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TOC-VCPH/CPN & TOC-Control V Software

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1. Backflow IC Reagent Prevention Vessel IC Reagent Trap Supply Pump Diluent Acid ets Drain ASI Solenoid Phosphoric Acid Joes es nes E Sample Backflow IC Reagent LightSource i Chemiluminescence Prevention i Detector Slide TC Sparge Valve Sample oe Solenoid f Injector i JV NDIR 1 re Tandem Cell Ozone Halogen Scrubber Sample Cell Generator 3 5mL Syringe i g Ozone ae Membrane Ozone 0 Source Flow Control Dehumidifier Filter Detector Treatmen Air Flow Capillary Exhaust Unit Meter Combustion Pure Wh fs Carrier Gas Tube TC Water i Flowmeter W Trap l NALE Pi sorber Gaie Mass Flow l JA A LL Drain Pot i eeh Solenoid Cnotroller Cooling Tubing l Pressure DE PI A HI Bai Carrier Pressure Gas Inlet Gas Inlet Valve qe TNM 1 TOC VcPH TNM 1 Figure 2 8 Flow Diagram TOC VcPH TNM 1 IC R Backflow ae Prevention Trap IC Reagent Diluent TOR Pump Acid ak 6 Backflow i Prevention Valve Drain Sample
2. Figure 4 147 Sample Wizard Page 6 Calibration Curve Window Second Analysis Sample Wizard Page 7 Injection Parameters A second Injection Parameters window is only displayed when more than one analysis type has been specified This window is the same as Page 4 of the Sample Wizard which is described above Verify the analysis type in the Analysis text box at the top of the page and make the appropriate selections j Sample Wizard Page 7 Injection Parameters Parameters Cal Curve Gen Info Figure 4 148 Sample Wizard Page 7 Injection Parameters Window Second Analysis LLL TOC fm 97 Sample Wizard Page 8 Peak Time Parameters A second Peak Time Parameters window is only displayed when more than one analysis type has been specified This window is the same as Page 5 of the Sample Wizard which is described above Verify the analysis type in the Analysis text box at the top of the page and make the appropriate selections Sample Wizard Page 8 Peak Time Parameters Figure 4 149 Sample Wizard Page 8 Peak Time Parameters Window Second Analysis Sample Wizard Page 9 USP EP The USP EP window is displayed only for TC or NPOC methods and is used to enable samples to be checked in accordance with USP EP standards This window is the same as Page 6 of the Sampl
3. Part Number Part Name 24mL 40mL 638 41462 Vials 24mL 100 038 00165 21 Vials 40mL with cap septum 72 638 20074 01 Cap 24mL 100 038 00165 48 Septum 24mL 100 638 52337 Rinse water bottle 1 1 072 603 10 03 Wiring band TM 53M 2 2 631 51869 20 Name plate SAMPLE 631 51869 21 Name plate GAS 072 60301 Wiring band Nylon TY 23M 638 74027 Cable ASSY ASI signal 638 41448 01 Needle regular type 24 40 TOC VCPHI CPN 299 300 6 3 8 6 4 Standard Accessories PC Hardware Requirements Table 6 5 Standard Accessories List 3 OCT 1 8 Port Sampler Part Number Part Name 8 Port 8 Port Details Sampler 1 Sampler 2 631 20265 Plug 35154 1 1 Rotor for replacement maintenance 638 41443 03 Common Tubing C 1 Common port connection tubing 638 41443 04 Additional Common Tubing C2 Common port connection tubing 638 41443 05 Common Tubing W Common port connection tubing 638 41443 06 Additional Common Common port connection Tubing W2 tubing 638 41337 03 Flanged Tubing C 1 1 Sample tubing for combustion analyzers CSH CSN CPH CPN 631 41660 Flanged Tubing W 1 1 Sample tubing for wet chemical analyzers WS WP 638 74004 01 Power Cable 1 Cable for connection to the main unit 638 74028 01 Power Cable 1 Cable for connection to the main unit 638 74028 02 Power Signal Ca
4. Combustion Tube TC nv Cooling Tubing Halogen gt _a Dehumid Water Trap We Drain Pot TOC VcPHI CPN Construction 2 1 7 Flow Diagrams Light Source CO Absorber NDIR Tandem Cell Halogen Scrubber Sample Cell pq Dehumidifier kemang Detector TOC VcPN Light Source iyi nE oy obs q Chemiluminescence ZN Detector NDIR QV 3 Tandem Cell zone Ser bber Sample Cell Generator al Ozone ifier Membrane Ozone Source Filter Detector Treatment Air Flow Exhaust Meter ie i i NO Absorber Pressure l Pressure Valve Sensor Gas Inlet TNM 1 Figure 2 11 Flow Diagram TOC Vcpn TNM 1 TOC VcPN TNM 1 TOC VCPH CPN 13 2 2 Autosampler ASI V Option 2 2 1 Front View 2 2 Autosampler ASI V Option 2 2 1 Front View Needle Replacement Window Sample Tubing Stirrer Speed Sample Cover Control option Figure 2 12 Front View 2 2 2 Rear View Rinse Solution Tubing Signal Cable Terminal Power Cable attached to AS Drain Tubing Figure 2 13 Rear View 14 TOC VcPHI CPN 2 3 8 Port Sampler OCT 1 Option 2 3 1 Front View 8 Port Valve Figure 2 14 Front View 2 3 2 Rear View 8 Port Sampler 1 8 Port Sampler 2 Signal Pow
5. ccececceeseeseeteereeneeees 288 6 2 Analysis Related Technical Information ceccceseeceeseeeeeeeceeeeeeeeeaeees 289 6 2 1 Peak Area Analysis eeccecccesseeseessessecsseesecseceseeeecnseseceseeeeeeaeeneeeneeeeeaeenaes 289 6 2 2 gt Peak Shape ss sceccestecels EEE aH ea ANA a 289 6 2 3 Calibration Guryeseescssecsists scdvsstesersesdees dedsocctalsasesttucadssisdvss as deers sages 290 6 2 3 1 Types of Calibration Curves 0 cccccecseesecsseeteeteceecesecesceseeeeenseeseeees 290 6 2 3 2 Shifting of Calibration Curves ccccecesseesecsseeseceeceteeteeeseeseeeeeees 290 6 2 4 Sparging During Standard Solution Analysis cccesecseeseeeceteeeeeeceeenee 292 6 2 5 Automatic Selection of Optimum Calibration Curve ececeeeeteeeeeeees 292 6 3 6 4 6 5 6 6 6 7 6 8 6 9 Table Of Contents SpPecifiGatlons otec c ceesseckanecat a a ataa aatan aa assai atto 294 G3 TOC VEPRICPN nininini h N N EEE E 294 EFE AREN a eich wei A E N A RNE 295 6 3 3 OCT 1 8 Port Sampler esanen enren n i 295 GSA TNM a a a a n a S 295 63 9 POOR raa E and gale hid E ATT tia dl ora 296 6 3 6 Carner Gas Purifier Kites s aaicn a svconie E iat 296 6 3 7 Manual Injection Kit Gas Sample Injection Kit eeeeesseeteeeeetees 296 6 3 8 PC Hardware Requirements ccccceecccsecssecseceseeeecesceeecescesseesecaeenseeseenaees 297 Standard ACCESSOLICS ccccecseessesseceteceseeeecescecsaecsaececeeeseseecseecseen
6. cccccesesesseeseeseecseeeseceeceeeeteerees 207 LAGT Stop gt Halts eran Was eee a eee r a eE 207 4 4 7 Maintenance Menu iicccccecesccccsscdedececctedi dee cceenses sedan R 208 FAS Tools MMU ei sec Setdecaece sh a a a a a eel a tock rT aT 208 448 1 Control Charts ace E ET 208 448 2 Method Validation cnn tit eee ie i E a l 208 4 4 8 3 Administration cceceecesesseceeceseeseeesceseeeeceseeeeecseeeeceeseececnseeseens 208 AAS 4A Sereen Ok isi cesses Giecceivedehicvisegvesieesleceesscviweecieecceeectvas views 209 44 9 Options Memia eare iheasvends ae eera eE a aens aS 210 4 4 9 1 General Informationerne gianna 210 4 4 9 2 Default Measurement Parameters s sessesseseeseeessseeesersrserssereseese 212 4 4 9 3 Display Settings gt Display Font s sesseseeseneesesseersseessersrsersrseeseese 213 4 4 9 4 Display Settings gt Table Settings cc eceeeescesseeseeseeeecseeeeeeens 214 4 4 9 5 Display Settings gt Notification Bar Settings ccceceseseeteeeeees 215 4 4 9 6 Display Settings gt Floating Point Number Formats 000 216 LAOT Directories e aar a seenazess ea e a ne aei a 217 Table Of Contents AAO gt Window Menu ivcsseecsocussitie R ott thos tesesatean teeta E 218 AANON Cascades ciciaiincieelnmaniaiiaiintadisuadetadaguene atin 218 AA VODs 7 ADAG C ATAA ca AII scuvace casos E ITE A A e TEA ETA 218 44 10 33 Arran Be Icons oe e e eK E tee E TRE EAK 218 44 11 Help MEn ra a a ett E
7. cceseesceseesecseeeeneeneees 148 System Tabien herea dieses 147 ASCII File Exporting Control Charts 383 ASI V See Autosampler Auto Dilution cece cee eeceeeneeeeneeees Auto Generate Auto Regeneration of IC Solution Auto Restart I 232202 s aseshease gcaeonthimeesiinenteteverenresnettoers Autosampler cise tudes catey df chests decssennastisnschecsecne baatdet Cables Connecting cceeeseserereeee Cover Installation cccccecececeseeseeseeeeneeneeee Drain Tank Installation Front View High Sensitivity Analysis mitali iiae e E E Trnstallation ceececcecseeseescescesceseeeeeeeeeeeeeeeeeeees Maintenances sirsa a E Needle Change ccccccssessesseseseeeeeeeeeeeeees Needle Types Needle Coaxial Needle Sample NPOC Analysis POSITIONING 00 eeeeeeseeeeeeceeceeceseesecaeeaeeseeneeneees ROA VieW sseisesecsesseeissiealeatemaseneaeereiieniienies Rinse Bottle Inspection ceeeeeeeereees Rinse Bottle Installation Rinse Pump Head Replacement Sample Catcher Inspection Shipping Screw ccccscsccescescsseeeeeeeeteeneens Software Settings ccceseseeseeeeeeeeeeeeees Specifications ccececscsseseeenecsecsecseeseeneens Turntable Installation Vial Positions Vial Rack Change cc eecsseceeeeecneeecseeneees Vial Rack Installation 0 cccccceeeseceeteeeee Blank Systemy arenan ana deed 291 Buzzer Setti
8. eceececesceeceseeteeeeseesecseeneeneeneees Maintenance eeeeeeceeeeees Ozone Source Airflow Rate Power Source seses Power Supply cineres esiin Principles ineeie e s Rear View vecscdc secs cxsssccgsles cle ces onted Specifications eisean Standard Solution Index 9 Index TN Unit Gas Tubing Connection ccceceeeseseneeeseees 330 TOC Principles isccenctherasing detain gies Setting Parameters 0 cccesesecesereeeceseseeeenees Setting Parameters in Software eee TOC window of the Instrument Setup Wizard TOC TN Catalyst ccccccecsesseeccesceseeeeeseeseeeeceeeeeceees TOC Control V Administration Tool cece esses ceeeseenees 21 Administrator Window ceeeeseeeereeecneeeeeeeee 21 TOC V ConstructiOn 4 ateneieneat ase eee 8 Front Views saciid tendinitis e ea 8 Grounding o n i AZ High Sensitivity Catalyst oe eeeeeeeeeeeeees 37 Inside Front View ccceeeseseeeesereeseeseeeeeeeeees 10 Inside Top View ceeeeseeseeeesetesseeseeeeseeeees 11 Installation cece seceeeseeeceeeseeecneeeeeeees Left Side VIEW sseeg araneon e aged eases Rear View Right Side View Specifications 4 Standard Catalyst e eeseeeeeeeeeeeeeseeeeeeesrreseereesee 37 Troubleshooting sseeseeeeeeseeeeereereereeeee 274 277 Units eain eye 87 130 138 163 171 188 212 Vial Puliti g e oer a e 72 Placing in R
9. ERROR ASI Turntable Position Detection The ASI V turntable position could not be detected Either the rack is not prop erly seated in the turntable or some object may be blocking a position detec tion notch on the periphery of the rack Switch off power to the TOC V main unit Make sure the rack is properly seated and remove any objects that may be blocking the position detection notch on the periphery of the rack After eliminating the cause of the problem place the cover on the ASI V and switch on the power to the instrument again ERROR TN Reactor Temperature The TNM 1 reactor temperature does not rise Switch off power to the TOC V main unit After switch ing on the power and running the instrument again see if the same error is generated TOC VCPH CPN 273 274 5 7 Troubleshooting 5 7 2 Troubleshooting Table 5 4 Error Message List 4 Error Message Description Corrective Action 8 Port Sampler 1 posi 8 Port Sampler 1 operation error tion detection occurred due to foreign matter infiltra 8 Port Sampler 1 opera tion into 8 port valve ete tion Switch off instrument Remove 8 port valve rotor from 8 Port Sampler 1 remove debris etc and wash valve 8 Port Sampler 2 posi 8 Port Sampler 2 operation error tion detection occurred due to foreign matter infiltra tion into 8 port valve etc 8 Port Sampler 2 operation Swit
10. Ensure that gas cylinders never reach temperatures higher than 40 C e Make sure there are no open flames anywhere within 2 meters of a gas cylinder e Secure cylinders with bands or other fasteners to prevent tipping and falling e When finished using gas immediately and completely turn OFF all valves on the cylinder e Inspect the operation of the pressure gauge at least once every three 3 months Gas Supply Pressure Supply gas at a constant stable pressure of 300kPa 44PSI at the gas inlet connection of the TNM 1 Note Keep the carrier gas supply pressure to the instrument from exceeding 600kPa 87PSD Gas Tubing Connections The special accessory Air Supply Tubing Set includes nylon tubing and connectors two 2 half unions Connection Inlet Half Union Nylon Tubing Figure 6 20 Gas Tubing Connection 330 TOC VCPH CPN 6 8 Installation 6 8 6 Installing the TN Unit Procedure 7 Connect the half unions to the carrier gas inlet on the instrument and the connection outlet 4 NPT of the gas supply source 2 Connect the nylon tubing 4mm O D 2 5mm I D between the gas supply source and the instrument Note The nylon tubing can be connected simply by firmly inserting it into the half union When disconnecting the tubing pull off the tub ing while pushing down firmly on the green colored ring of the half union using a screwdriver 3 After connection check to see that there are no g
11. TOC VCPH CPN 4 1 Analysis Preparation 4 1 7 Acid Preparation 4 1 7 Acid Preparation This section describes the preparation of acid used for IC removal in NPOC analysis or for IC analysis with the N Type instrument Procedure 1 Prepare 2 M HCI by diluting 1 part commercially available concentrated HCL 12 M with 5 parts pure water A final concentration accuracy of 2 is acceptable Note The pure water used as the diluent must have a TOC concentration no greater than 0 5 mg L Since the TOC value of the diluent pure water can have a large effect on the analysis result with high sensitivity analysis low TOC concentrations it is necessary to use pure water having a very low TOC concentration N caution Hydrochloric acid is a hazardous chemical Use precautions to avoid contact when handling this substance For details refer to Section 6 9 Material Safety Data Sheets 2 Acid Intake Tubing Hydrochloric Acid Container Transfer the prepared acid to the 250 mL bottle provided as a standard accessory and place it to the left of the instrument toward the front Pass the acid intake tubing through the hole in the cap Secure the tubing using a wire clamp about 100mm from the end of the tubing to prevent the tubing and cap from separating Place the cap on the container Note Verify that the tip of the acid intake tubing nearly reaches the bottom of the container Cap Fig
12. cccecceeeescesceeseeeeeeeesecseeeeeneensees 267 5 6 9 AST Rack Change eenn Baten inden ttt 267 5 6 10 ASI Needle Change sniene nrin r e a i 268 KONE Change Syrin gean ea T E E E E eee 268 5 6127 Blank Check none ae E EEEE A AE REE REO E RE 269 5 6 13 Maintenance L g orez rnran e a n i athe eed ete 269 eer e a E E E N O EN EET 269 5 06 15 Sparge Gas Valyen nieni E EEE EE EAE EEE RAEE S 269 5 6 16 Adjust Sparging Flow Rate Wet Chem cccccecseeseesserseeecseeeteeneeesees 269 5 7 Troubleshooting nesnenin A OE htes 270 Sided Error Messages n en ER EERE E a e e e EEEE 270 S722 Troubleshootint n e e a eni asa 274 SLAE TOCNE e EER nee ese cea maa wae 274 D122 gt ASV uaaa enna linn Miva ah chad alien anehan ahead 278 5 7 2 4 Corrective Actions for Poor Reproducibility 00 0 0 ceeeeeeeeeeeee 280 Reference Information ccccccsssssscscccccccsssssssssscsccccesccesescscsccsceseess LOD 6 1 Principles of Analysis O AE R 284 6 1 1 Principles of TC Total Carbon Analysis ee eecsecseeceeeceeeeeeeeereneees 284 6 1 2 Principles of IC Inorganic Carbon Analysis cccccecceeseeseeteereeneeees 285 6 1 3 Principles of NPOC Non Purgeable Organic Carbon Analysis 286 6 1 4 Principles of POC Purgeable Organic Carbon AnalySis scene 287 6 1 5 Principles of Measuring TOC ccccsesseessesseeseceeeesececeeeeenseeeeeeeeeneeaes 288 6 1 6 Principles of Measuring TN Total Nitrogen
13. 2227 Group Of Samples 181 High Sensitivity s c2 lt cst sp cavsicevtiesetee ape iesestenne 75 E ENEE E E te dere 56 Individual Sample sssseseeseeeeeeeeeeseseeeeeeeesrereees 185 Manual Injectionsissrsyissssniriisiinisni 219 Method Parameters cccsscsssssseseesseneeneenee 136 Preparation cccceescecceceeceeeeeeeeeeeeceeceseaes 36 82 Principles s e sesseessssessesersssesesrrsesrsessesesse 284 288 ProcedUTesiscscrirerciincairiarciniiiiii 89 121 Sample Parameters cccccesescesceseeeeeeeeeeeees 186 Sample Run 108 Suspended Solids 0 eecesesecseescessensenseeseeseees 69 Technical Information 289 293 DN session e a aa seston SE ok 59 Viewing Data in Real Time eee 167 Background Monitor ccseeseseceeeeeecreeeseeeeeeeeeeee 203 Base Effect on Instrument ccceccesseeseeeseesseeeee 71 Blank Check eee Analysis Using Area in Calculations 139 189 198 Numerics Installation anonanse EE Maintenance c cccccceescceesseecesceseseeeenee Rear View cccecccssceceeseeseeeees Sealing the Sample Containers 8 Port Valve Replacing Rotor 8 Port Sampler 4 254 Replacing Rotor Syringe Pump 06 246 Application Operations cceseeseeseeseereeneeee 219 233 ASCII Export Options D ta Tabore a a 147 Header Wabi cess cesses nee ttre a iann 146 Miscellaneous Tab
14. 5 7 Troubleshooting 5 7 1 Error Messages Table 5 4 Error Message List 4 Error Message Description Corrective Action ERROR ROM Write Error An error occurred while writing to memory Switch off power to the instrument Contact your Shi madzu representative ERROR Electric Fur nace Overheating The electric furnace overheated With the power ON wait approximately 20 minutes for the oven temperature to decrease then switch OFF the instrument After switching on the power and running the instrument again see if the same error is generated ERROR Electric Fur nace Sensor The oven temperature does not rise ERROR Syringe Posi tion Detection The syringe is not operating normally Switch off power to the instrument After switching on the power and running the instrument again see if the same error is generated ERROR Syringe Opera tion The syringe is not operating normally due to clogging of the tubing connected to the 8 port valve Switch off the instrument and remove any foreign parti cles from the line After switching on the power and running the instrument again see if the same error is generated ERROR Syringe Zero Point Detection The syringe is not operating normally Switch off the instrument After switching on the power and running the instrument again see if the same error is generated ERROR 8 Port Valve Position Detec
15. Setting Item Description Enable history log Select this option to enable the software to monitor all modi fications to the system Once the History Log is enabled it cannot be disabled If the History Log is not required it need not be enabled as the software works properly without it User has to comment all Select this option to require comments or approval for all modifications modifications LLL OC me 277 4 4 9 2 Default Measurement Parameters The Default Measurement Parameters command is used to enter the default values for samples methods and calibration curves The Default Measurement Parameters window contains a separate tab for each analysis type into which the default values are entered The SSM TC and SSM IC tabs are items associated with the installation of SSM 5000A For details refer to the SM 5000A User s Manual Default Measurement Parameters Figure 4 174 Default Measurement Parameters TN Tab The parameters shown on each of the tabs are similar and are described below Parameter Description Units Select the default concentration units No of Injections Enter the default minimum maximum number of injections No of Washes Enter the default number of times the syringe is to be washed with sample prior to the first injection Note that if the Auto Dilution option was selected the sample will be diluted and the syringe will then be washed with the diluted sample 212 Wl TOC VcPHicPN i
16. Start Vial Enter the starting vial position for the sample group Enter an integer ranging from 0 to 9 or 1 to 100 depending on the sample tray size The default value is 1 This field is disabled if an autosampler is not a component of the configured sys tem Sample Name Sample ID The default designations for these fields are obtained from the method or calibration curve identified in Page 1 of the Sample Group Wizard Enter other names if desired Index Start Select this option to start the counting index Each sample added receives an increased counting index number 182 WE TOC VcPmcPn Sample Group Wizard Page 3 Calibration Curves The Calibration Curves window is used to identify the calibration standards in the sample group and to specify their placement in the group The window is also used to revise the list of calibration curves that will be used to quantitate samples in the group Sample Group Wizard Page 3 Calibration Curves C Program Files Shimadzu TC C Program Files Shimadzu TN Figure 4 140 Sample Group Wizard Page 3 Calibration Curves Setting Item Description Perform Calibration Select one of the available options for when calibration should be performed At the beginning of the sample group or Always after a selected number of Samples have been ana lyzed Add button Use this button to add a calibration curve Delete button Highlight a calibration curve listed in the window and cli
17. 4 1 15 Sample Preparation 4 1 15 1 High Sensitivity Analysis High sensitivity analysis refers to use of the high sensitivity analysis kit to measure trace amounts commonly 0 5mg L or less of TOC in samples such as ultra pure water The precautions described in the sections below should be followed when conducting trace analysis on the order of 10 100ug L Precautions for High Sensitivity Analysis Use TOC high sensitivity catalyst Carefully fill the combustion tube with high sensitivity catalyst to prevent contamina tion of the combustion tube Measuring high concentration samples using TOC high sensitivity catalyst that is intended for the analysis of ultra pure water will influence the results of subsequent analyses on ultra pure water samples This is primarily caused by remaining sample residue The residue may be removed by running repeated analyses of zero water Since removal is difficult with residual salt alkali or highly acidic samples a separate combustion tube containing TOC high sensitivity catalyst should be prepared for use only with ultra pure water samples Verify that both ends of the combustion tube are sealed when storing catalyst that is to be used only for ultra pure water samples Measure samples immediately Samples containing trace carbon such as ultra pure water should be measured immedi ately after collection If analysis cannot be performed immediately store the sample in a dark location at 0 10
18. Connecting the Combustion Tube N caution The instrument is sealed sufficiently if the combustion tube does not move when it is pulled upwards The quartz glass combustion tube will break if the compression fitting is over tightened Do not allow organic contaminants such as grease or oil to touch the inner or outer surfaces on the tip of the combustion tube and gas connection parts of the ferrules This is especially important for high sensitivity analysis TOC VCPH CPN 43 4 1 Analysis Preparation 4 1 2 Connecting the Combustion Tube we Combustion Tube Figure 4 7 Connecting the Combustion Tube 5 Secure the sample injector with the knurled thumbscrew as shown in Figure 4 8 Securing the Sample Injector Knurled Thumbscrew Figure 4 8 Securing the Sample Injector 6 To prevent heat escape from the furnace pack the space around the capillary part of the combustion tube with the provided ceramic fiber N caution Use caution to avoid inhaling ceramic fibers when inserting the fibers into the combustion tube 44 TOC VcPHICPN 4 1 Analysis Preparation 4 1 3 Installing the Syringe 4 1 3 Installing the Syringe This section describes the procedure for attaching the syringe to the syringe pump assembly Depending on the instrument status flow lines are connected to each of the 8 ports of the syringe pump valve If the syringe is installed or removed without foll
19. ssseeeeeeeeeeeeeeeeererreereeees 207 Stop Peak Stop ccccececeseeseeceeeeeeeeeeneeneens 207 Suspended Solids cccccececcsseeseeteeseeseeneeeeneees 54 69 Syringe Changing oo ececeeeecceeceeceteeeeeeeeeseeneeee 226 268 Installation cece reinn 45 Manual Injection Kit ee eeseeseeseeteeneeneeee 226 Plunger Tip eces crrr noi 244 Plunger Tip Backlash Replacing iscc seesicceds cocinan eiei 45 Residue Removal sesessseseeeeeeeseseersrrererrereeseee 263 Washing with Sample 0 138 188 212 Washing with Standard eee 130 172 Syringe Pump 8 Port Valve Rotor ce ceeseeecreseseeeeeeenees 246 Zero Point Detection ccecececeseeteeteeteeteeeees 47 System Administration Add Event Logeren anre setters Change Password Tittroduction cee eceeeeseeseseeeeesesessceeeeeeseseeeeeeens Screen Lock i t 3 untested System Blank 0 0 ccccccscesesceeeeesceeeeeceeeeseeseseeeeeeeees System Description ccccecsesseeseeeeseeecesceeceeeeeees System Information Window Instrument Setup Wizard 00 eee eeeeeeneeeeeeeee 94 TN Analysis Preparation ccceceeeesseneeeceeeeeeeene Analysis New Catalyst Connecting Ozone Source Air Front and Right Side Views Gas Exhaust Tubing eeecesecseeseereeneeeees Grounding 0 0 eeeeeseeseeseeseesceseesceeeeeeeeeceeeeeeaees Inside Front View ccccccescescescessesseeeeeeceeceseeaes Installation
20. 4 5 1 Manual Injection Analysis Samples can be injected manually to perform analysis without the sample injector syringe when the optional manual injection kit is installed 4 5 1 1 Analysis Preparation Installing the Manual Injection Kit 7 Remove the knurled thumbscrew that secures the slider then remove the TC TN injector slider Figure 4 184 Removing the Slider 2 Install the TC TN block provided in the kit TC TN Block Figure 4 185 Installing the TC TN Block TOC VcPHICPN 219 220 4 5 Application Operations 4 5 1 Manual Injection Analysis 3 If the IC reactor kit is being used remove the IC injector slider and install the IC block provided in the manual injection kit Figure 4 186 Installing the IC Block Note When installing the block be sure that it is aligned with the injection port Software Settings Select the Manual Injection Kit option in the Instrument Setup Wizard Options window during System Setup Refer to Section 3 2 2 Options Window Note Selecting the Manual Injection Kit option disables operation of the TOC V injec tor syringe TOC VCPH CPN 4 5 1 2 Measurement Measurement procedures using the manual injection kit are similar to those described in Section 4 3 Measurement Procedures and Tutorial Calibration Curve Measurement Procedure 7 From the File menu select New The New dialog box is displayed Figure 4 187 New Dialog Box 2 Double
21. 5 Help Menu About ContrCharts Use the About command to view copyright and version information 384 E TOC VcPrcPn i i iii Index 8 Port Sampler Analysis Using cceccececcssesseeseneeeseeseeseeeeeeeeeees 80 Connecting Two Units Connection Front View ccccccsccecseccsssceessecesseceseeceseecesseees 15 High Sensitivity eseeeeeeeeeseeeeeeessrsrrerrrerrrrrsreese 82 Initializing seeeeseeeeeeeeeseeeeeessetseeressrrereerssreseees 267 ACCES SOTI ES E a AE 298 303 Speciales ieia nha ia 303 Sta dard ineaca e RSA 298 Acid Addition in NPOC sseseseesessesseseseessse 76 189 Addition VolUme ccecceceeseeseeteeeceeeeneeneeee 139 Checking Volume ccecececceceseeteceeeneeneenee 236 Effect on Instrument ccececeeeeeeeeeeeeeeeeeeee 71 Hydrochloric Phosphoric 000 Preparation eee Add Event Log eeessscesesesseeseeeeecneeeceecseteceesneees Administration cece seeseeeeeesereeseeeeeeeeenees Air Low Pressure Safety cccccscseeseceeseeeeeeeteees 331 Alkaline Samples inanon e 71 Analysis Blank Checkiiscncacnsscsesnh sravsachtocdetes 66 Calibration Parameters 128 Calibration RUM cceccecceseeseeseeseeteceeenseneenee 100 Control Sample Parameters sseeeeeeee 196 Creating New Method cceeeceseesseeeeeeneenes 135 Ending vivesicsccescsccctest oes cot sesso adsaceccencescvecssvbenses 120 Gas Sample
22. 64 characters maximum This field can be edited No of Determinations Displays the number of times 1 10 the sample is to be mea sured Note that determinations and injections are different each determination is made up of one or more injections This field can be edited Perform sample checking Select to enable USP sample checking according to USP EP Current Method Displays the file name of the current method Changes cannot be made to this field 162 W TOC VcrHichn iii TC Tab Setting Item Sample Method Properties Figure 4 118 Sample Method Properties Window TC Tab Description Analysis Parameters Units Displays the concentration units This field can be edited by selecting another option from the drop down list No of Injections Displays the minimum maximum number of injections for the samples analyzed with this method This field can be edited No of Washes Displays the number of times the syringe is to be washed with sample prior to the first injection Note that if the Auto Dilution option was selected the sample will be diluted and the syringe will then be washed with the diluted sample This field can be edited SD Max Displays the maximum standard deviation If this value is met no additional injections are required However if both this value and the CV Max value are exceeded the samples are automatically reinjected up to the maxi mum number of times specified in
23. Black O ring Figure 5 8 Replacing the Sliding Sample Injector O rings If a gas leak develops between the injector block and the combustion tube replace the O ring there as well L cau TION Do not scratch the O rings or the O ring seat when replacing the O rings TOC VCPHICPN 245 5 2 Periodic Inspections 5 2 10 Replacing the Syringe Pump 8 port Valve Rotor 5 2 10 Replacing the Syringe Pump 8 port Valve Rotor The fluororesin rotor of the syringe pump 8 port valve gradually becomes worn and scratched after prolonged use due to suspended particles in the samples This wear eventually causes leaks from the 8 port valve The following symptoms are associated with leaks from the 8 port valve and indicate that rotor replacement is necessary Droplets of liquid around the 8 port valve especially around the upper shaft e Decreased analysis reproducibility e Presence of bubbles in the syringe If the leakage is great sample remaining in the tubing after it is drawn into the syringe may flow back into the sample container This is most likely due to a sampling tubing flange or connection problem L cau TION Switch OFF the instrument before replacing the 8 port valve rotor Procedure 7 Shut down the instrument and turn OFF the power 2 Verify that the O mark on the 8 port valve interrupt plate is directed toward the No 1 port If not the instrument was not shut down using the appropriate procedure In this case
24. C without freezing and perform analysis as soon as possible To collect the water introduce water into a well washed container leaving no head space and seal the container Use glass sample containers Glass containers are optimal for samples containing trace carbon Commercially avail able 500mL to 1 L glass screw lid jars with Teflon seals generally referred to as heat resistant screw top jars or hermetic jars are appropriate for use as water collection and transport containers Note Exercise caution with plastic containers as elution of TOC containing components can occur TOC VCPH CPN 63 64 4 1 Analysis Preparation 4 1 15 Sample Preparation e Use NPOC analysis for ultra pure water samples Use the NPOC method for analysis of ultra pure water samples Measuring TOC in ultra pure water samples by using the difference between TC and IC is prone to large analysis errors for the following reasons e The TOC value is significantly affected since a large portion of TC often comprises IC Errors in TC analysis and IC analysis are additive e Carbon dioxide is absorbed from the atmosphere during sample collection and anal ysis During the elapsed time between TC analysis and IC analysis the sample absorbs more carbon from the atmosphere causing the IC result to be higher than the IC content in the TC result As a result subtracting the elevated IC result from the TC result yields a biased TOC value The TO
25. CAT NO CAS NO 7732 18 5 NAME Water OTHER NAME Dihydrogen Oxide MOLECULAR WEIGHT 18 CHEMICAL FORMULA H20 SECTION I HAZARDS IDENTIFICATION EMERGENCY OVERVIEW Not applicable HEALTH RATING 0 None FLAMMABILITY RATING 0 None REACTIVITY RATING 1 Slight CONTACT RATING 0 None LAB PROTECTIVE EQUIP Goggles lab coat STORAGE COLOR CODE Orange General Storage SECTION II HEALTH EFFECTS POTENTIAL HEALTH EFFECTS Water is non hazardous INHALATION Not applicable INGESTION Not applicable SKIN CONTACT Not applicable EYE CONTACT Not applicable CHRONIC EXPOSURE Not applicable AGGRAVATION OF PRE EXISTING CONDITIONS Not applicable SECTION III FIRST AID MEASURES INHALATION Not applicable INGESTION Not applicable SKIN CONTACT Not applicable EYE CONTACT Not applicable SECTION IV FIRE FIGHTING MEASURES FIRE Not applicable EXPLOSION Not applicable FIRE EXTINGUISHING MEDIA Use extinguishing media appropriate for surrounding fire SPECIAL INFORMATION In the event of a fire wear full protective clothing and NIOSH approved self contained breathing apparatus with full facepiece operated in the pressure demand or other positive pressure mode SECTION V ACCIDENTAL RELEASE MEASURES Non hazardous material Clean up of spills requires no special equipment or procedures SECTION VI HANDLING AND STORAGE Keep container tightly closed Suitable for any general chemical storage area Protect from freezing Water is con
26. Calibration points are distrib uted uniformly over the con centration range Edit calibration points manu ally Calibration curve according to DIN 38402 P 51 Calibration curve according to USP EP Select this option to calculate the calibration point concentra tions automatically The software will calculate the concen trations by distributing them in equal amounts over the measuring range of the calibration curve Select this option to enter the calibration point concentrations manually on a subsequent Wizard page the Calibration Points List Select this option to create a calibration curve according to DIN 38402 This type of curve consists of 10 calibration stan dards with 10 injections of the lowest and highest standards and a single injection of the intermediate standards Select this option to create a calibration curve that consists of 2 calibration standards with concentrations between 0 and 500ug L and one control sample with a concentration of 500ug L Calibrations using automatic dilution Dilution Factor Manual Set ting Dilution Factor Automatic Setting Use Source Dilution Function TOC VCPH CPN For manually setting dilution factor of standard solution Enter the dilution factor Automatically calculates dilution factor for standard solution and performs measurement using that dilution factor Prepares standard solution automatically inside the instru ment and performs measurement using tha
27. Displays the Open dialog box and allows a selected calibration curve to be added to the Sample Table 4 4 1 2 Status Bar and Notification Bar The Status Bar displays the status of various software functions and is displayed at the bottom of the open window for all applications If the Status Bar is not visible select Status Bar from the View menu The Notification Bar displays information about the status of the TOC Control V software the connection between the instrument and the PC measurement events and operation errors Use the Options gt Display Settings gt Notification Bar Settings window to enable disable or select settings for the Notification Bar Refer to Section 4 4 9 5 Display Settings gt Notification Bar Settings 7 i 1 Notification Initializing TOC started x eh fall nay Sts Ready ar Instr Sts Ready str Mode Initializing i ial Rdy Sts Ready oa El Instr Sts Moving Instr Mode Initializing k amp Notification Communication stop 3 Bi v Status Bar PEA A Notifications TCA System A Errors A Events A Debug LL For Help press F1 System l NUM 7 Figure 4 72 Status Bar and Notification Bar 124 TOC VcPHI CPN 4 4 2 File Menu 4 4 2 1 New TIP Figure 4 73 File Menu The New command opens the New dialog box which displays the options for all new file types The options are Sample Run Calibration Curve Method Control Sample Template and Parame
28. EXTINGUISHING MEDIA Water spray carbon dioxide dry chemical powder or appropriate foam SPECIAL FIREFIGHTING PROCEDURES Wear self contained breathing apparatus and protective clothing to prevent contact with skin and eyes UNUSUAL FIRE AND EXPLOSIONS HAZARDS Emits toxic fumes under fire conditions SECTION IX ACCIDENTAL RELEASE MEASURES Wear respirator chemical safety goggles rubber boots and heavy rubber gloves Sweep up place in a bag and hold for waste disposal Avoid raising dust Ventilate area and wash spill site after material pickup is complete SECTION X STABILITY AND REACTIVITY STABILITY Stable INCOMPATIBILITIES Strong oxidizing agent HAZARDOUS COMBUSTION OR DECOMPOSITION PRODUCTS Toxic fumes of carbon monoxide carbon dioxide HAZARDOUS POLYMERIZATION Will NOT occur SECTION XI SPECIAL PRECAUTIONS AND COMMENTS The above information is believed to be correct but does not purport to be all inclusive It shall serve only as a guide Shimadzu shall not be held liable for any damage resulting from handling or contact with the above product Users should make their own determinations regarding the suitability of this information for their particular purposes TOC VCPH CPN 6 9 Material Safety Data Sheets 6 9 13 Water 6 9 13 Water Shimadzu Scientific Instruments Inc 7102 Riverwood Drive Columbia MD 21046 Control No Tel 1 800 477 1227 Date MATERIAL SAFETY DATA SHEET SECTION I PRODUCT IDENTIFICATION
29. Instrument Calibrations Samples Header Miscellaneous I Print system information System Used options Detector Syringe Catalyst JASI Tray Type No of needle washes No of flow line washes Cell length K K Preview Select All Select None Default Cancel Figure 4 104 Page Setup Window Instrument Tab Calibrations Tab The Calibrations tab displays a list of calibration information items that can be printed on the report Page setup a x Instrument Calibrations Samples Header Miscellaneous Print calibration curve information Title OCY Max Excluded Comment ONo Washes MDate Time Sample Name Density WMlPeak Profile Sample ID MMean Area OSD Area Cal Curve MMean CNY OCY Area Type Mlini No Abs C Analysis Area CNY Acid Add MAnalysis Inj M Wweight Sparge Time Mlni Yol OVolume SD Max MhRemarks MGraph lt a UKK K KKK K gt Preview Select All Select None Default Cancel Figure 4 105 Page Setup Window Calibrations Tab 152 TOC VCPH CPN Samples Tab The Samples tab displays a list of sample information items that can be printed on the report i Page setup Ml nalysis Ini Mlini Vol Remarks Excluded Cal Curve Date Time JSD Cone CCV Area Figure 4 106 Page Setup Window Samples Tab Header Tab The Header tab displays a list of header items that can be printed on the
30. N caution Corrosion of the instrument may occur if spilled sample is allowed to remain in the sample catcher Keep the sample catcher clean TOC VCPH CPN 5 3 Autosampler ASI V Maintenance 5 3 3 Replacing the Pump Head of the Rinse Pump 5 3 3 Replacing the Pump Head of the Rinse Pump The rinse pump is located inside the autosampler and supplies rinse water to the rinse port The rinse pump is a roller type pump that uses a rotating roller to flatten the rubber tubing carrying the rinse water thereby feeding rinse water into the system This rubber tubing gradually deteriorates requiring periodic replacement The life of the rubber tubing is generally about 300 hours of pump operation It is recommended that 300 hours be entered as the warning value in the Maintenance History dialog box For details refer to Section 4 2 4 Maintenance History Settings Replacement Procedure Use the following procedure to replace the pump head 1 2 Remove the rectangular pump access cover on the back left side of the autosampler Grasp the latch on the pump head by hand and pull the white pump head from the black pump body On the left side of the pump head disconnect both of the yellow rubber tubes from the Teflon tubes Connect the new rubber pump head tubing to the Teflon tubes Replace the pump head by following the above procedure in reverse and then replace the pump access cover Pump Lae Head O F
31. P N 630 00999 which are located in the holder behind the instrument CO Absorber Disposal Procedure Used CO absorbers should be disposed of according to local industrial waste disposal regulations It must be clearly disclosed using an industrial waste manifest that the used CO absorber contains soda lime Reference For details on replacing the CO absorbers refer to Section 4 1 8 Installation of the CO Absorber 24 TOC VcCPH CPN 5 2 Periodic Inspections 5 2 6 Replacing the Halogen Scrubber 5 2 6 Replacing the Halogen Scrubber The absorbent inside the halogen scrubber turns black as it absorbs chlorine The discoloration band advances toward the outlet as the amount of chlorine absorbed increases Replace the scrubber with a new halogen scrubber when the front of the discoloration band reaches the position shown in Figure 5 4 Halogen Scrubber Replacement Procedure 1 Unclip the upper and lower clips that secure the halogen scrubber 2 Remove the upper and lower connection clamps 3 Disconnect the Viton connectors and remove the halogen scrubber Replace Scrubber When Discoloration Band Reaches Gas Flow Direction this Point _ To Sample Dehumidifier co HALOGEN SCRUBBER Cell Inlet Halogen Reactant filled Cylinder Figure 5 4 Halogen Scrubber The baseline may fluctuate immediately after replacement Allow the instrument to run for a short time until the baseline stabilizes Stabili
32. Repeat the procedure Click the Finish button when all measurements are complete Sample Measurement Procedure 7 From the File menu select New The New dialog box is displayed Sample Run Calibration Curve Method Control Sample Template Figure 4 189 New Dialog Box 2 Double click the Method icon The Method Wizard opens The System Information window of the wizard page 1 is displayed Method Wizard Page 1 System Information Parameters Cal Curve Gen Info System Figure 4 190 Method Wizard Page 1 System Information 3 Select the system that was configured with the Manual Injection Kit and used to create the calibration curve Advance to page 2 of the Method Wizard Analysis Information and enter the new method name in the text box at the bottom of the window 4 Advance to page 3 of the Method Wizard Calibration Curves Select the appropriate calibration curve file 5 Enter 1 in the No of Injections field on page 4 of the Method Wizard Injection Parameters LLL TOC VcPHchN mm 223 224 4 5 Application Operations 4 5 1 Manual Injection Analysis 6 10 11 12 13 14 15 TOC VCPH CPN Select the desired options on pages 5 6 and 7 of the Method Wizard which list peak time parameter USP EP check and history se
33. SSM Window SSM TC Furnace On Select this option for TC measurement SSM IC Furnace On Select this option for IC measurement LLL TOC Vc ly 29 3 2 6 Communication Window The Communication window of the Instrument Setup Wizard is used to set parameters for communication between the instrument and the PC Instrument Setup Wizard Communication Figure 3 11 Instrument Setup Wizard Communication Window Com Port Select the communication port from the drop down list Options include Com1 Com2 Com3 and Com4 Stop Bits The Stop Bits value is determined by the hardware and is set automatically based on the Com Port selection This field is disabled and cannot be edited by the user Parity The Parity value is determined by the hardware and is set automatically based on the Com Port selection This field is disabled and cannot be edited by the user 30 W TOC VcrHiCPN ieee 3 2 Instrument Setup and System Properties 3 2 7 History Function Window 3 2 7 History Function Window The History Function window of the Instrument Setup Wizard is used to enable the History Log The History Log records all modifications to the system properties The History Log can be set to require users to enter comments for each modification Note Once the History Log is enabled it cannot be disabled All modifications to the system properties will be tracked If the mandatory comment option is selected the user will be required to enter
34. Sample injection volume 10 2000uL variable Sample dilution function Dilution within syringe dilution factor 2 50 times Pretreatment for IC Automatic acid addition and sparging Carrier gas High purity air from cylinder Carrier gas pressure Approx 300 600kPa Carrier gas flow rate TOC VCPH 150mL min 230mL min when performing in syringe sparging TOC VCPN 230mL min Ambient temperature 5 35 C Power requirements AC 100 120V 10 or AC 220 240V 10 6 A 50 60Hz power consumption approx 230VA Fuse 8A T 100V Systems 15A T 200V Systems Approximate dimensions W 440 x D 560 x H 460mm excluding projections Weight Approx 40kg 294 TOC VCPH CPN 6 3 2 ASI V 6 3 Specifications 6 3 2 ASI V Sample containers 24mL vial rack 24mL External diameter 23 x Height 85mm 100 vials 100 septum equipped caps 40mL vial rack 40mL External diameter 27 x Height 9mm 72 vials 72 septum equipped caps Vial rack capacity 24mL vial rack 93nvials 40mL vial rack 68 vials Sample pretreatment e Acid addition and sparging possible for NPOC analysis e Needle rinse possible Stirring with magnetic stirrer with optional magnetic stirrer Ambient temperature 5 35 C Approximate dimensions W 370 x D 540 x H 490mm excluding projections Weight Approx 13kg
35. TOC Standard Catalyst The TOC standard catalyst is appropriate for both the TC IC method and NPOC method of analysis Note Analyze TOC high precision samples with expected concentrations of about lmg L using the TOC high sensitivity catalyst because smaller blank peaks are generated Filling Combustion Tube with TOC Standard Catalyst 7 Insert two sheets of platinum mesh into the combustion tube 2 Layer about 5mm of quartz wool onto the platinum mesh using the catalyst filling rod 3 Fill the TOC standard catalyst to a height of about 100mm Combustion Tube TOC Standard Catalyst Cd ae ates KY rola KOLS RO ye x4 ow Ky O SIK Ya er 3 100mm m ae 8 AS CH im Be CA AY xe C ee oS re Quartz Wool aaas Platinum Mesh Figure 4 1 Combustion Tube with TOC Standard Catalyst TOC High Sensitivity Catalyst H Type only Use the TOC high sensitivity catalyst for low level TC analysis The blank values are controlled to negligible levels and analysis is performed primarily for trace TOC in pure water 1mg L or less TOC VCPH CPN 37 4 1 Analysis Preparation 4 1 1 Catalyst Filling Samples containing IC in excess of 5mg L The detection rate for IC decreases with increasing concentration As a result use the NPOC method instead of the TC IC method when analyzing samples that contain IC concentratio
36. ground resistance 100W or less see Electrical Facilities Engineering Standards for details is recommended e Perform grounding separately and avoid contact with water supply pipes gas pipes and lightning rods 6 8 3 2 Changing the Power Supply Voltage The instrument is set up before shipment to match the power supply voltage in the locale where it will be used In the event that it becomes necessary to change the power supply voltage please contact your Shimadzu representative Depending on the voltage change an authorized Shimadzu service engineer may be required to rewire connections to the terminal block to change the power supply voltage and or perform changes to the main board 6 8 3 3 Connecting Gas Use one of the following as the carrier gas supply for this instrument e Cylinders filled with high purity air e Compressed air or instrumentation air Requires special Carrier Gas Purifier Kit accessory High Purity Air Cylinders High purity air is synthetic air manufactured from pure nitrogen and pure oxygen It must be guaranteed to contain less than one 1ppm of each of the following impurities carbon dioxide carbon monoxide and hydrocarbons The cylinder must be equipped with a pressure regulator to supply it at 300kPa to the gas connection inlet of the instrument Note If the carrier gas contains excessive impurities analysis accuracy is diminished and good results will not be obtained TOC VCPH CPN 313
37. sample will be spattered onto the cap seal Adjust the sparge gas flow rate to avoid this undesirable spattering To verify that enough IC is removed during sparging using the autosampler to enable unhindered NPOC analysis perform IC analysis on the remaining sample following NPOC analysis L caut ION When the vials are capped and sparging is performed without automatic acid addition via autosampler pierce the caps before analysis by using the tip of a provided needle or other instrument This allows the sparge gas to vent If sparge gas is not vented from the vials pressure will build inside the vials and prevent effective sparging TOC VCPH CPN 77 4 1 Analysis Preparation 4 1 16 Sample Preparation 4 1 16 7 Stirrer Preparation This section describes the procedure for enabling the optional stirrer Procedure 1 Open the TOC Control V Sample Table Editor 2 From the Instrument menu select Properties The Instrument Properties dialog box is displayed 3 Click the ASI tab then click in the Stirrer On check box to enable the stirrer 4 Click the OK button Adjusting the Rotation Speed Turn the knob at the bottom of the right side of the autosampler to adjust the stirring speed Note Capabilities of the Optional ASI V Magnetic Stirrer e The stirrer bar rotates inside the vial to agitate and mix suspended solids in the sample The magnetic stirrer cannot be expected to pulverize and homogenize suspended solids e
38. 1 connection tube for combustion TOC V add on Table 6 22 e Maintenance Parts List 5 Manual Injection Kit Part Number Part Name Comment 630 00261 Open Close valve TC injection port 638 60733 01 Microsyringe MANU10 10uL 638 60733 02 Microsyringe MANU25 25uL 638 60733 03 Microsyringe MANU50 50uL 638 60733 04 Microsyringe MANU100 100uL 638 60733 05 Microsyringe MANU250 250uL 638 60733 06 Microsyringe MANU500 500uL TOC VCPH CPN 309 6 8 Installation 6 8 1 Before Installation 6 S Installation 6 8 1 Before Installation Parts Inspection Confirm that all of the components listed in Section 6 4 Standard Accessories have been included in the shipping package 6 8 2 Installation Site Be sure to take into account the size of the instrument how it will be used and the installation conditions indicated below when selecting an installation site Instrument damage or measurement errors may occur based on the conditions of the installation site 6 8 2 1 Installation Site Selection The instrument is designed for use on a desk or bench The external dimensions of the instrument are shown in Figure 6 3 External Dimensions of Instrument with ASI V A space of at least 200mm is required on either side of and behind the instrument to enable unhindered operation and maintenance TOC V Main Unit 635mm Autosampler TOC V Main Un
39. 2 4 Maintenance History Settings for more details 5 6 14 History Use this option to view the operational history of various instrument components and to set limits for various parameters of the components When a limit is exceeded for an instrument component a warning message will be generated on the PC screen to remind the user to perform maintenance on the component Refer to Section 4 2 4 Maintenance History Settings for a detailed description of this function 5 6 15 Sparge Gas Valve Select this option to start and stop the flow of sparge gas when the external sparge kit is used 5 6 16 Adjust Sparging Flow Rate Wet Chem Use this function to adjust the sparge gas flow rate This option is available only when the wet chemical oxidation method is used TOC VcPHICPN 269 270 5 7 Troubleshooting 5 7 1 Error Messages 5 7 Troubleshooting This section describes the error messages displayed by the TOC Control V software and the actions recommended to resolve the underlying causes 5 7 1 Error Messages The following error messages are displayed on the PC screen when setting or operation errors are made or when problems with instrument operation occur Take the corrective actions indicated in the table below Table 5 1 Error Message List 1 Error Message Description Corrective Action WARNING Dilution water depleted Actual amount of dilution water used exceeds value set in the Maintenance His
40. 314 Installation Installation Procedure Precautions for Handling Gas Cylinders The handling and safety management of high pressure gases is strictly regulated by high pressure gas control laws general high pressure gas safety codes and fire laws The gas used in the instrument is not dangerous but mistakes in handling of high pressure gas cylinders can be extremely hazardous Carefully read and obey the following precautions e Place gas cylinders in a well ventilated location out of direct sunlight Ensure that gas cylinders never reach temperatures higher than 40 C e Make sure there are no open flames anywhere within 2 meters of a gas cylinder e Secure cylinders with bands or other fasteners to prevent tipping and falling e Turn OFF immediately and completely all valves on the cylinder when finished using gas Inspect the operation of the pressure gauge at least once every three 3 months Compressed Air or Instrument Air Purified with the Carrier Gas Purification Kit Using the Carrier Gas Purification Kit enables air from a compressor or instrumentation air or high impurity pressurized air in a cylinder to be used as the carrier gas Since there are limits to the capabilities of the Carrier Gas Purification Kit the following conditions must be met when supplying compressed air e Provide an air filter in the supply line to remove dust oil mist water drops and other contaminants Place an air filter in
41. 5 2 Periodic Inspections 5 2 2 Washing or Replacing Catalyst Removal Procedure 7 Remove the compression fitting joints at the top and bottom of the carrier gas purification tube 2 Detach the TC TN sample injection block from the combustion tube Refer toSection 4 1 2 Connecting the Combustion Tube 3 Extract the carrier gas purification tube from the electric oven by pulling upward Replacing Catalyst L ca UTION The top nut of the compression fitting joint is hand tightened Do not use tools to tighten or loosen this nut Because the tube is constructed of quartz glass over tightening or aggressive handling may result in damage Procedure 7 Remove the catalyst from the carrier gas purification tube through the opening at the top 2 Remove the quartz wool using a thin tube or other instrument 3 Insert a small amount of new TOC standard catalyst into the combustion tube from the bottom straight end 4 Pack a small amount of quartz wool into the tube from the bottom Note The quartz wool is inserted to prevent the catalyst from falling out of the bottom Packing too much quartz wool into the tube will greatly impede airflow so do not use too much quartz wool To prevent contamination of the catalyst or the inclusion of foreign particles use the same precautions used when filling the combustion tube with TOC platinum catalyst 5 Insert the straight end of the carrier gas purification tube down into the front 8mm diameter hole in t
42. 6 3 3 OCT 1 8 Port Sampler No of sample containers accommodated 8 containers 16 containers using 2 OCT 1 units Ambient temperature 5 35 C External dimensions Approx W 245 x D 245 x H 440mm excluding protruding parts Weight Approx 3 5 kg 6 3 4 TNM 1 Analyte TN total nitrogen Measurement principle Thermal decomposition NO detection chemiluminescence method Measuring range 0 4000mg L Measurement time Approx 4min Repeatability CV within 3 Ambient temperature 5 35 C Power requirements AC 100 120V 10 or AC 220 240V 4 consumption approx 230VA 10 6 A 50 60Hz power Approximate dimensions W 160 x D 235 x H 400mm excluding projections Weight Approx 8kg TOC VCPH CPN 295 296 6 3 Specifications 6 3 5 POC Kit 6 3 5 POC Kit Analyte POC Measurement method Sparging CO removal combustion oxidation CO removal method Absorption via lithium hydroxide removal Measuring range 0 500mg L Measurement time Approx 4min Repeatability CV within 5 6 3 6 Carrier Gas Purifier Kit Gas purification method Combustion oxidation CO removal Carrier gas supply Pressurized air or oxygen free of dust oil mist water droplets etc Carrier gas supply pressure 300 600kPa 6 3 7 Manual Inj
43. 84 O ring 4D P 10A For slider 5pcs 036 11408 84 O ring Teflon P10 For slider 5pcs 036 11219 84 O ring 4D P20 For TC reaction tube 5pcs 630 00635 01 Potassium biphthalate 25 g 630 00962 01 Sodium carbonate 25 g 630 00963 01 Sodium bicarbonate 25 g 046 00044 11 Membrane filter 017 30812 01 Silicone grease H V G 638 60074 Ceramic fibers 631 20265 8 port valve rotor 638 59213 01 Plunger tip 638 92206 02 Consumables set Refer to Table 6 13 for contents TOC VCPH CPN 305 306 6 3 8 6 6 Consumable Parts List PC Hardware Requirements Table 6 13 e Consumable Parts List 3 TOC VCPH CPN Part No Description Qty Remark TOC VCPN 638 41323 Combustion tube in case 2 2 638 60116 TOC regular catalyst 2 2 630 00996 TOC high sensitive catalyst 1 0 630 00557 Quartz wool 1 1 630 00999 CO absorber 1 1 630 00992 Halogen scrubber 2 2 036 11209 84 O ring 4D P 10A 1 1 5 pes 036 11408 84 O ring Teflon P10 1 1 5 pes 036 11219 84 O ring 4DP 20 1 1 5 pes 630 00635 01 Potassium hydrogen 1 1 phthalate 25g 630 00962 01 Sodium carbonate 25g 1 1 630 00963 01 Sodium bicarbonate 25g 1 1 638 60074 Ceramic fiber 1 1 042 00405 11 IC reagent supply pump head 1 0 631 20265 8 port valve rotor 1 1 638 59213 01 Plunger tip 2 2 Table 6 14 e Consumable
44. A R eatees 381 B41 Gonttol Chart Option Sheene a e en ai 381 BAX Foolen A E E N E csanedeantesdvia aeeeevents 381 B 4 3 Floating Point Numbering Format 0 cccccccsceesececeeteeeeceeeeseeeeeeeeeneeeneeaes 382 B 4 4 ASCH Export OptionS s essseseseesesersrersseesssrsseesseresstsrsseeresessesesstereseesesees 383 B 4 5 Enabl Excl si h sser ireen eee oiea ina EE aan eias 383 BS Help Menur reo e e E E E EE E EE ER 384 LLL TOC i xxi xxii E TOC VecpHicrn iene Overview This chapter provides an overview of the instrument and operational precautions for its use 1 1 Overview Provides an overview of the TOC VCPH TOC VCPN instrument 1 2 Operational Precautions Lists precautions necessary to ensure that the instrument is used correctly 2 1 1 Overview l 3 l Overview The TOC VcPH TOC VCPN hereinafter referred to as TOC V instrument measures the amount of total carbon TC inorganic carbon IC and total organic carbon TOC in water Purgeable organic carbon POC can also be measured when the POC accessory is installed Oxidative combustion infrared analysis is a widely used TOC measurement method that has been adopted by the JIS and other international standards The TOC V instrument can also measure total water borne nitrogen TN if the optional TN unit is installed TN is measured using the principles of oxidative combustion chemiluminescence Moreover when the ASI V Autosampler or
45. A T E E E TI te TENE 144 4426 SAE n e i AE EA ous EN EE E A 144 LAZ SIVE A Snoen cate oat hs eek E R A A A A AE 145 4 4 2 8 ASCII Export Options eseeeseseseeseesessesersesersrsreseosererssseeseesersrerereses 146 442 9 Database Export ene e E as rates ended eee 148 AA 2 10 Print Tables nn e ER ven E ERER 149 44 211 Print Sample Report s erunsnnnonenn e n a ERR 150 4 4 2 12 Print Preview gt Table cccececeeceseeescesceseeesecseeeaecaeeaeeeenseeteneeees 150 4 4 2 13 Print Preview gt Sample Report ccccecceesceeseesceceseeeeeeseeeenseeseens 151 AA DTA Print Setups sccg eke eek ok sect eee n leet E E dacs ee bt ent ta e OEDS 151 A ADS RAGE SCUUp ENERE AENT E tigen EEE 152 BADEN EAD soe cece a S E NE E casestaven tang avon S 155 TOC VCPH CPN xv XVI TOC VCPH CPN Table Of Contents AAS Ya EA ence fis EEE teh des eaah inated bees d web nected need oh 156 BABY UNO iss hearth a aain a a a AL 156 44 32 Cut Copy Paste a ait hao ik Sle EE E Pestcees 156 4 4 3 3 Replace ites ssc ie aE E a ea re es 157 AeA BAY E T iYe ASAE SE E ons oa babd tint eee ccotee cok ees 157 AABeS Exelude ie nrt i EERE ER R ieee eal a R eel 158 44 356 V R calcalate gt Ale n E E EEEE E EE 158 4 4 3 7 Recalculate gt Highlighted 0 0 0 ce cceecceseeeseeeceseeeeceeneeceeeseeteerees 158 4 4 3 8 Delete DataSAlle x e E EEEE ieee 158 4 4 3 9 Delete Data gt Highlighted s ssenenseeseseeeeseeseseeseersseesesersrseesseeesee
46. Calibration Curve Type x Calibration points are distributed uniformly over the Cal Pts o E Analysis Cal Type C Edit calibration points manually Calibration curve according to DIN 38402 P 51 Calibration curve according to USP EP Div Standard Solutions Fixed Dilution Dilution 1 E Div Standard Solutions auto correction of dilution factor Dilution from Standard Solution Enter the calibration curve type Calibration points can be modified later _ cok CAT ca Figure 4 46 Calibration Curve Type 4 Click the radio button for Calibration points are distributed uniformly over the concentration range In the future other options may be more appropriate Refer to Section 4 4 2 2 Calibration Curve for a detailed description of the calibration curve types Click the Next button LLL TOC my OL 5 Page 3 of the Calibration Curve Wizard is displayed The following options for calibration analysis are displayed e Analysis e Default Sample Name e Default Sample ID e Calculation Method Linear Regression or Point to Point e Check box for Zero Shift e Check box for Multiple Injections e Calibration File Name Select the following options as shown on the figure below e Analysis TC e Default Sample Name Standard e Default Sample ID Tutorial e Calculation Method Linear Regression e Check box for Zero Shift Deselect this option e Check box for Multiple Injections Deselect t
47. Corporation T 003201 Methods Tutorial met System C Calibration Curve po Edit parameters manually Parameters Se enana Sere erp pre eer jparameters from the source Enter the parameter source for the sample Back Cancel Figure 4 60 Sample Wizard Page 1 Parameter Sources 78 Click the Method radio button By selecting this option the sample will be analyzed using the measurement parameters specified in the method file we created previously Enter the name of the method file 7utorial met or click the Browse button to search for the file Click in the Skip remaining Wizard pages and use measurement parameters from the source check box By selecting this option the analysis parameters for the unknown sample are copied from the source method file The parameters do not need to be entered manually and the remaining pages of the Sample Wizard do not need to be displayed 79 Click the Finish button The Sparging Acid Addition window is displayed 20 Enter the vial position 2 for the unknown sample the 50ppm TC 10ppm TN calibration standard directly into the Vial column of the table 21 Verify the information then click the OK button The third row of the Sample Table now contains the measurement parameters for the unknown sample Note that a value will not be displayed in the Result column until measurement is complete 22 Save the Sample Table by selecting Save from the File m
48. Curve or click the Calibration Curve button on the toolbar The Calibration Curve Properties window for the TC calibration is displayed 3 Select the Graph tab to view the TC calibration curve data in graph form Common Parameter Analysis Data Graph History Cal Curve 441865 1 30000 Area 20000 10000 0 Conc ppm Slope 380 2 Intercept 38 17 Cal curve OK r2 0 999988 Figure 4 64 Calibration Curve Properties Graph Tab The coefficient of determination r value is a measure of the linearity of the relationship between concentration and area An r value was calculated for the TC calibration and displayed in the window because we selected the linear regression calculation when we created the calibration file Use the r value to determine the success of the calibration A 1 value of 1 indicates a perfectly linear relationship between concentration and area Application methods used for future analyses may specify an acceptable limit for the r value 4 Select the Data tab to view calibration statistics such as Standard Deviation SD and Coefficient of Variation CV These statistics can also be used to evaluate the success of the calibration TIP 4 successful calibration can be used for future analyses by specifving the calibration file name cal in the method 5 Close the TC Calibration Curve Properties window when the evaluation is complete Checking the TN Cal
49. DATA SEE SECTION 5 SECTION VII FIRST AID MEASURES In case of contact immediately flush eyes or skin with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes IF inhaled remove to fresh air If not breathing give artificial respiration If breathing is difficult give oxygen If swallowed wash out mouth with water provided person is conscious Call a physician Remove and wash contaminated clothing promptly SECTION VIII FIRE FIGHTING MEASURES EXTINGUISHING MEDIA CARBON dioxide dry chemical powder or appropriate foam SECTION IX ACCIDENTAL RELEASE MEASURES Shut off all sources of ignition Wear self contained breathing apparatus rubber boots and heavy rubber gloves Sweep up place in a bag and hold for waste disposal Ventilate area and wash spill site after material pickup is complete SECTION X STABILITY AND REACTIVITY INCOMPATIBILITIES Strong oxidizing agents organic materials HAZARDOUS COMBUSTION OR DECOMPOSITION PRODUCTS Nature of decomposition products not known Hazardous polymerization will not occur SECTION XI SPECIAL PRECAUTIONS AND COMMENTS The above information is believed to be correct but does not purport to be all inclusive It shall serve only as a guide Shimadzu shall not be held liable for any damage resulting from handling or contact with the above product Users should make their own determinations regarding the suitability of this information for their particular pu
50. FIRE FIGHTING MEASURES EXTINGUISHING MEDIA Carbon dioxide dry chemical powder or appropriate foam UNUSUAL FIRE AND EXPLOSIONS HAZARDS Material may have an exothermic reaction above 200 c with halocarbon vapors and may produce toxic hydrochloric acid and phosgene SECTION IX ACCIDENTAL RELEASE MEASURES Shut off all sources of ignition Wear self contained breathing apparatus rubber boots and heavy rubber gloves Sweep up place in a bag and hold for waste dis posal Ventilate area and wash spill site after material pickup is complete SECTION X STABILITY AND REACTIVITY Stability Stable Incompatibilities Strong acids strong bases chlorine trifluoride ethylene oxide halocarbons oxygen difluoride sodium nitrate vinyl acetate strong oxidizing agents organic materials Protect from moisture Hazardous combustion or decomposition products Nature of decomposition products not known Hazardous polymerization will not occur SECTION XI SPECIAL PRECAUTIONS AND COMMENTS The above information is believed to be correct but does not purport to be all inclusive It shall serve only as a guide Shimadzu shall not be held liable for any damage resulting from handling or contact with the above product Users should make their own determinations regarding the suitability of this information for their particular purposes TOC VCPH CPN 6 9 Material Safety Data Sheets 6 9 9 Potassium Nitrate 6 9 9 Potassium Nitrate Shimadzu Scien
51. Gas Sample Analysis cccccecesceseetereeseeee 232 Viewing Properties s ssssessseesseseeseseseseesesesese 161 i Method Properties Common Tabiano a 161 History Tab 0 cccecececeecesseseeeeseesecseeseeneeneens 166 NPOC and POC Tabs c cscssesseseeeseeeteeseeeees 165 Parameter Tarare a Aes 162 TC Tabah a A a aA 163 A MAEA K oE E TT 165 Periodic Inspection eeceseeeeeeeereees 238 251 Method Validation cee eeeeeetereeeeee 208 347 365 Software Controlled oo teeeeeeeeeeeeees 261 269 According to DIN ee eeseteeeeeeeeeees 347 364 EN eet hideeeatieeess Creating New File eeecececeseeseeseeseereeneeneeee 349 Warning Message Limits Editing File cceccececeseeseeseesectecseeeeeeneens 356 Manual Contents Overview Exporting Data To ASCII cece cree 363 Manual Injection Kit cece eseseeseetecreeeeeeeeneees Main Window ceccecesceseeteeteeecseeseeneeneeneens 348 AMalySiS ceecceccescesceseeseeseesecsecsecaecaecaeeneeneeneees Opening File oo ee ceeseescesceeeeeeeeeeeeeeeeeeeees 350 Calibration cccceccecsesseeeescesceeceeceseeseeeeaeensenes Printing File ccccsecseessescesceseeseeeeeeeeeeeeeeeeees 351 Trnstallation ceeeceescescesceseeseeseeseeeeseceeeaeensenee Savie File w ccccseveavsavascescatvsscnncenennenrcieeorians 351 Maintenance wis Setting Number Display Format 362 Specifications Viewing Parameters 00 0 sseeeeesete
52. If the History Log was not enabled previously it can be enabled on the History tab Calibration Curve Properties a x Common Parameter Analysis Data Graph History MV Enable hi 03 03 2003 03 11 3 03 03 2003 03 11 2 03 03 2003 03 10 3 03 03 2003 11 37 2 Zero Shift Sample Name Sample ID Cal curve created Figure 4 130 Calibration Curve Properties Window History Tab Setting Item Description Enable history log User has to comment all modifications ACSII Export Select this option to enable the software to monitor all modi fications to the system If the History Log is not required it need not be enabled as the software operates properly with out it Once this is enabled it cannot be disabled Select this option to require comments or approval for all modifications f the History Log is not required it need not be enabled as the software operates properly without it Once this is enabled it cannot be disabled The displayed items in the list are exported as tab delimi nated text files A list of the Comment dialog box contents is shown below Table 4 6 e Comment dialog box contents Item Description Date Time Displays the date and time of the modification User Displays the user who made the modification Changed item Describes the parameter that changed From Displays the previous parameter value To Displays the new parameter value Commen
53. New dialog box without making a new file 4 4 2 2 Calibration Curve The Calibration Curve command is used to insert a calibration curve into the Sample Table Selecting the command displays the File gt Open dialog box Look in E CalCurves x El c a TCtutorial 2001_01_15_10_31_08 cal a TCtutorial cal a TNtutorial 2001_01_15_10_36_08 cal a TNtutorial cal Filename EE Files of type Calibration Curves cal 7 Cancel Parameter Figure 4 75 Selecting Insert gt Calibration Curve displays the File gt Open dialog box A table of calibration information is displayed in the window at the bottom of the Open dialog box after a calibration curve is selected Click the OK button to insert the selected calibration curve into the Sample Table Click the Cancel button to abort the operation Note The Insert gt Calibration Curve command is not available during sample analysis e An error message is displayed if the selected file does not have the correct format or is not a calibration curve 126 TOC VcCPHI CPN To create a new calibration curve for insertion into the Sample Table click the New button to open the Calibration Curve Wizard The Calibration Curve Wizard consists of several windows each of which defines specific parameters for the calibration curve as described below TIP The Calibration Curve Wizard can also be accessed by selecting File gt New and double clicking the Calibration Curve icon
54. Note Typically 2 flow line rinses are sufficient Three to four rinses are recommended for samples containing acid base or salt Rinse Enables automatic rinsing of the sample needle and sparge needle between each sam ple using water from the dilution water bottle Note Rinsing between each sample prevents carryover from one sample to the next Rinsing is not necessary if all samples contain similar analyte con centrations e Rinsing is not recommended when analyzing ultra pure water samples with expected concentrations of less than a few hundred pg L The con centration of carbon in the rinse water may affect the sample results Rinsing with ultra pure water will not reduce this effect as the concen tration of carbon in the rinse water will increase with exposure to the atmosphere Rinse after acid addition Enables automatic rinsing of the sample needle and flow lines after each acid addi tion Note Rinsing the needle after each acid addition is not necessary if all samples contain similar NPOC concentrations Eliminating the rinsing operation will save time during the analysis sequence Stirrer On Enables the magnetic stirrer Select this option to stir the samples while measurement is being performed Note Stirring a sample during measurement prevents settling or clump ing of suspended solids thereby including suspended solids when the sample is drawn into the syringe 86 TOC VCPH CPN 4 2 Setting General M
55. OCT 1 8 Port Sampler is used in combination with the main unit a fully automatic system is created allowing automatic analysis of multiple samples This instruction manual covers both the TOC VCPH and TOC VCPN models These models will be referred to in relevant descriptions as the H Type and N Type respectively Read this user manual carefully before using the TOC V instrument to ensure its proper use The manual should be stored in a convenient location for future reference N caution Safety may be compromised if the instrument is used in a fashion other than that indicated in this user manual Pay particular attention to the CAUTION sections to ensure safety when using the instrument 1 JIS K 0102 Industrial Waste Water Testing JIS K 0551 Total organic carbon TOC testing methods for ultra pure water U S Pharmacopoeia EPA 415 1 EPA 9060A ASTM D2575 Standard Methods for Examination of Water and Waste Water 5310B TOC VCPH CPN 1 2 Operational Precautions l 2 Operational Precautions Take the following precautions when using this instrument N caution Do not touch the electric furnace while it is heating The center of the electric furnace near the combustion tube insertion opening reaches very high temperatures and burns may result lt Burn prevention gt To prevent high sensitivity catalyst from being forced upward in the combustion tube verify that carrier gas is flowing when heating the elect
56. Opening Calibration Curve Wizard sesseseesseseeseeee 125 Control Sample Wizard cccceeeseeseeteeseeee 126 Method Validation File ce ceeeseeseneeseees 350 Method Wizard cccesesccscesecsscssensensenseeseees 126 Sample Group Wizard ccececeseseeeceeeeeeeees 181 Sample Table 96 125 143 Sample Wizard ccceeceeeeeeeeeceeceecesceeeeaes 185 Sparge Gas Valve oo ccecseseseeeceecrseeceeeeeeeens 269 Page Setup Calibrations Tab 0 0 ecececesccseeseceeessensenseeeess 152 Header Tab 153 Instrument Tab eee eceeseceecnecneeneeneeeeeeseees 152 Miscellaneous Tab ccccecsesseeseecenseeseeseees 154 Samples Tab ives sistessassasesttstvanaleateedaeeceterestys 153 MSDS iarirnzwcnsielan uid liuachadsebeyataths CO Absorber Halogen Scr bber nimus penie 337 High Sensitivity Catalyst ssseeeesee eseese 339 Hydrochloric acid ccecesecseeseeseeseereereeeeeeees 333 Lithium hydroxide eccseeseeseeseereereeeeneene 336 Normal Sensitivity Catalyst eseese 340 Phosphoric acid cesceseeseeseesecseceescenseneeeeees 334 Potassium hydrogen phthalate 344 Potassium nitrate oe eeeeeseneeeeceeeeeeneeees 341 Quartz W O01 scccesteassdinnslaieadivannt 338 Sodium bicarbonate cccceeseeeceecneeneeeeeees 342 Sodium carbonate cc cceeeeeeecseeeceeceeeeeeees 343 Water dnain an ne oats 345 Multiple Injections ssseseseeseeeeeeeeeeee eee
57. Parameters Cal Curve Gen Info 3 TE i Figure 4 145 Sample Wizard Page 4 Injection Parameters Parameter Description Analysis Displays the analysis type This field cannot be changed Units Enter the concentration units Injection Volume Enter the injection volume Expected Conc Range Enter the maximum expected sample concentration No of Injections Enter the minimum and maximum number of injections for the sample SD Max Enter the maximum standard deviation If this value is met no additional injections are required However if both this value and the CV Max value are exceeded the sample is automatically reinjected up to the maximum number of times specified in the No of Injections field The SD Max field is disabled if the No of Injections is 1 or if the minimum is equal to the maximum CV Max Enter the maximum coefficient of variation If this value is met no additional injections are required However if both this value and the SD Max value are exceeded the sample is automatically reinjected up to the maximum number of times specified in the No of Injections field The CV Max field is disabled if the No of Injections is 1 or if the minimum is equal to the maximum No of Washes Enter the number of times the syringe is to be washed with sample prior to the first injection Note that if the Auto Dilu tion option was selected the sample w
58. Parts List 4 ASI V Part Number Part Name Comment 038 00165 21 Vial set 40mL 72 vials septa and caps 638 41462 Vial 24mL 100pcs 038 00165 48 Septum 24mL 100pcs 038 00165 50 Septum 40mL 100pcs 638 20074 01 Cap 24mL 100pcs 038 00165 40 Cap 40mL 200pcs 042 00405 11 Rinse pump head Table 6 15 e Consumable Parts List 5 8 Port Sampler OCT 1 Part Number Part Name Comment 631 20265 8 Port valve rotor TOC VCPH CPN Table 6 16 Consumable Parts List 6 TNM 1 638 65232 Ozone treatment catalyst 300g included 638 71162 Ozone treatment unit ASSY 631 43818 Reactor packing 631 40316 Viton joint reactor outlet 036 19004 19 O ring Ozone treatment unit Ipc 017 40533 01 Potassium nitrate 25 g Table 6 17 Consumable Parts List 7 Carrier Gas Purifier Kit 638 42013 L shaped combustion tube in case 630 00556 Soda lime Carrier gas purifier kit 500g included 638 60116 TOC regular catalyst LLL TOC VePrHiceN fm 307 6 7 Maintenance Parts List 6 3 8 PC Hardware Requirements 6 7 Maintenance Parts List Table 6 18 Maintenance Parts List 1 TOC VCPH Part Number Part Name Comment 638 56135 8 port valve 638 59213 Syringe 638 41337 03 Flared tubing 631 41660 Flared tubing for dilution water 638 65383 Tandem cell in case Table 6 19 e Maintenance Parts L
59. Rate of Volatile Organic Substances using Sparging Nitrogen Gas Organic Substance Pre Sparging Conc Post Sparging Conc Residual Rate ppm ppm Methanol 117 5 116 98 6 Ethanol 106 5 105 98 5 Isopropyl alcohol 129 127 98 5 n butyl alcohol 117 115 98 3 Acetone 106 101 95 3 Acetaldehyde 130 117 90 0 Ethyl acetate 102 88 86 3 Tyrosine 117 116 5 99 5 Benzene 85 2 5 2 9 Cyclohexane 79 2 2 5 TOC VCPH CPN 6 1 Principles of Analysis 6 1 4 Principles of POC Purgeable Organic Carbon Analysis 6 1 4 Principles of POC Purgeable Organic Carbon Analysis POC analysis is used to measure the volatilized component of TOC which is produced during the NPOC sample sparging process As a result NPOC POC is equivalent to TOC POC analysis is performed as follows Sparge gas containing the volatilized CO and POC components of the sample is carried to the lithium hydroxide filled CO absorber to eliminate the CO that was converted from the IC in the sample The gas which now contains only the POC component of the sample then passes through the combustion tube to be oxidized The POC component is converted to CO during oxidation and the CO is detected by the NDIR Data processing is conducted in the same manner as for TC POC is not precisely defined Factors that determine whether or not or to what degree a volatile organic carbon component is volatilized during sparging include the type of
60. Sus pended Solids kit is used TOC VCPH CPN 83 84 4 2 Setting General Measurement Parameters 4 2 2 ASI Parameter Settings Buzzer Enables the internal buzzer function Select this option to allow the buzzer to sound during measurement Auto regeneration of IC solution Enables the automatic regeneration of IC solution This option is enabled only when IC measurement is being performed and is typically selected Refer to Section 3 2 3 TOC Window for a detailed description of this option Enable ready status check Enables the Ready Status Check function When the function is enabled the software always verifies that the instrument is in the Ready state prior to starting measurement Enabling the Ready Status Check function is recommended When the function is deselected measurement can be performed when the instrument is not in the Ready state an option that is mainly for use by service personnel TN Power Source Select this item if the optional TNM 1 unit is installed to perform TN analyses TC Furnace Select the desired TC furnace temperature by clicking the appropriate radio button If Combustion is the selected oxidation method select 680 or 720 If Wet Chemical is the selected oxidation method the TC Furnace field is set to Off and disabled 4 2 2 ASI Parameter Settings The following parameters must be set when using the ASI V Tray type Needle Number of needle washes Number of flow line wa
61. TOC standard catalyst into the combustion tube to a height of 140mm from the top end of combustion tube A Introduce a small amount of ceramic fiber to cover the catalyst M Lightly press with a catalyst filling rod so that the thickness of the ceramic fiber is 10mm Note The thickness of the ceramic fiber must be uniform covering the entire surface of the catalyst or a poor TN detection rate may result e The filling heights of the catalyst and ceramic fiber influence the TN detection rate so it is important that the dimensions are close to those indicated below Catalyst 140mm from the top end of combustion tube Ceramic fiber 10mm Combustion Tube 140mm Ceramic Fiber TOC Standard Catalyst Quartz Wool Platinum Mesh Figure 4 3 Filling Combustion Tube with Catalyst for TOC TN Analysis TOC VCPH CPN 39 40 4 1 Analysis Preparation 4 1 2 Connecting the Combustion Tube 4 1 2 Connecting the Combustion Tube The procedure for installing the combustion tube differs depending on whether the instrument is the H Type or the N Type The procedure for each type is described below N caution Due to the potential for burns maintenance of the combustion tube and catalyst should be performed after the electric furnace temperature has cooled to room temperature When connecting the combustion tube handle it carefully to avoid breakage The combustion tube is constructed of quartz glass an
62. The General Information dialog box is used to view and edit information about the method validation file such as the system used to create the file the file version the operator who created the file and the date on which the file was created Some information fields may be disabled Comments about the file are displayed in the Comment field LLL TOC VerHiceN fm 359 A 5 2 Method Validation Parameter The Method Validation Parameter command displays the Method Validation Parameter window which contains detailed information about the method as described below Method Validation Parameter Mi 01 19 01 10 33 12 AM January 5 val January 5 ce Figure A 18 Method Validation Parameter Window Item Description Enable manual editing Unit Analysis Type Date Time Title Calibration curve file name Select to allow data tables to be edited manually This option is disabled for files linked to TOC Control V calibration curves If this option is deselected it is disabled and cannot be selected again This option is selected by default Displays the calibration curve units This option is disabled if the Enable manual editing option is not selected Displays the analysis used to create the calibration curve This option is disabled if the Enable manual editing option is not selected Displays the date and time the file was created Displays the title of the method validation file Displays the name o
63. and the IC in the sample is converted to carbon dioxide and detected by the NDIR TOC VcPHICPN 285 286 6 1 Principles of Analysis 6 1 3 Principles of NPOC Non Purgeable Organic Carbon Analysis 6 1 3 Principles of NPOC Non Purgeable Organic Carbon Analysis After acidifying the sample to pH 2 to 3 sparge gas is bubbled through the sample to eliminate the IC component The remaining TC is measured to determine total organic carbon and the result is generally referred to as TOC However in the TOC V this analysis value is referred to NPOC to distinguish it from the TOC value obtained by calculating the difference between TC and IC NPOC stands for non purgeable organic carbon and refers to organic carbon that is present in a sample in a non volatile form NPOC and TOC obtained by IC elimination described in the TOC related standard methods and referred to in water quality related test methods JIS ASTM EPA EN are identical Purgeable organic substances in the sample can be lost during the sparging process Consequently when the sample contains purgeable organic substances TOC should not be measured by the NPOC method If the dissolved purgeable organic component in the water sample is large the amount volatilized during sparging is relatively small Generally the amount of purgeable organic substances in natural environmental public and purified water is small as a result NPOC can be referred to as TOC Table 6 1 e Residual
64. appear in the Method Wizard window Method Wizard Page 1 System Information Method Wizard Page 1 System Information Parameters Cal Curve Gen Info Figure 4 84 Method Wizard Page 1 System Information Setting Item Description System Select one of the configured instruments Operator Displays the current operator name Date of Creation Displays the current system time Comment Enter a comment 512 characters maximum if desired LLL TOC fy 735 Method Wizard Page 2 Analysis Information The Analysis Information window is used to set analysis parameters for the method being created Method Wizard Page 2 Analysis Information 2 Parameters Cal Curve Gen Info Figure 4 85 Method Wizard Page 2 Analysis Information Setting Item Description Analysis Select the analysis type from the drop down list Default Sample Name Enter the default sample name 64 characters maximum Default Sample ID Enter the default sample ID 64 characters maximum Dilution Enter the preparation dilution factor which will be used to calculate concentration results The default value is 1 No of Determinations Enter the number of times each sample is to be measured Note that determinations and injections are different each determination is made up of one or more injec
65. are additive For samples that have a comparatively large IC concentrations relative to TOC concentrations the TOC analysis error is large if it is determined by the difference between TC and IC results Samples of this type include samples from water treatment facilities or from the natural environment such as rivers lakes swamps oceans and groundwater Using the difference between TC and IC to determine TOC is not appropriate for purified water or ultra pure water samples The CO in air dissolves in the sample and is measured as IC causing the concentration to vary In such cases the sample is pretreated with aeration or sparging before analysis to remove the IC The sample is then subjected to TC analysis immediately followed by TOC analysis using the NPOC method Sparge Sequence There are two methods for sparging with this instrument 1 Sparging in the sample injector syringe This is performed only when the instrument is set for automatic sparging before analysis 68 TOC VCPH CPN 4 1 Analysis Preparation 4 1 15 Sample Preparation 2 Independent sparging of sample using the optional external sparge kit Sample is introduced into a clean sample container acidified and then sparged A glass container with an external diameter of 24 25mm and a height of 200 250mm is appropriate for use as the sample container Test tubes stopper equipped test tubes and chromatography tubes of suitable size are available commercially If the
66. authorized Shimadzu service engineer or someone who has been properly trained in the procedure Contact your Shimadzu representative to request replacement at the appropriate time Confirming Operation Time The ozone generator operating time is displayed in the Maintenance History window which is accessed through the Sample Table Editor From the Instrument menu select Maintenance gt Maintenance History N caution If the ozone generator is used after 8000 hours of operation ozone generation may not be sufficient for analysis or ozone may leak from inside the generator Replace the ozone generator without fail 5 5 4 Replacing the NO Absorber The NO absorber absorbs NO gas generated in the TN unit A CO absorber is used for the NO absorber The CO absorber was previously used for purging the NDIR detector optical system Section 5 2 5 Replacing the CO Absorber and is still effective for this application During the annual replacement of the CO absorber used to purge the optical system of the NDIR detector replace the NO absorber for the TN unit with the used CO absorber from the TOC V Discarding the NO Absorber CO Absorber Place a request to an authorized industrial waste contractor to process the used NO absorber CO absorber Clearly indicate in the industrial waste material manifest that the absorber contains soda lime TOC VCPH CPN 5 6 Software Controlled Maintenance Functions 5 6 1 Zero Point Detect
67. calculated automatically based on the values entered into the Standard Solution Conc and Auto Dilution fields Enter the minimum and maximum number of injections Enter the maximum standard deviation or coefficient of vari ation values Calibration Curve Wizard Page 6 Peak Time Parameters The Peak Time Parameters window is used to set peak detection parameters Calibration Curve Wizard Page 6 Peak Time Parameters Figure 4 82 Calibration Curve Wizard Page 6 Peak Time Parameters Setting Item Description Use default settings Select this option to use the default peak detection parame ters When this option is selected all other options in this window are disabled Allowed peak start delay The allowed peak start delay is the amount of time in min utes that can elapse before the analysis is stopped because a peak is not detected Enter a number between 0 and 20 00 Total integration time The total integration time is the amount of time in minutes that analysis continues after the end of the peak is detected Enter a number between 4 50 and 20 00 LLL TOC Vcc fy 7133 Calibration Curve Wizard Page 7 History The History window is used to enable the History Log The History Log records all modifications to the calibration curve properties The History Log can be set to require users to enter comments for each modification If the History Log is not required it need not be enabled as the software operates
68. culation Select to enable the instrument to automatically adjust the injection volume and dilution factor when the peak height for the initial injection exceeds full scale After the adjustment measurement will be repeated TOC VCPH CPN 139 Method Wizard Page 5 Peak Time Parameters The Peak Time Parameters window is used to set peak integration parameters Method Wizard Page 5 Peak Time Parameters Figure 4 88 Method Wizard Page 5 Peak Time Parameters Setting Item Description Analysis Displays the previously selected analysis type Use default settings Select this option to use the default integration parameters When this option is selected all other options in this window are disabled Allowed peak start delay The allowed peak start delay is the amount of time in min utes that can elapse before the analysis is stopped because a peak is not detected Enter a number between 0 and 20 00 Total integration time The total integration time is the amount of time in minutes that analysis continues after the end of the peak is detected Enter a number between 4 50 and 20 00 140 QQ ON PN ee Method Wizard Page 6 USP EP The USP EP window is displayed only for TC or NPOC methods and is used to enable samples to be checked in accordance with USP standards Select the check box to enable the function Method Wizard Pag Figure 4 89 Method
69. danger of burn injury allow the oven temperature to cool to room temperature before starting any maintenance procedure involving the combustion tube or catalyst Procedure 1 Thoroughly wash the catalyst with tap water to remove any accumulated salts 2 Neutralize the alkalis with dilute hydrochloric acid 5 1 3 Thoroughly wash the catalyst with tap water to remove the hydrochloric acid 4 Rinse with pure water ion exchange water acceptable and then dry N caution e Dry the catalyst at a temperature lower than 700 C to avoid the degradation of catalyst activity that occurs at higher temperatures e A large quantity of steam is produced when the regenerated catalyst is placed in the oven and heated Due to the danger of burn injury leave the outlet of the combustion tube open until no more steam is released TOC VcPHICPN 239 240 5 2 Periodic Inspections 5 2 2 Washing or Replacing Catalyst 5 2 2 2 Replacing Catalyst If performance is not restored after washing the catalyst it must be replaced Replace the catalyst with new platinum catalyst alumina spherical support Keep extra platinum catalyst on hand for such a contingency One bottle of platinum catalyst is enough for one replacement Use the following procedure to replace the platinum catalyst Procedure 7 Wash the platinum mesh and the inside of the combustion tube with 1 2 hydrochloric acid 1 part concentrated HCl and 2 parts water 2 Ri
70. dialog box shown above is displayed after any change is made in the Instrument Properties dialog box 3 2 9 Removing a Configured System Systems are removed from the TOC Control V software using the main window To remove a system right click the appropriate system icon and select Delete Once a system is deleted it cannot be restored TOC VCPH CPN 33 BOC NN Lee Operation This chapter describes procedures for pre analysis preparations setting measurement parameters starting up the instrument generating calibration curves and conducting sample analysis This chapter also includes a tutorial that covers setup and measure ment procedures 4 1 4 2 4 3 4 4 4 5 Analysis Preparation This section describes instrument preparation procedures such as catalyst filling combustion tube connection and syringe replacement as well as other preparation procedures for actual sample analysis Setting General Measurement Parameters This section describes procedures for setting TOC ASI and default measurement parameters using the TOC Control V software Measurement Procedures and Tutorial This section describes and provides a tutorial for measurement procedures such as instrument startup calibration curve generation method development sample analysis halting of analysis and instrument shutdown Sample Table Editor This section provides a detailed description of the TOC Control V Sample Table Editor me
71. dilute hydrochloric acid is injected onto the catalyst Be sure to verify that sufficient hydrochloric acid is in the instrument acid reservoir before starting the procedure Regeneration of TC Catalyst Regeneration of TC Catalyst d d d d d d d d dd od oe oo od Figure 5 25 Regeneration of TC Catalyst Dialog Box Click the Start button to begin the procedure A progress bar is active until the TC catalyst is regenerated Click the Close button 5 6 3 Regeneration of the IC Solution Use this function to restore the acidity of the IC solution which decreases over time as the acid reacts with IC sample constituents During the procedure IC reagent is automatically pumped to the IC reaction vessel This option is available only if an IC unit is connected to the system Regeneration of IC solution Regeneration of IC solution i d d d d d dd ddad dddid Figure 5 26 Regeneration of IC Solution Dialog Box Click the Start button to begin the procedure A progress bar is active until the IC solution is regenerated Click the Close button 262 TOC VCPH CPN 5 6 4 Residue Removal Use this function to remove residue from the flow lines and syringe Residueremoval er fe De DD J J se os Figure 5 27 Residue Removal Dialog Box Click the Start button to begin the procedure A progress bar is active until the residue removal procedure is complete Click the Close button 5 6 5 Replace Flowline Content Sel
72. directory from the drop down Drive and Directory lists then select it by clicking the OK button Click the Network button to access at network drive a Program Files E Shimadzu Corporati 4 toc3201 Ce Figure 4 181 Folder Dialog Box Delete Click the Delete button to delete a selected directory from the list Up Click the Up button to move the selected directory up one line in the list The order of the directories in the list is the order in which the directories will be searched during instrument operation Down Click the Down button to move the selected directory down one line in the list The order of the directories in the list is the order in which the directories will be searched during instrument operation LLL TOC Vc le 277 4 4 10 Window Menu Figure 4 182 Window Menu 4 4 10 1 Cascade The Cascade command is used to stack all open windows so that the title bars are visible 4 4 10 2 Tile The Tile command is used to size all open windows so that each window occupies an equal portion of the screen 4 4 10 3 Arrange Icons The Arrange Icons command is used to neatly organize windows that have been minimized or reduced to icons 4 4 11 Help Menu Figure 4 183 Help Menu About The About command is used to view copyright software registration and software version information 218 Wl TOC VcrHicrn nnn 4 5 Application Operations 4 5 1 Manual Injection Analysis 4 5 Application Operations
73. edb dl babe bey 100 EEELEEEETSS rrr iiss Signallmv 600 E 100 08 20 Time min Figure 4 102 Print Preview gt Report Window 4 4 2 14 Print Setup The Print Setup command is used to set print options Select this command to open the Print Setup dialog box which may have a variable display depending on the installed printer driver Modifications to the Print Setup dialog box are saved until the TOC Control V software is exited Print Setup Figure 4 103 Print Setup Dialog Box 4 4 Sample Table Editor 4 4 2 File Menu 4 4 2 15 Page Setup The Page Setup command is used to select items to be printed on a report or table and to specify format parameters such as margins headers and footers Selecting the command displays the Page Setup window which consists of several tabs Each tab contains a list of page setup options shown in the figures below On each tab certain options are selected by default Individual options can be selected or deselected by clicking in the check box Use the Select All and Select None buttons to quickly select and deselect all options on a tab Use the Default button to select the default options for a tab Click the Cancel button to exit the Page Setup window without saving changes Click the OK button to save changes and exit the Page Setup window Instrument Tab The Instrument tab displays a list of instrument information items that can be printed on the report Page setup xj
74. eed vee hia eee 24 B23 TOC Window eocenie nie ii sedan E E R n e n e 26 PAA AST Window e E N 28 ILT SSM WON ae EAE tos hese E EATA 29 3 2 6 Communication WindoW ssesesesesessssseeeresrstesstsrstsrstsestssesestststrerseseseessee 30 3 2 7 History Function Window s ssssesesessessssessseeseseesrsresrerssernesersreeesseressesesses 31 3 2 8 Instrument Properties Dialog BOX sssssssssesssesesersssrsrsresseressrsesseeressesesees 32 3 2 9 Removing a Configured SystemM esssessssessssessesesseesseerssersesrsrsreseesessesesses 33 4 Operation ssssssessissesorssoroessossetsriso sous ss posest saa oase asie spant sesso 4 1 Analysis Preparation ccccccccsssscesscesceesecseceseeseeeeseeeseeeaeceaeceeeeeeeenseenaees 36 4 1 1 Catalyst Filling perar erree E RE E E EE ERR T E ek 36 4 1 1 1 Catalyst for TOC Analysis 0 ccceeccecceeseesecscecseceseeseceeeeteeseeseeeeeeees 37 4 1 1 2 TOC TN Catalyst Option 0 ccecceeceesesseececseceseeeceeeeeceeeseeeeeeeereees 39 4 1 2 Connecting the Combustion Tube ccceceesceseeeseesceseeeeecseeseeceeereeeeeens 40 41 3 Installing th Syringe meniren narn aiken Rh eid nth 45 4 1 3 1 Syringe Pump Zero Point Detection ccesceseeseeeeeeeeeeeeseeeeeenes 47 4 1 4 Water Supply to the Cooler Drain Container 0 ceeceseseeseereeeeeteneeeeeeees 48 4 1 5 Filling the Humidifier with Water cccccsccecceseesscesceeeeeeceseeeeceeeseeeenaees 49 4 1 6 Preparation of D
75. gt Open dialog box Select this option to insert a sample without defining a source Sample mea surement parameters will be entered in subsequent pages 1 12 of the Sam ple Wizard Select this option to accept all measurement parameters from the source file The Next button will become a Finish button and subsequent pages of the Sample Wizard will not be displayed This option is disabled if Edit parame ters manually is selected TOC VcPHICPN 185 Sample Wizard Page 2 Analysis Information Sample Wizard Page 2 Analysis Information Parameters Sample Cal Curve s Gen Info Tutorial 1 0000 Figure 4 143 Sample Wizard Page 2 Analysis Information Parameter Description Analysis Select the analysis type from the drop down list Default Sample Name Enter the sample name Default Sample ID Enter the sample identification Dilution Enter the preparation dilution factor No of Determinations Use the spin controls to enter the number of times the sample is to be measured Note that determinations and injections are different each determination is made up of one or more injections Enter an integer from 1 to 10 Note For combined analyses such as TC TN or POC NPOC subsequent Sample Wiz ard windows may appear more than once so that parameter modifications spe cific to each analysis type can be made The analysis type that is associate
76. impurities contained in the alkali reagents used for neutralization All salts of nitric acid generate acidic gas under thermal decomposition as a result neutralization is ineffective When the sample contains hydrochloric or hypochlorous acid hydrochloric acid gas is generated from salts that are readily subject to thermal decomposition such as ammonium chloride calcium chloride and magnesium chloride The instrument is equipped with a halogen scrubber however the scrubber s main function is absorb hydrochloric acid gas generated by corrosion of the gold plating on the internal surface of the NDIR cell Alkaline samples When performing TC analysis on alkaline samples the following problems can arise e Rapid decrease in sensitivity and loss of reproducibility e Rapid degradation of catalyst or wear of the combustion tube e Likelihood that IC will be high due to absorption of carbon dioxide For these reasons the NPOC analysis is suitable for alkaline samples In NPOC analysis dilute hydrochloric acid is added to adjust the solution to a pH of 2 3 thereby forming a salt For example calctum chloride will be formed as a salt if the sample contains calcium hydroxide as the base Since it is preferable for this salt concentration to be low alkaline samples should be diluted as much as possible Salt accumulation Samples should be diluted as much as possible to reduce the salt concentration and extend the life of the combustion tube
77. involves two steps creating a calibration file which stores information about calibration standard measurements and inserting the calibration standard runs in the Sample Table Separate calibration files are created for the TC and TN analyses The calibration is a three point curve generated using standard mixtures of potassium hydrogen phthalate and ammonium chloride Creating the TC Calibration File 7 Open the Sample Table From the File menu select New The New dialog box is displayed Click the Calibration Curve icon T Calibration Curve Figure 4 44 Creating a New Calibration File 2 Click the OK button to open the Calibration Curve Wizard Specific information about the calibration will be entered in the wizard Calibration Curve Wizard Page 1 System Information Cal Pts Analysis Cal Type Figure 4 45 System for Analyses of the Calibration Standard 10 0 WE TOC VcrHichN eee 3 Select the system to be used for the analyses from the drop down list on page 1 of the Calibration Curve Wizard Click the Next button Page 2 of the Calibration Curve Wizard which lists options for calibration curve type is displayed The four types of calibration curves available are e Calibration points are distributed uniformly over the concentration range e Edit calibration points manually e Calibration curve according to DIN38402 P 51 e Calibration curve according to USP EP Calibration Curve Wizard Page 2
78. limits to values slightly less than the remaining volume of each respective liquid A warning message will be generated before each liquid is completely consumed Click the Reset button to the right of a parameter to clear its current value TOC VCPH CPN 4 3 Measurement Procedures and Tutorial 4 3 1 Starting Up the Instrument 4 A 3 Measurement Procedures and Tutorial 4 3 1 Starting Up the Instrument 4 3 1 1 Turning on the Power Turn on the power to the instrument by pressing the power key on the bottom right of the front panel Note Press the power key again to turn off power to the instrument 4 3 1 2 Carrier Gas Pressure Procedure for setting the carrier gas pressure 7 Set the supply pressure of the carrier gas to 300kPa using the pressure regulator at the carrier gas supply source cylinder Note If compressed air or instrumentation air is used verify that the supply pressure is greater than 300kPa and does not exceed 600kPa 2 Open the front door of the instrument and adjust the carrier gas pressure to 200kPa using the carrier gas pressure regulation knob Carrier Gas Pressure Regulator CARRIER GAS Carrier Gas Pressure Regulation Knob PRESSURE Figure 4 30 Setting the Carrier Gas Pressure TOC VCPH CPN 89 4 3 Measurement Procedures and Tutorial 4 3 1 Starting Up the Instrument 4 3 1 3 Carrier Gas Flow Rate Procedure for setting the carrier gas flow rate 7 Ope
79. measurement occurs information in the appropriate Injection Table row is completed Previous injections are shown above the current row Use the scroll bar to see all of the information and use the tabs at the bottom of the table to toggle between analysis types between TC and TN in this case e To view the peak profile of the measurement in progress click the asterisk of Sample No To view a previous measurement click that row e When the Sample Window is opened the text on the graph may be overly enlarged In that situation close the Sample Window and then open it again During measurement even if All Peaks is selected because it takes time for the screen to update the peak display may not change In this case select All Peaks following measurement e When the measurement Type is TC TN NPOC TN TOC TN or POC NPOC TN the peak profile of the selected measurement type may not be displayed even after clicking the measurement type for example TC and TN toggle tab in the Sample Window In that situation click the data in the Sample Window corresponding to the peak you wish to display 77 Statistical information about the current set of injections is calculated and displayed in the Sample Window As a result preliminary decisions about the measurements can be made while the analysis is still in progress Note Information about the current injection is shown in the status box in the upper right portion of the Sam
80. new blank Sample Table is displayed E Untitled NG TN base ae Type Analysis Sample Na Sample ID ObjectD Origin Dilution Rest 5 Figure 4 40 New Sample Table a TOC fy 97 Connecting to the Instrument 7 To establish communication between the software and the instrument either select Connect from the Instrument menu or click the Connect toolbar button The Parameter Configuration dialog box is displayed Click the Use Settings on PC button The Sequence dialog box is displayed Open Port 100 TOC Initialize now Initializing Figure 4 41 Connection in Progress 2 The Sequence dialog box displays information about the attempt to establish communication between the software and the instrument Creating a Sample Table Step 3 Procedure Creating a Sample Table involves three steps First enter the default analysis parameters for the Sample Table t32 file 7 From the Options menu select Default Measurement Parameters 2 Three injections of each calibration standard and unknown sample will be made On the TC tab change the No of injections value to 3 The other default measurement parameters should not be changed 3 On the TN tab change the No of injections value to 3 The other default measurement parameters should not be changed Default Measurement Parameters x loom a St St p a PEER E Figure 4 42 Default Measurement Parameters Dialo
81. not breathe dust Do not get in eyes on skin or on clothing Avoid prolonged or repeated exposure Wash thoroughly after handling Corrosive harmful solid Keep tightly closed Hygroscopic Store under nitrogen in a cool dry place SECTION II PHYSICAL DATA Melt Boil Density Vapor Vapor Evaporation Odor Color Phase Water Point Point Pressure Density Rate Solubility N A N A 1 510 N A N A N A N A White Crystals N A SECTION IV REACTIVITY DATA Substance is strongly alkali In contact with or mixed with acid reaction is extremely strong Aluminum and zinc are corroded by this substance and not suitable as containers Corrosive effect is enhanced in presence of humidity or water Absorbs CO from air Containers made of steel stainless steel glass ceramic and many synthetic compounds are relatively durable Nature of decomposition products not known SECTION V FIRE AND EXPLOSION HAZARD DATA FIRE This substance is nonflammable Use water mist powdered extinguishing reagents foam or carbon dioxide gas Cool container using water mist and move container to safe location EXPLOSION Not considered to be an explosion hazard EXTINGUISHING MEDIA Carbon dioxide dry chemical powder alcohol or polymer foam Special Firefighting Procedures Use full protective clothing and NIOSH approved self contained breathing apparatus with full face piece operated in the pressure demand or other positive pressure mo
82. of the pump head from the Teflon tubes Connect the new rubber tubing to the Teflon tubes of the pump head Replace the pump head by following the above procedure in reverse Figure 5 12 Replacing the Pump Head of the IC Reaction Solution Pump 5 2 Periodic Inspections 5 2 14 Replacing the Filler of the Optional POC Analysis CO Absorber 5 2 14 Replacing the Filler of the Optional POC Analysis CO Absorber The CO absorber for POC analysis is filled with about 6 grams of lithium hydroxide which is sufficient to absorb carbon dioxide gas for several hundred analyses under normal conditions Airflow resistance gradually increases with use and may become excessive irrespective of adequate carbon dioxide absorbency Replace the lithium hydroxide in the CO absorber with a new batch if analysis values become unstable or carrier gas flow is impeded For the procedure on filling the CO absorber with lithium hydroxide refer to Section 4 1 12 Preparation for POC analysis N caution e Lithium hydroxide is a corrosive strongly alkali powder Be carefuel not to spill or touch it during handling For details refer to Section 6 9 Material Safety Data Sheets e Used lithium hydroxide should be disposed of by a certified industrial waste handler according to local industrial waste disposal regulations It must be clearly disclosed using an industrial waste manifest that the waste is lithium hydroxide e Lithium hydroxide cry
83. organic compound the gas liquid contact with the sparge gas and the ambient temperature during sparging The target of POC analysis is the organic component present in the aqueous phase As a result organic compounds that are highly soluble in water such as methanol or ethanol and not easily volatilized by sparging produce almost no peaks in POC analysis Organic compounds with low solubility in water such as methylene chloride or chloroform produce sharp peaks in POC analysis Over a long period of time compounds such as acetone and methyl isobutyl ketone generate extremely broad tailing peaks with no specific end time The lithium hydroxide filled CO absorber eliminates the carbon dioxide that was generated along with the POC substances Therefore POC components that are easily caught in the CO absorber such as esters produce low values in POC analysis POC results obtained using this technique are not absolute The user should take all the above factors into consideration when measuring POC using this instrument TOC VcPHICPN 287 288 6 1 Principles of Analysis 6 1 5 Principles of Measuring TOC 6 1 5 Principles of Measuring TOC TOC can be measured using the following 3 methods e TC IC Method e NPOC Method e POC NPOC Method TC IC Method In the TC IC method TOC is measured as the difference between the TC and IC analysis values The TC IC method is not recommended for samples that contain more IC than TOC sa
84. parameter and history settings respectively Click the Finish button to create the new calibration curve Note Select the settings described in Section 4 2 Setting General Mea surement Parameters Create a Sample Table for the calibration curve From the Insert menu select Calibration Curve Select the newly created calibration curve from the list of files in the Open dialog box Connect the instrument by selecting Connect from the Instrument menu Then select Start from the Instrument menu The Manual Injection Parameter dialog box is displayed Draw an appropriate amount of sample into the syringe Note Draw in and discharge the sample 3 or 4 times before filling the syringe for measurement Enter the injection volume in the Manual Injection Parameter dialog box and click the Set button Verify that the instrument is ready for measurement and click the Start button For TC or TN measurement open the injection port valve and insert the syringe needle into the injection port For IC measurement insert the syringe needle into the injection port septum Note Insert the syringe needle as far as possible into the injection port e To obtain reproducible results perform all injections at the same speed Withdraw the syringe from the injection port For TC or TN measurement close the injection port valve The results are displayed when measurement is complete Click Additional Measurements to perform repeat measurements
85. properly without it Note Once the History Log is enabled it cannot be changed All modifications to the calibration curve properties will be tracked If the mandatory comment option is selected the user will be required to enter a comment each time any parameter in the calibration curve is modified Calibration Curve Wizard Page 7 History Figure 4 83 Calibration Curve Wizard Page 7 History Setting Item Description Enable history log Select this option to enable the software to monitor all modi fications to the system Once the History Log is enabled it cannot be changed if GLP is selected during installation The GLP laboratory guidelines require that a history of changes be maintained for the system User has to comment all Select this option to require the user to comment all modifi modifications cations 134 QQ VON APN Lee 4 4 2 3 Method Wizard The Method Wizard is used to set method parameters and is accessed by selecting File gt New gt Method The Method Wizard consists of several windows each of which is described below The Back and Next buttons are used to navigate between windows Note that each set of parameters selected for a specific method applies only to that method Note Selected windows in the Method Wizard will be repeated for combined analysis types such as TOC POC NPOC Each duplicate window represents one analy sis type Parameters that are not applicable to an analysis type will not
86. quickly as possible using caution to avoid inclusion of external contaminants If a water purification apparatus is the source of purified water allow the water to flow for a few minutes prior to use as the initial water will have a higher TC concentration Alternate the flasks a number of times while filling them with water to equalize as much as possible the TC concentration of the purified water Use fresh purified water when filling the volumetric flask to the graduation line Do not use rinse bottle water that has been standing for a long period of time because the TC concentration continually increases with time TOC VCPH CPN 4 1 Analysis Preparation 4 1 15 Sample Preparation Instrument Preparation The blank peaks present at the start of high sensitivity analysis will become progressively smaller and gradually stabilize As a result calibration curves generated too soon after the start of analysis may be inaccurate because they contain data collected during unstable conditions To prevent this problem perform 5 or more measurements of purified water containing 2 3 drops of 1M HCI per 100mL of water prior to analyzing the calibration standards Use the same measurement parameters injection volume sparge time that will be used for the calibration standards and samples Calibration Curve Analyses Calibration curves are generated using the following two methods 1 Using standard solution in a 250mL volumetric flask Inser
87. samples are automatically reinjected up to the maximum number of times specified in the No of Injections field The Max SD field is disabled if the Number of Injections is 1 or if the minimum is equal to the maximum The default value for Max SD is 0 1 e Max CV Enter the default maximum coefficient of variation that is acceptable for repeat measurements If this value is met no additional injections are required However if both this value and the Max SD value are exceeded the samples are automatically reinjected up to the maximum number of times specified in the No of Injections field The Max CV field is disabled if the Number of Injections is 1 or if the minimum is equal to the maximum The default value for Max CV is 2 Note The maximum No of Injections field refers to the maximum number of repeat injections to be performed when the automatic additional measurement function is enabled Additional measure ments are performed when both the Max SD and Max CV settings are exceeded When both of these values are exceeded for the set number of sample injections the additional measurement function is automatically activated and the sample is reinjected TOC VCPH CPN 87 4 2 Setting General Measurement Parameters 4 2 4 Maintenance History Settings 4 2 4 Maintenance History Settings Enter limits for the following parameters to display a warning message when the limits are exceeded e Combustion Tube Sample Injection Volume Refe
88. selected location in a table Print Sends the data from the currently displayed window to the printer Clicking the button starts printing immediately using the current printer settings Help About Provides information about the TOC Control V software Background Monitor Displays the Background Monitor window which displays the status of the ASI and the instrument detector s TOC VCPH CPN 4 4 Sample Table Editor 4 4 1 Sample Table Window Overview Connect Opens or closes the electronic connection between the instrument and the PC Standby Shuts down or reactivates the instrument Start Continue Starts measurement Either the Manual Injection Parameter or Sparging Acid Addition window is displayed depending on the instrument settings Stop Stops the measurement sequence after all injections of the current sample are complete Halt Immediately stops the current measurement and discards data from the inter rupted measurement Peak Stop Stops the measurement sequence and aborts analysis of the current sample The peak in progress is treated as if it were a completed analysis Properties Displays the Sample Method Properties dialog box Calibration Curve View Displays the calibration curve data Highlight the calibration standard row in a Sample Table to select the calibration curve to examine Sample Opens the Sample Window which displays detailed information for each sample injection and can be used to view m
89. systems by collecting information such as installed instrumentation instrument settings and communication parameters Also describes procedures for viewing the properties of and removing previously configured systems 20 3 1 Introduction to System Administration Functions 3 1 1 Screen Lock Function 3 1 Introduction to System Administration Functions This section describes the various system administration functions in the TOC Control V software that are available to the user For a description of system administration functions that can be performed by the system administrator refer to the TOC V Administrator s Manual 3 1 1 Screen Lock Function If user must temporarily leave the PC during measurement the screen can be locked to protect the data from another individual making improper or malicious operations in TOC Control V This function can be used only if the User ID Password item is checked in the Security dialog box Consult with the system administrator to implement changes in the security settings To lock the screen select Screen Lock in the Tools menu The screen is locked and the Re enter Password dialog box displayed Once the screen is locked it can only be unlocked by entering the User ID and Password of the user who was logged on at the time the screen was locked Doe Gl amp Ba Ontol Charts Method Validation Administration History Database i ETOC 20031 a6 Toc 200302 If
90. the Ready state an option that is mainly for use by service personnel TN Power This item is displayed if TN was selected as an option in the previous screen Select this item to perform TN analyses TC Furnace Select the desired TC furnace temperature by clicking the appropriate radio button Select 680 C for regular or high sensitivity catalyst Select 720 C for TC TN catalyst TOC VCPH CPN 27 28 3 2 Instrument Setup and System Properties 3 2 4 ASI Window 3 2 4 ASI Window The ASI window of the Instrument Setup Wizard is displayed if ASI was selected in the Options window of the Wizard Use the ASI screen to set the autosampler parameters Instrument Setup Wizard ASI x Iray Type Needle No of Needle Washes 2 Z Binse No of Flow Line Washes 2 a IV Rinse after acid addition I Stier On Notice If tray type is 125ml vial needle type should be Single or Coaxial Combustion Specify the ASI parameters lt Back Next gt Cancel Figure 3 9 Instrument Setup Wizard ASI Window Tray Type Select the ASI tray type from the drop down list Options are 24mL Vial and 40mL Vial Needle Select the needle type from the drop down list Options are Sample for analysis using only a sample needle Sample Sparge for analysis using both a sample needle and a sparge needle Coaxial for analysis using an integrated sample and sparge needle Coaxial Sparge fo
91. the No of Injections field This field can be edited CV Max Displays the maximum coefficient of variation If this value is met no additional injections are required However if both this value and the SD Max value are exceeded the samples are automatically reinjected up to the maxi mum number of times specified in the No of Injections field This field can be edited Acid Addition Displays the quantity of acid to be added to each sample This value is expressed as a percent or the sample volume and is available only for NPOC and related analyses This field can be edited 4 4 Sample Table Editor 4 4 4 View Menu Setting Item Description Peak Time Parameters Use default settings Select this option to use the default settings for peak inte gration Allowed peak start delay Displays the amount of time in minutes that can elapse before the analysis is stopped because a peak is not detected This field can be edited by entering a number between 0 and 20 00 This option is disabled when Use default settings is selected Total integration time Displays the amount of time in minutes that analysis continues after the end of the peak is detected This field can be edited by enter ing a number between 4 50 and 20 00 This option is disabled when Use default settings is selected Multiple Injections Select this option to enable the syringe to draw up a single sample aliquot with a volume equal to that required for all injections of
92. the instrument 90 TOC VCPH CPN 4 3 1 5 TN Unit 4 3 Measurement Procedures and Tutorial 4 3 1 Starting Up the Instrument When TN analysis is to be performed using the optional TN unit power to the TN unit and ozone generator must be turned on Turning Power to the TN Unit ON 1 5 In the TOC Control V main window double click the icon for the desired instrument The Instrument Properties dialog box is displayed Click the TOC tab Click in the TN Power check box to select the option Click the OK button The screen returns to the TOC Control V main window Turning Power to the Ozone Generator ON 1 TIP Power Button positions Press the power switch at the lower right of the TN unit we ON a O OFF 4 3 1 6 Ozone Source Airflow Rate for the TN Unit Adjust the ozone source airflow knob on the TN unit to indicate 500mL min on the flow rate gauge TOC VCPH CPN 91 92 4 3 Measurement Procedures and Tutorial 4 3 2 Tutorial 4 3 2 Tutorial This tutorial gives step by step instructions on the use of the TOC Control V software The tutorial assumes that the hardware and software have been installed in the manner described in Chapters 2 and 3 and that users have a configured system that includes the TOC VcpH ASI and TNM 1 unit Note If your system does not include the ASI and TNM 1 units please adjust the tutorial procedure as appropriate In the tutorial a three point TC TN calibration c
93. the sample When this option is not selected the syringe will draw up a separate sample aliquot for each injection as a result selecting this option reduces analysis time Auto correction of inj Select this option to enable the instrument to automatically adjust the injection volume and dilution volume and dilution factor when the peak height for the initial injection exceeds full scale After the adjustment measurement will be repeated Auto Dilution Displays the factor by which the instrument will automatically dilute the sam ple This field can be edited Inj Volume Displays the injection volume This field can be edited Expected Conc Range Enter the expected concentration if it is known Use area retrieved from Select to include blank check result in the concentration calculation the blank check Calibration Curve 1 2 3 Displays the name s of calibration curve s used to quantitate samples ana lyzed by the method These fields can be edited by entering a calibration curve file name or clicking the Browse button to search for the file IC Tab The IC tab options are similar to those described above for the TC tab Parameter IC History Analysis Parameters _ Peak Time Parameters Units nd IV Use default settings No of Ini fe g M1 20 Allowed peak start delay No of Wash p 00 00 0 0 20 0 min SD Max o t000 Total integration time CV Max 2 00 z 0330 3 30 20 0 min I Multiole I
94. the source is displayed Enter the dilution factor If a source method or calibration file was specified on Page 3 of the Control Sample Wizard the default dilution factor is displayed Enter the calibration file name that is to be used to calculate control sample concentration If a source method or calibra tion file was specified on Page 3 of the Control Sample Wiz ard the default calibration curve name from the source is displayed 4 4 Sample Table Editor 4 4 5 Insert Menu Control Sample Wizard Page 5 Injection Parameters Control Sample Wizard Page 5 Injection Parameters x Analysis fe Units em gt eee Injection Volume 0 full 100 000 No of Injections 2 B H n 20 SD Max 01000 0 9999 CvMax 200 10100 No of Washes fo 4 Auto Ditton fT H peat Use area retrieved from T Multiple Injections the blank check Enter the injection parameters lt Back Next gt Cancel Figure 4 155 Control Sample Wizard Page 5 Injection Parameters Parameter Description Analysis Displays the analysis type This field cannot be changed Units Select the concentration units Injection Volume Enter the injection volume Expected Conc Range Enter the maximum expected concentration No of Injections Enter the minimum maximum number of injections for the control sample The setting range is from 1 20 SD Max Enter the maximum standard deviation that is acceptable for the in
95. the trap is emptied This step is repeated using another 6mL aliquot from the dilution water bottle Next the trap and the system is washed with ultra pure water The ultra pure water used to wash the trap is created when a 2mL aliquot of water from the dilution water bottle is injected through the TC injector and onto the catalyst The ultra pure water resulting from the analysis fills the trap and is then drawn into the syringe and discharged a total of 4 times 2 Preparation of purified water for blank check The ultra pure water that will be used for the Blank Check procedure is created as follows Six 2mL aliquots of water from the dilution water bottle are injected through the TC injector and onto the catalyst The ultra pure water resulting from the analysis is caught in the ultra pure water trap Water in the trap is further purified by injecting it onto the catalyst five more times in 2mL aliquots 3 Blank check analysis Using the ultra pure water created in Step 2 and caught in the purified water trap TC analysis is conducted 5 times The results of each analysis are stored in the data file Steps 2 and 3 are then repeated 9 more times Note The magnitude and stability of the system blank value can be evaluated from the blank check results If the blank value is not stable repeat the Blank Check procedure until the magnitude of the blank peak stabilizes 4 1 15 3 Pretreatment for IC Removal Sparging Errors for TC and IC analyses
96. the tubing near the gas connection inlet of the instrument when a compressor is used e Select the Oil less Carrier Gas Purification Kit when a compressor is used e There are cases where the organic gas concentration is too high to be removed completely by the gas purifier Analysis accuracy is poor in atmospheres containing high concentrations of volatile gases from exposed organic solvents and gasoline or high concentrations of automobile and diesel engine exhaust If the possibility of the presence of these kinds of gases cannot be avoided use a filter to remove organic particles and or gases Gas Supply Pressure Ensure that the gas supplied to the gas inlet of the instrument maintains a constant stable pressure of 300kPa When using compressed air or instrumentation air verify that the gas supply pressure is greater than 300kPa and less than 600kPa Note Do not allow the carrier gas supply pressure to exceed 600kPa Gas Tubing Connections The special accessory Air Supply Tubing Set includes nylon tubing and connectors two 2 half unions TOC VCPH CPN 6 8 Installation 6 8 3 Installation Procedure Procedure Connection Inlet x Nag Nylon Tubing Figure 6 6 Gas Tubing Connection Half Union Connect the half unions to the carrier gas inlet on the instrument and the connection outlet 4 NPT of the gas supply source Connect the nylon tubing 4mm OD 2 5mm ID between the gas supply source and the in
97. this section Analysis Related Technical Information This section summarizes technical information related to analysis including peak area analysis and calibration curve selection Specifications This section lists specifications for the TOC VCPH CPN main unit autosampler TN unit and the various optional kits Standard Accessories The standard accessories are listed in this section Special Accessories The optional accessories are listed in this section Consumable Parts List The consumable parts are listed in this section Maintenance Parts List The maintenance parts are listed in this section Installation The installation site requirements and installation procedures for future relocation of the instrument are described here Material Safety Data Sheets Material Safety Data Sheets are provided in this section 284 6 1 Principles of Analysis 6 1 1 Principles of TC Total Carbon Analysis 6 l Principles of Analysis Two types of carbon are present in water organic carbon and inorganic carbon Organic carbon TOC bonds with hydrogen or oxygen to form organic compounds Inorganic carbon IC or TIC is the structural basis for inorganic compounds such as gas carbonates and carbonate ions Collectively the two forms of carbon are referred to as total carbon TC and the relationship between them is expressed TOC TC IC Nitrogen is also present in water in two types organic and inorganic The sum of these is refer
98. those specified in the No of inj per sample field LLL TOC VerHiceN fy 37 Control Charts File Menu Control Chart Wizard History Window The Control Chart Wizard History function is identical to other history functions in the TOC Control V system Refer to Section 4 4 2 3 Method Wizard for more details about the History function The History window provides information on all control chart changes when enabled Control Chart Wizard Page 6 History x A Once the history function is enabled it cannot be cl Enable disable history functions lt Back Cancel Help Figure B 7 Control Chart Wizard History Window Setting Item Description Enable history log Select this option to enable the History Log which is used to monitor all modifications to the control charts Once the His tory Log is enabled it cannot be turned off Operator has to comment on Select this option to require the user to enter comments or all modifications obtain approval for modifications to the control charts B 1 2 Following Control Chart Select the Following Control Chart menu item to create a Following Control Chart It is recommended that a new control chart be created after 50 samples have been entered in the control period The new control chart uses the calculated standard deviation from the control period as the new control chart limits Control chart options are Setting Item Description File Na
99. water The pure water does not flow into the combustion tube It is driven out of the injection port by the carrier gas flowing through the needle guide pipe Wipe off the water coming out of the injection tube with soft tissue paper The internal injection port and inside of the needle guide pipe are now clean Measurement of service water or contamination free environmental water such as river water often reveals that IC is the major part of TC when the TOC content is around 1ppm For these types of samples it is preferable to remove the IC content before measuring TOC through the TC channel Errors for TC and IC analyses are additive For samples that have a comparatively high IC content relative to the TOC content the TOC analysis error will be large if it is determined by the difference between TC and IC results TOC VcPHICPN 225 226 4 5 Application Operations 4 5 1 Manual Injection Analysis 4 5 1 4 Maintenance Replacing the IC Injection Port Septum Cushion O Ring The septum used with the IC injection port is a consumable item The septum typically can be used for 200 or more injections however it should be replaced if there is deterioration in reproducibility or peak shapes Part number for replacement cushion O ring 20 pcs P N 630 01559 01 Replacement Procedure 7 Loosen and remove the injection port bushing 2 Remove the old septum and insert a new one 3 Replace the bushing and tighten it N caut
100. window Note On each tab in the Page Setup window certain items are checked selected by default To deselect these options click the item 374 E TOC VcPrcPn p Data Tab The Data tab displays a list of items that can be selected for printing Select the desired items and click the OK button Grid Tab Page Setup x E M TAAA ol M Figure B 10 Page Setup Window Grid Tab The Grid tab displays a list of format items for the report Option Description Row Headers Column Headers Print Frame Vertical Lines Horizontal Lines Only Black and White First Rows then Columns First Columns then Rows Vertical Horizontal Prints row headers in the table Prints column headers in the table Prints a frame around the table Prints vertical lines in the table Prints horizontal lines in the table Prints only in 2 colors without gray backgrounds or other colors Prints rows first followed by columns when more than one page is printed Prints columns first followed by rows when more than one page is printed Prints the table on the vertical center of the page Prints the table on the horizontal center of the page LLL TOC fy 375 Miscellaneous Tab Page Setup Figure B 11 Page Setup Window Miscellaneous Tab The Miscellaneous tab displays a list of format items for the report as described below Setting Item Description Margins Use the spin cont
101. 0 34 300 5 fe 01 20 34 300 53 m Percent Values Number of significant digits fi 1 01 20 3 300 Number of digits after the decimal point B 4 1 01 20 34 300 52 Figure B 18 Floating Point Format Window Common Floating Point Numbers Setting Item Description Number of significant digits Number of digits after the decimal point Percent Values Setting Item Select this option to display common floating point numbers using a specified number of significant digits Use the spin control to set the number of significant digits The default value is 4 Select this option to display common floating point numbers using a specified number of digits after the decimal point Use the spin control to set the number of digits after the deci mal point The default value is 2 Description Number of significant digits Number of digits after the decimal point 382 TOC VcPHI CPN Select this option to display percent values using a specified number of significant digits Use the spin control to set the number of significant digits The default value is 4 Select this option to display percent values using a specified number of digits after the decimal point Use the spin control to set the number of digits after the decimal point The default value is 2 Control Charts Options Menu B 4 4 ASCII Export Options The ASCII Export Options function is used to expor
102. 000 ppm 3 3 0 1000 2 00 2 10 00 ppm 3 3 0 1000 2 00 3 20 00 ppm 3 3 0 1000 2 00 4 Edit Add Delete Delete All Edit the single calibration points ome Figure 4 52 TN Calibration Points List Complete the TN calibration file by viewing but not changing pages 6 and 7 of the Wizard and clicking the Finish button The TN calibration curve file is now complete and has been saved Reference Refer to Section 4 4 2 2 Calibration Curve for a detailed description of the Calibration Curve Wizard Entering the Calibration Standard Runs in the Sample Table Now that the calibration files have been created and saved the calibration standard runs must be inserted into the Sample Table The TC and TN calibration standards are inserted separately 7 2 Insert the TC calibration standard runs by placing the cursor in the first line of the Sample Table From the Insert menu select Calibration Curve Specify the name of the TC Calibration Curve TCtutorial cal and click the Open button The Sparging Acid Addition window is displayed Notice that the TC calibration stan dards have been automatically added to the table TOC VcPHICPN 105 4 Enter the vial positions 1 3 for the calibration standards directly into the Vial column of the table As vial positions are entered in the table they are highlighted on the tray diagram in the Sparging Acid Addition window Sparging Acid Addition Figure 4 53 S
103. 126 Parameter Source Window csseceeseeeerees 195 Peak Time Parameters Window 00 198 System Information Window ceeee 193 Cooler Drain Container ccc eeteeeeecseeeeseeeeeeeeenees 48 Corrective Action Eliminate Syringe Bubbles Poor Reproducibility Poor Sample Injection eee eeeeeeeerereeeee Data Deleting iui anaana aa 158 Exporting to Database 148 Importing from ASCII 0 eee eeeeecreeeeeees 159 Recalculating cc cecececeseeseceeceeceecnsenseeeeee 158 Replacing o ornini needa iT 157 Database Exporting Data to ssseseseeseeseeeeereseereees 148 Default Measurement Parameters 00 87 212 Default Measurement Parameters Dialog Box 98 Deleting All Sample Table Data Configured System ccecescseesseseeseereeeeeeeeeeees Selected Sample Table Data 0 e eee 159 Description System cceceseesecsecseesecsecneeeeneens 7 18 Detector Chemiluminescence 0 cccessseecseseceeeeeeeeeees 259 Viewing Status oo eecceccesceseesecsececseceeneeeeneees 203 Edit Menu Sample Table Editor eee 156 Editing Calibration Point Parameters 0 0 0 0 eee 132 Control Charts 0 0 00 cceeseeeerees Method Validation File Sample Table a Electric Shock Warning ceseseesecseeneeneeeeneees ili Ending Measurement c ccceccesceseesecsecneeeeneeneens Error Messages ccecececes
104. 129 139 189 Multi Point Calibration Curvye seseseseeeeseerereeseee 290 Notation Conventions cceseceesseeecseseeeeeseeeseserees vi Notification Bar ceceseecseseceecneeecteceeeens 124 215 NO Absorber Connecting ac sietysitecaineawecgannae 59 Replac Mentiyescsi isieiesclechcleeteeicetest 260 Using a CO3 Absorber eee ceeeneeeeenes 59 NPOC Acid Addition oo ee ceeceecseeecteceeeeceeeeceeeneeeenees Analysis Principles Number of Injections Options Menu Sample Table Editor O tlier TeSt ssiri niian Oxidation Method Selecting seseseeeesseeeeeereseereeee Ozone Connecting SOUrCe sssssssesesseseseseseseses sesers ses 329 Generator Replacement 0 0 0 cececeeseeeeeeeeeee 260 Generator Low Air Supply Safety 0 0 331 Generator Source Air Pressure c 0 c008 330 Source Airflow Rate c ccecececesecsecseeteeneeeeeee 91 Treatment Unit cc ececeesecseeseerceeeeeeeeeeeeeeee 256 Parameter SOUrCC ccceececeeceneeeeceeeeeseceseeeneeneeeaes Parameter Table in Sample Window Index Parts Consumable ASV beni hie Gin Sieh B iin dba ans 306 Carrier Gas Purifier Kit eee 307 TM e a divuiesess eines 307 TOC V PHnrenninisnanininini voneeees 304 TOC VOPN o ccceccecssceececsecescesseseceseenseeeees 305 Maintenance ya te EAEE E E AE TE 308 Manual Injection Kit eee 309 TOC VOH ia Se 308 TOC VCPN asesiisisedsbactsicieshensnanesi
105. 3 Installation Procedure 6 8 3 1 Connecting Power Supply and Ground Connecting Power Supply Connect the instrument to a stable AC 100 127V 100V System or AC 220 240V 200V System 50Hz or 60Hz single phase power supply with sufficient capacity to accommodate 6A or greater current N caution The instrument may not operate properly if the power supply voltage exceeds the range of AC100 127V 10 or AC 220 240V 10 Unstable voltage may cause problems during high sensitivity analysis Note The instrument is compatible with both 50 Hz and 60 Hz power supplies and can be used with either frequency Grounding The included power cord is a three conductor cable including a ground wire and a 2P plug with ground at the end If the power outlet does not have ground receptacle use the included 2P no ground adapter Connect the external ground terminal to the ground The voltage terminals AC and ground terminal ACC on the power plug of this instrument are arranged as shown in Figure 6 5 Power Plug Connect them so that they match the power outlet being used Voltage terminal AC Ground terminal ACC Ground terminal G Be sure to ground completely Figure 6 5 Power Plug TOC VCPH CPN 6 8 Installation 6 8 3 Installation Procedure N caution e In addition to the consideration of safety complete grounding is necessary to prevent as much as possible the occurrence of signal noise A Type 3 ground
106. 4 Sparging During Standard Solution Analysis 6 2 4 Sparging During Standard Solution Analysis Standard solutions that have TC concentrations so low as to be affected by the amount of dissolved carbon dioxide in the solution should be sparged with carrier gas prior to measurement Sparging eliminates the dissolved carbon dioxide thereby preventing it from affecting the concentration of the standard solution The amount of dissolved carbon dioxide in water used for standard solution preparation is affected by factors such as water purification method length and condition of storage and the concentration of carbon dioxide in the atmosphere Concentrations of dissolved carbon dioxide increase when the water is exposed to the atmosphere during the standard solution preparation process Refer to Table 6 2 e CO Content ppm in Distilled Water Equilibrated with Atmosphere Temperature C for the dissolution rates of atmospheric carbon dioxide in water It is important to consider both the concentration of the standard solution and the concentration of TOC contained in the preparation water when deciding whether to use the sparging function Use of sparging is appropriate if the TOC contained in the water is low enough to not substantially affect the standard solution concentration but not low enough to be ignored Note Do not use sparging with IC standard solutions as sparging decreases the IC con centration Table 6 2 CO Content p
107. 58 Samples From Control Charts 377 383 Exporting Control Charts sic arara a eases 383 Data to ASCH File oo eeeeeeeeesereeecneeneees 146 Data to Database eee seeeeseneeeeceeeeeeeeeneeee 148 Method Validation Data ccc eseese 363 Flow Diagrams ccecceseseeseesecsecececeeeeeeeeeeees 11 13 Flow Line Replacing Content cececeseeseeseeseeteeneeneeee 263 Replacing Parts and Slider eeeeeeeeeeeee 54 Residue Removal sessies 263 Setting Washes in Software eee eeeeeeeee 86 Washitign ctoccaNia isa cine 264 Index 3 Index 4 Index Flow Rate Cartier Gas eene a aE O el da iene 90 OZONE SOU Rai hee Bl e a Oa 91 Sparse GaSe ereo a 53 Sparge Gas Wet Chemical seseeeeseeeeeeeee 269 General Information Window ccccccsscseeeeesees 125 General Measurement Parameters 6 83 88 Graph in Sample Window sssesseseeseeesessesesssesseseese 167 Halogen Scrubber MSDS is ited ies tee 337 Replacing ticissanicanviaudunetandcauceaves 243 High Purity Air Cylinder eee 242 313 High Sensitivity PASEI YSIS 43 EN tee head cht ston E 63 Catalyst wee 37 240 339 Combustion Tube 0 cece eee ceeeseseneneees 40 Using 8 Port Sampler oo eee eeeeeeeeeeeeeeeeee 82 High Temperature Warning ceeeseeeceeereeeeneeees vii EE EEE A S E E A 285 Analysis Preparation Injection Port Septum 7 Principl s tipanan a a pe deli Reaction Solution s s
108. 638 94241A M393 E189 PC Controlled Total Organic Carbon Analyzer TOC VCPH CPN amp TOC Control V Software User Manual Read this manual carefully and keep it with the instrument for future reference SHIMADZU CORPORATION ANALYTICAL amp MEASURING INSTRUMENTS DIVISION KYOTO JAPAN TOC VCPH CPN Copyright Shimadzu Corporation 2003 All rights reserved including those to reproduce this publication or parts thereof in any form without permission in writing from Shimadzu Corporation Read and understand this manual before operation Save this manual Information in this publication is subject to change without notice and does not represent a guarantee on the part of the vendor Any errors or omissions which may have occurred in this publication despite the utmost care taken in its produc tion will be corrected as soon as possible but not necessarily immediately upon detection We appreciate notifica tion of any errors or omissions Shimadzu does not have any responsibility for errors or injuries resulting from following the instructions in this manual Windows is a registered trademark of Microsoft Corporation TOC VCPHI CPN Introduction Thank you for purchasing the TOC VcPH TOC VCPN Total Organic Carbon Analyzer and the TOC Control V software This instruction manual is a TOC V user manual It provides operation and maintenance procedures for the TOC V The procedures related to TOC Control V software
109. 94 Block M INJ TC ASSY 1 638 10195 Block M INJ IC ASSY 1 631 43291 Syringe packing 10 Table 6 8 Standard Accessories List 6 POC Measurement Kit Part Number Part Name Qty 630 00557 Quartz wool TOC VCPH CPN 301 Table 6 9 Standard Accessories List 7 Carrier Gas Purifier Kit 638 42013 L shaped combustion tube in case 1 638 60116 TOC regular catalyst 1 630 00557 Quartz wool 1 638 52578 01 CO absorber container 1 630 00556 Soda lime 1 638 40168 Compression fitting elbow 4 016 37504 Teflon tube 3x4 2 9m 040 82074 03 Filter 1 035 65 104 Union 2 016 43284 01 Nylon tube 0 1m 302 W TOC V cPHICPN nnn 6 3 8 6 5 Special Accessories 6 5 Special Accessories PC Hardware Requirements Table 6 10 Special Accessories List Part Number Part Name CommentComment 638 93 141 04 Autosampler ASI V 24mL 24mL vials 638 93 141 08 Autosampler ASI V 40mL 40mL vials 638 93150 01 8 Port sampler OCT 1 For TOC VCPH CPN CSH CSN 638 93150 11 8 Port sampler OCT 2 unit second For TOC VCPH CPN CSH CSN 638 91065 01 TN unit TNM 1 For AC 100 127V 638 91065 02 TN unit TNM 1 For AC 220 240V 638 91066 POC measurement kit 638 72596 Option wiring kit Required to install the POC kit or external sparge kit for the TOC V CPH 638 41447 Carrier gas purifier kit 638 77152 Extern
110. 98 6 4 Standard Accessories 6 3 8 PC Hardware Requirements 6 4 Standard Accessories Table 6 3 e Standard Accessories List 1 TOC VCPH CPN Part Number Part Name TOC VcpH TOC VCPN 638 41323 Combustion tube in case 2 1 638 92069 02 TOC regular catalyst set 1 1 638 92070 01 TOC high sensitivity catalyst set 1 638 16023 Catalyst filling rod 1 1 630 00999 CO absorber 1 1 630 003 15 09 Plastic tube 9mm ID x 12mm OD 2m 2m 071 608 13 Adapter ground 1 1 071 608 14 01 Power cord set 100 127V 1 1 071 608 14 06 Power cord set 220 240V 1 1 638 59213 01 Plunger tip 1 1 630 00635 01 Potassium biphthalate 2g 1 1 630 00962 01 Sodium carbonate 25g 1 1 638 59213 Syringe 1 1 017 30812 01 Silicone grease 1 1 072 60359 01 Wiring band 2 2 630 00963 01 Sodium bicarbonate 25g 1 1 072 02004 25 Fuse 218 008 100 127V 2 2 072 02004 27 Fuse 218 015 220 240V 2 2 631 20265 Plug 35154 1 1 631 78002 Wrench for 8 port valve 1 1 638 52337 Rinse water bottle 1 1 638 20072 Cap 1 638 60074 Ceramic fibers 1 1 638 64727 CD ROM TOC Control V 1 1 638 74029 Cable RS 232C 1 1 631 81214 Plate for CO absorber 1 1 035 55026 02 Half union 1 1 038 00292 04 Plastic bottle 2 1 638 94241 Instruction manual TOC VCPH CPN 6 3 8 6 4 Standard Accessories PC Hardware Requirements Table 6 4 Standard Accessories List 2 ASI Unit
111. A Method Validation sccssscssssscssssssscsssssssssssssssssssssseees 347 Ask Main Wild O We eeaeee eea e a aae aeee a S ae i a te aE 348 A2 Hal MOB U asec face sit Sas tate e do data atadienaibenaeo St iealvon denen abbensieides tan beee 349 DM gt SING Wiesscin hints Ses hated c te teh lt Soot ted atin eer AE A AE 349 A22 t OP Cth nennen e EAER EAEE EEEE O dbase aca dea bvocuash canna set AE S 350 ALD Sie DAVES poen era ar a E R tenes 351 ADL SWEA iie sien oie EE A OER EEEE tee ne 351 ADD PUIG EAA EEEE Areata ea de Re EEE E eee 351 VIA S Print Preview eg foes Sei bac cs oes as ese Ao eg oo cee E dated 352 Al Print Setup ne a O E ose aera ee Re 353 AD 38 gt A EAI EE EAEE AE EAE 353 AXI EXGt e ka ri a e a e Pelee ee 355 A3 Edit Ment sonant ma ae i E E EN EE EA REN 356 yae P BE TE EAE EE E EE E A EE S AS 356 A32 Cut Copy Paste occ sities N 356 AS Ben ISL ROW aas ceca bokat oe tten A bomeametinn SES 356 AcBA Delete ROW nenien neriie iia cen dBc geval EE RE tence ie 357 A335 Insert Column r piel ceo e A et nb dees uee ee eben 357 A386 Delete TOILE aT a E EE tin ha teh hee ees 357 AS Recalculate t c a5 ccsuesei wi aise eatin BA host a Hi eA 357 AA r View Menus oaea E a A A cased A es 358 AS Options Men s initierea na aaa a Ea E aa E E EE RA 359 AS General Parameter aenn n e E A AAE 359 A 5 2 Method Validation Parameter e seeenseeseseesessesesessestsrsesseeseseesesrrsrereseene 360 AS gt FON re en a
112. ASI Rack Change Preparation Start Busy aod od od ool od Finish Re Figure 5 34 ASI Rack Change Window Click the Preparation Start button to begin the procedure A progress bar is active while the rack moves to the position where it can be replaced When the progress bar begins blinking replace the rack Click the Finish Replacement button to initialize the ASI and complete the rack change process Click the Close button TOC VcPHICPN 267 5 6 Software Controlled Maintenance Functions 5 6 10 ASI Needle Change 5 6 10 ASI Needle Change Use this function to change the ASI needle This option is disabled if an ASI is not connected to the system ASI Needle Change ASI Needle Change Preparation Start Busy Finish Replacement Figure 5 35 ASI Needle Change Window Click the Preparation Start button to begin the procedure A progress bar is active while the needle moves to the position where it can be replaced When the progress bar begins blinking replace the needle Click the Finish Replacement button to initialize the ASI and complete the needle change process Click the Close button 5 6 11 Change Syringe Use this function to replace the syringe Preparation Start a Verify Syringe Busi Ww Movement ata Err Stop Finish Replacement Figure 5 36 Syringe Change Window Click the Preparation Start button to begin the procedure A progress bar is active while the syringe moves to the position wh
113. ATA SHEET SECTION I PRODUCT IDENTIFICATION CAT NO 630 0557 00 CAS NO 14808 60 7 NAME Quartz Wool OTHER NAME N A SECTION II PRODUCT USE Support for catalyst in reaction tubes of TOC instruments consult instrument manuals for proper use SECTION III PHYSICAL DATA Melt Boil Density Vapor Vapor Evaporation Odor Color Phase Water Point Point Pressure Density Rate Solubility N A N A N A N A N A N A N A Grey Fibrous N A SECTION IV HAZARDS IDENTIFICATION Possible eye and skin irritation Avoid contact SECTION V TOXICITY DATA INERT SECTION VI HEALTH HAZARD DATA INERT SECTION VII FIRST AID MEASURES In case of contact immediately flush eyes with copious amounts of water for at least 15 minutes In case of skin contact immediately wash skin with soap and copious amounts of water SECTION VIII FIRE FIGHTING MEASURES N A SECTION Ix ACCIDENTAL RELEASE MEASURES N A SECTION X STABILITY AND REACTIVITY N A SECTION XI SPECIAL PRECAUTIONS AND COMMENTS The above information is believed to be correct but does not purport to be all inclusive It shall serve only as a guide Shimadzu shall not be held liable for any damage resulting from handling or contact with the above product Users should make their own determinations regarding the suitability of this information for their particular purposes TOC VCPH CPN 6 9 Material Safety Data Sheets 6 9 7 High Sensitivity Catalyst 6 9 7 High Sensitivity Catalyst Shimadzu Sc
114. ATION Not regulated SECTION XIII OTHER INFORMATION NFPA RATINGS Health 0 Flammability 0 Reactivity 0 LABEL HAZARD WARNING Not applicable LABEL PRECAUTIONS Keep in tightly closed container LABEL FIRST AID Not applicable PRODUCT USE Laboratory Reagent SECTION XIV SPECIAL PRECAUTIONS AND COMMENTS The above information is believed to be correct but does not purport to be all inclusive It shall serve only as a guide Shimadzu shall not be held liable for any damage resulting from handling or contact with the above product Users should make their own determinations regarding the suitability of this information for their particular purposes TOC VCPH CPN 345 346 E TOC VcPrcPn i _ iii Appendix A Method Validation The Method Validation function tests the variance and the linearity of the data The function also determines performance characteristics according to the requirements of DIN 38402 Part 51 The Method Validation function displays the data used for executing method validation performs the required calculations and displays the results Data can either be imported directly from the TOC Control V Sample Table or entered manually into the data table Data can also be exported to ASCII files stored and printed A 1 Main Window The Main Window is separated into three sections The upper left section of the window displays the calibration curve the upper right section displays the calculated validation results an
115. Acute effects Harmful if swallowed inhaled or absorbed through skin Material is extremely destructive to tissue of the mucous membranes and upper respiratory tract eyes and skin Inhalation may be fatal as a result of spasm inflammation and edema of the larynx and bronchi chemical pneumonitis and pulmonary edema Symptoms of exposure may include burning sensation coughing wheezing laryngitis shortness of breath headache nausea and vomiting To the best of our knowledge the chemical physical and toxicological properties have not been thoroughly investigated SECTION VIII FIRST AID An antidote is a substance intended to counteract the effect of a poison It should be administered only by a physician or trained emergency personnel Medical advice can be obtained from a POISON CONTROL CENTER In case of contact Immediately flush eyes or skin with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes Assure adequate flushing of the eyes by separating eyelids with fingers If inhaled remove to fresh air If not breathing give artificial respiration If breathing is difficult give oxygen If swallowed wash out mouth with water provided person is conscious CALL A PHYSICIAN Wash contaminated clothing before reuse Discard contaminated shoes For complete information see actual entry in RTECS VX965000 SECTION IX SPILL OR LEAK PROCEDURES Occupational spill Evacuate area Wear self contained b
116. Auto regeneration of IC solution check box will be enabled on the Instrument Setup Wizard TOC screen Specifies that the TN accessory is installed Ifthe TN Unit is selected as an option the TN Power check box will be enabled on the Instrument Setup Wizard TOC screen Specifies that the Sparge Kit accessory is installed and that external sparging is desired If the Sparge Kit is selected as an option the Nee dle parameter will be enabled on the Instrument Setup Wizard ASI screen Specifies that the Manual Injection Kit accessory is installed The ASI SSM and POC accessories cannot be used simultaneously with the Man ual Injection Kit If the Manual Injection Kit is selected as an option the options for ASI SSM and POC are deselected and disabled Select this option when one 8 port sampler accessory is installed 8 Port Sampler 1 cannot be selected if the ASI or SSM are selected Select this option when two 8 port sampler accessories are installed 8 Port Sampler 2 can only be selected if 8 Port Sampler 1 is selected TOC VcPHICPN 25 3 2 Instrument Setup and System Properties 3 2 3 TOC Window 3 2 3 TOC Window The TOC window of the Instrument Setup Wizard is used to set TOC instrument parameters Catalyst Type Tubing Diameter Regular z Cell Length Long z TC Fumace Deg C Je Autovegeneration of I solution Off IV Enable ready status check 680 I TN Power C 720 Specify the TOC para
117. C fm 257 258 5 5 TN Unit TNM 1 Maintenance 5 5 1 Replacing the Catalyst in the Ozone Treatment Unit 4 N TOC VCPH CPN Remove the cap from the ozone treatment unit and take out the used catalyst and polypropylene packing material Figure 5 21 Emptying and Removing the Ozone Treatment Catalyst O Pack a small amount of new polypropylene packing material into the bottom of the ozone treatment unit then fill with approximately 60 grams of catalyst Insert a small amount of new polypropylene packing material on top of the catalyst Place the cap back on the container Remove the Viton coupling connecting the detector exhaust opening to the inlet of the ozone treatment unit Replace this Viton coupling with a new one whenever the catalyst is replaced Inspect the Viton tubing at the outlet of the ozone treatment unit and replace it if cracked or damaged Reconnect the Viton tubing and Viton coupling and reinstall the ozone treatment unit L caution Used catalyst should be disposed of according to local industrial waste disposal regulations It must be clearly disclosed using an industrial waste manifest that the catalyst contains manganese dioxide 5 5 TN Unit TNM 1 Maintenance 5 5 2 Chemiluminescence Detector 5 5 2 Chemiluminescence Detector The light receiving window of the chemiluminescence detector may become soiled by components in the samples Inspect and clean the window and gasket at least once a y
118. C for the first time Only users with administrative privileges can configure the instrument If the system has already been configured proceed to Step 2 of the tutorial 3 From the TOC Control V main window double click the New System icon The User dialog box is displayed 4 Enter your user name and password as shown below x User ID Password a Paes eoe cece E U derit have a user account yet contact the TOC Contol System Administrator Figure 4 33 Enter User Name and Password LLL TOC fy 93 Click the OK button The Instrument Setup Wizard opens Instrument Setup Wizard System Information TC TN System o Figure 4 34 Enter the Name of the System 5 Inthe System Information window of the Instrument Setup Wizard enter the System Name and Instrument Serial Number Click the Next button The Options window of the Instrument Setup Wizard is displayed Reference For details on the System Name and Instrument Serial Number refer to Section 3 2 1 System Information Window Instrument Setup Wizard Options 18Port Sampler 1 z Figure 4 35 Configured Options 6 Specify the options that are configured on the system by clicking in the appropriate check boxes as shown in the above figure Click the Next button The TOC window of the Instrument Setup Wizard is displayed 94 TOC NM CPN Lea amp Select the TOC analysis parameters as shown in the figure below Note Be sure that th
119. C value can also be greatly influenced if standard solutions are not prepared and measured carefully Errors are compounded since two calibration curves must be generated for TC and IC The calibration curves are used in sample analysis by extending a two point calibra tion curve through the origin e In NPOC analysis POC may be volatilized from the sample during sparging for IC removal This is not a problem since the ultra pure water contains practically no POC Cautions in Calibration Curve Generation and Sample Measurement Using High Sensitivity Analysis The case below describes the generation of a 2 point calibration curve shifted through the origin The calibration standard concentrations are Oug L and 400yg L Preparation of Standard Solutions A 2 point calibration curve using Oug L and 400ug L is generated The calibration curve is shifted through the origin to correct for the TC contained in purified water used for preparation of the standard solutions The Oug L and 400ug L TC standard solutions should be prepared at the same time using the same purified water Wash well two 250mL volumetric flasks with purified water preferably water containing low TC concentration Carefully introduce 1mL of 100mg L TC standard stock solution for a 400ug L solution into one of the volumetric flasks Distilled water is introduced up to the graduation line in both volumetric flasks Standard preparation procedures should be performed as
120. CPH CPN Construction 2 1 1 Front View Start Button Front Door P itch Stop Button ower Switc Figure 2 1 Front View 2 1 2 Right Side View Tubing and Wiring Opening for the TN Unit Drain Tubing Figure 2 2 Right Side View 8 E TOC V cP H C PN nnn 2 1 TOC VcPH cPN Construction 2 1 3 Left Side View 2 1 3 Left Side View Sample Tubing Hydrochloric Acid Dilution Water Bottle IC Reagent 2 1 4 Rear View Carrier Gas Inlet CO Absorber AC Cord Socket Figure 2 4 Rear View 1 Flash ROM rewrite switch 2 Printer cable terminal 3 RS 232C terminal 1 4 RS 232C terminal 2 5 ASI V OCT 1 signal cable connector 6 ASI V OCT 1 power cable connector TOC VCPH CPN 9 10 2 1 TOC VcPH CPN Construction 2 1 5 Inside Front View 2 1 5 Inside Front View 1 2 3 4 5 6 O O O 16 O BAN Co ol qo 7 ovo OCE a 4 6 2o O 8 15 o F Q O 9 14 S P o P a 10 13 E Q Front Door 12 11 Figure 2 5 Inside Front View 1 Sliding sample injector H Type only 2 IC reagent vessel H Type only 3 Solenoid valve for IC drainage H Type only 4 Carrier gas pres
121. Catalyst oreren e e R E ten ieee Aegis 239 52 22 Replacing Catalyst essenin pee dali ein aed 240 5 2 2 3 Replacing the Carrier Gas Purification Tube and Catalyst 240 5 2 3 Washing Replacing the Combustion and Carrier Gas Purification Tubes 242 5 2 4 Replacing the High Purity Air Cylinder eeeesceceeceseeeseereeneeteeneees 242 5 2 5 Replacing the CO ADSOrDbET eee eeeecceecneeseeeeenececeeeesecseeeseeceecneeaeesneaes 242 5 2 6 Replacing the Halogen Scrubber cceeeccescesceescesceeeeeeeeeeeeseeeeeseeseeneees 243 5 2 7 Replacing the Syringe Plunger Tip ccccceceseecesceeecesceeeeceeeeenseeneensees 244 5 2 8 Replacing Ferrules at the Combustion Tube Outlet Connection 245 5 2 9 Replacing the Sliding Sample Injector O rings occ eeeeeseeteeeeereneeneees 245 5 2 10 Replacing the Syringe Pump 8 port Valve Rotor 00 0 cceesseseeseeeeeteeeeeees 246 5 2 11 Replacing the CO Absorber for the Optional Carrier Gas Purifier 248 5 2 12 Replenishing IC Reaction Solution cccceecceseeeceeeeseeeceeeeeeeeneeeseeeeeneees 249 5 2 13 Replacing the Pump Head of the IC Reaction Solution Pump 250 5 2 14 Replacing the Filler of the Optional POC Analysis CO Absorber 251 5 3 Autosampler ASI V Maintenance ececescceececeeseeeeeeeeeceaeeaeeaeeaeees 252 5 3 1 Rinse Bottle Inspection ceececceseeseesceeseceeceeeeecesceseceeeeeeeeeeeaeesaeeneeaees 252 5 3 2 Sample
122. Catcher Inspectii incean a E E 252 5 3 3 Replacing the Pump Head of the Rinse Pump ccececeeesseteeereeeeeeeeees 253 5 4 8 Port Sampler OCT 1 Maintenance 0 ee eeeeceseeceeceeeeeeeceeceaeeaeeaeees 254 TOC VcCPHICPN xvii xviii TOC VCPH CPN Table Of Contents 5 5 TN Unit TNM 1 Maintenance eccecccesseeseesseceecseeeeseeesseeseesseeseeennes 256 5 5 1 Replacing the Catalyst in the Ozone Treatment Unit eeeeeeseeeee 256 5 5 2 Chemiluminescence Detector cceccccccsessseceeceseeseceseeeeeeceeeeneeeseeeeeaeenaes 259 5 5 3 Ozone Generator Replacement ccecceesceceseeescesceeeceseeseeeseenseeneenseenees 260 5 5 4 Replacing the NO Absorber ec eceseesseecrsesesseseseesesseaeeeeaeeneaeeneas 260 5 6 Software Controlled Maintenance Functions ccccecseeteeeteeeeeeeeeeees 261 5 61 Zero Point Detection searen e ra Ate este tee hitaee Roe E 261 5 6 2 Regeneration of the TC Catalyst 0 c cc ccccccssesseesecesceeceeceeeeereeseeaeessecneeeaes 262 5 6 3 Regeneration of the IC Solution cece ccceseeseceeceseceeeeeceseeeeceseeseeeneenaes 262 5 6 4 R sid e Removal eien n conast nab n bet eeui hanna Aes 263 5 6 5 Replace Flowline Content ss sssesesessseeessesesseereseesesetsrsesreressesesseseesersee 263 5 6 6 Flowline Washing ic aseciadsiaien a E lain E EE ae 264 S67 Mechanical C OOE a a raae a aerea aa aae aE A a anaona AoE Ea ia osa tas iaoa 265 5 6 8 ASI 8 Port Sampler Initialization
123. Comparison between control charts window Comparison between control charts a oo an Tas Mean Value Control Period Mean Value Preparation Period Variance Control Period a ae A Mean Value Control Period E Mean Value Preparation Period Variance Control Period Figure B 15 Comparison Between Control Charts Window Setting Item Description Previous control chart Displays the file name of the previous control chart if appli cable Mean value t test Displays the results of the T test in the text box beneath the Item and Value lists The T table value and the calculated test value are also displayed in the Item and Value list The test value is calculated based on the mean values and variances obtained from the control and preparation period The T test result shows whether the long term deviation of the control samples is significant F test Displays the results of the F test in the text box beneath the Item and Value list The F table value and the calculated test value are also displayed in the Item and Value list B 3 3 Out of Control Events The Out of Control Events window displays a list of all out of control events Out Of Control Events Figure B 16 Out of Control Events Window Spl No Displays the sample number for which the out of control event occurred Event Describes the out of control event B 3 4 Toolbar Status Bar The View gt Toolbar and View gt Stat
124. Connecting Combustion Tube to the Compression Fitting N caution The instrument is sealed sufficiently if the combustion tube does not move when pulled upwards The quartz glass combustion tube will break if the compression fitting is over tightened Use only the provided Teflon ferrules for the front and rear ferrules Do not use any other material such as metal Do not allow organic contaminants such as grease or oil to touch the inner or outer surfaces on the tip of the combustion tube and gas connection parts of the ferrules This is especially important for high sensitivity analysis TOC VcPHICPN 4 4 1 Analysis Preparation 4 1 2 Connecting the Combustion Tube Combustion LH Tube i a x z t S a Ley Ct a ae y i gt ial Figure 4 5 Connecting the Combustion Tube 5 Secure the sample injector with the knurled thumbscrew Knurled Thumbscrew Figure 4 6 Securing the Sample Injector 6 To prevent heat escape from the furnace pack the space around the capillary part of the combustion tube with the provided ceramic fiber N caution Use caution to avoid inhaling ceramic fibers when inserting the fibers into the combustion tube 42 TOC VCPH CPN 4 1 Analysis Preparation 4 1 2 Connecting the Combustion Tube Verify that the gap between the adjustable base at the bottom of the instrument and the bottom most part of the compression fitting is 1mm or less preferably no
125. D DATA Exposure to large amounts can cause gastrointestinal disturbances nausea vomiting headaches or dizziness SECTION VII FIRST AID MEASURES In case of contact immediately flush eyes with copious amounts of water for at least 15 minutes in case of skin contact immediately wash skin with soap and copious amounts of water if ingested and subject is conscious immediately give large amounts of water get medical attention SECTION VIII FIRE FIGHTING MEASURES EXTINGUISHING MEDIA Appropriate to surrounding fire Possible formation of toxic copper fumes Use appropriate respiratory support SECTION Ix ACCIDENTAL RELEASE MEASURES N A SECTION X STABILITY AND REACTIVITY INCOMPATIBILITIES Strong acids active halogens such as chlorine fluorine iodine and bromine ammonia SECTION XI SPECIAL PRECAUTIONS AND COMMENTS The above information is believed to be correct but does not purport to be all inclusive It shall serve only as a guide Shimadzu shall not be held liable for any damage resulting from handling or contact with the above product Users should make their own determinations regarding the suitability of this information for their particular purposes TOC VCPH CPN 337 338 6 9 Material Safety Data Sheets 6 9 6 Quartz Wool 6 9 6 Quartz Wool Shimadzu Scientific Instruments Inc 7102 Riverwood Drive Columbia MD 21046 Control No Tel 1 800 477 1227 Date MATERIAL SAFETY D
126. DECOMPOSITION PRODUCTS Carbon monoxide carbon dioxide SECTION XI SPECIAL PRECAUTIONS AND COMMENTS The above information is believed to be correct but does not purport to be all inclusive It shall serve only as a guide Shimadzu shall not be held liable for any damage resulting from handling or contact with the above product Users should make their own determinations regarding the suitability of this information for their particular purposes TOC VCPH CPN 343 344 6 9 Material Safety Data Sheets 6 9 12 Potassium Hydrogen Phthalate 6 9 12 Potassium Hydrogen Phthalate Shimadzu Scientific Instruments Inc 7102 Riverwood Drive Columbia MD 21046 Control No Tel 1 800 477 1227 Date MATERIAL SAFETY DATA SHEET SECTION I PRODUCT IDENTIFICATION CAT NO 630 00635 01 CAS NO 877 24 7 NAME Potassium Hydrogen Phthalate OTHER NAME Phthalic Acid Monopotassium Salt Khp Primary Standard SECTION II PRODUCT USE Specifically for use as an organic carbon standard in the Shimadzu TOC 500 TOC 5 000 and TOC 4 000 instruments Consult the appropriate instrument manual for proper use SECTION III PHYSICAL DATA Melt Boil Density Vapor Vapor Evaporation Odor Color Phase Water Point Point Pressure Density Rate Solubility 295 300 C N A N A N A N A N A N A White Crystals N A SECTION IV HAZARDS IDENTIFICATION Irritant irritating to eyes respiratory system and skin Possible sensitizer In case of c
127. DUDOOODOUDOUUOODOO i Oho Oo OO m Due to the danger of electric shock do not remove this cover In the event that the cover must be removed first disconnect the TNM 1 power cord CAUTION HAZARDOUS VOLTAGE To avoid electric shock turn off the power supply before opening this cover TOC VCPH CPN Warning Labels Used on this Instrument Injury Warning The sample injection components of this instrument move during operation To prevent injury keep hands away from this mechanism A CAUTION MOVING PARTS DO NOT open except to replace syringe During operation the pressure in the CO absorber of the gas purifier is about 200kPa To prevent injuries turn off the carrier gas and switch off power to the TOC main unit Wait until the pressure inside the container and the instrument flow lines return to normal atmospheric pressure before performing any maintenance CAUTION RISK OF INJURY 200kPa 29PSl of pressure is applied to this container Ensure that the pressure is released before opening TOC VCPH CPN ix X Warning Labels Used on this In
128. HE Toc_200 HW a 128 TEST TEST2 E wet Figure 3 1 Screen Lock Command Re enter Password The screen has been locked Enter the User ID and Password again User ID Password Figure 3 2 Re enter Password Dialog Box TOC VCPH CPN 3 1 2 Change Password This function is used to change the password of a registered user Select Change Password in the TOC Control V Administrator window to open the Change Password dialog box This function can be used only if the User ID Password item is checked in the Security dialog box Refer to Section 3 2 4 Security in the Administrator s Manual for more information TOC Control Administrator Figure 3 4 Change Password Dialog Box LLL TOC my 2 22 3 1 Introduction to System Administration Functions 3 1 3 Add Event Log 3 1 3 Add Event Log This function is used when a comment is to be included with the operation history This function is useful for documenting items in the operation history such as the replacement of catalyst that cannot be recorded automatically through the software Only users with access rights to Add Event Log can use this function This function can be used only if Audit Trail is checked in the Security dialog box Refer to Section 3 2 4 Security in the Administrator s Manual for more information When Add Event Log is selected in the TOC Control V Administrator window the Add Event Log dialo
129. IC Analysis Preparations L caution The IC reaction solution is acidic Use care not to spill or touch the fluid when handling it For details refer to Section 6 9 Material Safety Data Sheets TOC VCPHICPN 249 5 2 Periodic Inspections 5 2 13 Replacing the Pump Head of the IC Reaction Solution Pump 5 2 13 Replacing the Pump Head of the IC Reaction Solution Pump The IC reaction solution pump is a roller type pump that uses a rotating roller to flatten the rubber tube carrying the IC reaction solution thereby feeding solution into the system This rubber tubing gradually deteriorates requiring periodic replacement of the pump head The life of the rubber tubing is generally about 300 hours of pump operation It is recommended that 300 hours be entered as the warning value in the Maintenance History dialog box Refer to Section 4 2 4 Maintenance History Settings CAUTION The pump head and rubber tubing inside the IC reagent pump are filled with IC reagent solution This solution is acidic Use care to avoid touching or spilling the solution when changing the pump heads For details refer to Section 6 9 Material Safety Data Sheets Replacement Procedure Use the following procedure to replace the rubber tubing of the pump head 1 Z 250 TOC VCPH CPN Grasp the front and rear stops of the pump head by hand Pull the white pump head from the black pump body Disconnect both of the yellow rubber tubes on the left side
130. Item Description Number of significant digits Number of digits after the decimal point Percent Values Setting Item Select this option to display common floating point numbers using a specified number of significant digits Use the spin control to set the number of significant digits The default value is 4 Select this option to display common floating point numbers using a specified number of digits after the decimal point Use the spin control to set the number of digits after the deci mal point The default value is 2 Description Number of significant digits Number of digits after the decimal point 362 TOC VcPHI CPN Select this option to display percent values using a specified number of significant digits Use the spin control to set the number of significant digits The default value is 4 Select this option to display percent values using a specified number of digits after the decimal point Use the spin control to set the number of digits after the decimal point The default value is 2 A 5 5 ASCII Export Options Use the ASCII Export Options function to export method validation data to an ASCII file ASCII Export Options Tabulator a Figure A 21 ASCII Export Options Dialog Box Setting Item Description Header Select this option to export method validation file header Data Select this option to export method validation data Results Select this option to export method va
131. Measurement Parameters 4 2 1 TOC Parameter Settings 4 2 Setting General Measurement Parameters 4 2 1 TOC Parameter Settings The following parameters must be set for analysis using the PC controlled TOC V analyzer The items available for editing change depending on the options that are installed Tubing Diameter Buzzer Auto regeneration of IC solution Ready status check TN Power Source Setting Procedure 1 3 In the TOC Control V main window double click the icon for the desired instrument The Instrument Properties dialog box is displayed Instrument Properties E x System Options TOC asi SSM Communication History Main Unit Ver o Catalyst Type C TN z Tubing Diameter Regular v F UY Lamp Cell Length Lona z F Reactor Temp Gn T Buzzer F TC Furnace Deg C I Auto regeneration of IC solution C Off IV Enable ready status check C 680 720 I TN Power Cancel Figure 4 26 Instrument Properties Dialog Box TOC Tab Click the TOC tab The Main Unit Version field displays the instrument version number this field cannot be changed by the user Enter the parameters as described below Tubing Diameter Specifies the diameter size of the sample injection tubing Select the tubing diameter from the drop down list Available options are e Regular 0 5mm diameter e Suspended Particle 0 8mm diameter The typical tubing diameter is 0 5mm Select a tubing diameter of 0 8mm if the
132. Move Tray Use the directional arrows to move the ASI tray to the desired position Click the Reset button to return the tray to its home position Arm Use the directional arrows to move the arm vertically Use the drop down list to move the arm horizontally Vial Position Use the spin controls to enter a vial position then click the Move button to verify that the arm moves to the specified vial position This is the only option that is enabled for systems using the OCT 1 8 port sampler Magnetic Stirrer Use the On and Off buttons to start and stop the magnetic stirrer 266 EE TOC VcrHicPN m 5 6 Software Controlled Maintenance Functions 5 6 8 ASI 8 Port Sampler Initialization 5 6 8 ASI 8 Port Sampler Initialization Use this function when first connecting the instrument to establish communication between the TOC Control V software and the ASI or 8 Port Sampler This option is disabled if an ASI or 8 Port Sampler is not connected to the system Initialize ASI 8Port Sampler Initialize ASI 8Port Sampler aod od Er se ee ed ed dod Figure 5 33 Initialize ASI 8 Port Sampler Window Click the Start button to begin the procedure during which a progress bar is active The progress bar becomes inactive after the ASI or 8 Port Sampler is initialized Click the Close button 5 6 9 ASI Rack Change Use this function to change the ASI rack This option is disabled if an ASI is not connected to the system ASI Rack Change
133. No of Injections field The CV Max field is disabled if the No of Injections is 1 or if the maximum and minimum values are the same No of Washes Enter the number of times the syringe is to be washed with sample prior to the first injection Note that if the Auto Dilu tion option was selected the sample will be diluted and the syringe will then be washed with the diluted sample 138 E TOC VcPmcPn iinet Setting Item 4 4 Sample Table Editor 4 4 2 File Menu Description Auto Dilution Sparge Time Acid Addition Multiple Injections Use blank check area Auto correction of inj vol and dilution Enter a dilution factor for the samples The instrument will automatically dilute the samples by this factor and the result will be multiplied by the factor to obtain the final concentra tion The default Auto Dilution value is 1 Enter the desired sparge time This option is available only for POC NPOC and related analyses The default Sparge Time value is 1 Enter the desired quantity of acid to be added This option is available only for NPOC or related analyses Select to enable the syringe to draw up a single sample ali quot with a volume equal to that required for all injections of the sample When this option is not selected the syringe will draw up a separate sample aliquot for each injection Select ing this option reduces analysis time Select to include blank check result in the concentration cal
134. OH NAOH soda lime Shimadzu Scientific Instruments Inc 957003 7102 Riverwood Drive Columbia MD 21046 Control No Tel 1 800 477 1227 November 1995 MATERIAL SAFETY DATA SHEET SECTION I PRODUCT IDENTIFICATION CAT NO 630 00556 00 CAS NO 80006 28 8 NAME Soda Lime OTHER NAME Soda Lime Soda and Lime PRODUCT USE CO Scrubber in Shimadzu TOC Analyzers SECTION II PRECAUTIONS TO BE TAKEN IN HANDLING Protect skin eyes and clothing Avoid prolonged or repeated exposure Wash thoroughly after handling Safety shower and eye bath Use 8 minimum face shield Store as a corrosive Keep tightly closed and store in a cool dry place Air and moisture sensitive Use as directed in the TOC 4000 Instruction Manual SECTION III PHYSICAL DATA Melt Boil Density Vapor Pressure Vapor Density Evaporation Odor Color Phase Water Point Point Rate Solubility N A N A N A N A N A N A N A White Granules various sizes N A SECTION IV REACTIVITY DATA Incompatible with strong acids Absorbs CO2 moisture inactivates SECTION V FIRE AND EXPLOSION HAZARD DATA EXTINGUISHING MEDIA Dry chemical fire extinguisher Wear self contained breathing apparatus and protective clothing to prevent skin and eye UNUSUAL FIRE HAZARD Ernits tonic fumes in a fire SECTION VI TOXICITY DATA RAT MOUSE LD50 RTECS OSHA PEL ACGIH TLV TWA N A VX965000 N A N A SECTION VII HEALTH HAZARD DATA
135. ON II PRDUCT USE This product is specifically for use in the IC channel of the TOC 500 TOC 5000 and TOC 4000 series of TOC analyzers Refer to the appropriate instruction man ual for directions on proper use Keep tightly sealed in a cool dry well ventilated place Store separate form flammable and combustible materials Wear appropri ate protective clothing and eye protection SECTION III PHYSICAL DATA Melt Boil Density Vapor Vapor Evaporation Odor Color Phase Water Point Point Pressure Density Rate Solubility N A N A 2 16 N A N A N A N A White Solid Powder or Completely Crystals Soluble SECTION IV HAZARDS IDENTIFICATION Corrosive causes burns harmful if swallowed Target organ s liver blood In case of contact with eyes rinse immediately with plenty of water and seek medical advice Take off all contaminated clothing Wear suitable protective clothing gloves and eye face protection SECTION V TOXICITY DATA ORL RAT LD50 4090mg KGIHL RAT LC50 2300mg M3 2H ORL MUS LD50 6600mg KG IHL MUS LC50 1200mg M3 2H SCU MUS LD50 2210mg KG IHL GPG LC50 800mg M3 2H SECTION VI HEALTH HAZARD DATA Harmful if swallowed inhaled or absorbed through skin causes severe irritation High concentrations are extremely destructive to tissues of the mucous mem branes and upper respiratory tract eyes and skin Symptoms of exposure may include burning sensation coughing wheezing laryngitis shortness of bre
136. Palatino Linotype xl r Sample AaBbYyZz Script Westem X Figure 4 175 Font Dialog Box TOC VCPH CPN 213 4 4 9 4 Display Settings gt Table Settings The Display Settings gt Table Settings function is used to select the parameters that will be displayed in the Sample Table window The Table Options window contains two tabs one that lists Sample Table parameters and one that lists Injection Table parameters Note that on each tab certain options are selected by default Individual options can be selected or deselected by clicking in the check box Use the All and None buttons to quickly select and deselect all options on a tab Use the Default button to select the default options Sample Table Tab Select the parameters that will be displayed in the Sample Table x Sample Table Samples Sample Table Columns v v v q Figure 4 176 Table Options Window Sample Table Tab Samples Tab Select the parameters that will be displayed in the Injection Table Sample Table Spl Std No Sample Name Mlini No VS ample ID Std Conc M rea sis VMean Area VResult MConce Unit Mean Conc Dilution MResult Control Checking MVRemarks File name Status MVConc avial f 1 I ANa nf eal nnints 1 a Figure 4 177 Table Options Window Samples Tab 214 TOC VM PCN Lee 4 4 Sample Table Editor 4 4 9 Options Menu 4 4 9 5 Display Setting
137. Procedure 1 2 TOC VCPH CPN Open the Sample Table and place the cursor in the row where the control sample will be inserted From the Insert menu select Control The Open dialog box displays the available control sample template files Select the appropriate control sample template and click the Open button The Open dialog box closes and the Sparging Acid Addition window is displayed Enter the ASI vial position for the control sample into the appropriate cell in the Sparging Acid Addition window Click the OK button The Sparging Acid Addition window closes Scroll through the Sample Table to verify that the control sample has been inserted at the correct location 4 4 Sample Table Editor 4 4 6 Instrument Menu 4 4 6 Instrument Menu The Instrument menu contains commands for connecting starting and stopping the instrument and for instrument maintenance functions Background Monitor Is Connect EB Standby Start Continue Stop V Maintenance Properties Figure 4 160 Instrument Menu 4 4 6 1 Background Monitor The Background Monitor command is used to open the Background Monitor window which displays the status of the autosampler and all installed instrument detectors The real time signal and ready status for various detectors can be viewed by toggling between the individual instrument tabs The command is available only when an instrument is connected to the software Inst
138. RE EE E E eae ee 361 A 5 4 Floating Point Numbering Format essesesseeessesesseesesersrsresreressesesseseesesss 362 ASS ASCIT Export Options seisein reiii iei i E E e 363 A 5 6 Validation Strictly Following DIN38402 sssseesessseerssesieersrerrerrrsreessese 364 A6 Help Menu esana a a a a eee e a n 365 Appendix B Control Charts sessessoesoossessoesoossoesoesooesoesoesoossossoessossosssesssee 307 Bell File Mehu Seeron a a iaa TA E ia Ri iE 368 BLE NEW irani RAE RRE EE ERRE sie aan 368 Bil2 Following Control Chart cccscicccccccies annene en ees es 372 BT Opens E e a ashen Mote hater aa aes EEA E EEE 373 jm E ES n AE EE E E E E E E EE E 373 BLS Save A S E E E E 373 B 16 Print Data arne cccciiecc ccecs veces cc cececseves oleeeceeecadeban deuce ATRE ER EE 373 BIT iPrint gt Graphiesitecs cette ie Sh he E E A aS 373 B 1 8 Print Preview gt Data Print Preview gt Graph cccccceceeceseesseeeeeeeeeneeseeenes 373 Bil 9 Print SetuP n Roeeceses Bk ens Hen eho a 374 B110 Page Setup Nitong ie a E EEOAE EE EAEE 374 BIIT Exit eedonia aE K E E E ERA E E EE 376 Bide Edi tMeni sgannan a a a Ta 377 XX TOC VCPH CPN B3 View Menu secate en e Gain ca edt rt debs Rieat aces 378 B315 StatistiGsisceecseskes Sa Ges see Re dk E a eee 378 B32 Compari soHi a onic wwiGiies eitade ieee mete a ae 379 B 3 3 Out of Control Event sessirnir 380 B 3 4 Toolbar Status Bar s is itaient evee ror oui n iaa 380 B4 Options M OAU A
139. TOC VerHiceN fm 7137 Method Wizard Page 4 Injection Parameters The Injection Parameters window is used to specify the injection parameters for the method Method Wizard Page 4 Injection Parameters Parameters Cal Curve Gen Info J okt Ty TA i Figure 4 87 Method Wizard Page 4 Injection Parameters Setting Item Description Analysis Displays the previously selected analysis type Units Select the concentration units to be used for samples Injection Volume Enter the injection volume Expected Conc Range Enter the expected sample concentration if it is known No of Injections Enter the minimum maximum number of injections for the samples that will be analyzed using this method SD Max Enter the maximum standard deviation that is acceptable for the injections If this value is met no additional injections are required However if both this value and the CV Max value are exceeded the samples are automatically reinjected up to the maximum number of times specified in the No of Injec tions field The SD Max field is disabled if the No of Injec tions is 1 or if the minimum is equal to the maximum CV Max Enter the maximum coefficient of variation that is acceptable for the injections If this value is met no additional injections are required However if both this value and the SD Max value are exceeded the samples are automatically reinjected up to the maximum number of times specified in the
140. Wait for the furnace temperature to rise before executing the catalyst regeneration procedure ERROR Vial rack not present Operation cannot continue because there is no vial rack in the turntable Mount a vial rack and then execute the operation again ERROR Vial rack has been exchanged Measurement cannot be performed because the vial rack specified in the settings differs from the type actu ally detected Verify the type of vial rack mounted in the ASI V and then set the vial rack type in the soft ware ERROR Vial rack type not set The measurement parameters cannot be validated because the vial rack type is not specified in the software Set the vial rack type in the software ERROR ASI Cover is open The ASI V cover is open The ASI V operation has stopped as a safety measure Close the ASI V cover The following messages indicate that an error has occurred that prevents measurement from continuing Take the appropriate corrective actions as indicated in the following table If the cause of the problem cannot be discovered or if the same error message appears after taking the indicated corrective actions contact your Shimadzu representative Note When the following errors are generated power to the instrument oven is auto matically stopped When power to the oven is switched on again wait until the temperature rises before starting measurement TOC VCPH CPN
141. Wizard Page 6 USP EP LLL TOC fy 747 Method Wizard Page 7 History The History window is used to enable the History Log The History Log records all modifications to the method The History Log can be set to require users to enter comments for each modification Note Once the History function is enabled it cannot be changed All modifications to the method will be tracked If the mandatory comment option is selected the user will be required to enter a comment each time any method parameter is modified Method Wizard Page 7 History Figure 4 90 Method Wizard Page 7 History Setting Item Description Enable history log Select this option to enable the software to monitor all modi fications to the system Once the history log is enabled it cannot be changed User has to comment all Select this option to require comments or approval for all modifications method modifications If the History Log is not required it need not be enabled as the software operates properly with out it 142 QQ ON PN 4 4 Sample Table Editor 4 4 2 File Menu 4 4 2 4 Open The Open command is used to select and open a Sample Table Method Calibration Curve Parameter or Control Sample Template file Save the open Sample Table before executing the Open command More than one Sample Table can be opened at the same time Selecting the Open command displays the Open dialog box s
142. Wizard Page 9 Failure Action Figure 4 159 Control Sample Wizard Page 9 Failure Action Setting Item Description Action when the failure event Select the action to be taken the first time a control sample occurs the first time exceeds the control limits Options available from the drop down list are Continue notify Select this option to allow the analysis sequence to continue normally and display a failure message in the Notification Bar Stop Whole Sample Run Select this option to stop the sam ple run and display a failure message in the Notification Bar Repeat From last control or calibration Select this option to automatically reanalyze all samples analyzed after the pre vious valid control sample or calibration curve whichever occurred most recently and display a failure message in the Notification Bar Action when the failure event Select the action to be taken the second time a control sample occurs the second time exceeds the control limits The options available from the drop down list are Continue and Stop The Repeat option is not available Save the control sample template and close the Control Sample Wizard by clicking the Finish button 202 4 4 Sample Table Editor 4 4 5 Insert Menu Inserting a Control Sample into the Sample Table Once the control sample template has been created a control sample can be entered into the Sample Table by following the procedure below
143. a comment each time any system parameter is modified Instrument Setup Wizard History Function Eg EE commentis required for allimoditications Enable modification tracking as desired lt Back Cancel Figure 3 12 Instrument Setup Wizard History Function Window Enable History Log Select this option to enable the software to monitor all modifications to the system properties Once the History Log is enabled the check box is disabled and the log cannot be turned off The History Log is maintained on the History tab of the Instrument Properties dialog box Refer to Section 3 2 8 Instrument Properties Dialog Box If the History Log is not required it need not be enabled as the software operates properly without it A Comment is Required for All Modifications Select this option to require the user to comment on or obtain approval for all modifications Once this option is selected the check box is disabled and the option cannot be turned off If the History Log is not required it need not be enabled as the software operates properly without it Finish Button The History Function window is the final screen in the Instrument Setup Wizard Make the appropriate selections then click the Finish button The new instrument is created and saved and its icon appears in the TOC Control V main window TOC VCPH CPN 3 3 2 Instrument Setup and System Properties 3 2 8 Instrument Properties Dialog Box 3 2 8 Instrument Pr
144. able Three Holes at Center of Turntable Figure 6 14 Installing the Turntable Installing the Vial Rack 7 Place the vial rack on top of the turntable 2 Rotate the vial rack until the guides of the turntable fit into the vial rack This secures the vial rack in place Installing the Cover 7 Place the cover on the ASI V Note There is a magnet at the left rear of the cover Verify that the cover and ASI V are in contact at the magnet Install the Rinse Bottle and Drain Tank Installation of the rinse bottle and drain tank is explained below Rinse and drain tubing are attached to the autosampler and are respectively labeled RINSE and DRAIN Use the rinse water tubing as is and cut the drain tubing to an appropriate length TOC VcPHICPN 323 324 6 8 Installation 6 8 4 Installing the Autosampler N caution Verify that the drain tubing remains lower than the drain port of the ASI V and that the end of the drain tubing remains above the surface of the liquid in the drain tank Corrosive substances such as acids may be present in the drainage liquid Avoid touching or spilling these liquids Preparation The rinse bottle is provided as a standard accessory The drain bottle is a special accessory P N 638 52344 A suitable substitute may be used as the drain container Procedure 7 Place the rinse bottle on the bench with the TOC V and the autosampler 2 Place
145. ack eee eeeecreteeseeeeeeseeneeees 74 Rack Installation ce eeeeeeseneeeceeeeeee 74 323 Deane theo eee eee TE 73 Setting Position eeeeseeereeecneeees 106 179 Type Sherin enea A E 72 Warning Cormroslones fi eed A hee x Electric Shock c svseinecunnndinedaedace viii High Temperature Vil TUE oa naiara a diese ese ix Warning Labels ccceceseeseesesseeseeseeeeeseeseeseeseeeeeeees vii Warning Message Maintenance s seseeeeseereeseeee 88 Wattanty wees cies easensesnesvedneoretesareorsaceantunevusductucnuanerneates iv Washing Catalyst oe Combustion Tube Plow Linies enn Glen ceed dete Syringe with Sample 138 188 212 Syringe with Standard cece 130 172 Zero Point Detection eeeeeeseseeeeeeeeeeeee 47 261 Zero Shift Toolbar Sample Table Editor CUStOMIZING eee eseeeeecteceeeecneteeeeeeeeetseneeees 177 Display ss hiomaan ah 178 Functions senenn ra A ES 122 Total Carbon See TC Total Nitrogen See TN Total Organic Carbon See TOC Troubleshooting eese 270 281 Autosampler 278 280 Flow Charts pe aa i 274 TOG V rasanan anatia 274 277 Tubing Diameters issor aeryen 83 Turntable Installation 00 0 0 cecccecceecesseceseeeenseees 323 Pitot alesse se eis 92 119 Calibration RUS cceeeeeeecreeeceseretecneeees 100 Configuring the Instrument te eee 93 Connecting the Instrument eee 96 98 Creating a Sample Table 00 98 Evaluating Results cse
146. agent contains phosphoric acid Use care while handling to prevent contact or For details refer to Section 6 9 Material Safety Data Sheets Preparing and Placing the IC Reagent Proc 1 TOC VCPH CPN edure Prepare the IC reagent by diluting 50 mL of commercial 85 phosphoric acid ACS Reagent grade to a final volume of 250 mL with pure water Note Since the specific gravity of 85 phosphoric acid is about 1 7 the concentration of the phosphoric acid is about 25 weight in the prepared IC reagent A final concentration accuracy of 2 is acceptable Transfer the prepared acid to the 250 mL bottle provided as a standard accessory and place it on the left side of instrument toward the front Pass the tip of the IC reagent tubing through the hole in the cap Secure the tubing using a wire clamp at a point about 100mm from the end of the tubing tip to prevent the tubing and cap from separating Replace the cap on the container 4 1 Analysis Preparation 4 1 11 IC Analysis Preparations Replenishing IC Reaction Vessel with IC Reagent Use the following procedure to replenish the IC reagent Procedure 1 Verify that the lever of the 3 way valve at the bottom of the IC reaction vessel is positioned to the left as shown in Figure 4 18 Lever Position of IC Reaction Vessel 3 O xX x Figure 4 18 Lever Position of IC Reaction Vessel 3 Way Valve 2 Open the TOC Control V Sample Table Editor and connect the i
147. ailed descriptions of generating calibration curves using the TOC Control V software Sample Analysis Use the calibration curve generated in the previous section to measure NPOC in the sample Measure the sample using the same method used for the calibration standards If the values gradually decrease with each repeated analysis using the optional external sparge kit extend the sparge time to ensure sufficient sparging The shape of the sample container the sample amount the amount of sparge gas and the IC content of the sample all have a bearing on the required sparge time Determine the appropriate sparge time in accordance with these parameters Reference Refer to Section 4 3 2 Tutorial and Section 4 4 5 2 Sample for detailed descriptions of conducting sample analysis using the TOC Control V software TOC VCPH CPN 65 66 4 1 Analysis Preparation 4 1 15 Sample Preparation 4 1 15 2 TC Blank Check Analysis A TOC system invariably contains substances in the instrument flow lines that produce peaks These peaks are referred to as blank values or system blank values and are present even in water samples containing absolutely no carbon The magnitude of peaks in the blanks differs based on various factors such as system construction and the catalyst used For the TOC V every effort has been made to minimize these peaks which can affect the accuracy of TC analyses Accuracy is particularly affected when trace TOC is measured s
148. al sparge kit 638 93 149 03 Manual injection kit 638 41460 Suspended solids kit when used with TOC V alone 638 93151 Suspended Solids Kit when autosampler is used 638 53044 01 Sample rack and vial sets for 24mL sample vials 24mL sample rack 24mL sample vials Vial caps Septa 638 53044 02 Sample rack and vial sets for 40mL sample vials 40mL sample rack 40mL sample vials Vial caps Septa 638 67075 Stirrer for 24mL vials For autosampler 24mL vials 638 67076 Stirrer for 40mL vials For autosampler 40mL vials 046 00617 02 Stirrer bar for 24mL vials Stirrer bar for 24mL vials 1 required for sample measurement 046 00617 03 Stirrer bar for 40mL vials Stirrer bar for 40mL vials 1 required for sample measurement 630 00960 High purity air cylinder Recommended that user provide this item 630 08585 05 Cylinder pressure regulator User can provide this item 638 41204 Air supply tubing set with 20 meters of tubing User can provide this item 630 02525 01 High speed homogenizer 638 52344 Drain bottle for ASI TOC VCPH CPN 303 304 6 6 Consumable Parts List 6 3 8 PC Hardware Requirements 6 6 Consumable Parts List Table 6 11 e Consumable Parts List 1 TOC VCPH Part Number Part Name Comment 638 41323 Combustion tube in case 638 60116 TOC regular catalyst 630 00105 01 Platinum mes
149. all a physician Wash contaminated clothing before reuse Discard con taminated shoes SECTION VIII FIRE FIGHTING MEASURES EXTINGUISHING MEDIA Carbon dioxide dry chemical powder or appropriate foam SPECIAL FIREFIGHTING PROCEDURES Wear self contained breathing apparatus and protective clothing to prevent contact with skin and eyes UNUSUAL FIRE AND EXPLOSIONS HAZARDS Emits toxic fumes under fire conditions SECTION IX ACCIDENTAL RELEASE MEASURES Evacuate area Wear self contained breathing apparatus rubber boots and heavy rubber gloves Cover with dry lime or soda ash pick up keep in a closed container and hold for waste disposal Ventilate area and wash spill site after material pickup is complete SECTION X STABILITY AND REACTIVITY INCOMPATIBILITIES Strong bases finely powdered metals HAZARDOUS COMBUSTION OR DECOMPOSITION PRODUCTS Thermal decomposition may produce toxic fumes of phosphorus oxides and or phosphine SECTION XI SPECIAL PRECAUTIONS AND COMMENTS The above information is believed to be correct but does not purport to be all inclusive It shall serve only as a guide Shimadzu shall not be held liable for any damage resulting from handling or contact with the above product Users should make their own determinations regarding the suitability of this information for their particular purposes TOC VCPH CPN 6 9 Material Safety Data Sheets 6 9 3 CO Absorber CA OH s KOH NAOH soda lime 6 9 3 CO Absorber CA OH K
150. all modi fications to the system If the History Log is not required it need not be enabled as the software operates properly with out it Once this is enabled it cannot be disabled User has to comment all Select this option to require comments or approval for all modifications modifications If the History Log is not required it need not be enabled as the software operates properly without it Once this is enabled it cannot be disabled ACSII Export The displayed items in the list are exported as tab delimi nated text files A list of the Comment dialog box contents is shown below Table 4 3 e Comment dialog box contents Item Description Date Time Displays the date and time of the modification User Displays the user who made the modification Changed item Describes the parameter that changed From Displays the previous parameter value To Displays the new parameter value Comment Lists the reason for the modification TOC VCPH CPN 4 4 Sample Table Editor 4 4 4 View Menu 4 4 4 3 Sample Window TIP The Sample Window is used to display detailed measurement information The information displayed in the Sample Window varies based on the type of analysis performed To view the Sample Window open a Sample Table place the cursor in the row of the Sample Table that contains the desired sample and select Sample Window from the View menu The Sample Window is displayed To view measu
151. alysis is complete Each tab contains the same command buttons OK Cancel and Apply Click the OK button to save changes and exit the Sample Method Properties window Click the Cancel button to exit the Sample Method Properties window without saving changes Click the Apply button to save changes without exiting the Sample Method properties window Sample Method Properties x Common Parameter 1E History System Our OC User Date of Creation 02 28 2003 01 33 45 Ph Comment Figure 4 116 Sample Method Properties Window Common Tab Common Tab Setting Item Description System Displays the system currently in use Changes cannot be made to this field User Displays the name of the user who created the method Changes cannot be made to this field Date of Creation Displays the date on which the method was created Changes cannot be made to this field Comment Enter a comment 512 characters maximum TOC VCPHICPN 161 Parameter Tab Sample Method Properties Figure 4 117 Sample Method Properties Window Parameter Tab Setting Item Description Analysis Displays analysis type Changes cannot be made to this field Dilution Displays the preparation dilution factor which will be used to calculate sample concentrations This field can be edited Sample Name Displays the default sample name 64 characters maximum This field can be edited Sample ID Displays the default sample ID
152. ample Wizard Note that a sample can also be added to the Sample Table without specifying a source an option that is desirable when a sample is to be analyzed using different parameters than those specified in the method or calibration files In this case unique measurement parameters for the sample will be entered on subsequent pages of the Sample Wizard Sample Wizard Page 1 Parameter Source x Create the sample by using parameters from Method Cal C eon ite Ju Corporation T 003201 Methods Tutorialmet System C Calibration Curve E C Edit parameters manually Parameters kip remaining Wizard pages and use measurement jparameters from the source Enter the parameter source for the sample Cancel Figure 4 142 Sample Wizard Page 1 Parameter Source Parameter Description Method radio button Calibration Curve radio button Edit parameters manually radio button Skip remaining Wizard pages and use measure ment parameters from the source Select this option to use the sample measurement parameters from a specified method This is the default option Enter the method name in the text field or use the Browse button to select the file using the File gt Open dialog box Select this option to use the measurement parameters from a specified cali bration curve Enter the calibration curve name in the text field or use the Browse button to select the file using the File
153. an area value from all non excluded injec tions No of Injections Displays the minimum and maximum number of injections Excluded E indicates calibration point has been excluded SD Max Displays the maximum standard deviation CV Max Displays the maximum coefficient of variation SD Displays the standard deviation CV Displays the coefficient of variation Additional buttons are displayed below the data columns and can be used to manipulate the calibration parameters The buttons are described below Refer to Section 4 4 2 2 Calibration Curve for more detailed descriptions Button Function Edit Edit the parameters for the selected calibration point Add Add a new calibration point Delete Delete the selected calibration point Delete All Delete all calibration points Exclude Exclude the selected calibration point TOC VCPH CPN Graph Tab The Graph tab displays the calibration curve in a graphic format Calibration Curve Properties Cal Curve Conc ppm Figure 4 129 Calibration Curve Properties Window Graph Tab Setting Item Description Slope Intercept r 2 The values for Slope Intercept and r are displayed for the selected calibration curve LLL TOC VerHiceN fy 775 176 4 4 Sample Table Editor 4 4 4 View Menu History Tab If the History Log was enabled when the calibration curve was created the History tab displays a list of changes made to the calibration curve parameters
154. ance can also be set using this command Toolbars Menu bar loobarnane M al Figure 4 133 Toolbar Window 4 4 4 8 Status Bar The View gt Status Bar function toggles the display state of the status bar between Show and Hide If the status bar is currently displayed selecting this option will hide the status bar If the status bar is not displayed selecting this option will display the status bar 178 EE TOC VcrHicen tenet 4 4 4 9 ASI 8 Port Sampler Vials This function displays the ASI or 8 Port Sampler dialog box and allows the user to enter vial numbers for measurement using the ASI or the 8 Port Sampler To access this command either create or open a sample table and select View gt ASI 8 Port Sampler Vials The Sparge Acid Addition dialog box opens automatically when the Start command is made The OK button saves the changes and closes the dialog box Using the Autosampler apang a dadanan Figure 4 134 Sparge Acid Addition Dialog Box for the ASI V Autosampler Using One 8 Port Sampler Sparging Acid Addition vit P AcidAddtion 00 x SpargeTime T sec Total Injection Volume 5000 ul Figure 4 135 Sparge Acid Addition Dialog Box for One 8 Port Sampler Using Two 8 Port Samplers Sparging Acid Addition Total Injection Volume ul Figure 4 136 Sparge Acid Addition Dialog Box for Two 8 Port Samplers LLL TOC me 779 4 4 Sample Table Edito
155. and catalyst Conducting a large number of analyses on samples containing salts will allow the salts to accumulate in the combustion tube gradually increasing resistance to the flow of carrier gas and resulting in decreased analysis reproducibility When decreased reproducibility is observed perform the combustion tube maintenance procedure described in Section 5 2 3 Washing Replacing the Combustion and Carrier Gas Purification Tubes TOC VCPH CPN 71 4 1 Analysis Preparation 4 1 16 Sample Preparation Identifying Salt Accumulation The following situations arise when salts accumulate and clog the catalyst e The sound of gas release is heard when the slider moves during analysis e A dramatic fluctuation in carrier gas flow is noticed after the sample is injected 4 1 16 Sample Preparation 4 1 16 1 Vial Types Two types of autosampler vials are available The sample volume associated with each vial type is shown below Introduce the specified volume of sample into the vials introducing too little sample may result in insufficient sample for analysis Table 4 1 Vial Types Vial Typical Sample Volume Sample Volume for NPOC Analysis 24mL 24mL 20mL 40mL 40mL 35mL Note 1 Sample volume when sample is introduced to the bottom of vial cap Note 2 Sample volume when sample is introduced to about 1cm from bottom of vial cap In NPOC analysis the sample volume is decreased to reduce its contact wit
156. and one plunger Table 4 9 Relationship Between Appropriate Peak Height and CO Gas Concentration Injection Volume Gas Concentration CO3 Gas Injection Volume TC 100ppm 10mL 1000ppm ImL 1 500uL 10 300uL 100 30uL IC 100ppm 6uL 1000ppm 600uL 1 300uL 10 200uL 100 20uL The values indicated in this table are reference values only Data will vary slightly among instruments TOC VCPH CPN 233 234 OM NLL Maintenance Inspection and maintenance of the TOC V instrument are required to ensure normal operation and reliable and accurate data acquisition 3d a 5 3 5 4 Dood 5 6 5 7 Daily Inspection Describes the daily inspection procedures that should be performed before instrument startup Periodic Inspections Describes periodic inspection procedures for the TOC V Autosampler ASI V Maintenance Describes periodic inspection procedures for the autosampler 8 Port Sampler OCT 1 Maintenance Describes periodic inspection procedures for the 8 Port Sampler TN Unit TNM 1 Maintenance Describes periodic inspection procedures for the TN unit Software Controlled Maintenance Functions Describes maintenance functions controlled by the TOC Control V software Troubleshooting Describes the error messages and troubleshooting procedures 5 1 Daily Inspection 5 1 1 Checking Dilution Water 5 l Daily Inspection Check the levels of dilution water ac
157. and time This field cannot be changed Comment Enter a comment 512 characters maximum LLL TOC fm 7193 Control Sample Wizard Page 2 Control Sample Type The Control Sample Type window is used to identify the type of control sample Control Sample Wizard Page 2 Control Sample Type C Program Files Shimadzu Corporation TOC3201 T Bk ne gt Cancel Figure 4 152 Control Sample Wizard Page 2 Control Sample Type Parameter Description Control Sample Select this option to define individual sample parameters This is the default option Control Chart Sample Select this option to add the control sample to a defined con trol chart Enter the file name or use the Browse button to select the control chart file from the File gt Open dialog box System Suitability Test for Select this option to check the control sample using USP EP USP EP criteria Save the data in a control Enter a file name for the control sample template sample template 194 TOC NM PN SSS 4 4 Sample Table Editor 4 4 5 Insert Menu Control Sample Wizard Page 3 Parameter Source The Parameter Source window is used to specify the source of the control sample measurement parameters The source can either be a method file or a calibration file When one of these sources is selected the control sample will be analyzed using the
158. ap with quartz wool and screw the cap back on the container AN CAUTION To maintain an airtight seal a rubber O ring is placed between the container and the screw cap Inspect the O ring to verify that it is not scratched or twisted then attach the cap TOC VCPH CPN 5 2 Periodic Inspections 5 2 12 Replenishing IC Reaction Solution 6 Using the elbow joints connect the carrier gas purifier CO absorber to the two tubes exiting the back of the instrument as follows e Tubing labeled L Affixed to the connection port of the CO absorber container labeled L e Tubing labeled S Affixed to the connection port of the CO absorber container labeled S L ca UTION Tighten the nut by hand only Do not use tools 7 Place the carrier gas purifier CO absorber container on the stand behind the instrument Used soda lime should be disposed of according to local industrial waste disposal reg ulations It must be clearly disclosed using an industrial waste manifest that the mate rial contains soda lime L ca UTION Soda lime is a corrosive chemical substance Be careful not to touch it with bare hands For details refer to Section 6 9 Material Safety Data Sheets 5 2 12 Replenishing IC Reaction Solution For the H Type verify that there is sufficient IC reaction solution in the IC reaction solution vessel before performing IC analysis If not replenish the IC reaction solution referring to Section 4 1 11
159. as leaks L caution Do not allow any acute bends in the tubing e When tubing and connectors are prepared by the user be sure to use clean components that are free of oils or other contaminants on their inner surfaces e Copper tubing or stainless steel tubing may also be used Low Ozone Air Supply Pressure Safety Mechanism To ensure safety the TN unit is equipped with an ozone air gas pressure sensor that will automatically cause the ozone generator to be switched off when the ozone air gas pressure decreases below 50kPa If this occurs the red lamp labeled PRESS at the lower right of the TNM front panel will illuminate Take the appropriate measures to correct the low pressure problem TOC VcPHICPN 33 6 8 Installation 6 8 6 Installing the TN Unit 6 8 6 3 Connecting Gas Exhaust Tubing Because the unit uses a chemiluminescence system for the detection of TN components it is equipped with an internal ozone generator The ozone and NO generated are removed by the ozone treatment unit and NO absorber and are then exhausted However in the event that the performance of the ozone treatment catalyst and NO absorber deteriorate ozone and NO gas may be expelled in the exhaust gas Be sure to discharge exhaust gas to the outdoors or to an exhaust pit using a 5mm I D flexible vinyl hose caution To minimize resistance leave the gas exhaust tubing open to the atmosphere e Be sure to connect the gas exha
160. ath head ache nausea and vomiting To the best of our knowledge the chemical physical and toxicological properties have not been thoroughly investigated SECTION VII FIRST AID MEASURES In case of contact immediately flush eyes or skin with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes Assure adequate flushing of the eyes by separating the eyelids with fingers If inhaled remove to fresh air If not breathing give artificial respiration If breathing is diffi cult give oxygen If swallowed wash out mouth with water provided person is conscious Call a physician wash contaminated clothing before reuse Discard con taminated shoes SECTION VIII FIRE FIGHTING MEASURES NONCOMBUSTIBLE Use extinguishing media appropriate to surrounding fire conditions SPECIAL Wear self contained breathing apparatus and protective clothing to prevent contact with skin and eyes UNUSUAL FIRE AND EXPLOSIONS HAZARDS Emits toxic fumes under fire conditions SECTION IX ACCIDENTAL RELEASE MEASURES Evacuate area Wear self contained breathing apparatus rubber boots and heavy rubber gloves Wear disposable coveralls and discard them after use Sweep up place in a bag and hold for waste disposal Avoid raising dust Ventilate area and wash spill site after material pickup is complete SECTION X STABILITY AND REACTIVITY INCOMPATIBILITIES Strong acids aluminum protect from moisture HAZARDOUS COMBUSTION OR
161. ation Odor Color Phase Water Point Point Pressure Density Rate Solubility 50 C N A 2 16 N A N A N A N A White Solid Powders 10 SECTION IV HAZARDS IDENTIFICATION Possible eye and skin irritation Avoid contact SECTION V TOXICITY DATA N A SECTION VI HEALTH HAZARD DATA Exposure to large amounts can cause gastrointestinal disturbances SECTION VII FIRST AID MEASURES In case of contact immediately flush eyes with copious amounts of water for at least 15 minutes In case of skin contact immediately wash skin with soap and copious amounts of water SECTION VIII FIRE FIGHTING MEASURES N A SECTION Ix ACCIDENTAL RELEASE MEASURES N A SECTION X STABILITY AND REACTIVITY N A SECTION XI SPECIAL PRECAUTIONS AND COMMENTS The above information is believed to be correct but does not purport to be all inclusive It shall serve only as a guide Shimadzu shall not be held liable for any damage resulting from handling or contact with the above product Users should make their own determinations regarding the suitability of this information for their particular purposes TOC VCPH CPN 6 9 Material Safety Data Sheets 6 9 11 Sodium Carbonate 6 9 11 Sodium Carbonate Shimadzu Scientific Instruments Inc 7102 Riverwood Drive Columbia MD 21046 Control No Tel 1 800 477 1227 Date MATERIAL SAFETY DATA SHEET SECTION I PRODUCT IDENTIFICATION CAT NO 630 0092 01 CAS NO 497 19 8 NAME Sodium Carbonate 100 OTHER NAME N A SECTI
162. ation Operations 4 5 2 Gas Sample Analysis 4 5 2 1 Analysis Preparation Installation of the Manual Injection Kit Installation Procedure 7 Remove the knurled thumbscrew that secures the slider then remove the TC TN injector slider and install the TC TN block provided in the kit 2 Ifthe IC reactor kit is being used remove the IC injector slider and install the IC block provided in the manual injection kit Note When installing the block be sure that it is aligned with the injection port Software Settings Select the Manual Injection Kit option in the Instrument Setup Wizard Options window during System Setup Refer to Section 3 2 2 Options Window Note Selecting the Manual Injection Kit option disables operation of the TOC V injector syringe Reference Refer to 4 5 1 1 Analysis Preparation 228 TOC VcPHICPN 4 5 2 2 Measurement The procedure for setting the various parameters is the same as described in Section 4 2 Setting General Measurement Parameters Section 4 3 Measurement Procedures and Tutorial and Section 4 4 2 2 Calibration Curve Calibration Curve Measurement Procedure 1 Prepare standard gas containing a known concentration of carbon Note For IC carbon dioxide analysis prepare a standard gas with a known carbon dioxide concentration For TC analysis another organic gas for example methane of known concentration can be used 2 From the File menu select New The New dialo
163. ation points click the Delete All button TOC VCPHICPN 13 132 4 4 Sample Table Editor 4 4 2 File Menu Click the Edit and Add buttons to display the Edit Calibration Point Parameters window This window is used to enter calibration points manually and to edit the parameters of existing calibration points Edit Calibration Point Parameters x Calibration Point No fi Standard Auto Cal Point Solution Conc Dilution Conc Cancel p fi 4 p 000 No of Injections 2 4 g a 1 20 SD Max 01000 C Max 2 00 z Figure 4 81 Edit Calibration Point Parameters Window Parameter Description Calibration Point No Standard Solution Conc Auto Dilution Cal Point Conc No of Injections SD Max and CV Max TOC VCPH CPN Displays the calibration point number This field will reflect the number selected by clicking in the No field in the Cali bration Points List The number cannot be changed directly in the window Enter the concentration of the calibration standard solution When creating a calibration curve from a single standard solution by using the Auto Dilution function enter the con centration of the original standard solution in this field Enter the factor by which the instrument should automati cally dilute the calibration standard solution to obtain the desired concentration for the calibration point Displays the actual concentration of the calibration point The concentration is
164. ble 1 Cable for connecting 8 Port Sampler 1 to 8 Port Sampler 2 M393 E228 User Manual 1 Flanged tubing in C sets have an inner diameter of 1 0 mm This set is provided for use with the combustion type TOC V Connect this tubing to the common COM port of the 8 Port Sampler and port No 2 on the TOC V unit Flanged tubing in W sets have an inner diameter of 1 5 mm This set is provided for use with the wet chemical type TOC V Connect this tubing to the common COM port of the 8 Port Sampler and port 10n the TOC V unit TOC VCPH CPN 6 3 8 6 4 Standard Accessories PC Hardware Requirements Table 6 6 Standard Accessories List 4 TN Unit Part Number Part Name Qty 630 00999 CO absorber 1 638 60074 Ceramic fibers 1 017 40533 01 Potassium nitrate 072 02004 19 Fuse 218 002 020 46547 SS screw pan head M 4 x 8 5 631 81157 Mounting plate TNM 1 072 60301 Wiring band TY 23M 5 630 003 15 05 Plastic tubing 5mm ID x 7mm OD 5m 631 41200 02 Viton tubing 5mm ID x 8mm OD 0 45 638 52353 03 Ozone treatment unit ASSY 1 035 60690 97 Tee 2 016 43284 01 Tube 0 1m 072 60338 03 Clip 2 638 42035 Capillary 1 071 60813 Adapter 1 071 608 14 01 Power cord set 100 127V 071 608 14 06 Power cord set 220 240V Table 6 7 Standard Accessories List 5 Manual Gas Sample Injection Kit Part Number Part Name Qty 638 101
165. bration Curve 183 Controls ei 184 Measurement ParameterS cecceseeseeeeees 182 Opening 2 sessecscsecdecvesssiceessevec ses cssescdecebdescebesees 181 Parameter SOULCE eee cece ceessessesee tee eeeeee 181 Sample Table Editor ccccecececesceteeeneeeee 122 218 Auto Restart nosan deans 121 Background Monitot cccccecsesesseeeneeeseees 203 Closing a File eee 144 Connecting The Instrument 205 Creating New Sample Table 98 125 Deleting All Data ccccceesseeeseneeeeeesees 158 Deleting Selected Data 0 ect eeeeeeeeeeerees 159 Directories useen a EE 217 Edt Menus cioen 156 Editing Rows and Cells 156 Excluding Data gs we 158 Exin icici eaten acc 15D Exporting Data to ASCII oo eeeeceeteneneeeee 146 Exporting Data to Database cceeeeseeteereeee 148 File Men sespe raoi nnie 125 Finding Cell Content 0 ec eeeeeseeereeerees 157 General Information Window 125 Help Menu ou ce ceeeeseeseeteeee 218 Importing Data from ASCII we 159 Insert Menu cece cece cecesecsececsecssessesessenes 181 Inserting Calibration Curve cccceeeeseeeeee 126 Inserting Control Samples 0 cesses 193 Inserting Sample Group cceceeesesseeeeseeseees 181 Inserting Samples Instrument Menu Notification Bar Opening File eee ceceseesecnecseceeneeeeeeeseess Options Menu iesin ne ioes Qutliet Testen
166. breathing is difficult give oxygen If swallowed wash out mouth with water provided person is conscious CALL A PHYSICIAN Wash contaminated clothing before reuse discard contaminated shoes Additional information Large doses of lithium ion have caused dizziness and prostration and can cause damage if sodium intake is limited Dehydration weight loss dermatological effects and thyroid disturbances have been reported Central nervous system effects that include slurred speech blurred vision sensory loss ataxia and convulsions may occur Diarrhea vomiting and neuromuscular effects such as tremor clonus and hyperactive reflexes may occur as a result of repeated exposure to lithium ion SECTION Ix SPILL OR LEAK PROCEDURES Occupational Spill Evacuate area Wear protective footwear Sweep up and place in a bag and hold for waste disposal Waste Disposal Method For small quanti ties cautiously add to a large stirred excess of water Adjust the pH to neutral separate any insoluble solids or liquids and package them for hazardous waste dis posal Flush the aqueous solution down the drain with plenty of water The hydrolysis and neutralization reactions may generate heat and fumes which can be controlled by the rate of addition Observe all federal state and local environmental regulations Water Contamination Harmful to marine life Change in pH will result in alkaline damage to marine life SECTION X SPECIAL PRECAUTIONS AND COMMENTS The above in
167. but is also valid for TN analysis Analysis Restrictions Since Teflon tubing with an inner diameter of about 0 5mm is used in the instrument for injecting the sample suspended solids that do not pass through cannot be measured Analysis reproducibility is poor for samples that do not uniformly contain such solids even if they should pass through the tubing Solids that are heavy and readily form sediment such as silt can accumulate at the bottom of the syringe This can scratch the rotor of the sample injector 8 port valve causing leaks Sedimentation and separation should be performed to as great an extent as possible prior to analysis TOC VCPH CPN 69 70 4 1 Analysis Preparation 4 1 15 Sample Preparation Countermeasures The following types of processing operations are normally used for measuring samples containing suspended solids 1 2 3 4 TOC VCPH CPN TOC Analysis of Supernatant In situations when the suspended solids are of no great concern sedimentation occurs in the sample container and the supernatant sample is used Results depend on the sedimentation and separation properties of the suspended solids but usually the dissolved TOC DOC dissolved organic carbon is measured TOC Analysis of Filtrate The suspended solids are removed using glass fiber filter paper or a membrane filter and only the dissolved TOC is measured Because the filter paper or filter itself is likely to contain TOC t
168. cPHICPN 197 Parameter Description Multiple Injections Select to enable the syringe to draw up a single sample aliquot with a volume equal to that required for all injections of the sample When this option is not selected the syringe will draw up a separate sample aliquot for each injection as a result selecting this option reduces analysis time Use area retrieved from Select this option to subtract the blank check area from the measured area of the blank check the control sample This option is only available for TC and NPOC analyses that use the high sensitivity catalyst Control Sample Wizard Page 6 Peak Time Parameters The Peak Time Parameters window is used to set peak detection parameters for the control samples Control Sample Wizard Page 6 Peak Time Parameters Figure 4 156 Control Sample Wizard Page 6 Peak Time Parameters Setting Item Description Use default settings Select this option to use the default integration parameters When this option is selected all other options in this window are disabled Allowed peak start delay The allowed peak start delay is the amount of time in min utes that can elapse before the analysis is stopped because a peak is not detected Enter a number between 0 and 20 00 Total integration time The total integration time is the amount of time in minutes peak detection continues Enter a number between 4 50 and 20 00 1 98 WE TOC VcPmcPn ieee Control Sam
169. ch off instrument Remove 8 port valve rotor from 8 Port Sampler 2 remove debris etc and wash valve 5 7 2 Troubleshooting 5 7 2 1 TOC V 1 An error message is displayed Refer to error message 2 The Ready lamp will not light Access the Background Monitor screen by selecting Background Monitor from the Instrument menu Refer to the screen to see which parameters are not satisfied 3 The baseline stays over the auto zero range Baseline position never reaches the ready state Does carrier gas flow normally to the analysis cell Is dehumidifier within the specified temperature The infrared gas analyzer is bad Contact your Shimadzu representative TOC VCPH CPN Carrier gas leak Repair the leak The dehumidifier temperature setting is bad Contact your Shimadzu representative 4 The baseline is unstable Is carrier gas flowing normally NS YES Was the catalyst replaced NO YES Is the dehumidifier operating normally NO YES Are external conditions vibration temperature power voltage normal NO YES The infrared gas analyzer is bad Contact your Shimadzu representative 5 7 Troubleshooting 5 7 2 Troubleshooting Carrier gas leak Repair the leak Accumulated obstructing substance Replace the catalyst The dehumidifier is bad Contact your Shimadzu representa
170. chever is less Store in tightly closed containers in cool dry ventilated area Protect from physical damage and direct sunlight Iso late from incompatible substances Protect from moisture Remove and wash contaminated clothing promptly Wash hands thoroughly after handling This sub stance is classified as a POISON under the Federal Caustic Poison Act SECTION III PHYSICAL DATA Melt Boil Point Density Vapor Vapor Evaporation Odor Color Phase Water Solubility Point Pressure Density Rate N A N A N A N A N A N A Pungent Colorless Clear Fuming Infinite slight Liquid evolution heat SECTION IV REACTIVITY DATA Stable under ordinary conditions of use and storage Containers may burst when heated When heated to decomposition emits toxic hydrogen chloride fumes and will react with water or steam to produce heat and toxic and corrosive fumes Hazardous Polymerization will not occur Incompatibilities A strong mineral acid concentrated hydrochloric acid is highly reactive with strong bases metals metal oxides hydroxides amines carbonates and other alkaline materials Incompati ble with materials such as cyanides sulfides sulfites and formaldehyde SECTION V FIRE AND EXPLOSION HAZARD DATA FIRE Can react with metals to release flammable hydrogen gas EXPLOSION Not considered to be an explosion hazard EXTINGUISHING MEDIA If involved in a fire use water spray Special
171. cing the CO Absorber for the Optional Carrier Gas Purifier The NDIR baseline becomes unstable with a decrease in the carbon dioxide absorption in the carrier gas purifier CO absorber The baseline position rises and reproducibility diminishes making analysis impossible The soda lime must be replaced when this occurs The frequency with which soda lime must be replaced depends on the frequency of analysis quantity of organic impurities in the carrier gas and the TOC content of the samples It is recommended that soda lime be replaced once every four months Soda Lime Replacement Procedure N caution The carrier gas pressure applied to the carrier gas purifier CO absorber is approximately 200kPa It is dangerous to perform this maintenance procedure under these conditions Before replacing the soda lime lower the carrier gas pressure in the instrument to normal as follows Turn the supply valve of carrier gas source OFF Switch OFF the instrument Procedure 7 Remove the elbow joints of the carrier gas purifier CO absorber which are behind the instrument 2 Invert the CO absorber and remove the screw cap 3 Remove the used soda lime 4 Refill the absorber container with about 500g of new soda lime until it reaches about 5mm from the interior screw threads L caution Do not allow any soda lime to enter the tube in the center of the container when refilling the CO absorber 5 Fill the hollow in the screw c
172. ck the Delete button to remove the curve from the sample group Calibration Curves No Displays the number of the calibration point File name Displays the name of the calibration curve Analysis Displays the analysis type LLL TOC Vc fy 183 184 4 4 Sample Table Editor 4 4 5 Insert Menu Sample Group Wizard Page 4 Controls The Controls window is used to identify the control samples in a sample group and to specify their placement in the sample group Sample Group Wizard Page 4 Controls x Insert Control samples T At the beginning of the sample group T iays alter P At the end of the sample group Control Templates No Filename Analysis m a Delete f 10 Sample s Define the sequence of control samples lt Back Cancel Figure 4 141 Sample Group Wizard Page 4 Controls Insert Control Samples Use the options listed below to insert individual control samples in the sample group Setting Items Description At the beginning of the sam Select this option to add control samples at the beginning of ple group the sample group Always after number of Select this option to add control samples at defined intervals samples between unknown samples At the end of the sample Select this option to add control samples at the end of the group sample group Control Templates The Control Templates table displays a list of the control sample templates currently assigned to
173. ck the Cancel button to abort the Exit command TOCSpITbI oye se o cea Figure 4 109 Prompt to Save Data Changes If the software is connected to an instrument and the Exit command is selected a dialog box is displayed as shown below Click the OK button to disconnect the instrument before exiting the software Click the Cancel button to abort the Exit command Figure 4 110 Prompt to Disconnect Instrument LLL TOC fy 755 156 4 4 Sample Table Editor 4 4 3 Edit Menu 4 4 3 Edit Menu 4 4 3 1 Undo The Edit menu contains functions that allow a user to modify data To change data using the Edit menu functions a user must have the appropriate access rights Options such as Cut Copy and Paste are available only when a content selection from an open file is made Undo Ctrl Z amp Cut Chex Copy Ctrl C e Paste Ctrl V Replace Eind gt lt Evclude Recalculate Delete Data Import Figure 4 111 Edit Menu The Undo function is used to reverse the last change made in the active Sample Table and is only available after the user changes the content of a cell in the table The Undo function is not available during actual measurement or when the user has inserted or deleted completed samples calibration curves or control samples 4 4 3 2 Cut Copy Paste The Cut Copy and Paste functions are used to edit selected Sample Table cells and rows The Cut command deletes selected information from
174. click the Calibration Curve icon The Calibration Curve Wizard opens The System Information window of the wizard is displayed i Calibration Curve Wizard Page 1 System Information Cal Pts Analysis Cal Type System Figure 4 188 Calibration Curve Wizard Page 1 System Information 3 From the System drop down list select the system that was configured with the Manual Injection Kit during setup 4 Select the desired options on pages 2 and 3 of the Calibration Curve Wizard which list calibration curve type and analysis information settings respectively Enter the name of the new calibration curve in the text box at the bottom of page 3 of the wizard Note Select the settings described in Section 4 2 Setting General Mea surement Parameters LLL TOC fm 227 222 4 5 Application Operations Manual Injection Analysis 4 5 1 5 10 11 12 13 14 15 TOC VCPH CPN Enter the desired number of injections on page 4 of the Calibration Curve Wizard Calibration Measurement Parameters Enter the injection volume on page 5 of the Calibration Curve Wizard Calibration Points List Note An injection volume is displayed automatically The displayed value is based on the volume of the last injection that was per formed using the sample injector This value can be changed by the user as appropriate Select the desired options on pages 6 and 7 of the Calibration Curve Wizard which list peak time
175. ct this option to insert a control sample without defining radio button a source Control sample measurement parameters will be entered in subsequent pages of the Control Sample Wizard Skip remaining Wizard pages Select this option to accept all measurement parameters from and use measurement param the source file The Next button will become a Finish button eters from the source and subsequent pages of the Control Sample Wizard will not be displayed This option is disabled if Edit parameters man ually is selected TOC VCPH CPN 195 Control Sample Wizard Page 4 Analysis Parameters Control Sample Wizard Page 4 Analysis parameters Figure 4 154 Control Sample Wizard Page 4 Analysis Parameters Parameter Description Analysis Default Sample Name Default Sample ID Dilution Calibration Curve 196 EE TOC VcPrHicPN iene Select the analysis type from the drop down list If a source method or calibration file was specified on Page 3 of the Control Sample Wizard this field is disabled and the applica ble analysis type is displayed Enter the sample name If a source method or calibration file was specified on Page 3 of the Control Sample Wizard the default sample name from the source is displayed Enter the sample identification If a source method or calibra tion file was specified on Page 3 of the Control Sample Wiz ard the default sample identification from
176. cursor in the Calibration Curve 1 field Click the Browse 2 button Select the file for the TC calibration curve created previously TCtutorial cal Method Wizard Page 3 Calibration Curves Ea Parameters Cal Curve Gen Info System Figure 4 58 Method Wizard Page 3 Calibration Curves 7 Click the Next button Page 4 of the Method Wizard is displayed Method Wizard Page 4 Injection Parameters Parameters Cal Curve Gen Info System JL Tis Te Figure 4 59 Method Wizard Page 4 Injection Parameters LLL TOC fm 109 110 4 3 Measurement Procedures and Tutorial 4 3 2 Tutorial 10 11 12 13 14 15 16 The following TC analysis parameters can be entered e Analysis disabled Units Injection Volume disabled e Number of Injections SD Max e CV Max e Number of Washes e Auto Dilution e Acid Addition e Expected Concentration Range e Multiple Injections e Use blank check area e Auto reinjection If both the CV max and SD max values have been exceeded Click the Next button Page 5 of the Method Wizard is displayed View but do not change the default settings for options on this page Click the Next button The Method Wizard Page 3 Calibration Curve screen is displayed Enter the TN measurement parameters Click the box beside Calibration 1 an
177. d Operation eeeeesceeceeceeceeeeeseeseeseeneens 35 233 History LO gin sis scdsscsscescastcscesstbsenseveveecsces cessed ces 31 OVMEIVIE Wits mest tehetculiestiaco naan 1 5 Needle Seiseanan aea enana eari 28 POWEL enie sateen eniti E EKSS 89 Options Window sseeseesseseseeeeesrereererrereeees 24 94 SetuP a e e awaken es 23 33 Oxidation Method cccceeseeeesceeceeceeceseeaeenes 24 Shut Down Procedure 0 0 ceceesceesseeeeneeeeeeees 120 Ready Status Check ll Standby Window cccccseesesceseeeeeeseeeeeeeeees 206 SSM Window ccccccsecsecscesceneeseeeeeeeceeeeeeeeeeees 29 Starting isisisi 89 207 System Information Window 23 94 Viewing Properties cccccceeseeseeseeeeeeeeeeeeees 32 TOC Widow neire a a a 26 Instrument Properties Dialog BoX cceceeeeeeees 32 Tubing Diameter oo cece eeeeeeeeeceeceeceeeeeeaeenes 26 Tinttrod ction ceceeseeeesesesseesesessceeeceseseeecseeeeeseeeees iii System Administration ccccceseseeseeeeeeeeeeees 20 L Left Side View Lithium hydroxide MSDS s ssesseseeeeeerereeeereerereeeeee 336 TOG V a A L EEEE ES 9 M Malittenance sorna 235 281 Measurment 8 Port Sampler sessseseseesesesreeeeeseerersesen 254 255 8 Port Samplet niiina aneateen 80 Autosampler sieniin enia 252 253 Mechanical Check Chemiluminescence Detector cee 259 Method Daily Inspection cc eeeeceseneeecteeeeeee 236 237 Creating NeWsiocsinn ennie ie det 135
178. d either select the TNtutorial cal file or enter the calibration curve file Click the Next button The Method Wizard Page 4 Measurement Parameters screen is displayed Set the TN measurement parameters in the same way as for TC measurement Click the Next button The Method Wizard Page 5 Peak Detection Time screen is displayed Do not change the default settings on this page Click the Next button Page 6 of the Method Wizard is displayed View but do not change the default settings for options on this page Click the Next button Page 7 of the Method Wizard is displayed View but do not change the default settings for options on this page Click the Finish button The Method Wizard closes The method file is now complete and has been saved Insert the sample into the Sample Table Reference Refer to Section 4 4 2 3 Method Wizard for a detailed description of the Method Wizard TOC VCPH CPN 4 3 Measurement Procedures and Tutorial 4 3 2 Tutorial 77 Insert the unknown sample by placing the cursor in the third line of the Sample Table From the Insert menu select Sample Page 1 of the Sample Wizard Parameter Source is displayed TIP Zoset up multiple analyses using a previously created method select the Auto Generate Table command from the Insert menu Refer to Section 4 4 5 1 Auto Generate Sample Wizard Page 1 Parameter Source x Create the sample by using parameters from Method Cal C on ie Ju
179. d for the GLP GMP 21 CFR item in System Administration Tools of the TOC Control V main menu the History Log function is automatically activated 13 Click the Finish button An icon for the system now appears in the TOC Control V main window TC TN System To edit the system configuration double click the system icon in the TOC Control V main window or when in the Sample Table Editor window select Properties from the Instrument menu The Instrument Properties dialog box opens and system configuration options are displayed on tabs in the dialog box Connecting the Instrument Step 2 Opening a New Sample Table 1 2 In the TOC Control V main window double click the Sample Table Editor icon The User dialog box is displayed Sample Table ditor Enter your user name and password Click the OK button Open a new Sample Table by either selecting New from the File menu or clicking the New J toolbar button The New dialog box is displayed alibration Curve Control Sample Template Method Cancel Figure 4 38 Sample Run Icon Click the Sample Run icon then click the OK button The General Information dialog box opens TOC VCPH CPN 5 Click the System tab and select the desired system from the drop down list 6 Select Save File As in the File menu Enter Tutorial and click the Save button 6 14 032 Figure 4 39 Save As Dialog Box 7 Click the OK button A
180. d injury is possible Do not use a wrench or other tool Injury could result if the combustion tube breaks Installation for the H Type 7 2 TOC VCPH CPN Push the capillary end of the catalyst filled combustion tube downward into the center of electric furnace about 22mm diameter Apply an extremely thin layer of the provided high vacuum silicone grease to the outside of the combustion tube tip part in contact with O ring Note Use the smallest possible amount of silicone grease Absolutely no grease should be applied to the interior of the combustion tube Insert the tip of the combustion tube with the silicone grease securely into the opening at the bottom of the sample injector Note At this point be sure to connect the drain tubing exiting the slide injector to the Y fitting of the system drain line Connect the tubing at the bottom end of combustion tube as shown in Figure 4 4 Connecting Combustion Tube to the Compression Fitting Push the narrow end of the combustion tube into the compression fitting Adjust the distance between the bottom of the compression fitting and the base of the instrument to 1mm or less and then tighten the top compression fitting nut firmly by hand 4 1 Analysis Preparation 4 1 2 Connecting the Combustion Tube TC Combustion Tube Nut Rear Ferrule Sleeve Set 6F T oe P N 035 62994 03 Front Ferrule TC Combustion Tube Stainless Tubing toward detector Figure 4 4
181. d off and the furnace cools down The power to the instrument is automatically turned off when the countdown is complete Auto restart Select this option to shut down the instrument but automati cally restart it at a specified time Set the restart time using the spin controls for Auto start time The default settings are the current system date and time Keep TC furnace heating Select this option to keep the TC furnace on during the Standby mode This option is available only when the Auto restart option is selected Keep carrier gas flowing Select this option to keep the carrier gas flowing during the TOC VCPH CPN Standby mode This option is available only when the Auto restart option is selected 4 4 Sample Table Editor 4 4 6 Instrument Menu 4 4 6 4 Measurement Start Click the Measurement Start command to open the Standby dialog box if the ASI is included in the system configuration If the ASI is not included the Measurement Mode dialog box is displayed To start measurement open the Sample Table define a new sample and connect to the instrument x Normal Continious C Non Stop Mode Cancel Figure 4 167 Measurement Mode Dialog Box Item Setting Description Normal Mode Select this option to conduct analysis sample by sample Between samples the instrument waits for the user command before starting the next measurement Multiple Row Continuous Select this option to perform continuous uninterrupt
182. d the lower portion displays the data table which contains all relevant data for performing the validation The toolbar options such as Open Save Cut Copy and Paste are similar to those described in Section 4 4 2 File Menu and Section 4 4 3 Edit Menu ATE ee Cal Curve Area 10000 8000 6000 5000 sooo EEEE EAFE Sooo SB pee CARA RHARARARAR si 2 s2 2 Test Value P Value ting the linearity Regression Coeff Gd Regression Coeff b gt Regression Coeff Co Residual SD CSy gt Process SIDCSX REL ProcessCV CVS Figure A 1 Method Validation Main Window Linear Regres The windows can be resized by dragging the dividers between the sections 348 COC NP LLL A 2 File Menu Figure A 2 File Menu A 2 1 New Use the New command to create a new empty method validation file A new file can also be created by clicking the New toolbar button If a file that contains modified and unsaved data is open when the New command is selected a prompt is displayed in a dialog box Select one of the options in the dialog box to determine if the unsaved data should be saved before opening a new method validation file Click the Yes button to save the document and create a new method validation file Click the No button to create a new document without saving previous data Figure A 3 Prompt for Saving Data LLL TOC fy 349 A 2 2 Open Use the Open command to
183. d with each Sample Wizard window can be found in the Analysis box at the top of the window 186 M TOC VcpmcPn p Sample Wizard Page 3 Calibration Curve The Calibration Curve window is used to identify the calibration curve s that will be used to calculate the sample concentration If more than one curve is identified the software automatically selects the curve to be used in calculating sample concentration Refer to Section 6 2 5 Automatic Selection of Optimum Calibration Curve Sample Wizard Page 3 Calibration Curve omar Parameters Cal Curve Gen Info Corporation TOC3201 CalCurves tctutorial cal System Figure 4 144 Sample Wizard Page 3 Calibration Curve Parameter Description Analysis Displays the analysis type This field cannot be changed Calibration Curve 1 2 3 Enter the name of the calibration curve or click the Browse button to select a file using the File gt Open dialog box Skip the injection parameter Select this item to skip the Measurement Parameters window pages of the wizard of the Sample Wizard Use this option when the sample mea surement parameters will be the same as those used for cali bration curve measurements LLL TOC fy 187 Sample Wizard Page 4 Injection Parameters Sample Wizard Page 4 Injection Parameters
184. de SECTION VI TOXICITY DATA RAT MOUSE LD50 RTECS OSHA PEL ACGIH TLV TWA N A 0j6307080 Lithium hydroxide Monohydrate N A N A REVIEWS STANDARDS AND REGULATIONS NOES 1983 HZD X6293000 TNF 60 NIS 6239 NOS 54 TNE 59941 TFE 6243 SECTION VII HEALTH HAZARD DATA Acute Effects Harmful if swallowed inhaled or absorbed through skin Material is extremely destructive to tissue of the mucous membranes and upper respiratory tract eyes and skin Inhalation may be fatal as a result of spasm inflammation and edema of the larynx and bronchi chemical pneumonitis and pulmonary edema Symptoms of exposure may include burning sensation coughing wheezing laryngitis shortness of breath headache nausea and vomiting Uncontrolled move ment muscle spasms and loss of consciousness may occur To the best of our knowledge the chemical physical and toxicological properties have not been thor oughly investigated SECTION VIII FIRST AID An antidote is a substance intended to counteract the effect of a poison It should be administered only by a physician or trained emergency personnel Medical advice can be obtained from a POISON CONTROL CENTER In case of contact Immediately flush eyes or skin with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes Assure adequate flushing of the eyes by separating the eyelids with fingers If inhaled remove to fresh air If not breathing give artificial respiration If
185. djust the flow rate to about 100mL min using the sparge gas flow rate adjustment knob Note The flow rate should be adjusted according to the size and shape of the sample container 5 Close the front door of the instrument I Sparge Gas Flow Rate Adjustment Knob H an Halogen Scrubber Figure 4 17 Sparge Gas Flow Rate Adjustment TOC VCPHI CPN 53 4 1 Analysis Preparation 4 1 10 Installing the Suspended Solids Kit 4 1 10 Installing the Suspended Solids Kit To analyze samples containing suspended solids the sample flow line diameter can be increased from 0 5mm to 0 8mm by installing the optional Suspended Solids Kit This section describes the installation of the Suspended Solids Kit There are two kits available 1 For TOC V TOC V main unit only 2 For TOC V ASI V used with TOC V and autosampler N caution Switch OFF the TOC V before attempting to install the Suspended Solids Kit Replacing the Flow Line Parts and Slider This procedure is used for both kits Procedure 7 Remove the bushing from port 7 of the 8 port syringe pump valve and disconnect the TC injection tubing For the H type remove the bushing from port 5 and disconnect the IC injection tubing 2 Remove the slider mounting screws from the TC and IC injection blocks and detach the sliders 3 Remove the slider bushings and replace the sample injection tubing wi
186. e Figure 4 137 Insert Menu The Auto Generate command opens the Sample Group Wizard which is used to create a group of unknown samples control samples and calibration standards and then insert the group into the active position of the Sample Table Sample Group Wizard Page 1 Sample Source The Sample Source window is used to specify the source of sample measurement parameters Sample Group Wizard Page 1 Sample Source Figure 4 138 Sample Group Wizard Page 1 Sample Source Setting Item Description Method radio button Method text field Calibration curve radio but ton Calibration curve text field Click this option to analyze the samples using the measure ment parameters from a specified method This is the default option Enter the desired method or select the method using the Browse button Click this option to analyze the samples using the measure ment parameters from a specified calibration curve Enter the desired calibration curve or select the curve using the Browse button LLL TOC my 87 Sample Group Wizard Page 2 Sample Parameter The Sample Parameter window is used to enter basic information about the sample group Sample Group Wizard Page 2 Sample Parameter Figure 4 139 Sample Group Wizard Page 2 Sample Parameter Setting Item Description No of Samples Enter the number of samples in the group Enter an integer ranging from 1 to 200 The default value is 1
187. e Enable ready status check option is selected Enabling the ready status check function means that the instrument will not begin a new injection until the instrument status is Ready Instrument Setup Wizard TOC emp arm D Aaaa E ee _ lt Back ne Figure 4 36 TOC Analysis Parameters Reference For details on TOC parameters refer to Section 4 2 1 TOC Parameter Settings 9 Click the Next button The ASI window of the Instrument Setup Wizard is displayed Verify that the ASI parameters match those shown on the figure below Instrument Properties Figure 4 37 Autosampler Parameters 70 Click the Next button The Communication window of the Instrument Setup Wizard is displayed 11 Verify the communication information COM Port Stop Bits and Parity Note If a Shimadzu representative installed your TOC Control V soft ware the correct settings for your system are already configured Please do not change the settings Refer to Section 3 2 6 Commu nication Window for more information on Communication set tings LLL TOC VePrHiceN fe 95 96 4 3 Measurement Procedures and Tutorial 4 3 2 Tutorial y 12 Click the Next button The History Function window of the Instrument Setup Wizard is displayed If desired enable the History Log to track all changes to the method Refer to Section 3 2 7 History Function Window for more information about the History Log Note If Audit Trail was checke
188. e 8 port valve and result in leaks Syringe Plunger Retaining Screw e Figure 4 10 Installing the Syringe 9 Verify that the syringe moves smoothly between the upper and lower positions by clicking the directional arrows on the Syringe Change dialog box 10 With the syringe in this position hand tighten the plunger retaining screw on the plunger holder 11 Click the Finish Replacement button to move the syringe to its initial position 12 Click the Close button Note Once the syringe is installed perform the syringe pump zero point detection operation See Section 4 1 3 1 Syringe Pump Zero Point Detection for details 46 TOC VCPH CPN 4 1 3 1 Syringe Pump Zero Point Detection This section describes the procedure for performing automatic detection of the syringe pump zero point Note Perform the zero point detection procedure whenever a new syringe is installed or the syringe is replaced Procedure 7 Open the TOC Control V Sample Table Editor and connect the instrument 2 From the Instrument menu select Maintenance gt Zero Point Detection The Zero Point Detection dialog box is displayed Zero point detection Zero point detection Std dtd dd dt Hdd dd dd Sd Figure 4 11 Zero Point Detection Dialog Box 3 Click the Start button A progress bar is active while the syringe moves to the position where the zero point can be detected When the progress bar stops blinking the procedure
189. e Wizard which is described above Select the check box to enable this function Sample Wizard Page 9 USP EP Figure 4 150 Sample Wizard Page 9 USP EP 192 Wi TOC VcprHicPN p 4 4 5 3 Control The Control command is used to insert a control sample into an existing Sample Table Note A control sample template must be created before a control sample can be inserted into a Sample Table A control sample template has a file extension of tpl and specifies measurement parameters for the Control Sample The following subsections describe the procedures for creating a control sample template and for inserting a control sample into a Sample Table Creating a Control Sample Template Control sample templates are created using the Control Sample Wizard To access the Control Sample Wizard select New gt Control Sample Template from the File menu The Control Sample Wizard consists of several windows each of which defines specific parameters for the control sample template as described below Control Sample Wizard Page 1 System Information ontrol Sample Wizard Page 1 System Information Cal Pts Analysis Cal Type Figure 4 151 Control Sample Wizard Page 1 System Information Parameter Description System Select the instrument Operator Displays the current operator name This field cannot be changed Date of Creation Displays the current date
190. e e OVET EW e e e ei al ee Page Setup Options Previewing Sample Report we 151 Previewing Sample Table w 150 Printing Options cceceseeseesecseceececensenseneeees 151 Printing Sample Report cee ceeeseeeeteneeee 150 Printing Sample Table eee eeeeeeeees Recalculating Data ccs eeecseeeeecreeeeeeneeees Replacing Data Reversing Last Action Searching for Text ceeseeecteseseeeeeeeeeeee Sequence Window ccececcesesseseceeceeeneeeenee Setting Vial Position Sparging Acid Addition Window Standby Window ceeeeeeeeeeees Starting Instrument cece ete seceeeeeeeeeees Status Baf sosisini ssnesd cases ses e iana Stopping the Instrument 0 0 eee ee eeenees To lbat seyrin Toolbar Customize View Menu seen Viewing Calibration Curve Viewing Cell Properties cc ceeseeeceeeeeeeee Viewing Data in Real Time Viewing Method Properties cesses Viewing Vial Positions ceeeseeeceeeeeeeee Window Menu cceccssessesseseesereeeesreeeeseneeees Injection Table Parameter Table ccccccceccseesseeseceseeeseeneeeees Sample Wizard Acid Addition cccecesseesecesseessceseecseceeeesseens 189 Analysis Information Window seseseeseeeeeee 186 Auto Dilution ccccccccceeecessecseseseeceeeeeeseens Calibration Curve 06 Calibration Curve Window Determinations ccecseeseeseesecseeneeeeee
191. e eye irritation may cause skin irritation Material may be irritating to mucous membranes and upper respiratory tract prolonged or repeated exposure may cause allergic reactions in certain sensitive individuals EXPOSURE CAN CAUSE Coughing chest pains difficulty in breathing gastrointestinal disturbances CHRONIC EFFECTS Prolonged exposure can cause damage to the lungs and bones TO the best of our knowledge the chemical physical and toxicological properties have not been thoroughly investigated TARGET ORGAN DATA Lungs thorax or respiration tumors tumorigenic neoplastic by RTECS criteria tumorigenic equivocal tumorigenic agent by RTECS criteria tumorigenic tumors at site of application only selected registry of toxic effects of chemical substances RTECS data is presented here see actual entry in RTECS SECTION VI HEALTH HAZARD DATA OSHA PEL 8H TWA SMG ME respirable fraction 8h TWA 10MG M3 total dust SECTION VII FIRST AID MEASURES In case of contact immediately flush eyes with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes If inhaled remove to fresh air If not breathing give artificial respiration If breathing is difficult give oxygen If swallowed wash out mouth with water provided person is conscious Call a physician Remove and wash contaminated clothing promptly In case of skin contact immediately wash skin with soap and copious amounts of water SECTION VIII
192. e results are displayed when measurement is complete Click Additional Measurements to perform repeat measurements Repeat the procedure Click the Finish button when all measurements are complete Sample Measurement Procedure 7 From the File menu select New The New dialog box is displayed Sample Run Calibration Curve Method Control Sample Template Figure 4 193 New Dialog Box 2 Double click the Method icon The Method Wizard opens The System Information window of the wizard page 1 is displayed Method Wizard Page 1 System Information Parameters Cal Curve Gen Info System Figure 4 194 Method Wizard Page 1 System Information 3 Select the system that was configured with the Manual Injection Kit and used to create the calibration curve Advance to page 2 of the Method Wizard Analysis Information and enter the new method name in the text box at the bottom of the window 4 Advance to page 3 of the Method Wizard Calibration Curves Select the appropriate calibration curve file 5 Enter 1 in the No of Injections field on page 4 of the Method Wizard Injection Parameters LLL OC fm 237 232 4 5 Application Operations 4 5 2 Gas Sample Analysis 6 Select the desired options on pages 5 6 and 7 of the Method Wizard which list
193. e text search Find Next Select to begin the search and to continue a search that has already begun Replace Select to replace the found text with the text in the Replace with field Replace All Select to replace all occurrences of found text with the text in the Replace with field Cancel Select to close the Replace dialog box The Find function is used to search for specified text Selecting the Find command opens the Find dialog box which is similar to the Replace dialog box and displays the options described below Refer to Section 4 4 3 3 Replace Setting Item Description Find what Enter the text to be searched for Match case Select to perform a case sensitive text search Direction Click the Up radio button to search the table backwards from the current location Click the Down radio button to search the table forward from the current location Find Next Select to begin the search and to continue a search that has already begun Cancel Select to close the Find dialog box TOC VcPHICPN 157 158 4 4 Sample Table Editor 4 4 3 Edit Menu 4 4 3 5 Exclude The Exclude function is used to exclude selected injections from the calculations A user must have access rights for updating data to use the Exclude function To exclude data highlight the desired injection shown in the Sample Window Injection Table and select Exclude from the Edit menu A confirmation dialog box is displayed Click the Yes button t
194. ear Maintenance Procedure Perform maintenance on the detector only after shutting down the instrument 7 After removing the tubing from the reactor as shown in the figure below loosen the 4 mounting screws and detach the reactor Detector Reactor Mounting Screws Figure 5 22 Removing the Reactor 2 Remove the gasket and confirm that it is not dirty or cracked Replace it if necessary 3 Confirm that the detector window is not dirty If necessary gently wipe the window clean with a cloth 4 Place the flat side of the gasket facing the detector window sandwiching it between the window and the reactor 5 Secure the gasket in place with the 4 mounting screws tightening them uniformly N caution Recheck the tubing after completing the maintenance work to make absolutely certain that there are no mistakes in the line connections and that everything has been properly tightened 6 Reconnect the tubing TOC VcPHICPN 259 260 5 5 TN Unit TNM 1 Maintenance 5 5 3 Ozone Generator Replacement 5 5 3 Ozone Generator Replacement Replace the ozone generator with a new one after 8000 hours of operation Set a warning generation value of 8000 hours in the Maintenance History dialog box For details refer to Section 4 2 4 Maintenance History Settings Ozone generator replacement must be carried out by an
195. easurement Parameters 4 2 3 Setting Default Measurement Parameters 4 2 3 Setting Default Measurement Parameters The Default Measurement Parameters window is used to enter the default values for sample measurement parameters The selections made in the Default Measurement Parameters window will be displayed as the default values when setting calibration curve and sample measurement parameters Procedure 7 From the Options menu in the Sample Table Editor select Default Measurement Parameters The Default Measurement Parameters window is displayed TC Jic Nroc roc TN ssm tc ssM c Units pm X No of injections e B Bp 1 20 No of washes 0 Max SD 0 1000 Mas V 12 00 Figure 4 28 Default Measurement Parameters TC IC INPOC POC TN Tabs 2 Enter the following parameters on each of the applicable tabs e Units Select the default concentration units for the measurement results e No of Injections Enter the default mintmum maximum number of injections No of Washes Enter the default number of times the syringe is to be washed with sample prior to the first injection In POC analysis and IC analysis with the N type this refers to the number of syringe rinses using dilution water e Max SD Enter the default maximum standard deviation that is acceptable for repeat measurements If this value is met no additional injections are required However if both this value and the Max CV value are exceeded the
196. easurement data in real time Method Opens the Method Properties window which contains the method parameters for a selected sample Exclude Excludes a selected sample or injection from the calculation Toggles to include an excluded sample Recalculate Highlighted Recalculates the highlighted sample results after applying a new calibration curve or excluding injections Recalculate All Recalculates all sample results after applying a new calibration curve or exclud ing injections Delete Highlighted Data Deletes the highlighted measurement data This function does not change the structure of the Sample Table Delete All Data Deletes the measurement data for all samples This function does not change the structure of the Sample Table TOC VCPH CPN 123 4 4 Sample Table Editor 4 4 1 Sample Table Window Overview Format Displays the Floating Point Format dialog box where options for numeric for mats can be modified Font Displays the Font dialog box where options for fonts can be modified Insert Sample Opens the Sample Wizard and allows a sample to be inserted in the active posi tion of the Sample Table Autogenerate Opens the Sample Group Wizard and allows a specified group of samples to be inserted in the active position of the Sample Table Insert Control Displays the Open dialog box and allows a selected control sample template to be added to the Sample Table Insert Calibration Curve
197. eate control charts Refer to Appendix B for a detailed description of the function 4 4 8 2 Method Validation The Method Validation function is used to validate analytical methods Refer to Appendix A for a detailed description of the function 4 4 8 3 Administration The Administration function is used to access the Administration program of the TOC Control V software Refer to Section 3 1 Introduction to System Administration Functions for a detailed description of the Administration program 208 WE TOC VcrHicrn jn 4 4 8 4 Screen Lock If the user must temporarily leave the PC he she is logged into the screen can be locked by using the password function to prevent another individual from performing operations in TOC Control V This function can be used only if the User ID Password item is checked in the Security dialog box To lock the screen select Screen Lock in the Tools menu The screen will then be locked and the Re enter Password dialog box is displayed To release the screen lock enter the user ID and password into the designated fields If the user ID and password entered are not the same as those used up to that point the screen lock will not be released The screen has been locked Enter the User ID and Password again User ID sd Password Figure 4 169 Re enter Password Dialog Box LLL TOC fm 209 4 4 9 Options Menu The Options menu contains commands for viewing and displaying system informat
198. eck if there is a problem with the instrument operation or if there is a problem with communication between the PC and the instrument The selected communication port is already open Verify that it is not used with another connection An attempt was made to open a communication port that has already been opened Check if the selected port is being used with another connection Cannot open communication port Check instrument status and trans mission settings The communication port failed to open Verify that the instrument is switched on and that the instru ment connection and communica tion port settings are correct Mode error Check instrument con dition If necessary restart instru ment The operation was not accepted due to the instru ment condition Verify the instrument operation If necessary restart the instrument TOC VCPH CPN 271 272 5 7 Troubleshooting 5 7 1 Error Messages Table 5 3 Error Message List 3 Error Message Description Corrective Action ERROR Syringe Zero Point Detection Syringe zero point detection could not be performed Syringe is not properly installed Properly mount the syringe Then select Zero Point Detection from the Maintenance menu WARNING TC furnace temper ature is too low to regenerate cat alyst TC furnace temperature is too low to perform the catalyst regeneration procedure
199. ect this command to replace the contents of the flow lines connected to the 8 port valve from the dilution solution bottle and the hydrochloric acid bottle Replace Flow Line Content godt d d d dd ed ed dd od od od od Figure 5 28 Replace Flow Line Content Dialog Box Click the Start button to begin the procedure A progress bar is active until the flow line content has been replaced Click the Close button LLL TOC fm 263 5 6 6 Flowline Washing Use this function to wash the selected flow lines a ar ee ee ee ee Ge stop Figure 5 29 Washing Dialog Box To perform flow line washing click the Select Flow Lines button to open the Wash Flow Lines dialog box Select the flow lines to be washed and click the Washing button The ports for the 8 Port Sampler 1 2 can be selected if the 8 Port Sampler 1 2 is being used Wash Flow Lines F Fort F Port 10 F Part 17 Port 12 F Port 13 F Port 14 F Port 15 F Port 16 Figure 5 30 Wash Flow Lines Dialog Box While this process is being executed the buttons in the Washing dialog box are disabled and progress bar activity is displayed 264 OC MN ae 5 6 Software Controlled Maintenance Functions 5 6 7 Mechanical Check 5 6 7 Mechanical Check Select this function to check mechanical components of the instrument or to make adjustments The Mechanical Check window consists of several tabs one for each connected instrument TOC Tab Mechanical Check x
200. ection Kit Gas Sample Injection Kit Analyte Liquid samples TC IC TOC TC IC Gas samples TC carbon dioxide TOC determined by TC carbon dioxide Carbon monoxide and other inorganic carbon containing gases aside from carbon dioxide are also measured as TOC Measurement of IC TOC and carbon dioxide is possible with the TOC VcPH Measurement principle 680 C catalytically aided combustion oxidation non dispersive infrared detection NDIR Measuring range Liquid sample e TC 0 20000mg L IC 0 20000mg L Gas sample 6ppm 100 CO Sample injection volume Liquid sample 1 150uL Gas sample 20uL 10mL Measuring time Liquid sample e TC Approx 3min e IC Approx 3min Gas sample 2 4min Repeatability Liquid sample CV within 2 CV is within 3 when sample concentration is 8000mg L or greater Gas sample CV within 2 Sample introduction Manual injection using microsyringe TOC VCPH CPN 6 3 8 PC Hardware Requirements PC IBM PC AT or compatible with 9 pin RS 232C connector CPU 233MHz or better Memory 32 MB or greater Hard drive 2 GB or greater OS Windows95 Windows98 Windows2000 WindowsNT 4 0 SP3 or later WindowsXP For compliance with FDA 21 CFR Part 11 use Windows2000 The User Authentication function cannot be used with WindowsXP Monitor resolution 800 x 600 or better 1024 x 768 suggested LLL TOC fm 297 2
201. ed mea Mode surement of multiple rows until the user stops the measure ment sequence Continuous Mode Select this to perform measurement using multiple measure ment modes without stopping measurement between modes Select OK to continue on to the measurement or select Cancel to cancel the start of measurement 4 4 6 5 Stop gt Peak Stop The Stop gt Peak Stop command is used to interrupt the current measurement The peak measured up to the stopping point is considered a complete peak After the Stop gt Peak Stop command is executed the next injection listed in the Sample Table is made and analysis continues normally 4 4 6 6 Stop gt Finish Current Sample The Stop gt Finish Current Sample command is used to interrupt measurement after all injections of the current sample are complete After the Stop gt Finish Current command is executed the instrument remains in Ready mode 4 4 6 7 Stop gt Halt The Stop gt Halt command is used to immediately interrupt the current measurement discard data from the current injection and return the instrument to Ready mode TOC VCPH CPN 207 4 4 7 Maintenance Menu Instrument maintenance procedures are described in Section 5 6 Software Controlled Maintenance Functions All maintenance functions can be initiated using the options displayed in the Instrument gt Maintenance menu 4 4 8 Tools Menu Figure 4 168 Tools Menu 4 4 8 1 Control Charts The Control Charts function is used to cr
202. eeee 330 Principles NPO wince Rivnn bie Sean mas 286 288 Of Analysis ceeeecesceeceteeteeeeeeneeneene 284 288 Print Control Charts cneccc ica se ei a ae 373 Method Validation File ee eceeeeeene teens 351 OptOisisaii aceite EE teaser PASE SOUP seesi r seeden re s roria Pr view Repoti e Preview Tabl nonnene enaa Sample Report Sample Table Product Warranty cccccescsseescescesceeceseeseeseceeneensenee i Purgeable Organic Carbon See POC Regenerating Catalyst F Beinat 2385 262 IC Sol t naera 27 262 Replacing Sample Table Data eee eeeeeteeeee 157 Replacing the NO Absorber eeeeeeteeeeeerees 260 Residue Removal cccseccsseceecreeecneeeceecneeecneees 263 Right Side View TOC V ccsccsccsseseseetseneeeeeeeeeeees 8 Rinse Bottle Needle Needle After Acid Addition ccccceeseceee 86 Pump Headset 253 Index 7 Index 8 Salt Effect on Instrument ccccceececssesseceseesseeeees 71 Sample PUAN esate case cet aaee EA at cee eae Catcher Container Containing Acid ececeseesecsecsecseereeeeeeeeeeeeees 71 Containing High IC Levels eee eeeeeeeeeee 38 Containing Salt 2 eee seeeeseteeseeeeeeeeneeees 71 Preparations 3 c s ecavteutstes verve deee eles 63 72 79 Report Printing 0 cece cesceeeceecsecneenseneeeenee 150 Suspended Solids cceeescesceceseesecseenecneeseenee 69 Sample Group Wizard Cali
203. eeeeeeee Injection Parameters cceeseseeeeeeeeeeeeeeees Injection Parameters Window cceceee 188 Injection VolUME ec eseeseesecseeneeeeeeeeeeeeeeee 188 Multiple Injections 0 0 0 ee eee eeeeteteeeeneeees 189 Number of Injections ccceseseseeseeseeeeeeees 188 Parameter Source Window csceseeeeeeees 185 Peak Time Parameters Window c ee 190 SDMaK Cae 188 Waits eile te eh oe ele oe eee eee 188 USP EP Window ececeeceescecesceseeseeeeteeeeeeees 192 Screen Lock eceschaidaneititasisesen aes 20 SD MaX 138 188 Sequence Window cccesssecsecsectecreeteeneeneeeeeeeees 205 Shipping Screw ecccccescesceccesceseeeceecseceeseeeeneeeeees 317 Sliding Sample Injector ececeeeseeseeseereeneeeeees 245 Sodium bicarbonate MSDS cccccecceeeeecesteeenee 342 Sodium carbonate MSDS 00 ceesecseeteereeneeeeees 343 Index Software Connecting To Instrument 0 cee eeeeeeeeeee 205 Creating New Method cc eceseceseeteeneeees 135 Maintenance Functions eeeseeeceeeneeneenee 261 Maintenance History Settings eee 88 Module naii cid seat tian Beenle aes 122 OVETVIE Was Sas stele EE AEE EEE 19 33 Ready Status Check ccceeseecseseeeeeteeeseeeees 84 Setting Measurement Parameters 83 87 Setting up a Sequence ceceeceeseeseeeereeeeeeees 125 Source Air TN Unit PHESSULE cyrr hosen en aA 330 Sparge Gas Flow Rates
204. eeneeeaes 298 Special ACCeSSOMes niona n a elaceeeedeetadarsiusloeeda locos 303 Consumable Parts Tisti sirini ane ta a ae e aae te 304 Maintenance Parts List cccescessceescesseesseeseceeceseeeseeeseeaeceseceseseneeeseesaes 308 Mista at Om sn E esa seen aes nye os sedans eee eae 310 6 8 1 Before Installationen nni e 310 6 8 2 Installation S Eaa a a iene ce ale E 310 6 8 2 1 Installation Site Selection c ce ceccecceesesceeseeesececeseeeeeneseeeeeeeneeeaes 310 6 8 2 2 Installation Site Conditions eceeceeseseessessececeeeeseeeeeeteeerenseeees 311 6 8 3 Installation Procedure ececceescescesseesecseecsececeseceeceseceeeseseeeeseeeseeaeenseeaees 312 6 8 3 1 Connecting Power Supply and Ground ceeeeeeeseeseeeeeereereeenes 312 6 8 3 2 Changing the Power Supply Voltage cccccseeseesseeseeeeeeteeeeeereees 313 6 8 3 3 Connecting Gaseni iii ii n E E E a lvesd deca i 313 6 8 3 4 Connecting the Drain Tubing sssssssesessesesseseeseeseseesteeesersesersrereses 316 6 8 3 5 PC Cable Connections ceceeeesceseeesceseeeeeeeeeeeeeaeeseecaeceeenseesenseens 317 6 8 4 Installing the Autosampler cccccecseesecsseeteceseesececeseeeceeeeenseeeeeeneeneeenes 317 6 8 5 OCT 1 8 Port Sampler Installation 2 0 0 0 eee eceeeescereeeeceeeesecnseseeeeeeees 325 6 8 5 1 Installation Procedure ceceseesceseeescesceeeeeseeeeeeaeeseecsececeseesenseens 325 6 8 6 Installing the TN Unit thet at
205. egration Allowed peak start delay Displays the amount of time in minutes that can elapse before the analysis is stopped because a peak is not detected Total integration time Displays the amount of time in minutes that analysis contin ues after the end of the peak is detected Data Tab The Data tab displays information about each calibration standard used in the calibration curve Common Parameter Analysis Data Graph History en Auto Dilution Ini VolumefV Calibration Points tu No Conc Mean Area No of Inj Excluded SD Max CVb 0 000 mg L 2 3 01000 Z 50 00 mg L 2 3 01000 Z 100 0 mg L 2 3 01000 Z 4 Edit Add Delete Delete Al Exclude Figure 4 128 Calibration Curve Properties Window Data Tab Setting Item Description Auto Dilution Displays the auto dilution factor Inj Volume Displays the injection volume which varies depending on the analysis type 174 4 4 Sample Table Editor 4 4 4 View Menu Columns of data are displayed in a window below the Inj Volume selection as described below Table 4 5 Data Tab Columns Column Name Description Auto Dilution Displays the dilution factor for auto dilution Standard Solution Concentra Displays the concentration of the standard solution used for tion analysis No Displays the calibration point number Conc Displays the concentration of calibration point Mean Area Displays the me
206. ends on the water temperature and carbon dioxide content of the air in contact with the water Refer to Table 6 2 e CO Content ppm in Distilled Water Equilibrated with Atmosphere Temperature C Instruments that prevent contact with air are not incorporated in water uptake retention or storage processes during common distillation and purification of water For this reason IC is present in most types of distilled and purified water In some cases the TC content of commercially available distilled water stored in plastic or glass containers is ppm Note The degree of purity required varies depending on the analysis range Use of commercially available purified water is acceptable when measuring samples with expected TC concentrations around 100ppm The quality of the zero water should be considered along with the analysis range Preparation of TC Standard Solutions 7 Accurately weigh 2 125g of reagent grade potassium hydrogen phthalate that was previously dried at 105 120 C for about hour and cooled in a desiccator 2 Transfer to a 1 L volumetric flask and dissolve in zero water 3 Add zero water to the 1 L mark and stir the solution The carbon concentration of the solution is 1000mgC L 1000mgC L 1000ppmC This solution is the standard stock solution Note The standard stock solution may be prepared at other concentrations For example a 2000mgC L solution can be used as the standard stock solution 4 The standard stoc
207. eneeees 134 Measurement Parameters Window 130 Opening sosenem ae 125 Peak Integration Parameters ccccseeseeeeee 103 Peak Time Parameters Window sese 133 System Information Window ccceeeeeees 127 Carrier Gas Connecting inne a aa Flow Rate Pressure Purification Tube eeeeeeeseseeseeeeeesenees 240 PUD er eshte ct atid E AEN TEREA 314 Kit Specifications 0 0 cee seeeeeeeeeerees 296 Replacing CO Absorber eee 248 Supply Pressure ceeeeeeeees Tubing Connections Catalyst Disposal c6 ciitA RG ees 240 Pulling esiisa leet e eenas 36 Filling Roderes merecanno morerna 37 38 High Sensitivity ccccccseesecseeseereereeeees 37 240 NeW Regenerating Replacitig iesca niniin Setting Typeset a ran Eor Eeit 26 Standard TOG iraa TOC TN Washing Ceramic Fiber ocssssssicsoniioiisiiiiriisiiiiii 39 42 Change Password sseeseeeesseseeeeeesseressesrsrerseseseererses 21 Dialog BOX oic ia E A eteee 21 Chemiluminescence Detector ccceeeeeeeeeees 259 COs Absorber esinin a oats 335 Disposal e etai iie A E ETT 242 Installation 52 58 MSDS orearen e E E EA 335 Replat tei irainen Ae 242 248 251 Used as NOx Absorber 59 Coaxial Needl spasiini 28 85 320 ComM POr aea a ER E tte ands 30 Combustion Tube Connecting s sseesessesesseesseserstsesresrsessesesesessesesse Filling with Catalyst Installating H Type 2 iy Insta
208. enu or by clicking the Save button amp in the toolbar Measurement can now be performed TOC VCPH CPN 4 3 Measurement Procedures and Tutorial 4 3 2 Tutorial Performing Measurement Step 6 Procedure 1 Prepare the three calibration standards Oppm potassium hydrogen phthalate Oppm ammonium chloride 50ppm potassium hydrogen phthalate 10ppm ammonium chloride and 100ppm potassium hydrogen phthalate 20ppm ammonium chloride and place them in autosampler tray vial positions 1 2 and 3 Note Calibration standards and unknown samples can be placed in any vial position when controlling the instrument with the TOC Control V software 2 Check the status of the instrument detectors before starting analysis From the Instrument menu select Background Monitor or click the Background Monitor button on the toolbar The Background Monitor window is displayed this window is used to monitor the real time signal from the ASI and the detectors On the TOC tab the status of the baseline should be OK for each parameter position fluctuation and noise 3 Click the TN tab to check the status of the nitrogen detector Background Monitor Toc tN Jasi Furnace E Dehumidifier BREE NDIR Baseline Pos Baseline Fluc Baseline Noise NDIR x1 x50 Chem Sep sare esse sete qs Signal m o 4 r 4 1 4 Time min Figure 4 61 Background Monitor 4 Close
209. er use the Font option Note that the Display Folder check box Max Number of Displayed Lines field and Font option apply only to the selected folder as a result these options must be set separately for each folder Note A folder will not be displayed in the Notification Bar unless the Display Folder option is selected and the Max Number of Displayed Lines field is set to a value greater than 0 TOC VCPHICPN 215 4 4 Sample Table Editor 4 4 9 Options Menu 4 4 9 6 Display Settings gt Floating Point Number Formats The Display Settings gt Floating Point Number Formats command is used to select display options for numeric results in the Sample Table Note that these options apply only to the manner in which numbers are displayed internal data retain their original values Floating Point Format x Display floating point numbers in the following format Common Floating Point Numbers Cancel p a 1 012 20 34 300 5 Number of digits after the decimal point F 3 1 01 20 34 300 52 Percent Values Number of significant digits 3 4 1 01 20 3 300 Number of digits after the decimal point B a 1 01 20 34 300 52 Figure 4 179 Floating Point Format Window Select settings for both common numbers and percent values as described below Common Floating Point Numbers Setting Item Description Number of significant digits Select this option to display common floating poi
210. er Signal Cable Cable Cable with Power Supply Figure 2 15 Rear View LLL TOC V fm 75 16 2 4 TN Unit TNM 1 Option 2 4 1 Front and Right Side Views 2 4 TN Unit TNM 1 Option 2 4 1 Front and Right Side Views Ozone Air Source Flowmeter POWER Power Lamp REACT Reactor Temperature Control Heater Lamp O3GEN Ozone Generator Status Lamp PRESS Ozone Source Air Supply Warning Lamp Ozone Generator Switch Figure 2 16 Front and Right Side Views TOC VCPH CPN 2 4 TN Unit TNM 1 Option 2 4 2 Inside Front View 2 4 2 Inside Front View Reactor Viton Joint Flowmeter Ozone Treatment Unit Ozone Source Airflow Adjustment Knob Figure 2 17 Inside Front View TOC VCPH CPN 17 2 4 TN Unit TNM 1 Option 2 4 3 Rear View 2 4 3 Rear View Ozone Source Air Inlet AC Cable Socket Gas Exhaust Port Figure 2 18 Rear View 18 TOC VcPHICPN Software Overview Administration and Setup This chapter provides an overview of the TOC Control V software and describes the software s Administration and Instrument Setup Wizard tools 3 1 Introduction to System Administration Functions Describes the system administration functions performed by the user 3 2 Instrument Setup and System Properties Describes the software s Instrument Setup Wizard which is used to configure new
211. ere it can be replaced When the progress bar begins blinking replace the syringe Verify that the syringe moves smoothly between the upper and lower positions by clicking the directional arrows Click the Finish Replacement button to move the syringe to its initialization position then click the Close button Note Perform the zero point detection procedure whenever a new syringe is installed or the syringe is replaced Refer to Section 4 1 3 1 Syringe Pump Zero Point Detection 268 TOC VcPHI CPN 5 6 Software Controlled Maintenance Functions 5 6 12 Blank Check 5 6 12 Blank Check Use this function to automatically determine the background TC level of the instrument Conducting the Blank Check procedure is recommended prior to performing high sensitivity measurements and after loading high sensitivity catalyst Open a blank Sample Table connect the instrument and select the Blank Check option from the Instrument menu Refer to Section 4 1 15 2 TC Blank Check Analysis for details Set the injection volume using the spin controls then click the Start button to begin the procedure Blank Check Parameters x Injection Volume 2000 El Cancel Press the Start button on this dialog or on the front panel of the instrument Figure 5 37 Blank Check Parameters Window Note Do not insert a sample into the Sample Table The Blank Check procedure only works in a blank Sample Table 5 6 13 Maintenance Log Refer to Section 4
212. essesseeecsecseeeeeeseees File Menu Sample Table Editor eee 125 Flow charts Troubleshooting 0 0 0 ceeeeeeeeeeeeeees 274 Flow Diagram TOC VCPH TOC VcPH TOC VcPH TOC VCPN TOC VcPN Corrosion Warning Cover Installation ccccccccccecessceesseecssceeeseeeesaees Creating Calibration Curve ccccccccccccscecssceesseeeesseeenes Control Charts ccccccccsesscessessecessesseeeseesseeees Method Validation File Sample Table 0 0 0 0 TC Calibration File cece eeeeeeeesereeeceeeeeees CV Max Setting in Method Wizard eee eeeeeees 138 Setting In Sample Wizard eee eeeeeeee 188 Determinations No Of c sees 136 162 186 Dialog Box Change Password cesesceseresseeseseeeceeeeeeens 21 Dilution Water Checking cscs eck cdhnienancane ie iene 236 Preparing onion ein E EE O ES 50 Display Settings Floating Point Number Formats 0 216 Notification Bar Settings ce eeeeeeeeeee 215 Table Settings sesccceasndecanerantseteeelanasss 214 Disposal Catalyst eenst sa gttlsss cided lavedineetleton ait 240 CO Absorber 0 0 eeete eee teesee ee seeeeeceneneeeeees 242 Drain Tank Installation 0 0 cccccecsseecesseceeeeessees 323 Drain Tubing Connecting 00 0 eeceeeseeseeseeteeneenes 316 Drain Vessel Water Checking cecceceeeeseeneeeee 236 Excluding Data from Sample Table eee eeeeeee 158 Injections from Calculations cece 1
213. eview Use the Print Preview command to view the method validation file before printing Y a January15 Method Validation Button Figure A 7 Print Preview Window Description Next Page and Previous Page One Page Two Page Zoom In and Zoom Out Close Print Click the Next Page button to display the next page of the report Click the Previous page button to display the previous page of the report The Next Page button is disabled when the last page of the report is displayed and the Previous Page button is disabled when the first page of the report is dis played Click the One Page button to display one page at a time in the Print Preview window After selection the button toggles to the Two Page button Click the Two Page button to display two pages side by side Click the Zoom In and Zoom Out buttons to change the mag nification of the displayed pages Three different zoom fac tors are available Repeated selection of either option will continue to increase or decrease the magnification as appli cable Click the Close button to close the Print Preview window and return to the previous window The Print Preview window must be closed to edit the report Click the Print button to print the report A 2 7 Print Setup Select Print Setup to open the Print Setup dialog box Print Setup HP Lasenet 474M Plus New AutoSelect Tray Figure A 8 Print Setup Dialog Box The print opt
214. f the TOC Control V calibration curve A 5 3 Font Use the Font command to select fonts for printed reports and display screens Selecting the Font command opens the Font dialog box TIP The Font command has a shortcut button on the toolbar AGaramond FP Algerian Andale Mono T Andale Mono IPA T Animals T Animals 2 Figure A 19 Font Dialog Box Choose a font for printed reports by selecting options from the Font Font Style Size Color and Script drop down lists A preview of the font appearance is visible in the Sample field on the lower portion of the Font dialog box LLL TOC fy 361 Method Validation Options Menu A 5 4 Floating Point Numbering Format Use the Floating Point Numbering Format command to select display options for numeric results in the method validation tables These options apply only to the manner in which numbers are displayed internal data retain their original values Floating Point Format x Display floating point numbers in the following format m Common Floating Point Numbers Cancel 012 20 34 300 5 Number of digits after the decimal point F 1 01 20 34 300 52 m Percent Values Number of significant digits fi 1 01 20 3 300 Number of digits after the decimal point fa 4 1 01 20 34 300 52 Figure A 20 Floating Point Format Window Common Floating Point Numbers Setting
215. f the active Sample Table TOC VCPH CPN 159 4 4 4 View Menu The View menu contains options for viewing calibration method and sample information and for selecting settings for the display screen Outlier Test Gl eroperties Customize V Toolbar v Status Bar Show all control bars ASI 8Port Sampler Vials Data Profile Figure 4 115 View Menu 4 4 4 1 Calibration Curve The View gt Calibration Curve command is used to view the calibration curve information associated with a sample Place the cursor in the desired row of the Injection Table and select the Calibration Curve command from the View menu The Calibration Curve Properties window is displayed Refer to Section 4 4 4 5 Properties TIP The Calibration Curve Properties window can also be displayed by clicking the Calibration Curve View button on the Toolbar 160 WE TOC VePHICPN iii 4 4 Sample Table Editor 4 4 4 View Menu 4 4 4 2 Method The View gt Method command is used to view the properties associated with a method Selecting the command displays the Sample Method Properties window which consists of several tabs including a separate tab for each applicable method Each tab lists options for method properties as shown in the figures below Individual options can be selected deselected or edited by clicking in the check boxes or entering information into the text fields Note that certain options will be disabled if sample an
216. fer to Section 5 2 2 Washing or Replacing Catalyst Regeneration Procedure The procedure for regenerating the TC catalyst is controlled by the TOC Control V software as described below 7 From the Instrument menu in the Sample Table Editor select Maintenance gt Regeneration of the TC Catalyst The Regeneration of TC Catalyst dialog box is displayed Regeneration of TC Catalyst d d d ddd i d ddadda Figure 5 3 Regeneration of TC Catalyst Dialog Box 2 Click the Start button to begin the procedure A progress bar is active until the TC catalyst has been regenerated 3 Click the Close button TOC VCPH CPN 5 2 Periodic Inspections 5 2 2 Washing or Replacing Catalyst caution Dilute hydrochloric acid is the only type of acid that can be used to regenerate TC catalyst Other acids particularly phosphoric acid cause abnormally high peaks and scattered peak values to occur If this happens the catalyst must be replaced 5 2 2 Washing or Replacing Catalyst Large quantities of salts accumulate in the catalyst when measuring samples with high salt concentrations If sensitivity and reproducibility do not improve after catalyst regeneration wash or replace the catalyst Refer to Section 5 2 1 Catalyst Regeneration 5 2 2 1 Washing Catalyst Standard catalyst can be washed and reused several times using the following procedure High sensitivity catalyst cannot be washed and reused warnine Due to the
217. firefighting procedures Use full protective clothing and NIOSH approved self contained breathing apparatus with full face piece operated in the pressure demand or other positive pressure mode SECTION VI TOXICITY DATA RAT MOUSE LDS50 RTECS OSHA PEL ACGIH TLV TWA 900mg kg hydrocloric acid concentrated N A Sppm TWA Ceiling 5ppm TWA Ceiling SECTION VII HEALTH HAZARD DATA Symptoms of overexposure Inhalation corrosive can cause coughing choking inflammation of the nose throat and upper respiratory tract Inhalation of higher concentrations may cause lung damage Ingestion corrosive swallowing product can cause immediate pain and burns of the mouth throat esophagus and gas trointestinal tract may cause nausea vomiting and diarrhea Contact with skin corrosive can cause redness pain and severe skin burns deep ulcers and discol ored skin severe burns and eye damage Chronic exposure long term exposure to concentrated vapors may cause erosion of teeth long term exposure seldom occurs due to the corrosive properties of the acid Persons with preexisting skin disorders or eye disease may be more susceptible to the effects of this substance SECTION VIII FIRST AID An antidote is a substance intended to counteract the effect of a poison It should be administered only by a physician or trained emergency personnel Medical advice can be obtained from a POISON CONTROL CENTER In case of contact Immediately flush eyes or skin with copious am
218. for all injections of the stan dard When this option is not selected the syringe will draw up a separate aliquot for each injection as a result selecting this option reduces analysis time File Name Enter the file name of the calibration curve LLL TOC mm 129 4 4 Sample Table Editor 4 4 2 File Menu Calibration Curve Wizard Page 4 Calibration Measurement Parameters The Calibration Measurement Parameters window is used to specify measurement parameters for the calibration standards Calibration Curve Wizard Page 4 Calibration Measurement Parameters Cal Pts Analysis Cal Type No of Cal Points 1 20 System Concentration Range Bi aeaee No of Injections 3 47 B 3 1 20 No of washes E 4 wo SD Max 0 10000 0 9999 CY Max 200 0 100 Acid Addition Joo a 0 0 20 0 Enter analysis parameters for all calibration points lt Back Next gt Cancel Figure 4 79 Calibration Curve Wizard Page 4 Calibration Measurement Parameters Parameter Description Units Concentration Range No of Cal Points No of Injections No of Washes SD Max and CV Max Sparge Time Acid Addition 130 TOC VCPH CPN Select the concentration units from the options on the drop down list Enter the maximum and minimum concentrations of the cali bration curve standard solutions Enter the number of calibration standards that will be used to create the ca
219. formation is believed to be correct but does not purport to be all inclusive and shall be used only as a guide SHIMADZU shall not be held liable for any damage resulting from handling or from contact with the above product Users should make their own investigations to determine the suitability of the infor mation for their particular purposes TOC VCPH CPN 6 9 Material Safety Data Sheets 6 9 5 Halogen Scrubber 6 9 5 Halogen Scrubber Shimadzu Scientific Instruments Inc 7102 Riverwood Drive Columbia MD 21046 Control No Tel 1 800 477 1227 Date MATERIAL SAFETY DATA SHEET SECTION I PRODUCT IDENTIFICATION CAT NO 630 0092 00 CAS NO 07740 50 8 NAME Halogen Scrubber OTHER NAME Copper Wool PRODUCT USE This product is for specific use with TOC instruments SECTION II PRODUCT USE For use specifically with the Shimadzu TOC 500 TOC 5 000 and TOC 4 000 instruments Consult the appropriate instrument manual for proper use SECTION II PHYSICAL DATA Melt Boil Density Vapor Vapor Evaporation Odor Color Phase Water Point Point Pressure Density Rate Solubility 1083 C 2595 C N A N A N A N A N A Reddish Solid Malleable N A Metal SECTION IV HAZARDS IDENTIFICATION Dust mist or fumes may cause eye and skin irritation Avoid contact SECTION V TOXICITY DATA RAT MOUSE LD50 RTECS OSHA PEL ACGIH TLV TWA N A GL5325000 N A N A SECTION VI HEALTH HAZAR
220. from the drain bottle YES Is the level of the water normal in the drain bottle NO Low water level YES Replenish water Was membrane filter NO replaced Clogged membrane filter YES Bad infrared gas analyzer Large resistance downstream of dehumidifier Contact your Shimadzu Replace the membrane filter representative Contact your Shimadzu representative TOC VCPH CPN 277 5 7 Troubleshooting 5 7 2 Troubleshooting 5 7 2 2 ASI V 1 The ASI V does not operate y ls connection cable and power cable properly connected Improperly connected cable Properly connect the cables Bad electrical system Contact your Shimadzu representative 2 Rinse water is not delivered from the rinse port Is there sufficient rinse water in rinse water bottle Insufficient rinse water Replenish the rinse water Is the rinse tubing properly inserted into the rinse water bottle The rinse tubing is not properly inserted into rinse water bottle Properly insert the tubing into the rinse water bottle The rinse pump is bad Contact your Shimadzu representative 278 TOC VCPH CPN 5 7 Troubleshooting 5 7 2 Troubleshooting 3 Reproducibility is poor Is there any material adhering to the sample needle YES Poor reproducibility due to foreign matter Remove the obstruction from the opening a
221. g Box Note The selected measurement parameters will appear as default values when setting up calibration and method files 98 EE TOC VcPHicPn M Reference For details refer to Section 4 2 3 Setting Default Measurement Parameters Modify the Sample Table window display settings so that all items contained in the Sample Table are shown on the screen The default display settings may not include all of the Sample Table parameters 4 From the Options menu select Display Settings gt Table Settings 5 Ensure that all items on both tabs in the Table Options window are selected If not click the Select All button Table Options MDate Time Figure 4 43 Table Options Window Note Use this window in the future to create custom Sample Table win dows that display only the desired items Save the Sample Table t32 file S From the File menu select Save As The Save As dialog box is displayed Enter Tutorial as the file name and click the Save button Note The name Tutorial appears at the top of the Sample Table win dow and for the directory name after the file is saved The basic instrument configuration and analysis parameters have been set up Reference Refer to Section 4 4 Sample Table Editor for detailed descriptions of the Sample Table Editor menus and commands LLL TOC VcrHiceN fy 99 Setting up the Calibration Standard Runs Step 4 Setting up calibration standard runs
222. g Box The Save As command saves the active current data to a new file name Enter the desired name in the File Name field Two different file types are available validation files val used for storing the data in binary files and ASCII files txt used for exporting the data Select the desired file type from the Save As Type drop down list Use the Save In window to select the location where the file should be saved For details about the Save As command refer to Section 4 4 2 7 Save As A 2 5 Print Use the Print command to print data from a method validation file Executing the Print command opens the Print dialog box displayed options vary based on the installed printer driver The Print command can also be executed by clicking the Print toolbar button Print BEI m Printer Name HP LaserJet 474M Plus New Properties Status Ready Type HP Lasenet 474M Plus PS SSI DOCUMENTHP4 SSI Where MIST Comment T Print to file m Print range Copies All Number of copies fi Pages from l to pi BD F Gollete t 2 ila C Selectior Cancel Figure A 6 Print Dialog Box Use the Print Range option to specify the range to be printed The All selection prints all pages in the file Specific pages can be printed by selecting the Pages option and entering the desired page numbers Use the Number of Copies field to select the number of copies to be printed TOC VCPH CPN 351 A 2 6 Print Pr
223. g box is displayed Add event log x Choose an item Administration General Operation Create Edit Data C HAW Settings Maintenance Error Comment 250 characters at most Figure 3 5 Add Event Dialog Box Select one of the items in the Select Item array and then enter a comment in the Comment text field If the Comment text field is left blank an error message is displayed and the comment is not added to the Event Log TOC VCPH CPN 3 2 Instrument Setup and System Properties 3 2 1 System Information Window 3 2 Instrument Setup and System Properties y This section describes the Instrument Setup Wizard which is used to configure new systems This section also describes procedures for viewing the properties of and removing previously configured systems The TOC Control V Instrument Setup Wizard is used to enter properties for a new system Access the Wizard by double clicking the New System icon in the TOC Control V main window Multiple instruments can be configured for the TOC Control V software system by entering information into the series of Wizard screens Use the Back and Next buttons to move among the various Instrument Setup Wizard windows 3 2 1 System Information Window The System Information window of the Instrument Setup Wizard is used to enter basic system information Instrument Setup Wizard_ System Information O O lt lt lt Setup W
224. g box is displayed Sample Run Calibration Curve Figure 4 191 New Dialog Box 3 Double click the Calibration Curve icon The Calibration Curve Wizard opens The System Information window of the wizard page 1 is displayed Calibration Curve Wizard Page 1 System Information Cal Pts Analysis Cal Type System Figure 4 192 Calibration Curve Wizard Page 1 System Information 4 From the System drop down list select the system that was configured with the Manual Injection Kit during setup TOC VcPHICPN W 229 230 4 5 Application Operations 4 5 2 Gas Sample 5 10 11 12 13 14 15 16 TOC VCPH CPN Analysis Select the desired options on pages 2 and 3 of the Calibration Curve Wizard which list calibration curve type and analysis information settings respectively Enter the name of the new calibration curve in the text box at the bottom of page 3 of the wizard Note Select the settings described in Section 4 2 Setting General Mea surement Parameters Enter the desired number of injections on page 4 of the Calibration Curve Wizard Calibration Measurement Parameters Enter the injection volume on page 5 of the Calibration Curve Wizard Calibration Points List Note An injection volume is displayed automatically The displayed value is based on the volume of the last injection that was per formed using the sample injector This value can be changed by the user a
225. g from the slider and remove any obstruction that may be adhering to the opening at the tip of the sample tubing Unacceptable Unacceptable Appropriate oblique spray scattered spray Figure 5 38 Sample Injection Patterns from Sample Tubing Ensure that the tip of the tubing does not protrude beyond the bottom surface of the slider The O ring or other seal parts will be scratched if the tubing protrudes resulting in gas leaks The sample is not properly injected unless the tip of the tubing extends into the depression in the bottom of the slider Check the state of the injection for TC analysis by looking through the TC combustion tube while it is attached to the instrument The sample injection tubing can be detached from the slider and water can be injected for inspection using the functions available in the Instrument gt Maintenance gt Mechanical Check screen 280 TOC VcPHICPN 5 7 Troubleshooting 5 7 2 Troubleshooting Salt or other substances adhering to the tip of the tubing after rinsing can allow large droplets of sample to remain on the tip of the tubing after injection A deformed tip on the sample injection tubing a beard like protrusion for example may cause the sample to be injected obliquely In either case reproducibility is adversely affected and the sample injection tubing should be replaced Another option available only if there is sufficient length of tubing remaining is to use a sharp cutting tool at a 90 angle
226. g the autosampler in NPOC measurement there is a danger that following measurement volatilization of acid in the sample could cause corrosion of the autosampler Do not switch off the power to the instrument Do not select Shutdown 120 TOC VCPHI CPN Reference 4 3 Measurement Procedures and Tutorial 4 3 3 Ending Measurement Auto Restart The Auto Restart function is used to shut down the instrument and then restart it at a specified time Selections are made for the date and time that measurement will next be performed as well as for the instrument restart settings After shutting down the instrument the carrier gas flow and power to the furnace are automatically turned off Approximately one hour before the restart time the furnace and the carrier gas will automatically be turned on to allow the instrument to achieve a Ready state by the restart time 7 Select Auto Restart in the Standby window 2 Select the appropriate instrument restart settings TC furnace carrier gas ozone generator and set the restart date and time If a check is placed in the box beside a unit the furnace power remains on and the carrier gas continues to flow In order to have the power turned off automatically do not place a check mark in any of these boxes 3 Click the Standby button Power to the instrument is automatically switched off and will be automatically switched on approximately one hour before the restart date and time Using Auto Res
227. gap If the gap is too large loosen the nut at the top of the compression fitting and pull the combustion tube upwards Since the TC combustion tube is inserted into the compression fitting pulling up on the combustion tube shortens the insertion length and ultimately lowers the compression fitting assembly When almost no gap remains firmly tighten the nut at the top of the compression fitting Note The sample rapidly vaporizes in the combustion tube when injected in large quantities with a gap present between the bottom most part of the compression fitting and the base of the instrument The pressure increases resulting in a separation at the connection between combustion tube and sample injector Installation for the N Type 1 2 Push the capillary part of the catalyst filled combustion tube downward into the center of electric furnace about 22mm diameter Apply an extremely thin layer of the provided high vacuum silicone grease to the outside of the combustion tube tip part in contact with O ring Note Use as small amount of silicone grease as possible Absolutely no grease should be applied to the interior of the combustion tube Insert the silicone grease coated tip of the combustion tube into the opening at the bottom of the sample injector Note Connect the drain tubing exiting the slide injector to the Y fitting of the system drain line Connect the tubing at the bottom of the combustion tube as shown in Figure 4 7
228. h To support catalyst 2 included 630 00557 Quartz wool To support catalyst 1g 630 00996 TOC high sensitivity catalyst 638 41308 01 Cooling coil 630 00999 CO absorber 630 00992 Halogen scrubber 036 11209 84 O ring 4D P 10A For slider 5pcs 036 11408 84 O ring Teflon P10 For slider 5pcs 036 11222 84 O ring 4D P22 For IC reaction tube 5pcs 036 11219 84 O ring 4D P20 For TC reaction tube 5pcs 035 62994 03 Sleeve set 6F T 042 00405 11 IC reaction solution supply pump head 630 00635 01 Potassium biphthalate 25 g 630 00962 01 Sodium carbonate 25 g 630 00963 01 Sodium bicarbonate 25 g 046 00044 11 Membrane filter 017 30812 01 Silicone grease H V G 630 08913 01 Chart paper 10 rolls 638 60074 Ceramic fibers 631 20265 8 port valve rotor 638 59213 01 Plunger tip 638 92206 01 Consumables set Refer to Table 6 13 for contents TOC VCPH CPN 6 3 8 6 6 Consumable Parts List PC Hardware Requirements Table 6 12 e Consumable Parts List 2 TOC VCPN Part Number Part Name Comment 638 41323 Combustion tube in case 638 60116 TOC regular catalyst 630 00105 01 Platinum mesh To support catalyst 2 included 630 00557 Quartz wool To support catalyst 1g 630 00999 CO absorber Contains 500mL 630 00992 Halogen scrubber 036 11209
229. h accommodating a different vial size The ASI V permits random access of vials in the vial rack Vials are measured according to the sequence set in the Sample Table Editor thus enabling analysis to start from any position number in the vial rack and for analysis to occur in non sequential vial positions TIP When samples are to be sparged using the optional external sparge kit analysis is performed more efficiently if the vials are placed in sequential rack positions without gaps This allows a vial to be sparged while an adjacent vial is being measured Installing the Vial Rack Install the rack using the following procedure 7 Insert the vials into the vial rack and place the rack on the ASI V turntable 2 Place the cover over the turntable Note During analysis the turntable must be covered The ASI V will not operate if the turntable cover is not detected 74 TOC VCPH CPN 4 1 Analysis Preparation 4 1 16 Sample Preparation 4 1 16 4 High Sensitivity Autosampler Analysis If samples with TOC concentrations of 100ug L or less such as purified water or ultra pure water are measured using an autosampler the following precautions associated with high sensitivity analysis must be considered Refer to Section 4 1 15 1 High Sensitivity Analysis for additional information 1 2 3 4 5 6 7 NPOC analysis is recommended TOC TC IC analysis tends to have a greater variation in measured values
230. h the sample cap during sparging Note Vials to be used for the first time should be washed with laboratory detergent and then rinsed well with water 4 1 16 2 Filling Vials with Sample In most cases vials can be placed in the ASI V turntable and analyzed without being sealed Vials must be sealed in the following situations 1 sparging with the autosampler for NPOC analysis 2 measuring acidic samples 3 IC analysis 4 POC analysis 5 low concentration samples as a guideline less than 10mg L 6 alkaline samples pH 7 or higher 7 samples that contain volatile organic hydrocarbon components 8 alarge number of samples to be measured 9 standard solutions 72 TOC VcPHI CPN 4 1 Analysis Preparation 4 1 16 Sample Preparation In situations 1 and 2 above corrosion of the instrument may occur due to spattering of sample which contains acid If the samples are left in the autosampler following measurement there is danger that the autosampler may be subjected to corrosion due to the volatilization of acid In situations 3 through 9 results may be affected by either volatilization of the TOC components in the sample or contamination from substances that absorb CO from the atmosphere If aluminum foil is used to cap the sample vial for NPOC or acidic sample measurement there is a danger of acid volatilization through the hole caused by insertion of the needle Do not use aluminum foil to cap the vials Meth
231. he IC Injection Port Septum Cushion O Ring The septum used with the IC injection port is a consumable item The septum typically can be used for 200 or more injections however it should be replaced if there is deterioration in reproducibility or peak shapes Part number for replacement cushion O ring 20 pcs P N 630 01559 01 Replacement Procedure 1 2 J TOC VCPH CPN Loosen and remove the injection port bushing Remove the old septum and insert a new one Replace the bushing and tighten it 4 5 Application Operations 4 5 2 Gas Sample Analysis N caution IC reaction solution may spatter close to the injection port septum and injection port however this poses no problem during analysis When replacing the septum wipe away any liquid taking care to avoid contact Gas tight Syringe For analysis use a needle length of 50mm or a 2 inch gas tight syringe The following gas tight syringes are available from Shimadzu Order replacement syringes as necessary Table 4 8 Gas Tight Syringes Option Part Name P N Capacity Gas tight syringe set 25uL 638 60733 02 25uL Gas tight syringe set 50uL 03 50uL Gas tight syringe set 100uL 04 100uL Gas tight syringe set 250uL 05 250uL Gas tight syringe set 500uL 06 500uL Gas tight syringe I1mL 046 00026 02 ImL Gas tight syringe set 5mL 03 5mL Gas tight syringe set 10mL 04 10mL Set comprises one replacement gas tight syringe needle
232. he oven 6 Using the compression fitting joints restore the tubing connections to their original condition TOC VCPH CPN 241 5 2 Periodic Inspections 5 2 3 Washing Replacing the Combustion and Carrier Gas Purification Tubes 5 2 3 Washing Replacing the Combustion and Carrier Gas Purification Tubes The inner surface of the combustion tube devitrifies becomes crystalline in texture and turns white when it reacts with salts contained in the samples The tube can continue to be used in this condition until it breaks or cracks During the catalyst washing or replacing process wash the interior of the combustion tube and carrier gas purification tube with 1 2 hydrochloric acid 1 part concentrated HCl and 2 parts water to remove the contaminants and accumulated salts Rinse with water dry and then reuse the tube s 5 2 4 Replacing the High Purity Air Cylinder A 47 liter cylinder of high purity air used as the carrier gas will last for approximately three months using the H Type instrument and two months using the N Type e Replace the cylinder when the residual pressure diminishes to a few hundredkPa Do not wait until it is completely empty e When connecting a new cylinder clean the connections thoroughly After connecting the cylinder do not allow dust or other matter to enter the instrument e Keep a spare cylinder available at all times 5 2 5 Replacing the CO Absorber Once a year replace each of the CO absorbers
233. heat closed containers may explode Emits toxic fumes under fire conditions SECTION VII ACCIDENTAL RELEASE MEASURES Absorb on sand or vermiculite and place in closed containers for disposal Ventilate area and wash spill site after material pickup is complete Evacuate the area Wear self contained breathing apparatus rubber boots and heavy rubber gloves SECTION VIII SPECIAL PRECAUTIONS AND COMMENTS The above information is believed to be correct but does not purport to be all inclusive It shall serve only as a guide Shimadzu shall not be held liable for any damage resulting from handling or contact with the above product Users should make their own determinations regarding the suitability of this information for their particular purposes TOC VCPH CPN 34 342 6 9 Material Safety Data Sheets 6 9 10 Sodium Bicarbonate 6 9 10 Sodium Bicarbonate Shimadzu Scientific Instruments Inc 7102 Riverwood Drive Columbia MD 21046 Control No Tel 1 800 477 1227 Date MATERIAL SAFETY DATA SHEET SECTION I PRODUCT IDENTIFICATION CAT NO 630 00963 01 CAS NO 144 55 8 NAME Sodium Bicarbonate 100 OTHER NAME Baking Soda SECTION II PRDUCT USE This product is specifically for use as a catalyst in the TOC 500 TOC 5000 and TOC 4000 series of TOC analyzers Refer to the appropriate instruction manual for directions on proper use SECTION II PHYSICAL DATA Melt Boil Density Vapor Vapor Evapor
234. hens AOR edna 328 6 8 6 1 Connecting the Power and Installation cceececesseeteeeeeeeeeens 328 6 8 6 2 Connecting Ozone Source AIL eeeecesceeeeseeeseeseceseeseceseneeneenseens 329 6 8 6 3 Connecting Gas Exhaust Tubing 000 00 cceececceeseessesceeeeeseeeeneenseens 332 Material Safety Data Sheets ccccccsccescessceseeseecseeeecseeeeseeeseeeeeeseeenes 333 6 9 1 Hydrochloric Acid HCH sencan e 333 6 9 2 Phosphoric Acid EA E ee cece dei a cteos ed basecdeceg os asttncas tess hades ede 334 6 9 3 CO Absorber CA OH KOH NAOH soda lime ue eee ees 335 6 9 4 Lithium Hydroxide monohydrate 00 0 ce cecceseeseceeceseeneeeeceeeeeeeeeeeneeeneenees 336 6 9 5 Halogen Scrubber vcs onien nreti E E E ERRAR eevee 337 e KO Quartz L010 AEEA OE NE EATER NE ETETE 338 6 9 7 High Sensitivity Catalyst cc ccceccccseseeseceseeseeeeceseeeceeceeeeeeeaeeeeeeaeeeseenees 339 6 9 8 Normal Sensitivity Catalyst ccceceesccsscesecesceseeesceseeeecenseseeceeceesaeeeenaees 340 6 9 9 Potassium Nitrate ss 0ci cA ccc csscesccdecsads ec dusdisaced duqees cds West T 341 6 9 10 Sodium Bicarbonate ccccccccsecseesecsecesececeeceseeeeceseeeeceseeeeeeaeeaeeeeeseeenees 342 69 11 Sodium Carbonate s20 0 3 5ce n een Oe R 343 6 9 12 Potassium Hydrogen Phthalate ec ceceecececeeseeeceseeeeeeseeeseceeeaeesseneees 344 PEI 2 WiatebiFici EE OE E N cbvesettus ney cuvelnivas cece covets 345 TOC VcPHI CPN Xix Table Of Contents Appendix
235. his option e Calibration File Name TCTutorial cal Calibration Curve Wizard Page 3 Analysis Information a Figure 4 47 TC Calibration Analysis Information 6 Click the Next button Page 4 of the Calibration Curve Wizard is displayed Notice that the No of Injections displayed matches the number entered when setting the default measurement parameters for the Sample Table in Step 3 of the tutorial 102 W TOC VcPHICPN iii Enter the TC calibration standard concentration range values of 0 to 100ppm Enter 3 as the number of calibration points Calibration Curve Wizard Page 4 Calibration Measurement Parameters la pai a pa E a al EE w a Figure 4 48 TC Calibration Standard Information amp Click the Next button Page 5 of the Calibration Curve Wizard displays the Calibration Points List 9 Notice that the Calibration Points List was completed based on information entered on the previous Wizard pages To make any changes select a row and click the Edit button Calibration Curve Wizard Page 5 Calibration Points List 01000 0 1000 0 1000 Figure 4 49 TC Calibration Points List 70 Click the Next button Page 6 of the Calibration Curve Wizard which specifies peak integration parameters is displayed 77 Settings can be made on this page to delay the peak detection start time or extend the pea
236. horough washing with water or sample is performed prior to use until no TOC is present in the eluate Perform heat treatment on the filter for glass fiber filter paper TOC Analysis of Stirred Samples To perform intentional analysis of suspended solids the sample is stirred using a magnetic stirrer or other instrument Simple stirring can lead to extreme variability in the results because the suspended solids contained in the sample may not be distributed uniformly throughout the suspension TOC Analysis after Homogenization of the Sample If the application requires that the suspended solids be included in the analysis it is critical that the solids are as fine as possible and distributed uniformly throughout the suspension Accurate and reproducible TOC results can be obtained when the sample is highly homogenized to form uniform micro size particles Homogenizing systems may include a mixer to perform high speed stirring or an ultrasonic system These are homogenizers with outputs of 150 300W Typical washing sonicators do not have sufficient output for this use Ultrasonic systems are generally more powerful though performance varies with the type of suspended solids Uniform suspension cannot always be achieved with all types of suspended solids Sludge like materials are comparatively easy to process while fibrous materials are more difficult 4 1 Analysis Preparation 4 1 15 Sample Preparation 4 1 15 5 Handling Samples Containi
237. hown below Open ix Look in ada O H El c a E File name Tutorial Files of type Sample Tables t32 z Cancel Ver 00 00 01E User System System TC TN Date of creation 07 12 01 12 01 24 PM Sw Serial nn TCF 1nnni Figure 4 91 Open Dialog Box TIP The Open dialog box can also be displayed by clicking the Open File button on the Toolbar Table 4 2 displays the types of files that can be opened using this function No other file types should be opened using this menu command Table 4 2 e Acceptable File Types for Open Function File Extension Description 32 Sample Table met Method cal Calibration Curve tpl Control Sample Template trd Data Profile The opened file replaces the currently displayed table or function depending on the type of file selected Dialog Box Options Description File name Enter the name of the file to be opened Look in Find the file to be opened by choosing the appropriate folder or accessing other directories The selected file will appear in the File name text box Files of type Select the type of file from the drop down list Choose only files of type t32 when opening a Sample Table Open button Opens the selected file Cancel button Aborts the Open operation TOC VcPHICPN 143 144 4 4 Sample Table Editor 4 4 2 File Menu 4 4 2 5 Close 4 4 2 6 Save TIP The Close command is used to close the current wi
238. ibration Curve Results Evaluate the TN calibration curve results by placing the cursor in the second row of the Sample Table which contains analysis information for the TN calibration Then follow Steps 2 through 5 in the procedure listed above for evaluating the TC calibration curve results TOC VCPHICPN 115 4 3 Measurement Procedures and Tutorial 4 3 2 Tutorial Viewing Peak Profiles View peak profiles by placing the cursor in the desired row of the Sample Table and either selecting Sample Window from the View menu or clicking the Sample button E on the toolbar The Sample Window is displayed this is the same window we used to observe the real time injections 2 To view the peak profiles for all injections in a Sample Table row select All Peaks from the drop down list at the top of the graph All peak profiles for the selected row are displayed in the graph TIP _ When All Peaks is selected from the drop down list at the top of the graph clicking in another row of the Sample Table will automatically update the Sample Window display with the peak profiles for that row 3 To view the peak profile for individual injections click in the appropriate row of the Injection Table and select Current Peak from the drop down list at the top of the graph Evaluating the Sample Results 7 Place the cursor in the third row of the Sample Table which contains analysis information for the sample 2 Examine the concentration res
239. ical Lines Prints vertical lines in the table Horizontal Lines Only Black and White First Rows then Columns First Columns then Rows Vertical Horizontal Prints horizontal lines in the table Prints only in 2 colors without gray backgrounds or other colors Prints rows first followed by columns when more than one page is printed Prints columns first followed by rows when more than one page is printed Prints the table on the vertical center of the page Prints the table on the horizontal center of the page 354 OC NP SSS Miscellaneous Tab Page Setup Figure A 11 Page Setup Window Miscellaneous Tab The Miscellaneous tab displays a list of format items for the report as described below Setting Item Description Margins Use the spin controls to enter the page margins in mm Footer Page No Select this option to print the page number in the footer of each page Header Organization Select this option and enter the name of the organization in the text box to print the organization name in the page header Logo Select this option to print a bitmap in the page header Use the Browse button to select the bitmap file Date Time Select this option to print the current system date and time in the page header Operator Select this option to print the current user name in the page header A 2 9 Exit Select Exit to close the Method Validation application If an active file con
240. icates only Step 4 Analyze the standards The results are saved in a cal file Step 5 Select Method Validation from the Tools menu in the Sample Table Editor The Method Validation main window is displayed Step 6 Select the Validation Strictly Following DIN from the Options menu Step 7 Select Open from the File menu Step 8 Select cal from the file type drop down list Step 9 From the list of file names select the cal file where the measurement data was saved Then select OK Step 10 The calculations are automatically performed and the validation data displayed Step 11 Select Save from the File menu assign a file name in the dialog box and select OK The validation data is saved with a va file name extension When the Validation Strictly Following DIN option is enabled a check mark is displayed in front of the menu item After selecting this option a confirmation message is displayed Meth al AN Changing the calculation parameter requires recaculation of the results and regresion curve Recalculate now J Figure A 22 Confirmation Message for Validation Strictly Following DIN 38402 Select Yes to execute recalculation The calibration curve and result sections of the Method Validation window are updated accordingly TOC VCPH CPN A 6 Help Menu About Meth Val Use the About command to view copyright and version information LLL TOC VerHiceN fy 365 366 EE TOC VcPHicPN nnn Appendix B Contr
241. id drain vessel water and humidifier water each day before starting the instrument 5 1 1 Checking Dilution Water Verify that the dilution water volume is sufficient for analysis If necessary replenish the dilution water as described in Section 4 1 6 Preparation of Dilution Water 5 1 2 Checking Acid Verify that the acid volume is adequate for analysis If necessary replenish the acid as described in Section 4 1 7 Acid Preparation Any container such as a small mouth glass 1 liter bottle can be used 5 1 3 Checking Drain Vessel Water Level MSE Overflow Tube Drain Vessel y Pure Water Figure 5 1 Drain Vessel Water Level Verify that the water level in the drain vessel inside the instrument is within 10mm of the overflow tube on the side of the drain vessel Replenish as necessary with purified water ion exchange water Reference Refer toSection 4 1 4 Water Supply to the Cooler Drain Container for details on adding purified water Confirm that the carrier gas does not leak from the tip of the drain tubing when the flow rate is 150mL min 236 TOC VCPH CPN 5 1 4 Checking Humidifier Water Level Supply Port Pure Water Lo Mark Figure 5 2 Humidifier Water Level Verify that the water level in the humidifier is above the Lo mark If the level is below the Lo mark replenish by adding purified water through the water supply port on
242. ientific Instruments Inc 7102 Riverwood Drive Columbia MD 21046 Control No Tel 1 800 477 1227 Date MATERIAL SAFETY DATA SHEET SECTION I PRODUCT IDENTIFICATION CAT NO 630 00996 00 CAS NO N A NAME High Sensitivity TC Catalyst OTHER NAME Platinum on Quartz Wool SECTION II PRDUCT USE This product is specifically for use as a catalyst in the TOC 500 TOC 5000 and TOC 4000 series of TOC analyzers Refer to the appropriate instruction manual for directions on proper use SECTION II PHYSICAL DATA Melt Boil Density Vapor Vapor Evaporation Odor Color Phase Water Point Point Pressure Density Rate Solubility N A N A N A N A N A N A N A Grey Fibrous Solid N A SECTION IV HAZARDS IDENTIFICATION FLAMMABLE Possible sensitizer Keep away from sources of ignition NO SMOKING Take precautionary measures against static discharges Keep container tightly closed and in a well ventilated place SECTION V TOXICITY DATA ACUTE EFFECTS May be harmful by inhalation or ingestion May cause eye irritation May cause skin irritation Material may be irritating to mucous membranes and upper respiratory tract Prolonged or repeated exposure may cause allergic reactions in certain sensitive individuals EXPOSURE CAN CAUSE Coughing chest pains difficulty in breathing To the best of our knowledge the chemical physical and toxicological properties have not been thoroughly investigated SECTION VI HEALTH HAZARD
243. igure 5 14 Replacing the Pump Head of the Rinse Pump TOC VCPH CPN 253 254 5 4 8 Port Sampler OCT 1 Maintenance 5 3 3 Replacing the Pump Head of the Rinse Pump 5 4 8 Port Sampler OCT 1 Maintenance 5 4 1 Replacing the 8 Port Valve Rotor The OCT 1 uses a fluororesin 8 port valve rotor The valve rotor may become worn or scratched after prolonged use due to the suspended particles in the samples This wear eventually causes leaks from the 8 port valve The following symptoms are associated with leaks from the 8 port valve and indicate that it is necessary to replace the rotor e Droplets of liquid around the 8 port valve especially around the upper shaft e Decreased analysis reproducibility e Presence of bubbles in the TOC V syringe If the leak is large sample remaining in the tubing after the syringe has been filled may flow back into the sample container This is most likely due to a sample tubing or flange connection problem N caution Switch OFF the power before replacing to the 8 port valve rotor Replacement Procedure 7 Shut down the TOC V unit and switch OFF the power Reference Refer to Section 4 3 3 Ending Measurement for details on shutting down the TOC V unit 2 Remove the 4 screws at the top of the 8 Port Sampler and take OFF the cover 3 Verify that the O mark on the 8 port valve cover is directed toward port No 1 Note Ifthe O mark is not directed toward port No 1 the instrument was
244. ill be diluted and the syringe will then be washed with the diluted sample Parameter 4 4 Sample Table Editor 4 4 5 Insert Menu Description Auto Dilution Sparge Time Acid Addition Multiple Injections Use blank check area Auto correction of inj vol and dilution Enter a dilution factor for the sample The instrument will automatically dilute the sample by this factor and the result will be multiplied by the factor to obtain the final concentra tion The default Auto Dilution value is 1 Enter the sparge time Enter the desired quantity of acid to be added This value is expressed as a percent of the sample volume and is available only for NPOC or related analyses Select this option to enable the syringe to draw up a single sample aliquot with a volume equal to that required for all injections of the sample When this option is not selected the syringe will draw up a separate sample aliquot for each injec tion Selecting this option reduces analysis time Select this option to subtract the blank check area from the measured area of the sample This option is only available for TC and NPOC analyses that use the high sensitivity catalyst Select this option to enable the instrument to automatically adjust the injection volume and dilution factor when the peak height for the initial injection exceeds full scale After the adjustment measurement will be repeated TOC VCPH CPN 189 Sample Wiza
245. ilution Water cccceccececeseeescesceesceeeeeeeesecseesaecaeenseeneens 50 41 7 Acid Preparation ssie whioniessigeaeeants eoe nt tess ai teaser 51 4 1 8 Installation of the CO Absorber eee ceceeceseneeeeceecneeseeeeesecaeeeessceaeeeseres 52 4 1 9 Adjusting Sparge Gas Flow Rate cc ccccceesecseceeceteeeecesceeeeeeeeeeeeeeeaeeeeenees 53 4 1 10 Installing the Suspended Solids Kit cece eeeeseesseeeeenseseeceeeseecseeeseeteeneens 54 4 1 11 IC Analysis Preparations morenen o E o E E E R 56 4 1 12 Preparation for POC analysis ccccecceeseecesseececeeesecaeenaecseceseceeeeneeneeees 58 4 1 13 TN Analysis Preparations sseisensein ieina 59 4 1 14 Preparation and Storage of Standard Solutions seseseeeeseeeeeeseereerrereeseee 60 4 1 14 1 Preparation of Standard Solutions sesesseesesseeessesessesresessesessrsesses 60 4 1 14 2 Storage of Standard Solutions ccceccecseeseesecseceseeteceeceseeeeeseeeeeeees 62 4 1 15 Sample Preparation cccccecsecscesseeseceeceseceeceeeeeceeceseeseecaeeeeecseseaeeaeenseeseens 63 4 1 15 1 High Sensitivity Analysis ccceceescesceesceceeeecsecsseeseceeceeensenseeereess 63 4 1 15 2 TC Blank Check Analysis cceecceceseeecsseeseceseeseeeeceteeeeeseeeereess 66 4 1 15 3 Pretreatment for IC Removal Sparging ccceccseeeeeeeeeeeeeereees 68 4 1 15 4 Analysis of Samples Containing Suspended Solids cece 69 4 1 15 5 Handling Samples Containing Acids Bases or Salt
246. in 4 4 Sample Table Editor 4 4 9 Options Menu Parameter Description Max SD Enter the default maximum standard deviation that is accept able for the injections If this value is met no additional injections are required However if both this value and the Max CV value are exceeded the samples are automatically reinjected up to the maximum number of times specified in the No of Injections field The SD Max field is disabled if the No of Injections is 1 or if the minimum is equal to the maximum Max CV Enter the default maximum coefficient of variation that is acceptable for the injections If this value is met no addi tional injections are required However if both this value and the Max SD value are exceeded the samples are automati cally reinjected up to the maximum number of times speci fied in the No of Injections field The CV Max field is disabled if the No of Injections is 1 or if the minimum is equal to the maximum 4 4 9 3 Display Settings gt Display Font The Display Settings gt Display Font function is used to select font options for both the general screen display such as in the Sample Table and Print Preview screens and printed reports Select a font type style size and color from the lists in the Font dialog box A preview of the font appearance is displayed in the Sample field Font style Size Regular 8 Cancel Modem O Monotype Corsiva T MS Outlook MS Sans Serif MS Serif O
247. in the New dialog box Calibration Curve Wizard Page 1 System Information Calibration Curve Wizard Page 1 System Information Cal Pts Analysis Cal Type Figure 4 76 Calibration Curve Wizard Page 1 System Information Parameter Description System Select the system to be used User Displays the user name This field cannot be changed Date of Creation Displays the current system date and time This field cannot be changed Comment Enter a comment 512 characters maximum LLL TOC Vc lm 127 128 4 4 Sample Table Editor 4 4 2 File Menu Calibration Curve Wizard Page 2 Calibration Curve Type The Calibration Curve Type window is used to specify the calibration curve type Calibration Curve Wizard Page 2 Calibration Curve Type x c Calibration points are distributed uniformly over the concentration range Edit calibration points manually Calibration curve according to DIN 38402 P 51 Calibration curve according to USP EP Calibration using automatic dilution Div Standard Solutions Fixed Dilution Dilution 1 Div Standard Solutions auto correction of dilution factor g Dilution from Standard Solution Enter the calibration curve type Calibration points can be modified later lt Back Cancel Figure 4 77 Calibration Curve Wizard Page 2 Calibration Curve Type Calibration Curve Wizard Page 3 Analysis Information Parameter Description
248. inage liquid Avoid touching or spilling these liquids 316 TOC VCPH CPN 6 8 Installation 6 8 4 Installing the Autosampler 6 8 3 5 PC Cable Connections This section describes the procedure for connecting the TOC V to the PC using the supplied RS 232C cable Procedure 7 Insert the supplied RS 232C cable into the RS 232C 1 connector on the back of the TOC V and tighten the retaining screws on both sides Figure 2 4 Rear View 2 Insert the plug at the other end of the RS 232C cable into the RS 232C connector of the PC and tighten the retaining screws on both sides 6 8 4 Installing the Autosampler This section describes procedures for installing the ASI V autosampler Positioning the Autosampler The autosampler is placed to the left of the TOC V as shown in Figure 6 8 Installing the Autosampler Figure 6 8 Installing the Autosampler Note Keep the distance between the autosampler and main unit to a minimum to allow a free range of motion of the autosampler If the autosampler tubing becomes stretched taut it may impede the movement of the autosampler arm resulting in operation errors and damage Removing the Shipping Screw The ASI arm is secured with a shipping screw to prevent damage during shipment Before connecting power to the instrument remove the ASI cover to access the shipping screw which is located on the retaining bracket Remove the shipping screw and re
249. indow and detach the window cover by pulling downward 5 Install the tubing clamp Needle Replacement Window Sample Catcher Figure 6 10 Tubing Installation 6 Install the bushing at the end of the sample tubing to the Number 2 port of the TOC V sample injector 8 port valve TOC VCPH CPN 319 320 6 8 Installation 6 8 4 Installing the Autosampler 7 Draw the sparge tubing out through the joint and connect the sparge tubing Sparge Tubing External Sparge Kit V H lt L External Sparge Unit S Advance Sparge Sampling Needle Peo Tubing Installation Label we Sparge Kit Sparge Tubing External Sparge Kit y 5 l lt Da N ASI V Cover Installation figure using the anvance sparge needle and the sampling needle Figure 6 11 Installing the External Sparge Kit Note Do not use the flow controller knob to turn off the sparge gas flow Installing the Needle This section describes installation of the ASI V needle There are two types of needles the sample needle same as the sparge needle and the coaxial needle which is a combined sample sparge needle When install
250. iners that can be used with the 8 Port Sampler It is only necessary that the containers be placed so the sample tubing from the various ports can be inserted directly into the containers Note Wash all sample containers with an appropriate laboratory detergent and rinse them thoroughly with water before using them for the first time Loading the Sample Although it is possible to perform measurement of a sample using the 8 Port Sampler while the container open in the following situations it is necessary to seal the sample container 1 When performing IC measurement 2 When performing POC measurement 3 When performing measurement of low concentration samples e g 10 mg L 4 When performing measurement of alkali samples of pH 7 or higher 5 When performing measurement of samples containing volatile organic carbon compounds 6 When the number of samples is so great as to require a long measurement time 7 When performing measurement of standard solutions Note Ifthe sample container openings are not sealed in the situations listed above measurement values may be influenced by such factors as absorption of atmo spheric CO contamination with carbon containing substances and evaporation of TOC constituents from the samples Sealing the Sample Containers Sample containers may be sealed using commercial sealing films such as Parafilm It is also possible to pierce the lid of the container and insert the sample tubing in
251. ing of Calibration Curves Shift to Origin The shift to origin function is used when the amount of TC and IC or TN in the pure water used for standard solution preparation cannot be ignored with respect to the standard solution concentration A correction must be made by shifting the calibration curve in a parallel fashion so that it passes through the origin This corrects for the TC and IC or TN concentration in the water used for standard solution preparation An example of a situation in which the shift to origin function is useful is described below When water containing 0 5mg L TC is used to prepare a 10mg L TC standard solution the actual TC concentration in the standard solution will be 10 5mg L 0 5mg L from the water 10mg L from the standard solution The 2 point calibration curve generated using such a solution is shown by the solid line in Figure 6 2 Shifting of Calibration Curve If this curve is used without correction the sample analysis values will always be 0 5mg L less than the true value By shifting the calibration curve so that it passes through the origin as shown by the broken line in Figure 6 2 Shifting of Calibration Curve the calibration curve is effectively corrected TOC VCPH CPN 6 2 Analysis Related Technical Information 6 2 3 Calibration Curves A system blank is water that contains absolutely no carbon zero water When measurement of a system blank produces a peak the TC concentrations mea
252. ing the needle remove the needle replacement window cover Refer to Figure 6 11 Installing the External Sparge Kit for the removal procedure TOC VCPH CPN 6 8 Installation 6 8 4 Installing the Autosampler Installation Procedure for the Sample Needle and Sparge Needle 1 2 J A Open the TOC Control V Sample Table Editor and connect the instrument From the Instrument menu select Maintenance gt ASI Needle Change Click the Preparation Start button The autosampler arm moves to the front of the needle replacement window allowing easy access Remove the screw and then detach the needle holder from the arm Insert the needle into the opening in the needle holder Secure the needle by turning the retaining bracket and tightening the screw at the top of the needle holder Note There are two openings the left opening is for the sample tubing and the right opening is for the sparge tubing Retaining Bracket Needle Holder Sample Needle Figure 6 12 Installing the Needle 1 Securely fit the sample tubing or sparge tubing onto the upper end of the needle Note Verify that the bushing is in position to secure the sample tubing onto the sample needle Insert the lower tip of the needle into the needle guide opening thrusting the needle holder into the pin of the arm and then tighten the screw TOC VCPH CPN 32 322 6 8 Installation 6 8 4 Installing the Autosampler 9 Reinstall the needle rep
253. ion File name Enter a name for the file The applicable file extension will automatically be added if it is not entered Save in Select the directory in which the file is to be saved by choos ing the folder or accessing other directories from the drop down list The currently selected directory appears in the Save in text field Save as type Select the type of file from the drop down list A list of avail able file types is listed in Table 4 2 E TOC fy 745 146 4 4 Sample Table Editor 4 4 2 File Menu 4 4 2 8 ASCII Export Options The ASCII Export function is used to export Sample Table data to an ASCII file Open a Sample Table that contains completed measurement data Select ASCII Export from the File menu The Save As dialog box is displayed Refer to Section 4 4 2 7 Save As Enter a file name for the ASCII file to be created and confirm that the Save as type field contains the ASCII file type txt If the entered file name matches a file that already exists a confirmation message is displayed Save As C Program Files Shimadzu Corporation TOC3201 Data test txt This file already exists Replace existing file Figure 4 94 Save As Confirmation Message Click the Yes button to overwrite the existing file and close the dialog box Click the No button to redisplay the Save As dialog box and enter a new file name Select the ASCH Export Options command from the File menu The ASCII Export Options dialog bo
254. ion 5 6 Software Controlled Maintenance Functions Maintenance functions that can be performed using the TOC Control V software are described below These functions can be accessed through the Instrument gt Maintenance menu Zero Point Detection Regeneration of the TC Catalyst Regeneration of the IC Solution Residue Removal Replace Flowline Content Washing Mechanical Check Initialize ASI 8Port Sampler ASI Rack Change ASI Needle Change Change Syringe Blank Gheck History Sparge Gas Valve Adjust Sparaing Flow Rate Wwet Ghem Figure 5 23 Instrument gt Maintenance Menu To access the menu select Instrument gt Maintenance in the Sample Table Editor 5 6 1 Zero Point Detection Use this function to determine the zero point of the syringe Click the Start button to begin the procedure during which a progress bar is active The progress bar becomes inactive after the syringe zero point is determined Click the Close button Zero point detection Zero point detection d di d ddd dood de oe oe oe od Figure 5 24 Zero Point Detection Dialog Box TOC VCPHICPN 261 5 6 Software Controlled Maintenance Functions 5 6 2 Regeneration of the TC Catalyst 5 6 2 Regeneration of the TC Catalyst Use this function to restore the sensitivity and efficiency of the TC catalyst which decrease over time as inorganic substances are deposited on the catalyst surface During the procedure
255. ion IC reaction solution may spatter close to the injection port septum and injection port however this poses no problem during analysis When replacing the septum wipe away any liquid taking care to avoid contact Gas tight Syringe For analysis use a needle length of 50mm or a 2 inch gas tight syringe The following gas tight syringes are available from Shimadzu Order replacement syringes as necessary Table 4 7 e Gas Tight Syringes Option Part Name P N Capacity Gas tight syringe set 25uL 638 60733 02 25uL Gas tight syringe set 50uL 03 50uL Gas tight syringe set 100uL 04 100uL Gas tight syringe set 250uL 05 250uL Gas tight syringe set 500uL 06 500uL Gas tight syringe 1mL 046 00026 02 ImL Gas tight syringe set 5mL 03 5mL Gas tight syringe set 10mL 04 10mL Set comprises one replacement gas tight syringe needle and one plunger TOC VCPH CPN 4 5 Application Operations 4 5 2 Gas Sample Analysis 4 5 2 Gas Sample Analysis If the optional manual injection kit is installed analysis of TC and IC in gaseous samples can be performed by using gas tight syringes or other applicable injectors to inject the gaseous samples Precautions for Gas Sample Analysis L caution Do not inject a large quantity of sample at one time when measuring combustible or explosive gases The combustion tube could break The injection volume should not exceed 10mL e Use caution when measuring co
256. ion and for setting default measurement parameters Figure 4 170 Options Menu 4 4 9 1 General Information The General Information command is used to view information about the system The General Information window contains two tabs one that displays System parameters and one that displays History information Most of the fields in the General Information window are disabled because they were set previously After changing an active field click the OK button to close the window and save the changes or click the Apply button to save the changes without closing the window Click the Cancel button to close the window without saving changes General Information Figure 4 171 General Information Window System Tab System Tab The System tab displays general parameters Parameter Description System Displays the instrument identification File Version Displays the instrument file version User Displays the name of the user who set up the system Date of Creation Displays the date the system was set up Comment Enter a comment 512 characters maximum if desired 21 0 WE TOC VcrHicPN inten History Tab General Information Ej se esto Comment all moniications Shs ones Figure 4 172 General Information Window History Tab The History tab is used to view the system s History Log or to enable the log if it was not previously selected Note Once the History Log is enabled it cannot be disabled
257. ion calculated from the area CV Area Displays the coefficient of variation calculated from the area SD Conc Displays the standard deviation calculated from the concen tration CV Conc Displays the coefficient of variation calculated from the con centration Status Displays the analytical status either measuring or fin ished Vial Displays the vial number for ASI samples only Excluded Displays the exclusion flag denoted as E for user exclusion of the sample ES for exclusion by the system or Not Excluded Modified Displays the modification flag of M if the sample was modified Inj Volume Displays the injection volume for each injection Dilution Factor Calibration curve TOC VCPH CPN Displays the dilution factor used in measurement Displays the calibration curve used 4 4 Sample Table Editor 4 4 4 View Menu 4 4 4 4 Outlier Test The Outlier Test also known as the Grubb test is used to determine whether a selected injection is an outlier The test also determines whether the injection with the highest deviation from the mean value is still within an acceptable range The Outlier Test can only be performed if the sample contains at least three non excluded injections Calculation based on C Cone Area CNV Deviation is not significant Exclude Figure 4 124 Outlier Test Window To perform the Outlier Test open the Sample Window and select the cell
258. ions available vary based on the printer installed Select the paper size and source from the drop down lists and select Portrait or Landscape to change the orientation of the printed pages Click the OK button to save the selections or click the Cancel button to close the dialog box without saving changes A 2 8 Page Setup Use the Page Setup command to select items to be printed and to select options for printing format such as margins headers and footers Page Setup Figure A 9 Page Setup Window Data Tab The Page Setup window consists of several tabs Use the OK button to save changes and exit the Page Setup window Click the Cancel button to exit the Page Setup window without saving changes Click the Apply button to update the parameters without closing the Page Setup window Note On each tab in the Page Setup window certain items are checked selected by default To deselect these options click the item LLL TOC fm 353 Data Tab The Data tab displays a list of items that can be selected for printing Select the desired items and click the OK button Grid Tab Page Setup x e M TAAA C g M Figure A 10 Page Setup Window Grid Tab The Grid tab displays a list of format items for the report as described below Option Description Row Headers Prints row headers in the table Column Headers Prints column headers in the table Print Frame Prints a frame around the table Vert
259. is complete 4 Click the Close button LLL TOC fy 47 48 4 1 Analysis Preparation 4 1 4 Water Supply to the Cooler Drain Container 4 1 4 Water Supply to the Cooler Drain Container The drain container must be filled with water to prevent carrier gas from being released from the drain tubing Procedure 1 2 3 SAMA Remove the rubber cap from the drain container Remove the drain container from the mounting clip Introduce pure water deionized water is acceptable into the cooler drain container up to the level of the drain discharge tube on the side of the container Cap the drain container with the rubber cap Return the drain container to its position in the mounting clip Verify that the cooler drain tube reaches to the bottom of drain container N caution Do not bend drain tubing as this may prevent drain discharge Rubber Cap O Drain Discharge Tube T Drain Tubing ee te Mounting Clip Drain Container Pure Water Figure 4 12 Filling the Cooler Drain Container with Water TOC VCPH CPN 4 1 Analysis Preparation 4 1 5 Filling the Humidifier with Water 4 1 5 Filling the Humidifier with Water The carrier gas must be humidified for high sensitivity analysis to ensure high analysis precision Water is supplied to the humidifier using the following procedure Procedure 7 Remove the cap from the water supply port at the top of the humidifier 2 Introduce water thr
260. ist 2 TOC VCPN Part Number Part Name Comment 638 56135 8 port valve 638 59213 Syringe 638 41337 03 Flared tubing 631 41660 Flared tubing for dilution water 638 65383 Tandem cell in case Table 6 20 Maintenance Parts List 3 ASI V Part Number Part Name Comment 638 41472 01 Needle sampling For 24mL and 40mL Ipc 638 41448 01 Needle sparging For 24mL and 40mL Ipc 638 41449 01 Needle simultaneous sparge type For 24mL 40mL Ipc 638 41450 01 Needle suspended solids kit For 24mL 40mL Ipc 0 8mm 638 42029 04 Tubing set sampling 1 sampling tube with retainer and tube seal 638 42029 05 Tubing set sparge 1 sparge tube with retainer and tube seal 638 42029 03 Tubing set sampling sparge for simultaneous sparge 1 each of sampling and sparge tube for simultaneous sparging with retainers and tube seals 308 TOC VCPH CPN 6 3 8 6 7 Maintenance Parts List PC Hardware Requirements Table 6 21 e Maintenance Parts List 4 OCT 1 8 Port Sampler Part Number Part Name Comment 631 20265 8 port valve rotor Spare rotor 638 41337 03 Flared tubing C Sampling tube for combustion type TOC V 638 41443 03 Common tubing C Main unit OCT 1 connection tube for combustion TOC V 1 unit 638 41443 04 Common tubing C2 Main unit OCT
261. it TN Unit 370mm Ata 440mm Jtsomm Figure 6 3 External Dimensions of Instrument with ASI V 310 TOC VcCPHI CPN 6 8 Installation 6 8 2 Installation Site TOC Main Unit TOC Y Main Unit 635 mm 245 mm somm mm 440 245 mm somm Figure 6 4 External Dimensions of Instrument with OCT 1 8 Port Sampler N caution When lifting the instrument lift from the bottom and at both sides of the instrument Do not lift the instrument by the front access door as this may cause damage 6 8 2 2 Installation Site Conditions Select an installation site with the following conditions A clean environment free of corrosive gases organic gases and dusts Note Contamination in the atmosphere will cause analysis errors especially for high sensitivity analyses e A strong level bench free of vibration and shock e A location with a stable ambient temperature e A location with access to a completely grounded stable power supply N caution Avoid locations where flames are prohibited Some internal parts reach high temperatures and could cause a fire hazard Avoid the following kinds of locations e Locations close to heat sources windows in direct sunlight or in direct contact with drafts from air conditioning vents e Near equipment that generates intense magnetic fields electrical fields or high frequency waves TOC VcPHICPN 311 312 6 8 Installation 6 8 3 Installation Procedure 6 8
262. izard System Information System Instr Serial No User Ersten Date of Creation 07 12 01 11 30 50 Comment f Enter the basic system information cme Figure 3 6 Instrument Setup Wizard System Information Window System Enter a unique name for the system using up to 32 characters A name must be entered before continuing to the next Wizard page If a system with the entered name already exists an error message is displayed requesting entry of a unique name Serial Number Enter the serial number of the TOC V The serial number of the unit is an 8 character number No that is printed on the plate attached to the lower right side of the instrument TOC VCPH CPN 23 User The name of the current user is automatically entered into the User field and cannot be edited Date of Creation The current date is automatically entered into the Date of Creation field and cannot be edited Comment Enter additional system information in the Comment text box The Comment field is optional and can contain up to 512 characters 3 2 2 Options Window The Options window of the Instrument Setup Wizard is used to specify the instrument hardware configuration and attached accessories Instrument Setup Wizard Options Sparge Kit Manual Inj Kit _ 8Port Sampler 1 a Figure 3 7 Instrument Setup Wizard Options Window Oxidation Select Combustion from the drop down list to specify the
263. j TOC ASI 8Port Sampler rm Syringe Pump m Solenoid Valves Combustin r Port Select E a ee oe a tere open open open oom on 7 e a Ser ioe coe coe coe orf 8 4 Reset eee cia eca TC Inj Port Acid Pump cau e a Nese Disin Meas Deen Cose open oen Gpen oe IC Ini Port d dadda Dran Meas Stop Figure 5 31 Mechanical Check Window TOC Tab Syringe Pump Use the buttons to move the syringe pump to the Zero Home or Sparge posi tions Click the Reset button to move the plunger to the highest position Solenoid Valves Use the buttons to open or close the various solenoid valves Different options are available depending on the instrument configuration and oxidation method Port Select Open the line between the syringe and an injection port by clicking the button for the desired port TC Inj Port Specify whether the port should be set to drain or measure by clicking the appro priate button IC Inj Port Specify whether the port should be set to drain or measure by clicking the appro priate button Acid Pump Use the buttons to open or close the IC acid pump lines TOC VCPH CPN 265 ASI 8 Port Sampler Tab Mechanical Check dd fd od od od oo od stop Figure 5 32 ASI 8 Port Sampler Tab of Operation Verification Dialog Box Rinse Use the On and Off buttons to start and stop the ASI flow line rinsing option
264. jections If this value is met no additional injections are required However if both this value and the CV Max value are exceeded the control sample is automatically reinjected up to the maximum number of times specified in the No of Injec tions field The SD Max field is disabled if the No of Injections is 1 or if the minimum is equal to the maximum CV Max Enter the maximum coefficient of variation that is acceptable for the injec tions If this value is met no additional injections are required However if both this value and the SD Max value are exceeded the control sample is automatically reinjected up to the maximum number of times specified in the No of Injections field The CV Max field is disabled if the No of Injections is 1 or if the minimum is equal to the maximum No of Washes Enter the number of times the syringe is to be washed with sample prior to the first injection Note that if the Auto Dilution option was selected the sample will be diluted and the syringe will then be washed with the diluted sample Auto Dilution Enter a dilution factor for the samples The instrument will automatically dilute the control sample by this factor and the result will be multiplied by the factor to obtain the final concentration The default Auto Dilution value is 1 Acid Addition Enter the desired quantity of acid to be added This option is available only for NPOC and related analyses Sparge Time Enter the sparge time TOC V
265. k detection time View but do not change the default setting on the page LLL TOC Vc fm 703 72 Click the Next button Page 7 of the Calibration Curve Wizard is displayed The History function can be enabled on this page of the wizard View but do not change the default setting 73 Click the Finish button The Calibration Curve Wizard closes The TC calibration curve file is now complete and has been saved Creating the TN Calibration File The TN calibration file is created by following the same steps used to create the TC calibration file with the exceptions described below 7 On page 3 of the Calibration Curve Wizard specify the Analysis as TN and enter TNtutorial cal as the calibration file name Calibration Curve Wizard Page 3 Analysis Information x Figure 4 50 TN Calibration Analysis Information 2 On page 4 of the Calibration Curve Wizard enter 0 to 20ppm for the Concentration Range and 3 for the number of calibration points Calibration Curve Wizard Page 4 Calibration Measurement Parameters A NEL Figure 4 51 TN Calibration Measurement Parameters 104 EE TOC VcPmcPn i iii 3 4 4 3 Measurement Procedures and Tutorial 4 3 2 Tutorial Page 5 of the Calibration Curve Wizard should match the following figure Calibration Curve Wizard Page 5 Calibration Points List x Auto Dilution Inj Volume 80 ul Calibration Points No Conc NoofIn SDMas CV Max 1 0
266. k solution is diluted with zero water to prepare standard solutions at the required concentrations Note The TC standard solution reagent need not be potassium hydrogen phthalate Depending on the application other substances are also acceptable e g sucrose etc TOC VCPH CPN 4 1 Analysis Preparation 4 1 14 Preparation and Storage of Standard Solutions Preparation of IC Standard Solution HV 7 Accurately weigh 3 50g of reagent grade sodium hydrogen carbonate that was previously dried for 2 hours in a silica gel desiccator and 4 41g of sodium carbonate previously dried for 1 hour at 280 290 C and cooled in a desiccator 2 Transfer the weighed materials to a 1L volumetric flask 5 Add zero water to the 1L mark 4 Stir well to mix In this instance the carbon concentration of 1000mg L is indicated as 1000mgC L The concentration of this solution is 1000mgC L 1000ppmC and is referred to below as the TC Standard Solution Preparation of TN Standard Solution 7 Accurately weigh 7 219g of special reagent grade potassium nitrate dried for 3 hours at 105 110 C and cooled in a desiccator 2 Transfer the weighed material to a 1L volumetric flask 3 Add zero water to the 1L mark 4 Stir well to mix In this instance the nitrogen concentration of 1000mg L is indicated as 1000mgN L The concentration of this solution is 1000mgN L 1000ppmN and is referred to below as the TN Standard Solution Prepa
267. lacement window cover and tighten the screw Figure 6 13 Installing the Needle 2 Installing the Coaxial Needle 1 2 J A 10 TOC VCPH CPN Open the TOC Control V Sample Table Editor and connect the instrument From the Instrument menu select Maintenance gt ASI Needle Change Click the Preparation Start button The autosampler arm moves to the front of the needle replacement window allowing easy access Detach the needle holder from the arm Insert the needle into the opening in the needle holder Secure the needle by turning the retaining bracket and tightening the screw at the top of the needle holder Install the provided 3 way joint on the top of the needle Connect the sample tubing to the top of the 3 way joint and the sparge tubing to the side of the joint Insert the tip of the needle into the needle guide opening thrusting the needle holder into the pin of the arm and then tighten the screw Reinstall the needle replacement window cover and tighten the screw at the lower left of the cover 6 8 Installation 6 8 4 Installing the Autosampler Installing the Turntable Vial Rack and Cover Installing the Turntable 7 Place the turntable on the ASI V Note There is no distinction between front and rear of the turntable so placement orientation is irrelevant 2 Place the turntable so that the 3 guides on the ASI V pass through the 3 holes at the center of the turnt
268. large the measurements are affected by the changing magnitude of the blank peaks resulting in errors in the analysis values Such errors are especially significant for high sensitivity TC analysis TC Analysis Using New Catalyst Catalyst regeneration should be conducted 1 2 times for TC analysis using new catalyst This reduces the size of the blank peaks Use continuous injections of pure water until the blank peak area becomes small and stable The blank peak magnitude depends on the quality of the water TC impurity concentration and the TC analysis range used for analysis For example a blank peak of 1mg L has little influence on results greater than 100mg L but has a significant influence on results equal to or less than 10mg L Analyses for expected concentrations around 10mg L must have stable blank peaks of 0 5mg L or less For TOC high sensitivity catalyst conduct the TC blank check analysis described in Section 4 1 15 2 TC Blank Check Analysis TN Analysis Using New Catalyst Blank peak magnitude poses no practical problems for TN analysis using new catalyst The blank peaks are fairly small and stable Perform analysis with distilled or deionized water to confirm the size of the blank peaks TOC VCPH CPN 4 1 Analysis Preparation 4 1 1 Catalyst Filling 4 1 1 1 Catalyst for TOC Analysis Either standard or high sensitivity catalyst can be used for TOC analysis The furnace temperature is set to 680 C for TOC analysis
269. le Connections The cable is connected between the main unit of the TOC V and the 8 Port Sampler N CAUTION Confirm that the power to the TOC V main unit is switched OFF before performing this procedure Connection Procedure 7 Remove the 4 screws at the top of the 8 Port Sampler and take off the cover 2 Connect the power and signal cable to the circuit board of the 8 Port Sampler 3 Connect the ground wire of the power cable to the grounding terminal on the circuit board of the OCT 1 4 Pass the cable through the rear panel and replace the cover of the 8 Port Sampler TOC VCPHICPN 325 326 6 8 Installation 6 8 5 OCT 1 8 Port Sampler Installation Rear Panel 8 Port Sampler SighI Cable 8 Port Sampler Power Cable Figure 6 16 Cable Connections TOC V and 8 Port Sampler 5 Connect the power cable to the power receptacle on the back of the TOC V 6 Connect the signal cable to the 8 Port Sampler connection on the back of the TOC V Installing Two 8 Port Sampler Units When installing two 8 Port Sampler units a signal cable standard accessory is connected between 8 Port Sampler and 8 Port Sampler 2 Installation Procedure 7 Remove the covers from both 8 Port Sampler units 2 Connect the signal cable exiting 8 Port Sampler 2 to the connector of 8 Port Sampler 1 8 Port Sampler 2 Fr are lt q S a f Signal Cable 8 Port Sa
270. le Editor and start measurement Refer to Section 4 4 4 1 Calibration Curve Acid addition for NPOC analysis can be performed automatically using the ASI V It is best to perform manual addition of hydrochloric acid for NPOC analysis on the order of 10ug L This is because automatic acid addition pierces the vial seal and allows CO contamination from the air To prevent rinsing of the needle deselect the Rinse option and set the No of Needle Washes field to zero in the Instrument Properties Dialog Box gt ASI Window Refer to Section 3 2 4 ASI Window Even if ultra pure water is used as rinse water the TOC concentration of the rinse water will increase during the time it is exposed For best results do not rinse the needle for analyses on the order of 100ug L Do not use the analysis value acquired from the first sample vial In sample analysis particularly analysis on the order of 10ug L the first sample measured may yield high results When using the optional external sparge kit perform sparging using a sparge gas flow rate of 100mL min As a guideline use sparge times of 5 to 10 minutes for 24 and 40mL vials Increase the gas flow rate or sparge time if sparging is insufficient TOC VCPH CPN 75 76 4 1 Analysis Preparation 4 1 16 Sample Preparation 4 1 16 5 Acid Addition in NPOC Analysis Automatic addition of acid is possible using the autosampler when the optional external sparge kit is installed Usi
271. lect the type of needle that is actually installed in the instrument No of Needle Washes Specifies the number of times the needle will be rinsed after sample injection This operation rinses the outside of the needle using water drawn from the dilution water bottle Rinsing the needle can prevent poor injection quality that results from salt buildup at the tip of the injection tube during sample analysis Such salt buildup is especially problematic when analyzing samples with high salt concentrations 1000ppm or greater Enter a number ranging from 0 to 10 in the No of Needle Washes field Note Needle rinsing is not required when samples contain low salt con centrations Three rinses are recommended for samples containing salt concentrations of 1 or more TOC VCPH CPN 85 4 2 Setting General Measurement Parameters 4 2 2 ASI Parameter Settings No of Flow Line Washes Specifies the number of times the flow lines will be rinsed after all samples listed in the Sample Table have been measured This operation rinses the flow line from the sample needle to the injection tube using water drawn from the dilution water bottle If the automatic acid addition option has been selected the flow lines will be rinsed the specified number of times following acid addition to each sample rinsing after acid addition removes acid that remains in the sample needle or flow lines Enter a number ranging from 0 to 10 in the No of Flow Line Washes field
272. ler COVET i iit nee ea eee oe Drain Tank Needle Coaxial cjcssciecsstecssensnaescictes 322 Needle Sample ccccceceseseeeeeeeeeeeeees 321 POSITIONING ececeeceseeseeteeeeeeeeneeeeneeeee 317 Rinse Bottle 00 cee esesceseeeecneeneeneeneeees 323 Shipping Screw cccceseeseceeeeeeeeeeeeeeees 317 Purmitabletcccecttod en cachivndcti abides 323 Vial Rack wo cceeceeseeseeseeseeeeeereeeeeeeees 74 323 CO Absorber srele nEn 52 58 Combustion Tube Preparation serene ch iin des Ree 310 Procedure 0 ceececcesceseeseceesecseeseesceseeeeeteeteeeees 312 Sieen E i i cs eee ee 310 Suspended Solids Kit eeeceseeseesecreeneeneees 54 SyriD gei necies TN Unit TOC V raae EEE EE Index Instrument Instrument Setup Wizard Auto Restart narnii ne i Ae 121 AST Window 0 ececeeseeseetecseeseeseeeeeneeneeeees 28 95 Background Monitor cccceeeecseseeeeeeeeeeeee 203 Auto Regeneration of IC Solution 27 Connecting And Disconnecting cceee 205 Autosampler Parameters ccceseeseeteeteeseereeee 28 Detector Stats o ccsesccsesssesees caseasnesiesnsvseossaeoosss 203 BUZZEL AA E E E E E T 27 Effects of Acid Base and Salt cece 71 Cell Length scesmesecsoiniiiiricirniniinrai 26 History LOg o ei r a E 31 Communication Window 30 Maintenance ceeeeececeeeeees 261 Configuration 4 24 Menu Sample Table Editor eee 203 Furnace Temperature se L
273. lete Data gt All function open a Sample Table that contains measurement data and select Delete Data gt All from the Edit menu A confirmation dialog box is displayed as shown in the figure below Click the Yes button to delete the data Click the No button to abort the operation A message is displayed on the Notifications tab in the Notification Bar when the data has been deleted TOC Control 2 Are you sure you want to delete all measured data i No Figure 4 114 Delete Data Confirmation Dialog Box TOC VCPH CPN 4 4 Sample Table Editor 4 4 3 Edit Menu 4 4 3 9 Delete Data gt Highlighted The Delete Data gt Highlighted function is used to delete the measurement data for selected samples To execute the command open the appropriate Sample Table highlight the samples to be deleted and select Delete Data gt Highlighted from the Edit menu A message is displayed on the Notifications tab in the Notification Bar when the selected data has been deleted 4 4 3 10 Import The Import function is used to import data from an ASCII file into a Sample Table Note that the Import function is not available during sample analysis To import data open the destination Sample Table and place the cursor in the row of the table into which data will be imported Select the Import function from the Edit menu The Open dialog box is displayed Select the ASCII file from which data will be imported The data is inserted in the current position o
274. libration curve Enter the minimum maximum number of injections for the calibration standards Specifies the number of times the syringe is to be washed with standard prior to the first injection Note that if the Auto Dilution option was selected the standard will be diluted and the syringe will then be washed with the diluted standard Enter an integer from 0 to 10 Specifies the maximum standard deviation and coefficient of variation that is acceptable for the injections Enter a value ranging from 0 to 9999 for SD Max and from 0 to 100 for CV Max If either of these values are met no additional injec tions are required However if both of these values are exceeded the calibration standards are automatically rein jected up to the maximum number of times specified in the No of Injections field The SD Max and CV Max fields are disabled if the No of Injections is 1 or if the minimum is equal to the maximum Enter the length of time sparging will occur 0 20 minutes Enter the desired quantity of acid to be added This option is available only for NPOC or related analyses 4 4 Sample Table Editor 4 4 2 File Menu Calibration Curve Wizard Page 5 Calibration Points List The Calibration Points List window displays a list of parameters for each calibration point The parameters can be edited by using the buttons below the list A user must have access rights for updating data to edit calibration information Calibratio
275. lidation results Separator Select the type of separator to be used between items in the ASCII file Export strings in quotation Select this option to add quotation marks to all exported marks strings To export a file create or open a method validation file Select the desired options from the ASCII Export Options dialog box and select OK The File gt Save As dialog box is displayed Enter a file name for the ASCII file and select the txt file type LLL TOC VePrHiceN fm 363 364 Method Validation Options Menu A 5 6 Validation Strictly Following DIN38402 Use the Validation Strictly Following DIN38402 option to conduct the validation calculation by DIN 38402 requirements that is only the area obtained from the first injection of every standard is used in the calibration calculation When this option is not selected the mean value of the area counts from all injections of each standard is used in the calibration calculation Perform method validation according to DIN regulations as follows Step 1 Select the estimated working range Step 2 Prepare 10 calibration standards with concentrations distributed uniformly over the complete working range Step 3 Create a Sample Table with 10 injections of the highest and lowest standard concentrations and a single injection for all other standards If more than one injection is made of the intermediate standards the linearity test is calculated with the results of the first repl
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277. lobal data B 1 File Menu Figure B 1 File Menu B 1 1 New The New function is used to define new control charts and displays the Control Chart Wizard Follow the Control Chart Wizard process to enter a new control chart The file extension cc is used for all control charts Note Control Chart parameters can be changed at a later time by selecting Options gt Control chart options from the main menu bar Control Chart Wizard System Information Window The first page of the Control Chart Wizard is used to enter basic system information and is similar to the System Information pages in the Method and Sample Wizards Refer to Section 4 4 5 2 Sample and Section 4 4 2 3 Method Wizard Control Chart Wizard Page 1 System Information Figure B 2 Control Chart Wizard System Information Window 368 Wy TOC VCPH CPN Control Chart Wizard Control Chart Type Window Select the type of control chart to be created and select the analysis type from the drop down list Control Chart Wizard Page 2 Control Chart Type Figure B 3 Control Chart Wizard Control Chart Type Window Control Chart Wizard Control Chart Parameters Window Enter the control chart parameter values and limits as described below Control Chart Wizard Page 3 Control Chart Parameters Figure B 4 Control Chart Wizard Control Chart Parameters Window Setting Item Description Automatic calculation of the Select
278. m hydroxide is a corrosive strongly basic powder Use care when han dling to prevent contact or inhalation Refer to Section 6 9 Material Safety Data Sheets for details e Lithium hydroxide is available in anhydrous and hydrated forms Since the abil ity of the hydrated form to absorb carbon dioxide is slightly inferior to that of the anhydrous form use anhydrous lithium to fill the CO absorber container e When introducing the quartz wool and lithium hydroxide into the container do not pack too tightly e The CO absorber container is constructed of glass Handle it carefully to prevent breakage Cap a il Nipple O Ring BD i es So e Sd x RS RISO IZIS RSSRSS RRR KINISS LSS Lithium Hydroxide lt gt Quartz Wool OO cece SO O 2 p O x Se lt gt Z X lt gt eee eee x SS 3 DS SS Figure 4 20 Preparing the CO Absorber for POC Analysis 58 TOC VCPH CPN 4 1 Analysis Preparation 4 1 13 TN Analysis Preparations 4 1 13 TN Analysis Preparations TN analysis can be performed if the optional TN unit is installed on the instrument The NO absorber also must be connected to perform TN analysis The CO absorber soda lime is used as the NO absorber Connect it to the instrument using the following procedure Procedure 7 Cut the tips of the rigid tubes 2 in the lid of the CO absorber with a knife 2 Connect
279. mbustible or explosive gases e Do not analyze samples that can release toxic substances during combustion The exhaust gas released during analysis passes through the CO detector to the CO absorber after which it is used as NDIR purge gas and then is vented inside the instrument Take appropriate countermeasures if there is a possibility that toxic substances could be included in the exhaust gas If appropriate countermeasures cannot be taken do not perform such analyses The sample analysis results are displayed according to the gas concentration used in cal ibration For example if CO is used to generate the calibration curve the sample anal ysis result is displayed based on a conversion using the CO gas concentration Gaseous samples have certain properties such as adsorption condensation and reactiv ity and some gaseous samples are partially liquid or contain a solid component Depending on the properties certain conditions may occur that cannot be ignored Some of these conditions are residual substances and contamination in the flow line which may result in peak tailing carryover baseline fluctuation or other analytical problems High concentrations of NO or SO in the sample or in the post combustion oxidized sample can interfere with the NDIR activity To evaluate the degree of the interference combine the analysis of the base gas without the TOC component together with the sample analysis TOC VcPHICPN 227 4 5 Applic
280. me Displays the name of the currently active control chart Save the current control chart Enter a new file name in this field to save the currently active as control chart to a new location or with a new file name A confirmation message is displayed to confirm the operation Create Select this option to create the Following Control Chart The new limits are calculated from the samples of the control period stored in the previous control chart Parameter Select this option to display the parameters of the newly cre ated Following Control Chart This function can also be accessed using the Options gt Control Chart Options command in the main window 372 TOC VcPHI CPN Control Charts File Menu B 1 3 Open The Open command is used to open files Select a cc file to open a control chart file Refer to Section 4 4 2 4 Open for further information on the standard File gt Open dialog box B 1 4 Save The Save command saves the current control chart B 1 5 Save As Use the Save As command to save files for the first time or to save a file using a new file name Files can be saved as file types cc or txt ASCII format For more information on the Save As function refer to Section 4 4 2 7 Save As B 1 6 Print gt Data Use the Print gt Data command to print data in spreadsheet format For more information on the Print function refer to Section 4 4 2 10 Print gt Table B 1 7 Print gt Graph U
281. me the calibration curve was created Comment A comment regarding the calibration curve may be entered here Print Prints the calibration curve information 170 TOC VcPHI CPN Parameter Tab 4 4 Sample Table Editor 4 4 4 View Menu Calibration Curve Properties a x Common Parameter Analysis Data Graph History Analysis TC 4 Status Defined Units x mast Sample Name Standard Sample ID Tutoria No of Cal Points E Calculation Method Linear Regression gt I Multiple Injections Calibration Curve File estocsz20 CalCurves mpCalCurve cal Figure 4 126 Calibration Curve Properties Window Parameter Tab Setting Item Description Analysis Unit Sample Name Sample ID No of Cal Points Catalyst Type Calibration Curve Type Calculation Method Displays the analysis method used to create the calibration curve This field can not be edited Displays the concentration units This field cannot be edited Displays the default sample name used for the calibration standards 64 characters maximum This field can be edited Displays the default sample ID 64 characters maximum This field can be edited Displays the number of calibration standards used This field cannot be changed Displays the type of catalyst used Displays the calibration curve type This field cannot be changed Displays the calibration curve calculation method This field can be edited by selecting a diffe
282. ment Setup and System Properties Section 4 2 Setting General Measurement Parameters and Section 4 4 Sample Table Editor 4 3 Measurement Procedures and Tutorial 4 3 3 Ending Measurement 4 3 3 Ending Measurement Follow the procedure below to end measurement Procedure 7 From the Instrument menu select Standby Standby x System TC TN Keep running ITN Pamer Auto start time Select the standby mode and press Standby Standby Close Escape Figure 4 71 Standby Window 2 Two procedures are available for ending measurement e Shut down instrument e Auto restart These procedures are described below Shut Down Instrument Use the Shut down instrument option to end measurement and switch off power to the instrument 7 Select Shut down instrument in the Standby window then click the Standby button A 30 minute countdown to instrument shutdown begins During the shutdown pro cess the carrier gas flow and power to the furnace are automatically turned off and after 30 minutes the power to the instrument is switched off 2 Toend TN measurement manually switch off the TN unit using the power switch located in the lower right area of the ozone generator Note When Shut down instrument is selected the instrument power is turned off and the power to the autosampler exhaust fan is turned off If acidic samples are being measured or if sparging is being performed usin
283. meters lt Back ne h Cancel Figure 3 8 Instrument Setup Wizard TOC Window Catalyst Type Select the type of catalyst to be used in TC or TC TN measurement from the drop down list Available options are e Regular for TC measurements concentrations of 500ppb or greater High Sense for TC measurements concentrations below 500ppb e TC TN for combined TC and TN measurements Note The instrument does not automatically recognize the type of cata lyst that is installed Be sure to select the catalyst type that is actu ally installed in the instrument The high sensitivity catalyst should be used when the expected sample concentrations are below 500ppb or when detection of minute changes in concentration is necessary Tubing Diameter Select the diameter size of the sample injection tubing from the drop down list Available options are e Regular 0 5mm diameter e Suspended Particle 0 8mm diameter The typical tubing diameter is 0 5mm Select a tubing diameter of 0 8mm if the Suspended Solids kit is used Cell Length Select the length of the NDIR detection cell from the drop down list Available options are e Long for typical measurements Short for measurements using the Suspended Solids kit 26 TOC VcPHICPN 3 2 Instrument Setup and System Properties 3 2 3 TOC Window Buzzer Enables the internal buzzer function Select this option to allow the buzzer to sound during measurement Auto regeneration of IC s
284. mple Result Displays the sample concentration Dilution Factor Displays the dilution factor The result will be multiplied by this factor to calculate the final concentration If the sample was not diluted do not change the default value of 1 TOC VCPH CPN 167 4 4 Sample Table Editor 4 4 4 View Menu Injection Table The lower section of the Sample Window displays the Injection Table which contains detailed information about the injections performed for the selected sample Asterisks are displayed in the Injection Table for the injection that is currently being measured Some columns in the Injection Table use the Merge Cell function to display information that is common to all the injections of a particular sample If the sample has been analyzed by more than one analysis method the Injection Table contains several folders displayed as tabs at the bottom of the window The columns in the Injection Table are described below Setting Items Description Spl No Displays the sample number Inj No Displays the injection number Area Displays the area value Mean area Displays the mean area value for all injections of the sample Conc Displays the concentration obtained for the injection Mean Conc Displays the mean concentration obtained for all injections of the sample Result Displays the analysis result Notes Displays any analysis flags or notations associated with that sample SD Area Displays the standard deviat
285. mple if vial number 20 is selected stirring is performed for vial 20 sam pling position and vial 21 advance processing position The stirrer bar may not work normally for other vial positions The stirrer bar rotation axis may shift depending on the shape of the vial bottom this has almost no effect on the effec tiveness of the stirring Adjust the stirrer rotation speed according to the sample properties Use the stirrer rotation speed adjustment control on the right side of the ASI V Increasing the speed excessively may cause the stirrer bar to jump around instead of rotate Turning the stirrer on and off repeatedly while the stirrer is set at the slowest speed could cause the rotation speed to become uneven In this situation adjust the rotation speed using the following procedure ON OFF control of the stirrer is performed on the screen Setting the Stirrer Rotation Speed Perform the following steps to achieve nearly equivalent rotation speeds in all of the instruments used 1 2 5 Turn the stirrer OFF Set the stirrer speed to the highest speed using the Stirrer Rotation Speed Adjustment Knob Turn the stirrer ON and OFF several times With the stirrer ON lower the stirrer speed TOC VCPH CPN 79 80 4 1 Analysis Preparation 4 1 17 8 Port Sampler Measurement 4 1 17 8 Port Sampler Measurement 4 1 17 1 Type of Sampler Container There are no restrictions on the type of sample conta
286. mple as uniform as possible After homogenizing the sample depending on the type of suspended substance precipitation and coagulation may occur after a period of time Prior to measurement mix the sample again using a magnetic stirrer to ensure that pre cipitated coagulated material is well dispersed throughout the sample Ifthe suspended material is present in large quantities clumping of the material and obstruction may occur inside the sample flow line even if the particles are of smaller diameter that the sample flow line diameter Take measures such as sam ple dilution to prevent flow line obstruction e The suspended solids measurement kit employs a 0 8mm Teflon tube for sample injection Diminished reproducibility may occur with small sample injection vol umes Make injection volumes as large as possible e When conducting IC measurement of suspended solid samples using the H type instrument obstruction of the IC measurement flow line drain tube may occur Sufficiently pulverize the suspended particles to allow free flow through the drain tube TOC VCPH CPN 55 56 4 1 Analysis Preparation 4 1 11 IC Analysis Preparations 4 1 11 IC Analysis Preparations Certain preparations are necessary for the H Type instrument These include installing and replenishing the IC reagent in the IC reaction vessel This section describes the procedures for installing and replenishing the IC reagent The I spills N caution C re
287. mpler 1 Figure 1 17 Connecting Two 8 Port Samplers TOC VCPH CPN 4 6 8 Installation 6 8 5 OCT 1 8 Port Sampler Installation Remove the port number label from the 8 Port Sampler 2 unit and replace it with the port number label provided with the unit Note The port that was originally labeled as port No 1 should be labeled as port No 9 Replace the covers on the 8 Port Samplers Connecting the Sample Tubing Use the following procedure to connect the sample tubing of the 8 Port Sampler Tubing Connection Procedure 1 The sample tubing differs according to the TOC V model that is used with the 8 Port Sampler Note Refer to Table 6 21 Maintenance Parts List 4 OCT 1 8 Port Sam pler for the appropriate part numbers Connect the fitting at one end of the tubing to the common COM port of the 8 Port Sampler Pass the sample tubing through the hole in the left side panel of the TOC V main unit Connect the fitting at the other end of the sample tubing to port No 2 of the 8 port valve of the TOC V sample injector Connect to port No 1 when installing 8 Port Sampler 2 Connect the sample tubing to ports 1 8 ports 9 16 for 8 Port Sampler 2 of the 8 Port Sampler Sample Tubing Figure 6 18 Tubing Connections Note Connection to the TOC V Main Unit e 8 Port Sampler 1 Connect the COM tubing to the common COM port of 8 Port Sampler 1 and port No 2 on the TOC V unit e 8 Port Sampler 2 Co
288. mples where TC consists almost entirely of IC the NPOC method is recommended for such samples The TOC value determined using the TC IC method includes errors associated with each of the individual TC and IC measurements and can therefore result in a large error in the TOC value Because detection accuracy decreases with increasing IC concentration the NPOC method is also recommended for samples containing IC concentrations exceeding 10ppm for TOC TN catalyst and 5ppm for high sensitivity catalyst NPOC Method The NPOC method is the most widely used TOC analysis method The NPOC method is not recommended for samples that foam during sparging Samples that become foamy during sparging tend to form bubbles that flow out of the syringe which removes the concentrated TOC sample components and leaves a small amount of TOC in the syringe The TC IC method is recommend in this situation POC NPOC Method The POC NPOC method should be used when the amount of POC present in the sample cannot be disregarded 6 1 6 Principles of Measuring TN Total Nitrogen When a sample is introduced into the combustion tube furnace temperature 720 C the TN in the sample decomposes to nitrogen monoxide Nitrogen gas does not become nitrogen monoxide under these circumstances The carrier gas which contains the nitrogen monoxide is cooled and dehumidified by the electronic dehumidifier The gas then enters a chemiluminescence gas analyzer where the nitroge
289. n Curve Wizard Page 5 Calibration Points List a x Auto Dilution Inj Volume 50 ul Calibration Points No Conc No ofiri SDMas CV Max 1 0 000 mg L 3 3 0 1000 2 00 2 50 00 mg L 3 3 0 1000 2 00 3 100 0 mg L 3 3 0 1000 2 00 4 4 Edit Add Delete Delete All Edit the single calibration points ial Figure 4 80 Calibration Curve Wizard Page 5 Calibration Points List Parameter Description No Displays the calibration point number Note that the standards will be analyzed in the order shown To add a calibration point at a certain position click the desired number in the No column then click the Add button and enter the appro priate information The new point will be added in the speci fied position and the point that was previously in that position will move down the list to the next position Inj Volume Displays the injection volume for the calibration standards Calibration Points Displays a table of measurement parameters such as those entered in the previous page of the Calibration Curve Wizard for each calibration point To edit the parameters for a cali bration point highlight the point in the table and click the Edit button To add a calibration point click the appropriate number in the No column to specify the insertion point then click the Add button To delete a calibration point highlight the point in the table and click the Delete button To delete all calibr
290. n Curves 6 2 3 Calibration Curves 6 2 3 1 Types of Calibration Curves 1 Point and 2 Point Calibration Curves The output signals of the TOC V are linearized As a result there are almost no factors in the reaction systems of the TC TN combustion and IC reaction components that might cause the concentration output characteristic to deviate from linearity Consequently calibration curves are commonly generated as 1 point curves consisting of 1 span point or 2 point curves consisting of 1 span point and the zero point The concentration of TC and IC or of TN varies with standard solutions prepared with pure water A calibration curve generated using concentrations greater than 50 100mg L will pass very close to the zero point In this case it is practical to generate a 1 point calibration curve Use a 2 point calibration curve when the concentration of TC and IC or TN in the pure water used to prepare the standard solutions cannot be disregarded with respect to the standard solution concentration For information on handling of this type of curve refer to Section 6 2 3 2 Shifting of Calibration Curves Multi Point Calibration Curves Calibration curves can be generated using up to 10 points Calibration curves consisting of 3 or more points can be generated as a point to point curve or as a regression line using the least squares method With the least squares regression curve a correlation coefficient is displayed 6 2 3 2 Shift
291. n monoxide is detected The detection signal from the chemiluminescence gas analyzer generates a peak and the TN concentration in the sample can then be measured Note TN Detection Rate In TN analysis the state crystalline state in which TN exists in the sample greatly affects the TN detection rate Nitrogen contained in nitrates nitrites ammonia and the majority of other organic nitrogen compounds exhibit high detection rates Conversely some organic nitrogen containing compounds such as hydrazines pyrazolones and azide compounds have detection rates ranging from 10 to 60 depending on the concentration TOC VCPH CPN 6 2 Analysis Related Technical Information 6 2 1 Peak Area Analysis 6 2 Analysis Related Technical Information 6 2 1 Peak Area Analysis When a sample is analyzed the TOC Control V software automatically detects the beginning and end of each peak produced and calculates the peak areas Detection of the beginning and end of each peak is based on the slope of the tangent which changes from moment to moment Peak detection begins when that slope exceeds a predetermined value and ends when a negative slope falls below a specified value Note Separated Peaks In TC analysis multiple peaks may occur when a large quantity of sample is injected Only the end of the last peak is detected The total area of the multiple peaks is calculated e Baseline Correction Baseline correction is performed for peaks prod
292. n standards directly into the Vial column of the table Because the calibration standards are TC TN mixtures enter the same vial positions 1 3 for the TN standards that were entered for the TC standards LLL TOC VerHiceN my 107 4 3 Measurement Procedures and Tutorial 4 3 2 Tutorial amp Click the OK button to display the Sample Table window Notice that the second row of the Sample Table now contains complete TN calibration standard measurement information Take a moment to scroll through the completed Sample Table Notice that the col umns in the left portion of the Sample Table contain the specified analysis parameters Actual measurement information will appear in the columns in the right portion of the Sample Table once the measurements are completed 9 Save the Sample Table by selecting Save from the File menu or by clicking the Save button El in the toolbar Setting up an Unknown Sample Run Step 5 In Step 4 of the tutorial you learned that information about calibration standard measurement is saved in a calibration file You also learned that setting up a calibration standard run involves two steps creating a calibration file and then inserting the calibration standards into the Sample Table By contrast information about unknown sample measurement is saved in a method file Setting up an unknown sample run involves two steps creating a method file and then inserting the unknown sample into the Sample Table In this tu
293. n the front door of the instrument 2 Turn the carrier gas flow adjustment knob For H Type adjust the flow rate to 150mL min as indicated on the flow rate gauge Carrier Gas Flow CARRIER GAS Rate Adjustment 4 a Knob Oo o Flow Rate Gauge PRESSURE Figure 4 31 Setting Carrier Gas Flow Rate Note Do not change the carrier gas flow rate during analysis The peak area changes in an inversely proportional relationship and may cause errors in analysis precision e With the N Type although the flow rate is adjusted to indicate 130mL min on the flow rate gauge the actual flow rate used is 230mL min 4 3 1 4 Electric Furnace The electric furnace power must be turned on for TC TOC NPOC POC and TN analyses The electric furnace does not need to be turned on if only IC analysis is performed When TN analysis is conducted the TN unit must also be turned on Turn On Power to the Electric Furnace 1 Inthe TOC Control V main window double click the icon for the desired instrument The Instrument Properties dialog box is displayed 2 Click the TOC tab 3 Set the TC furnace temperature to either 680 C or 720 C used for TN measurement 4 Click the OK button The screen returns to the TOC Control V main window Note It takes 30 40 minutes after the electric furnace power is turned on for the tem perature to reach the set value Refer to Section 4 3 3 Ending Measurement to turn Off
294. n the valve lt Part damage prevention gt TOC VCPH CPN 4 1 2 Operational Precautions Stop operation of the instrument when performing maintenance on any of the drive components such as connecting lines to the 8 port valve or connecting disconnecting lines on the sample injector If these parts are manipulated or if the lines are disconnected during operation the drive component could move and cause injury or discharge of liquid lt Injury prevention corrosion prevention gt To shut down the instrument first select Shut down instrument in the TOC Control V Standby window Refer to Section 4 3 3 Ending Measurement for more information The electric furnace turns off and after 30 minutes the power supply shuts off This shutdown process extends the life of the TC injection port parts by preventing unnecessary wear This procedure does not apply to emergency shutdown lt Maintaining durability of TC injection port parts gt The lever of the 3 way valve at the bottom of the IC reaction vessel should normally be turned to the left position Refer to Figure 1 2 Lever Position of 3 Way Valve on the IC Reaction Vessel The lever should never be turned to the lower position The lower position allows carrier gas to flow at a pressure of 200kPa upstream from the 3 way valve causing possible disconnection of joints and damage to parts such as the combustion tube O x x Carrier gas is discharged Never turn the lever to the fro
295. ndow and is an option only when a file is open If the open file has not been saved and the Close command is selected the Save As dialog box is displayed Refer to Section 4 4 2 7 Save As Enter a name for the file and click the OK button to save the file If the open file has been modified but not saved and the Close command is selected a dialog box is displayed as shown below Click the Yes button to save the file before closing Click the No button to close the file without saving the modified information Click the Cancel button to abort the Close command TOCSpiTbl x AN Save changes to Tutorial t32 Figure 4 92 Dialog box for Saving Modified Data The Save command is used to save data in the current active file If the file has not yet been saved and the Save command is selected the Save As dialog box is displayed Refer to Section 4 4 2 7 Save As The Save command can also be executed by selecting the Save File button on the Toolbar TOC VCPH CPN 4 4 2 7 Save As The Save As command is used to save the current active file with a new file name Selecting the command opens the Save As dialog box shown below Button options in the dialog box are similar to those in the Open dialog box Refer to Section 4 4 2 4 Open Click the Save button to save the data under the specified file name Click the Cancel button to abort the Save As operation PS Tutorial m Figure 4 93 Save As Dialog Box Dialog Box Options Descript
296. nect the instrument by selecting Connect from the Instrument menu gt From the Instrument menu select Maintenance gt Blank Check The Blank Check Parameters dialog box is displayed Blank Check Parameters Figure 4 22 Blank Check Parameters Dialog Box 4 Enter the desired injection volume and click the Start button The Standby dialog box is displayed OTC Furnace Carrier Gas OSSM TC Furnace OSSM IC Furnace Figure 4 23 Standby Dialog Box 5 Select an option to determine the condition of the instrument after the blank check is complete Options are e Keep running Shut down instrument e Auto Restart TC furnace carrier gas restart time 6 Fill the dilution water bottle to full capacity with purified water and place it in the specified position About 200mL of dilution water is used for the blank check measurement 7 Click the Standby button The Save As dialog box is displayed amp Enter a file name and click the Save button Data from the Blank Check procedure will be stored in the created file Blank check analysis begins The procedure that the instrument executes is described below LLL TOC fl 67 4 1 Analysis Preparation 4 1 15 Sample Preparation Description of TC Blank Check Analysis Procedure 1 Washing the inside of the trap First the trap is washed with water from the dilution water bottle A 6mL aliquot from the dilution water bottle is drawn into the ultra pure water trap and
297. nerator 5 5 1 Replacing the Catalyst in the Ozone Treatment Unit The ozone treatment unit breaks down ozone gas produced by the ozone generator The catalyst inside the ozone treatment unit must periodically be replaced Replace the catalyst once a year for an instrument that runs 8 hours a day and 5 days a week Perform maintenance to the ozone treatment unit only after stopping the instrument as described inSection 4 3 3 Ending Measurement N caution The interior of the ozone treatment unit is heated to 50 C Perform maintenance only after cooling for at least two hours Replacement Procedure Use the following procedure to replace the catalyst in the ozone treatment unit 7 Remove the knurled screw at the bottom of the unit and remove the installation bracket i Ozone Treatment Unit Knurled Screw Installation Bracket Figure 5 18 Removing the Ozone Treatment Unit Screw and Bracket 256 TOC VCPH CPN 2 Remove the hose clamp at the bottom of the ozone treatment unit and pull off the Viton tubing Hose Clamp Viton Tubing Figure 5 19 Removing the Viton tube 3 Remove the hose clamp at the top of the unit and remove it from the Viton coupling Hose Clamp Viton Coupling Figure 5 20 Removing the Ozone Treatment Unit LLL TO
298. ng Acids Bases or Salts Various problems can be encountered when measuring samples that contain acids bases or salts Such problems include corrosion of the NDIR analysis cell as well as detrimental effects on analysis values and the life of the combustion tube and catalyst If corrosion of the inner surface of the NDIR cell occurs baseline stability will decline and noise will increase Samples containing acids bases or salts should be handled as described below The concentration at which adverse effects are produced varies depending on the type of acid or salt and the TOC or TN concentration Prior to analysis dilute the sample so that acid base and salt concentrations are reduced to 1000mg L or less Neutralization is also required for bases The TOC V is equipped with an automatic dilution function to perform these dilutions Acids Acids should be diluted to a concentration of 1000mg L or less Concentrations up to 5000mg L can be used if this level of dilution cannot be reached The acidity of hydrochloric acid or sulfuric acid can be reduced to a pH of 2 3 with sodium hydroxide or potassium hydroxide This process produces thermally stable sodium chloride or sodium sulfate which prevent the generation of acidic gas when combusting the sample Neutralization of the acid is stopped at a pH of about 2 3 and TOC direct analysis NPOC analysis with sparging to remove the IC is performed It is necessary to consider the TOC associated with
299. ng in Software cece seeeeseeeceeeeeees 84 Index 1 Index Cable Connections iesene Et Cables Connecting ccccccseeseessereereeeeeeees Calibration Curve 1 Point and 2 Point Calculation Method Creating sicicscvsiveessececesadoedcnccesanestconseeedhes Entering Calibration Standard Levels 132 Gas Sample Analysis cccccccsesceeensenseees 229 High Sensitivity Analysis 0 00 0 cesses 65 Inserting into Method Inserting into Sample Table Inserting Into Sample Wizard 187 Manual Injection Kit cece eeceeeeeeeeeseeseees 221 M lti Point aoieanna 290 OptiIMUM ona e a E A EANES 292 OPONSE aseran EEEE 128 Points List 131 Points Parameters 132 Shifting To Blank Point 0 eee eee eeeeeee 291 Shifting to Origin eee 129 172 290 Types ae eepe cate aa eeess 128 290 Viewing Data cccecsecsecseesceseeeeeeeeeeeeeeeeceeees 160 Viewing Properties cescceeseeeeeeeeeeeeeeeees 170 Calibration Curve Wizard ceeeeeeeeteees 100 126 Analysis Information Window ceceeee 128 Analysis Options cceeeeeee gs 102 Calibration Points List 103 Calibration Points Window we 131 Curve Ty o EE EE E E E 101 Curve Type Window ccccecssessessenseeseeseees 128 Default Measurement Parameters 0 102 History auy an vetelal ahs athens a as 104 History Window ccceseseese
300. ng the ASI V acidification and sparging can be performed on samples during NPOC analysis To perform acid addition using the autosampler enter the desired amount in the Acid Addition field on the Injection Parameters window of the Sample Wizard refer to Section 4 4 5 2 Sample or Method Wizard refer to 4 4 2 3 Method Wizard When analysis is started acid is drawn from the acid bottle into the syringe and the set amount of acid is added from the sample needle into each of the vials that have been designated for acid addition Use 2M hydrochloric acid The acid addition ratio ratio of acid with respect to sample should be set to about 2 5 However a setting of about 0 5 is used for purified water analysis The hydrochloric acid concentration or amount added should be adjusted in accordance with the sample pH or buffering strength to bring the sample pH to 2 3 Prior to analysis verify that the pH is 2 3 using pH paper The pH need not be checked each time if the same type of sample is routinely measured N caution Hydrochloric acid is a hazardous chemical Exercise caution when handling to prevent contact and spills For details refer to Section 6 9 Material Safety Data Sheets If the sample pH does not reach a value between 2 and 3 increase the acid addition ratio or the acid concentration Excessively increasing the acid addition ratio will result in dilution of the sample On the other hand if the acid amount is too
301. niections r Auto correction of inj vol and dilution Auto Dilution Inj Volume Expected Cone Range p a fo u fpo Calibration Curve 1 ms Calibration Curve 2 Calibration Curve 3 Figure 4 119 Sample Method Properties Window IC Tab 164 TOC VCPH CPN NPOC and POC Tabs The NPOC and POC tab options are similar to those described above for the TC tab i Sample Method Properties Figure 4 120 Sample Method Properties Window NPOC Tab TN Tab The TN tab options are similar to those described above for the TC tab except that some options such as Use area retrieved from blank check are not available for TN measurements Sample Method Properties Figure 4 121 Sample Method Properties Window TN Tab LLL T OC VcH fy 165 166 4 4 Sample Table Editor 4 4 4 View Menu History Tab If the History Log was enabled when the method was created the History tab displays a list of changes made to the method parameters If the History Log was not enabled previously it can be enabled on the History tab Sample Method Properties x Common Parameter TC History VV Enable history log JV Comment Required for Modificatior Ascii export Changed Item 03 03 2003 02 24 3 Sy Method created Figure 4 122 Sample Method Properties Window History Tab Setting Item Description Enable history log Select this option to enable the software to monitor
302. nnect the COM tubing to the common COM port of 8 Port Sampler 2 and port No 1 on the TOC V unit TOC VCPH CPN 328 6 8 Installation 6 8 6 Installing the TN Unit 6 8 6 Installing the TN Unit 6 8 6 1 Connecting the Power and Installation Connecting the Power Supply Connect the TN unit to a stable AC100V 10 V 50Hz or 60Hz single phase power supply with sufficient capacity to accommodate 2A or greater current The symbol on the name plate indicates alternating current caution The instrument may not operate properly if the power supply voltage exceeds the range of AC100 127V 10 or AC 220 240V 10 Unstable voltage may cause problems during high sensitivity analysis Note The instrument is compatible with both 50Hz and 60Hz power supplies and can be used with either frequency Grounding The included power cord is a three conductor cable including a ground wire and a 2P plug with ground at the end If the power outlet does not have ground receptacle use the included 2P no ground adapter and ground the external ground tap terminal The voltage terminals AC and ground terminal ACC on the power plug of this instrument are arranged as shown in Figure 6 19 Power Plug Connect them so that they match the power outlet being used Voltage Terminal AC Ground Terminal ACC Ground Terminal G Be sure to ground completely Figure 6 19 Power Plug TOC VCPH CPN 6 8 Installation 6 8 6 I
303. not shut down properly If this is the case turn the TOC V on again and shut it down properly TOC VCPH CPN 5 4 8 Port Sampler OCT 1 Maintenance 5 3 3 Replacing the Pump Head of the Rinse Pump 4 Remove the nut using the wrench supplied with the TOC V Figure 5 15 Removing the Nut 5 Remove the 8 port valve by pulling it downward 6 Loosen the retaining nut using the provided wrench Retaining Nut Figure 5 16 Removing the Retaining Bracket 7 Note the orientation toward port No 1 of the flat surface of the spring equipped rod Remove the spring equipped rod and retaining nut amp Note the orientation of the rotor hole position Grasp the rotor with forceps and remove by pulling upwards Rotor Figure 5 17 Removing the Rotor 9 Insert a new rotor positioning the rotor hole to the original position 70 Reinsert the spring equipped rod and retaining nut with the flat surface directed toward port No 1 Tighten the retaining nut 11 Replace the 8 port valve in its original position and secure it using the nut 12 Replace the cover of the 8 Port Sampler and secure it with four screws 13 Switch on the TOC V unit TOC VCPH CPN 255 5 5 TN Unit TNM 1 Maintenance 5 5 1 Replacing the Catalyst in the Ozone Treatment Unit 5 5 TN Unit TNM 1 Maintenance Maintenance of the TN unit includes periodic inspection of the ozone treatment unit catalyst chemiluminescence detector and ozone ge
304. ns 308 Peak Phosphoric acid Plunger Tip Backlash POC Analysis Preparation Kit pce ei Pineiples derin eran en n SE Standard Solution esaeen POC NPOC Principles ceccseseeseeeeeneeneeeeneees Post Sal S rvice cipine nrn einir iv Potassium hydrogen phthalate MSDS 0 344 Potassium nitrate MSDS ccccceeseeecseeeseeeneeeeee 341 Power PUIACE EA E testes nantosnapronitone Instrument CLIN EAEE EA AE E escent Power Supply Changing Voltage ssssessssessessssessesersssesessesesse 313 Connecting tasmaniae 312 328 Quartz Wool acetone eunaien det 37 39 58 338 Ready Status Check 0 0 ecsesseseseeecesserenesereres 27 84 Rear View 8 Port Sampler seriernes 15 Autosampler c cccccececceccseesensenseeseeeeeeeeeeeeeesees 14 A DAAE EE E E E EE EAEE EA 18 TOC V a E ea e hetbeatoedd 9 Recalculating All Sample Table Data cece cceseseereereeee 158 Control Chart Limits see STL Selected Sample Table Data eee 158 Reference Information 0 0 0 ceceeeeeeeeeeeeee 283 345 Precautions noii enhe nesortate Gas Sample Analysis High Sensitivity Analysis sseeseseseeeeeeeeereeseeee 63 Preparation ANALYSIS eann aeann a ni Dilution Water 0 High Sensitivity Analysis Manual Injection Analysis Samples gis heii ie iets betes Standard Solution eceseeecseeeceecreeecneeeeees TEN Analysis enrenar Pressure Ozone Generator Source Alt eee eeeee
305. ns in excess of 5mg L Filling Combustion Tube with TOC High Sensitivity Catalyst Two cylindrical containers of catalyst are required for a single load 7 Place two sheets of platinum mesh in the combustion tube 2 Fit together the combustion tube opening and the opened end of the cylindrical catalyst container 3 Use the catalyst filling rod to push catalyst into the combustion tube from the other opened end of the cylindrical catalyst container 4 Transfer the contents of the two cylindrical catalyst containers to achieve a catalyst layer height of 130mm in the combustion tube Combustion Tube TOC High Sensitivity Catalyst 130mm Platinum Mesh Figure 4 2 Filling of TOC Combustion Tube with High Sensitivity Catalyst 38 TOC VCPH CPN 4 1 Analysis Preparation 4 1 1 Catalyst Filling 4 1 1 2 TOC TN Catalyst Option TOC TN catalyst is used for TN analysis and TOC TN simultaneous analysis The detection rate is low for the IC component when it exceeds 10mg L as a result TOC in samples containing more than 10mg L IC cannot be measured using the TC IC method and should be measured using the NPOC method The furnace temperature is set to 720 C for TOC TN and TN analysis Filling Combustion Tube with Catalyst for TN Analysis 7 Insert two sheets of platinum mesh into the combustion tube 2 Layer about 5mm of quartz wool onto the platinum mesh using the catalyst filling rod 3 Introduce the
306. nse with water 3 Dry and reuse these items 4 Fill the combustion tube as described in Section 4 1 1 Catalyst Filling TOC High Sensitivity Catalyst TOC high sensitivity catalyst cannot be washed and reused like standard catalyst If analysis sensitivity and reproducibility are not restored after catalyst regeneration replace the deteriorated high sensitivity catalyst with new high sensitivity catalyst The platinum mesh and combustion tube can be washed with hydrochloric acid and reused Disposal of Catalyst Used catalyst should be disposed of according to local industrial waste disposal regulations It must be clearly disclosed using an industrial waste manifest that the used catalyst contains platinum 5 2 2 3 Replacing the Carrier Gas Purification Tube and Catalyst The carrier gas purification tube burns the carrier gas and oxidizes carbon based impurities converting them to carbon dioxide The carbon dioxide is absorbed and eliminated by the CO absorber The carrier gas purification tube is filled with oxidation catalyst same as TOC standard catalyst The procedure for replacing the purification tube and catalyst is as follows Removal of Carrier Gas Purification Tube warnine Before attempting to remove the carrier gas purification tube be sure to allow the oven temperature to cool to room temperature There is a danger of burn injury if this procedure is performed while the oven is hot TOC VCPH CPN
307. nstalling the TN Unit N caution e In addition to the consideration of safety complete grounding is necessary to prevent as much as possible the occurrence of signal noise A Type 3 ground ground resistance 100W or less see Electrical Facilities Engineering Standards for details is recommended e Perform grounding separately and avoid contact with water supply pipes gas pipes and lightning rods 6 8 6 2 Connecting Ozone Source Air The TNM 1 incorporates an internal ozone generator requiring a source of air gas supplied at about 500mL min separate from the carrier gas supplied to the TOC V While it is possible to use TOC V high purity carrier gas by providing branch tubing the consumption of the combined use carrier gas would increase to about 150 250mL min Assuming operation at the rate of 8 hours day 5 days week the 47 L 12MPa air cylinder would require monthly replacement as compared to every 3 months when used for carrier gas alone Because air gas for ozone generation is not required to be the high purity air used as carrier gas it is recommended to use instrumentation air or compressor supplied air for ozone generation separate from the carrier gas Using Compressor Air or Instrumentation Air When using compressor air or instrumentation air for generation of ozone be sure that the following conditions are satisfied e Install an air filter in the air supply line to eliminate dust oil mist and water droplet
308. nstrument 3 From the Instrument menu select Maintenance gt Regeneration of the IC solution The Regeneration of IC solution dialog box is displayed Regeneration of IC solution Regeneration of IC solution Figure 4 19 Regeneration of IC Solution Dialog Box 4 Click the Start button The IC reagent will be delivered to the IC reagent vessel by the liquid delivery pump During the process the Start button is disabled x A progress bar is active until the IC reagent is completely regenerated Click the Close button TOC VCPH CPN 57 4 1 Analysis Preparation 4 1 12 Preparation for POC analysis 4 1 12 Preparation for POC analysis POC analysis can be performed if the optional POC analysis kit is installed on the instrument This section describes preparations required for POC analysis Installation of the CO Absorber for POC Analysis 7 Remove the CO absorber 2 Insert about 5mm of quartz wool into the bottom of the container 3 Add commercially available anhydrous lithium hydroxide to the container on top of the quartz wool until it reaches just below the screw threads of the container Note About 6g of anhydrous lithium hydroxide is required for a single load 4 Place about 5mm of quartz wool on top of the lithium hydroxide M Attach the O ring and nipple to the top of the container and firmly tighten the cap 6 Install the CO absorber for POC analysis in the original position L caution e Lithiu
309. nt numbers using a specified number of significant digits Use the spin control to set the number of significant digits The default value is 4 Number of digits after the Select this option to display common floating point numbers decimal point using a specified number of digits after the decimal point Use the spin control to set the number of digits after the deci mal point The default value is 2 Percent Values Setting Item Description Number of significant digits Select this option to display percent values using a specified number of significant digits Use the spin control to set the number of significant digits The default value is 4 Number of digits after the Select this option to display percent values using a specified decimal point number of digits after the decimal point Use the spin control to set the number of digits after the decimal point The default value is 2 216 TOC VcPHI CPN 4 4 9 7 Directories The Directories function is used to modify system directories Select Options gt Directories to display the Folder window m C Program Files Shimadzu Corporation T 003201 Data Figure 4 180 Folder Window Show all directories for Use the drop down list to access various directories Available directories are listed in the Folder text field Add Click the Add button to add a new directory to the list for a specified topic and the Folder dialog box is displayed Highlight the desired
310. nt of the IC to this position reaction vessel Turn the lever to this position only when detaching an IC reaction vessel that contains liquid Figure 1 2 Lever Position of 3 Way Valve on the IC Reaction Vessel To use the ozone generator of the TN unit verify that air is supplied at a rate of 0 5 L min to the ozone air source flow meter inside the instrument Refer to Figure 2 5 Inside Front View Turn ON the ozone generator This prevents ozone leaks and line corrosion lt Ozone leak prevention line corrosion prevention gt If ozone odor is detected during operation of the TN unit stop the gas supply by turning the ozone generator OFF and contact your Shimadzu representative to request maintenance Ozone can cause respiratory organ injury and equipment damage lt Prevention of injury to respiratory organs and equipment damage gt To shut down the TN unit turn the ozone generator OFF at least 3 minutes prior to switching OFF the TN unit power to stop ozone generation This prevents ozone leaks and line corrosion lt Ozone leak prevention line corrosion prevention gt TOC VCPH CPN 1 2 Operational Precautions The optional POC measurement circuit incorporates a carbon dioxide CO3 absorber packed with lithium hydroxide for removal of carbon dioxide gas Misuse of lithium hydroxide can cause bodily harm During packing or replacing the CO absorber container exercise adequate precaution After use treat the material as indu
311. nus and commands The Sample Table Editor is used for instrument startup calibration curve generation method development sample analysis halting of analysis and instrument shutdown Application Operations The procedures for performing manual injection analysis and gaseous sample analysis are described in this section 36 4 1 4 1 1 Analysis Preparation Catalyst Filling 4 l Analysis Preparation 4 1 1 Catalyst Filling Three types of catalyst are available TOC standard catalyst TOC high sensitivity catalyst H Type only and TOC TN catalyst option The procedures for filling the combustion tube with catalyst are described in this section For TOC standard and high sensitivity catalyst filling follow the procedure in Section 4 1 1 1 Catalyst for TOC Analysis For TOC TN catalyst filling follow the procedure in Section 4 1 1 2 TOC TN Catalyst Option Ncau TION Exercise caution when handling the combustion tube to prevent breakage as it is made of quartz glass Note When filling the combustion tube verify that the catalyst does not become con taminated Contamination will cause high blank values and abnormal analysis values Using New Catalyst Broad blank peaks are obtained when using new catalyst for the first time The blank peaks will become progressively smaller and more stable with repeated injections and their size will stabilize If calibration or analysis is performed while the blank peaks are
312. o exclude the selected data Click the No button to abort the operation TOC Control 2 Are you sure you want to toggle the exclusion status of the selected injections Figure 4 113 Exclude Confirmation Dialog Box 4 4 3 6 Recalculate gt All The Recalculate gt All function is used to recalculate the data for all measured samples in a Sample Table after applying a new calibration curve or excluding injections To execute the command open the appropriate Sample Table and select Recalculate All from the Edit menu A message is displayed in the Notify folder of the Notification Bar when the recalculation is complete 4 4 3 7 Recalculate gt Highlighted The Recalculate gt Highlighted function is used to recalculate the data for selected samples after applying a new calibration curve or excluding injections The function is similar to the Recalculate All function described in Section 4 4 3 6 Recalculate gt All To execute the command open the appropriate Sample Table highlight the samples to be recalculated and select Recalculate Highlighted from the Edit menu 4 4 3 8 Delete Data gt All The Delete Data gt All function can only be used if the GLP conformity was disabled during system installation The function is used to delete all measurement data in the Sample Table The Sample Table structure can then be used to enter new data A user must have access rights for updating data to use the Delete Data gt All function To use the De
313. o graphic file Figure 4 69 Page Setup Miscellaneous Tab 1 18 WE TOC VcrrHichN ieee SOHSSSHSSHSHSHSHSHSSHSHSHSHSHSSHSSHSHSHSHSHSHSSSHSHSSHSHSSHSHSHSHSHSHHSHSSHSHHHHSHHSHEHSHHSSEEHSEEEE Previewing the Report 7 Select the Preview button from any of the Page Setup tabs to preview the entire report before printing TIP The report can also be previewed from outside the Page Setup window by selecting Print Preview gt Sample Report from the File menu The Preview feature displays each page of the report exactly as it will be printed Notice that each item that was selected in the Page Setup window appears in the report 0 0 6 12 20 Timefmin Area 0 842463 mE o 110 Concfppm l a u Sisam 200 FopppE EEA ae Pe 100 EEELLEEEETSS 04812 20 Tmi Figure 4 70 Report Appearance TIP Magnify the view by clicking the magnifying glass tool or on the Zoom In button Move from page to page by clicking the Next Page and Previous Page buttons 2 Print the report by clicking the Print button This ends the Tutorial Reference The tutorial provided instructions for setting instrument configuration and analysis parameters adding calibration standard and unknown sample information to the Sample Table creating calibration curves and method files conducting measurements and checking and printing results More details on all of these procedures are discussed in Section 3 2 Instru
314. ods of Sealing Vials Two methods of sealing the vials are acceptable 1 Using the caps provided with the vials 2 Using a sealing material marketed under such names as Parafilm or Sealon Film Note Use caps only after washing them with water or washing them with laboratory cleaning solution and then rinsing with water Using Caps For 24mL vials Holed caps and seals are provided with the vials 7 Place a seal over the vial opening 2 Cap the vial over the seal Note Because the seals are perforated during injection discard the seals after use For 40mL vials Seal equipped caps are provided with the vials 1 Using a seal equipped cap provides an adequate seal for the vial Note Because the seals are perforated during injection discard the seal equipped cap after use Using Parafilm or Other Sealing Materials Procedure 7 Cut the Parafilm or other sealing material into approximately 25 x 25mm squares 2 Place a square over the opening of the vial and stretch it to seal to the edges of the vials TOC VCPH CPN 73 4 1 Analysis Preparation 4 1 16 Sample Preparation 3 Press the edges down so that they wrap around the outside of the vial Be careful that film edges do not descend below vial threads Figure 4 24 Sealing the Vial 4 1 16 3 Placing Vials in the Vial Rack Remove the vial rack from the ASI V before inserting the sample vials There are three different types of vial racks eac
315. of the PC power while it is controlling the TOC analyzer A shutdown of this nature would adversely affect performance Hand tighten the connectors to the 8 port valve of the 8 port sampler Over tightening with a tool may exert excessive force to the internal valve body causing deformation and internal leakage lt Part damage prevention lt Shut down the instrument before connecting or disconnecting tubing to the 8 port valve or performing maintenance to the drive parts Liquid may be discharged from tubes during operation lt Part corrosion prevention gt When utilizing the software s printing function set the paper size to letter or A4 and printer graphic resolution to 600 dpi TOC VCPH CPN 6 E TOC VcPHICPN iii System Description This chapter describes the components of the TOC VCPH CPN autosampler ASI V 8 port sampler OCT 1 and the TN unit TNM 1 2d ae fa 2 4 TOC VCPH CPN Construction Describes the construction of the TOC V unit using front right left rear and internal views of the instrument as well as flow diagrams Autosampler ASI V Option Describes the construction of the ASI V unit using front and rear views of the autosampler 8 Port Sampler OCT 1 Option Describes the construction of the 8 port sampler using front and rear views of the unit TN Unit TNM 1 Option Describes the construction of the TNM 1 unit using front right and internal views of the unit P l TOC V
316. ol Charts The Control Charts software monitors precision and accuracy of a defined data set The software supports five types of Control Charts Mean Value Control Charts Recovery Control Charts Blind Value Control Charts Spanwidth Control Charts User Defined Control Charts The Mean Value Control Chart checks the accuracy of an analytical method on an instrument Control value drifts may indicate a change in system performance The Recovery Control Chart tests an analytical method for matrix influences and provides a restrictive control of accuracy by testing proportional system errors Using certified standards will test the accuracy of the system as well as the recovery rate The Blind Value Control Chart is a special form of the Mean Value Control Chart used for quality assurance of the instrument and variable elements Unlike the Mean Value Control Chart the control value is the information value absorbance peak height peak area received from the analysis The Spanwidth Control Chart tests the precision of an analytical method and monitors the accuracy under actual conditions Drift Control For this type of Control Chart there are several existing models for calculating the control and warning limits Each type of control chart can be used to create charts for different working range and analysis methods For each control chart a file is created which contains general information about the type data structure and other g
317. olution Select this option to automatically regenerate the IC solution This option is enabled only if IC Unit was selected in the Options window of the Instrument Setup Wizard The acidity of the IC solution gradually decreases over time as the acid is used to convert the IC components in samples into carbon dioxide Unless the IC solution is periodically regenerated it eventually loses its ability to fully convert IC into carbon dioxide which can affect the accuracy of analysis When the Auto Regeneration option is selected the pH and volume of the IC solution are automatically maintained at the appropriate levels The instrument automatically pumps IC solution from the IC reagent reservoir in the following cases e When the instrument is turned on e Prior to the initial IC measurement following a preset number of injections and preset volume of injected samples e If peak tailing is observed during an IC measurement The system notifies the user of peak tailing by inserting a T into the Notes column of the Injection Table and the Remark column of the Sample Table Enable ready status check Select this option to enable the Ready Status Check function When the function is enabled the software always verifies that the instrument is in the Ready state prior to starting measurement Enabling the Ready Status Check function is recommended When the function is deselected measurement can be performed when the instrument is not in
318. one eetarea eeaeee eenst cata sesa anosa ree aaa a A Product Warranty and Post Sale Service cccccsesscescerseeseeeteceteeeteeseeeees iv Product Warranty renmen n docs E E ek R ee iv RIRE E DA EAE AE E T EEE TA iv Contents of This Manual 00 cccccccsccescesseeseecseeseceeeceseeeseeeseceseceeeeeeeaeesees v Notation Conventions ccceccccssceseceseeeeeeseesseceseceeceeseeeeecaaecseseeeeseeeseeseee vi Precautionary Conventions Used in this Manual vi Other Conventions Used in this Manual ssssseeseeeesesssseeseesesersessesseressrsesses vi Warning Labels Used on this Instrument cccceesceseceseeeeeeseeseeseees vii OVERVIEW Sicssceiciscecscesteectuseekcsenes cet cenceccccucestewcenececcoscescotccsocsesbecs sescssecseeccests L jes OVE ne er a anta 2 1 2 Operational Precauti h Sma E E ER EE Eta 3 System DESC rip HON essisciscsssndscassnnsccccenewedeniedstacdesucecespacscsdncseuscocsasenadabvodsens T 2 1 TOC VCPH CPN Construction ccccceccceesccesecesceseeeesecseeeseseecseeeeseeeeeeeeeaeenes 8 ZEL Front View cic 2c scccsci getsececei eel scecess jen ie E tees ei ees EE eee eee 8 212 RightSide View lt ccssnceieitnncgh ae does i echoes Wide oe te 8 DAB het Side Vilewss sie E E ete 9 DVWAs CREAR VIG W ao aare en eave TE sec bece ie tees ees ened 9 2 1 5 InsidesEront Viewer e a ovate ce E E E Gm tee ee ooese eeorseond 10 Q6 gt Inside Top View ocna enia iets leaded ee oe 11 Zi
319. only for documents that can be manually edited TOC Control V method validation documents have a fixed number of rows equivalent to the number of calibration points in the calibration curve TOC VCPH CPN Method Validation Edit Menu A 3 4 Delete Row Use the Delete Row command to delete a row from the data table The command is available only for documents that can be manually edited TOC Control V method validation documents have a fixed number of rows equivalent to the number of calibration points in the calibration curve The Delete Row function is not available if the number of rows is 4 or less Once a row is deleted the format of the remaining rows is updated A confirmation dialog box opens asking you to confirm the deletion Meth al EB 7 Are you sure you want to delete Row 1 to 2 Figure A 14 Delete Row Confirmation Dialog Box A 3 5 Insert Column Use the Insert Column command to add an additional column to the data table The command is available only for documents that can be manually edited TOC Control V method validation documents have a fixed number of columns equivalent to the maximum number of injections specified for the calibration points A 3 6 Delete Column Use the Delete Column function to delete a column from the data table The command is available only for documents that can be manually edited TOC Control V method validation documents have a fixed number of columns equivalent to the ma
320. ontact with eyes rinse immediately with plenty of water and seek medical advice Wear suitable protective clothing SECTION V TOXICITY DATA RTECS CZ4326000 1 2 BENZENEDICARBOXYLIC ACID MONOPOTASSIUM SALT ORL RAT LD50 gt 3200mg KG KODAK 21MAY1971 SKN GPG LD50 gt 1 GM KG KODAK 21MAY1971 Only selected registry of toxic effects of chemical substances RTECS data is presented here See actual entry in RTECS for complete information SECTION VI HEALTH HAZARD DATA ACUTE EFFECTS May be harmful by inhalation ingestion or skin absorption causes skin irritation vapor or mist is irritating to the eyes mucous membranes and upper respiratory tract EXPOSURE CAN CAUSE ASTHMATIC SYMPTOMS Cough hoarseness rhinorrhea wheezing and conjunctivitis nausea or vomiting Prolonged or repeated exposure may cause allergic reactions in certain sensitive individuals To the best of our knowledge the chemical physical and toxicological properties have not been thoroughly investigated SECTION VII FIRST AID MEASURES In case of contact immediately flush eyes or skin with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes If inhaled remove to fresh air if not breathing give artificial respiration If breathing is difficult give oxygen If swallowed wash out mouth with water provided per son is conscious Call a physician wash contaminated clothing before reuse SECTION VIII FIRE FIGHTING MEASURES
321. open a saved method validation file va A file can also be opened by clicking the Open toolbar button Start the method validation process by selecting a cal file application of DIN 38402 will begin The process can also be started by selecting the calibration curve row in the Sample Table and opening the method validation function using the Tools gt Method Validation command HE face e Pe January15 val PF Untitled val Pe Untitled yall val m oe aneta rea m Figure A 4 Open Dialog Box When the Open command is selected the File gt Open dialog box is displayed To open an existing file select the filename and choose the Open button To create a new method validation file type the filename into the File name text field then select the New button For further information on the standard functions of the Open dialog box refer to Section 4 4 2 4 Open Note An error message is displayed if a file that is not in a correct TOC Control V for mat is selected 350 W TOC VcPHicPN jinn Method Validation File Menu A 2 3 Save Use the Save command to save data in the current active file If the file has not been saved selecting the Save command opens the Save As dialog box The Save command can also be executed by clicking the Save toolbar button A 2 4 Save As Save in 5 Data z ce File name anuar 5 Save as type SAMT E SAAE 7 Cancel Figure A 5 Save As Dialo
322. operties Dialog Box Instrument parameters can be viewed and modified using the Instrument Properties dialog box shown below Open the dialog box by double clicking the instrument icon in the TOC Control V main window Instrument Properties a x System Options TOC as SSM Communication History System uoe Instr Serial No pomo Date of Creation 02720703080222 Comment o Print Cancel Figure 3 13 Instrument Properties Dialog Box System Tab The System tab displays the System Information window for the selected system and allows editing of the Comment field Options Tab The Options tab displays the oxidation method and instrument components that were selected in the Options window of the Instrument Setup Wizard Information on this tab can be viewed but not changed TOC Tab The TOC tab is identical to the TOC window in the Instrument Setup Wizard Some fields on the TOC tab can be edited If the History Log was enabled during setup edits to the TOC tab will be tracked and listed in the History tab ASI Tab The ASI tab is identical to the ASI window in the Instrument Setup Wizard Some fields on the ASI tab can be edited If the History Log was enabled during setup edits to the ASI tab will be tracked and listed in the History tab Communication Tab The Communication tab is identical to the Communication window in the Instrument Setup Wizard Some fields on the Communication tab can be edi
323. or ASI Solenoid Phosphoric Acid Light Source cin Sparge IC Reagent Solenoid Slide TC Absorber Sample Injector CO Absorber bin Tandem Cell Halogen Scrubber SampleCell 5mL Syringe E PA M ib Flow Control Dehumidifier ane L Capillary Detector Combustion Carrier Gas Tube TC Water Flowmeter Trap Pressure oy JJ SIIS Drain Pot Solenoid Gauge Mass Flow Cooling Tubing a Controller z Carrier Gas Pressure Inlet Valve Humidifier TOC VCPH POC Option Figure 2 9 Flow Diagram TOC VcPH POC Option 12 TOC VcPHI CPN Diluent Acid s fs Drain 6 2 ASI 1 l Sample Sparge Solenoid c 5mL Syringe Flow Control Capillary Carrier Gas Flowmeter Pressure Pressure Valve Carrier Gas Inlet Mass Flow Controller Backflow Prevention Valve O Humidifier Slide TC Sample Injector Tube TC Cooling Tubing Combustioon 2 1 Drain Pot Figure 2 10 Flow Diagram TOC Vcpn Diluent Acid ASI Sample Sparge Solenoid DOM 5mL Syringe Flow Control Capillary Backflow Prevention A Valve Slide TC Sample Injector Carrier Gas 0 Flowmeter Pressure Solenoid _ Sause Mass Flow Y A Controller a Carrier Pressure Gas Inlet Valve Humidifier
324. or Low Concentration Samples In manual injections of sample concentrations lower than lug mL it is necessary to take the following precautions to prevent contamination of the sample and the measurement process Injecting Sample into the Injection Port Use a separate micro syringe 500uL for high sensitivity measurement Any contamination on the sample injection port may affect the result for high sensitivity measurement The inside of the injection port can be contaminated by sample solution that adheres to the tip of the micro syringe needle When inserting the micro syringe into the injection port use extreme care to avoid touching the tapered portion of the inside of the sample injection port After filling the syringe wipe the excess solution from the needle surface with soft tissue paper Prevent excess drops of solution from forming on the tip of the needle by gently pulling back on the plunger Cleaning the Sample Injection Port Under normal operating conditions fill a 500uL micro syringe with pure water and insert it into the injection port Keep the bottom of the syringe barrel 8 10mm above the injection port Under normal operation the bottom of the syringe barrel is inserted until it comes into contact with the injection port allowing the needle tip to protrude from the needle guide pipe by about 5 6mm With the needle 8 10mm higher than normal operation the tip of the needle inside the needle guide pipe Slowly dispense the pure
325. ors in the two values are additive using TOC TC IC analysis This affect significantly influences TOC analysis For calibration measurement of standard solutions fill well washed containers with standard solutions to about 5 10 mm from the top of the container and immediately seal each container When placing the container below the 8 Port Sampler handle it carefully to avoid the standard solution contacting the sealing surface Low concentration standard solutions must be prepared each time they are used To ensure that the peaks are stable for generating the calibration curve perform 4 5 injections using the same analysis parameters prior to performing the calibration curve analysis For example to generate a 400ppb calibration curve set 400ppb as the Ist standard solution concentration and enter as the container number Actually place a Oppb solution in the container for port No 1 The objective at this point is not to generate a calibration curve but to inject water using the same injection volume that will be used to generate the calibration curve This not only stabilizes the instrument but also thoroughly washes the sampling needle with purified water In the 2nd row of the settings screen and using the same calibration curve number as above set the analysis parameters for Oppb and 400ppb When sample mea surement starts the calibration curve to be used will be created with the correct standard solutions 4 2 Setting General
326. ough the water supply port to the Hi marking on the side of the humidifier Note Use pure water containing as little TC as possible for high sensitivity analysis i Water Supply Port Pure Water oy Humidifier Hi Marking O Figure 4 13 Filling the Humidifier with Water TOC VCPH CPN 49 50 4 1 Analysis Preparation 4 1 6 Preparation of Dilution Water 4 1 6 Preparation of Dilution Water This section describes the preparation of water used to automatically dilute samples Procedure 7 Wash the provided dilution water bottle with laboratory glassware detergent rinse well with tap water then wash a number of times with pure water Fill the container with pure water to the 2 liter level Place the container to the left of the instrument toward the rear Pass the dilution water intake tubing labeled DILUTION through the hole in the cap Secure the tubing using a wire clamp about 200mm from the end of the tubing to prevent the tubing and cap from separating N MAY N Place the cap on the container Note Verify that the tip of the intake tubing nearly reaches the bottom of the container Dilution Water Intake Tubing Figure 4 14 Preparing Dilution Water Note About pure water e Use the purest water that can be obtained e Refer to Section 4 1 14 1 Preparation of Standard Solutions for details on the degree of purity of pure water
327. ounts of water for at least 15 minutes while removing contaminated clothing and shoes Assure adequate flushing of the eyes by separating eyelids with fingers If inhaled remove to fresh air If not breathing give artificial respiration If breathing is difficult give oxygen If swallowed wash out mouth with water provided person is conscious CALL A PHYSICIAN DO NOT INDUCE VOMITING If conscious give large quantities of milk or water Never give anything by mouth to an unconscious or convulsing person Get medical attention immediately SECTION Ix SPILL OR LEAK PROCEDURES Cleanup personnel should wear protective clothing and respiratory equipment suitable for toxic or corrosive fluids or vapors Isolate or enclose the area of the leak or spill Small spills Flush with water and neutralize with alkaline material soda ash lime etc Sewer neutralized material with excess water Larger spills and lot sizes Neutralize with alkaline material pick up with absorbent material sand earth vermiculite Provide forced ventilation to dissipate fumes For disposal neutralize with alkaline materials soda ash lime etc Dispose in a RCRA approved waste facility or sewer the neutralized slurry with excess water if local ordi nances allow Reportable quantity RQ CWA CERCLA 5000 labs Ensure compliance with federal state and local regulations SECTION X SPECIAL PRECAUTIONS AND COMMENTS The above information is believed to be correct but does not p
328. outer diameter of the container is too large the air to water contact efficiency is decreased requiring a longer sparge time Sparge Procedure 7 Refer to Section 4 1 9 Adjusting Sparge Gas Flow Rate for the sparge gas delivery procedure 2 Add 2M hydrochloric acid to the sample to adjust the pH to 2 3 3 Insert the sparge tubing into the sample To improve the sparging efficiency the tip of the sparge tubing should be as close to the bottom of the sample container as possible Note In this method sparge gas can be used independently While the first sample is being measured another sample can be sparged thereby improving analysis effi ciency 4 1 15 4 Analysis of Samples Containing Suspended Solids Effect on Analysis Large variations sometimes occur in TOC analyses of samples containing suspended solids because TOC is often contained in the suspended material This effect is evident when the same sample is analyzed on two different TOC analyzers Good results are not obtained if the suspended solids are handled differently in the gathering of biochemical oxygen demand BOD and TOC correlative data The suspended solids described here are primarily considered impurities in the sample that will pass through a 50 mesh strainer openings of approximately 0 28mm When larger solid particles are present analysis should be performed without drawing water into the instrument The procedure described below is for TOC analysis
329. owing the sequence described below acid can be released from the syringe connection port The sequence described below must be followed N caution Due to the potential for injury keep hands away from the sample injector during operation of the syringe pump unit The syringe barrel is made of glass and must be handled carefully to avoid break age Syringe Installation 1 2 A NAMM Open the TOC Control V Sample Table Editor and connect the instrument From the Instrument menu select Maintenance gt Change Syringe The Syringe Change dialog box is displayed Preparation Start a Verity Syringe SED vj Movement Iad ddj Stop Finish Replacement Figure 4 9 Syringe Change Dialog Box Click the Preparation Start button to begin the procedure A progress bar is active while the syringe moves to the position where it can be replaced When the progress bar begins blinking remove the screw at the bottom of the syringe pump cover and remove the cover Remove the sparge gas line from the syringe Remove the syringe from the syringe connection port of the 8 port valve Attach the new syringe to the syringe connection port of the 8 port valve TOC VCPH CPN 45 4 1 Analysis Preparation 4 1 3 Installing the Syringe amp Connect the sparge gas line to the syringe using the bushing and spacer Note Do not use tools when replacing the syringe hand tighten only Over tightening can deform the components of th
330. oxidation method Options Select the installed instrument components by clicking the appropriate check boxes The options include TOC ASI SSM solid sampler unit POC IC Unit TN Sparge Kit Manual Injection Kit 8Port Sampler 1 8Port Sampler 2 and ESU external scrubbing unit The selected options determine which Instrument Setup Wizard screens are displayed Select the IC Unit for the H type If Manual Injection Kit is selected the ASI SSM and POC options are disabled 24 ON PO CO Option 3 2 Instrument Setup and System Properties 3 2 2 Options Window Description TOC ASI SSM POC IC Unit TN Sparge Kit Manual Inj Kit 8 Port Sampler 1 8 Port Sampler 2 Displays the TOC screen of the Instrument Setup Wizard to allow TOC instrument parameters to be set Displays the ASI screen of the Instrument Setup Wizard to allow autosampler parameters to be set This option is disabled if the Manual Injection Kit option is selected Displays the SSM screen of the Instrument Setup Wizard to allow solid sampler unit parameters to be set This option is disabled if the Manual Injection Kit option is selected Specifies that the purgeable organic carbon accessory is installed Specifies that the instrument will be used to measure inorganic carbon Select this option for only instrument model TOC VcPH Do not select this option for instrument model TOC VcpN If the IC Unit is selected as an option the
331. parging Acid Addition Window for the ASI V Autosampler OCT 1 8 Port Sampler Sparging Acid Addition Window Figure 4 54 Sparging Acid Window for the OCT 1 8 Port Sampler TIP Zhe vial position for a sample can also be entered by placing the cursor in the appropriate row of the Sparging Acid Addition window and then double clicking the desired vial position in the tray diagram 106 WE TOC VcPrHichN inner 5 Verify the information then click the OK button The Sample Table is displayed Notice that the first row of the Sample Table now con tains complete TC calibration standard measurement information E Tutorial t32 Figure 4 55 TC Calibration Standard Information in the Sample Table 6 Insert the TN calibration standard runs by placing the cursor in the second line of the Sample Table From the Insert menu select Calibration Curve The Open dialog box is displayed Specify the name of the TN Calibration Curve TNtutorial cal and click the Open button CalCurves ca ce la TCtutorial cal B TNtutorial cal TNtutorial cal Calibration Curves cal _ Ver 00 00 01E User System System TC TN System Date of creation 01 15 01 01 50 47 PM H TOr AM A Figure 4 56 Select the TN Calibration File The Sparging Acid Addition window is displayed Notice that the TN calibration standards have been automatically added to the table 7 Enter the vial positions for the calibratio
332. peak time parameter USP EP check and history settings respectively Click the Finish button to create the new method Note Select the settings described in Section 4 2 Setting General Mea surement Parameters From the Insert menu select Sample Select the newly created method from the list of files in the Open dialog box Complete the remaining pages of the Sample Wizard amp From the Instrument menu select Start The Manual Injection Parameter dialog box is displayed 9 Draw an appropriate amount of sample into the syringe Note Draw in and discharge the sample 3 or 4 times before filling the syringe for measurement 70 Enter the injection volume in the Manual Injection Parameter dialog box and click the Set button 77 Verify that the instrument is ready for measurement and click the Start button 72 For TC or TN measurement open the injection port valve and insert the syringe needle into the injection port For IC measurement insert the syringe needle into the injection port septum Note Insert the syringe needle as far as possible into the injection port e To obtain reproducible results perform all injections at the same speed 73 Withdraw the syringe from the injection port For TC or TN measurement close the injection port valve 74 Click Additional Measurements to perform repeat measurements Repeat the procedure Click the Finish button when all measurements are complete Maintenance Replacing t
333. place the cover Label the shipping screw and store it for future use TOC VCPH CPN 317 6 8 Installation 6 8 4 Installing the Autosampler N caution To prevent instrument damage verify that the ASI arm is firmly attached to the retaining bracket with the shipping screw before shipping the instrument or moving it to another location Connecting Cables The TOC V and ASI V are connected using cables as described below L caution Verify that the TOC V is switched OFF before performing the following procedure Procedure 7 Connect the ASI V power cord at the rear of the ASI V to the ASI V power connector at the rear of the TOC V 2 Connect the provided signal cable to the ASI V signal connectors at the rear of the TOC V and the ASI V Figure 6 9 Connecting the Cables TOC V to ASI V 318 TOC VcPHICPN 6 8 Installation 6 8 4 Installing the Autosampler Connecting the Sample Tubing and Sparge Tubing External Sparge Kit The procedure for connecting the ASI V sample tubing and sparge tubing for the External Sparge Kit is as follows Procedure 7 Open the TOC Control V Sample Table Editor and connect the instrument 2 From the Instrument menu select Maintenance gt ASI Needle Change 3 Click the Preparation Start button The autosampler arm moves to the front of the needle replacement window allowing easy access 4 Remove the screw at the lower left side of the needle replacement w
334. ple Window The drop down list above the graph is used to set the graph display When Current Peak is selected the peak profile of the current injection is drawn in the graph as the measurement is performed Use this window to monitor the analysis as it occurs The blue peak denotes carbon while the red peak denotes nitrogen To see the peak profile of a previous injection click its row in the Injection Table To see the peak profile of all the injections for a sample select All Peaks from the drop down list at the top of the graph Use the graph right mouse menu to customize the peak profile graph Refer to Section 4 4 4 3 Sample Window for a detailed description of the Sample Window options 72 When the measurements are complete the autosampler moves to the rinse well for a flow line rinse and the instrument status tab displays a Ready status Close the Sample Window Evaluating the Results Step 7 The Sample Table now contains measurement information in the columns in the right portion of the table Use the scroll bars to view the measurement information We will check the calibration curve results and then evaluate the results for the unknown sample TOC VCPH CPN 4 3 Measurement Procedures and Tutorial 4 3 2 Tutorial Checking the TC Calibration Curve Results 7 Place the cursor in the first row of the Sample Table which contains analysis information for the TC calibration 2 From the View menu select Calibration
335. ple Wizard Page 7 History The History window is used to enable the History Log The History Log records all modifications to the control sample template properties The History Log can be set to require users to enter comments for each modification Note Once the History Log is enabled it cannot be disabled All modifications to the control sample template will be tracked If the mandatory comment option is selected the user will be required to enter a comment each time any parameter in the control sample template is modified Control Sample Wizard Page 7 History Figure 4 157 Control Sample Wizard Page 7 History Setting Item Description Enable history log Select this option to enable the software to monitor all modi fications to the control sample template Once the History Log is enabled it cannot be disabled If the History Log is not required it need not be enabled as the software operates properly without it User has to comment all Select this option to require comments or approval for all modifications modifications LLL TOC fm 199 Control Sample Wizard Page 8 Control Checking The Control Checking window is used to select options for control checks and control limits This window is not displayed if the USP EP system suitability criteria are used because the control limits are already defined Control Sample Wizard Page 8 Control Checking Figu
336. pm in Distilled Water Equilibrated with Atmosphere Temperature C Atmospheric CO 0 5 10 15 20 25 30 vol 0 030 1 00 0 83 0 79 0 59 0 51 0 44 0 38 0 033 1 10 0 91 0 76 0 65 0 56 0 48 0 42 0 044 1 47 1 22 1 02 0 87 0 74 0 64 0 56 The above CO content can be converted to IC using the following equation IC ppm CO mg L x 0 27 6 2 5 Automatic Selection of Optimum Calibration Curve Up to three different calibration curves can be selected for use in a method The curves are specified in the Calibration Curve 1 Calibration Curve 2 and Calibration Curve 3 fields on page 3 of the Method Wizard when the method is being created Refer to Section 4 4 2 3 Method Wizard for more information When more than one calibration curve is specified the TOC Control V software automatically selects the optimum calibration curve to be used for calculating measurement results TOC VCPH CPN 6 2 Analysis Related Technical Information 6 2 5 Automatic Selection of Optimum Calibration Curve The automatic selection process occurs on a measurement by measurement basis Measurement values are always calculated first using Calibration Curve 1 The TOC Control V software then evaluates the result applies the optimum calibration curve and recalculates the value if necessary The calibration curve with a concentration range that is greater than and closest to the measured value is used Example
337. preparation method described above 3 Introduce 100mL of each of the prepared standard solutions into a 1L volumetric flask 4 Add 25mL of 2M hydrochloric acid to the flask Add zero water to the 1L level NM Stir well to mix The hydrochloric acid concentration will be about 0 05M after dilution 4 1 14 2 Storage of Standard Solutions The standard solutions undergo concentration changes particularly when low concentration solutions are stored even for short periods As a result high concentration standard stock solutions for example 1000mgC L should be stored in airtight containers in a cool dark place Glass bottles are suitable storage containers Dilute the stock solution prior to each use Storage Time The limitation on storage of standard solutions is about 2 months for 1000mgC L standard stock solutions and about 1 week for diluted standard solutions for example 100mgC L The limitations are for cold storage in sealed containers Note IC standard solution absorbs atmospheric carbon dioxide and undergoes concen tration changes As a result it is particularly important to store IC standard solu tion in a sealed container Prepare fresh standard solutions e Ifreproducibility of analysis values is poor or concentration fluctuates Ifcontaminants including even small amounts of dust are present in the standard solution 62 TOC VcPHICPN 4 1 Analysis Preparation 4 1 15 Sample Preparation
338. r 4 4 4 View Menu When the mouse is positioned over a vial in the drawing of the of ASI or 8 Port Sampler a tool tip showing the vial number is displayed Click the vial to display the following items Parameter Description Vial No Displays the currently selected vial number Acid Addition rate Displays the acid addition rate for each vial Sparge time Displays the sparge time for each vial Total injection volume Displays the total injection volume for each vial TIP The desired vial position for a sample can be entered either directly into the Vial column or by placing the cursor in the appropriate row of the Sparging Acid Addition window and then double clicking the desired position in the tray diagram 4 4 4 10 Data Profile Displays the raw measurement data The data profile is never modified or processed following the initial collection It includes the corresponding measurement parameters The files which were created and named using the object ID each occupy a row in the sample table and are stored within the RawData folder in folders named using the date of creation The View gt Data Profile function is used to view the data profile for a sample Highlight the desired row of the Sample Table then select the command 180 TOC VCPH CPN 4 4 5 Insert Menu The Insert menu contains options for inserting sample groups calibration curves individual samples and control samples into the Sample Table 4 4 5 1 Auto Generat
339. r SHOW Difrae senenn a e est icine Is NSST 11 2 2 Autosampler ASI V Option cecccssecssesteceseceeceeeeeseeeseeeseceeeeseeeseeesees 14 DD HETON VIEW coran bes OR ER eee A 14 DIDS Rear Vi Weee ea tase E E wah oie uate eeaas ating pete aoe 14 2 3 8 Port Sampler OCT 1 Option 0 cccceeseceseceeeeseeesecneeceteeeeeeseeeeeenaes 15 2S Front Vie W mecene oc ar decent hosed WO a A A A ee eat 15 DBD SREAPNICW 6 dele AE A etce cei A bas a8 12 Cees doesds 15 2 4 TN Unit TNM 1 Option ec cccccccessesceestecneceeeeeeeeseeeseceeceeeeeseeeseenaees 16 2 4 1 Front and Right Side Views 0 ccsccssessessecesceeseesceseeseeeseeesecaeeaeeeenseeeeneeees 16 2 4 2 Inside Front View secs sec c ceccccecccdes kenij chs caen E E E RER 17 DAB RAT VIG Weens ennea ota te ese hee a Re RE RR 18 Software Overview Administration and Setup ccccccscsccsssreeee 19 3 1 Introduction to System Administration Functions cesceceeseereeeeeees 20 31 1 Sereen Lock Function sereni hacen dhs es ee Bess 20 3 1 2 Change Password wi 0 2ccc c a deiiinieeteicacleseteien oes aviv edie Peele 21 JEF Add Event EOT st s enr eea aa aE Eeee ea E e S ER 22 TOC VcCPH CPN xiii Table Of Contents 3 2 Instrument Setup and System Properties ccccccecscesseesseceseeeeeeteeeteeseens 23 3 2 1 System Information Window ccccccecseeseeseessesseeseceeceeeeeceeeerenseeeeenseenteees 23 32 2 Options Windows ated section
340. r analysis using both the coaxial needle and a sparge needle which allows a sample to be measured while the next sample is sparged The Needle field is enabled only if Sparge Kit was selected in the Options window of the Wizard Note The instrument does not automatically recognize the type of needle installed Be sure to select the type of needle that is actually installed in the instrument No of Needle Washes Enter the number of times 0 10 the outside of the needle will be washed with water from the dilution water bottle at the end of a sample run No of Flow Line Washes Enter the number of times 0 10 the flow lines will be washed after all samples listed in the Sample Table have been measured Water from the dilution water bottle is used to wash the flow lines TOC VCPH CPN Rinse Select this option to rinse the sampling needle between each sample with water from the dilution water bottle Rinse After Acid Addition Select this option to rinse the sampling needle after each acid addition with water from the dilution water bottle Stirrer On Select this item to use the optional magnetic stirrer during measurement 3 2 5 SSM Window The SSM window of the Instrument Setup Wizard is displayed if SSM was selected in the Options window of the Wizard Use the SSM screen to set the SSM parameters Refer to the SSM 5000A User Manual for details Instrument Setup Wizard SSM Figure 3 10 Instrument Setup Wizard
341. ration of POC Standard Solution using the optional POC analysis kit IC standard solution is used as the POC standard solution with this instrument for the following reasons In POC analysis the measured substance is an organic material that is volatile and poorly soluble in water for example benzene or chloroform Preparing a stan dard solution at an appropriate concentration using these types of organic sub stances is difficult Volatile and poorly soluble organic substances tend to undergo changes in concen tration during storage or handling after preparation e Standard solutions that are produced using volatile and poorly soluble organic sub stances are difficult to use Consequently the IC standard solution is used for this instrument The preparation method is listed above TC TN Mixed Standard Solution Preparation Procedure When TC or NPOC and TN analyses are performed simultaneously a mixed TC and TN standard solution is prepared The mixed standard solution is prepared by mixing the TC standard solution and TN standard solution The mixed standard solution must contain 0 05M hydrochloric acid TOC VCPH CPN 61 4 1 Analysis Preparation 4 1 14 Preparation and Storage of Standard Solutions Preparation of 100mgC L TC 100mgN L TN Mixed Standard Solution 1 Prepare 1L of 1000mgC L TC standard solution using the preparation method described above 2 Prepare 1L of 1000mgN L TN standard solution using the
342. rd Page 5 Peak Time Parameters Sample Wizard Page 5 Peak Time Parameters Figure 4 146 Sample Wizard Page 5 Peak Time Parameters Parameter Description Analysis Displays the analysis type This field cannot be changed Use default settings Select this option to use the default integration parameters When this option is selected all other options in this window are disabled Allowed peak start delay The allowed peak start delay is the amount of time in min utes that can elapse before the analysis is stopped because a peak is not detected Enter a number between 0 and 20 00 Total integration time The total integration time is the amount of time in minutes that analysis continues after the end of the peak is detected Enter a number between 4 50 and 20 00 190 WE TOC VcrHicen neem Sample Wizard Page 6 Calibration Curve A second Calibration Curve window is only displayed when more than one analysis type has been specified This window is the same as Page 3 of the Sample Wizard which is described above Verify the analysis type in the Analysis text box at the top of the page and make the appropriate selections Sample Wizard Page 6 Calibration Curve Parameters Cal Curve Gen Info orporation T 003201 CalCurves T Ntutorial cal System
343. re 4 158 Control Sample Wizard Page 8 Control Checking Setting Option Description Recovery Select this option to check recovery amounts in control sam ples Spiked Select this option to use an original and a spiked sample to Original Concentration Spiked Concentration Mean Value Concentration Blind Value Area Spanwidth Concentration Max Dev Low Up 200 Wim TOC VcrHicPN jinn calculate the recovery amount This option is enabled only when the Recovery option is selected Enter the original concentration of the spiked sample This field is enabled only when the Recovery option is selected Enter the concentration of the spiked sample This field is enabled only when the Recovery and Spiked options are selected Select this option to check the mean value of the measured concentrations Select this option to check the mean value of the measured area values Select this option to check the deviation of the measured con centrations Enter the maximum acceptable deviation This field is enabled only when the Spanwidth option is selected Enter the lower limit of the valid control range if the Blind Value option is selected Enter the upper limit of the valid control range if the Blind Value option is selected Control Sample Wizard Page 9 Failure Action The Failure Action window is used to specify the actions taken when a control sample exceeds the specified control limits ontrol Sample
344. reathing apparatus rubber boots and heavy rubber gloves Absorb on sand or vermiculite and place in closed containers for disposal Ventilate area and wash spill site after material pickup is complete SECTION X SPECIAL PRECAUTIONS AND COMMENTS The above information is believed to be correct but does not purport to be all inclusive and shall be used only as a guide SHIMADZU shall not be held liable for any damage resulting from handling or from contact with the above product Users should make their own investigations to determine the suitability of the infor mation for their particular purposes TOC VCPH CPN 335 336 6 9 Material Safety Data Sheets 6 9 4 Lithium Hydroxide monohydrate 6 9 4 Lithium Hydroxide monohydrate Shimadzu Scientific Instruments Inc 957002 7102 Riverwood Drive Columbia MD 21046 Control No Tel 1 800 477 1227 November 1995 MATERIAL SAFETY DATA SHEET SECTION I PRODUCT IDENTIFICATION CAT NO 630 00961 00 CAS NO 1310 66 3 NAME Lithium Hydroxide Anhydride 99 95 OTHER NAME Lithium Hydroxide Hydrate Lithium Hydroxide Anhydride DOT N2680 DOT TRADE NAME IC Absorbent PRODUCT USE This product is for specific use with TOC instruments SECTION IT PRECAUTIONS TO BE TAKEN IN HANDLING Wear appropriate NIOSH MSHA approved respirator chemical resistant gloves safety goggles other protective clothing Safety shower and eye bath Use only in a chemical fume hood Face shield 8 inch minimum Do
345. red to as total nitrogen TN The principles underlying TC and TN analysis are explained in the following sections 6 1 1 Principles of TC Total Carbon Analysis Sample is introduced into the TC combustion tube which is filled with an oxidation catalyst and heated to 680 C The sample is burned in the combustion tube and as a result the TC components in the sample are converted to carbon dioxide Carrier gas which flows at a rate of 150mL min to the combustion tube carries the sample combustion products from the combustion tube to an electronic dehumidifier where the gas is cooled and dehydrated The gas then carries the sample combustion products through a halogen scrubber to remove chlorine and other halogens Finally the carrier gas delivers the sample combustion products to the cell of a non dispersive infrared NDIR gas analyzer where the carbon dioxide is detected The NDIR outputs an analog detection signal that forms a peak the peak area is measured by the TOC Control V software The peak area is proportional to the TC concentration of the sample A calibration curve equation that mathematically expresses the relationship between peak area and TC concentration can be generated by analyzing various concentrations of a TC standard solution The TC concentration in a sample can be determined by analyzing the sample to obtain the peak area and then using the peak area in the calibration curve equation TOC VCPH CPN 6 1 Principle
346. reeeceeeneeee 359 Material Safety Data Sheets See MSDS Index 5 Method Wizard Acid Addition Volume ccecceseeeceeeeeeeeee 139 Analysis Information 0 cc eeseeseeeeeeeneeees 136 Auto Dilution c cece ccecceeseeseeceseeseeeeeeeeeeeeeeee 139 Calibration Curve ssiri 137 Creating New Method cccececessesseeeeeeseens 135 CV IMR eei 138 Determinations 136 History Log 142 Injection Parameters ccceceseeseeteeteeeeseeee 138 Injection Volume cceeesecseesecesenseeteeseeseees 138 Multiple Injections eeeeeeseeseeereeeees 139 Number of Injections ccccccecseeseeseereeeeeeeees 138 Opening i2 teen 126 Peak Integration Parameters 140 SD Maxi eodeni 138 System Information 0 0 0 ccecececeeeeeseeeeeeeeees 135 Using Blank Check Area wo teeters 139 WS PARP sc 25 2 aaciheas a des ei a 141 Needle Chante lt t 20cci ii needle eens 268 Coax al ssisacaccecvisdiscb ieiandaeiaeens 28 85 Coaxial Sparge cceccseesesseeseeseeeeseeeeeees 28 85 Installation Coaxial ccccccescecsecsscesseeseeeeees 322 Installation Sample eee eee eeeeeeeeeeeeees 321 Rins verifies ea Out ee a E S 85 Rinse after Acid Addition ccc esesesereereees 86 Samples ahina ee ee 28 85 Samplet Sparge cccccecesceceseeteeteeteeneeeeee 28 85 Setting in Software wo cee eeeseeeceereeeeee 28 85 TIPES eener a 28 85 320 OCT 1 2 See 8 Port Sampler
347. rement data in real time place the cursor in the row of the Sample Table that contains the current sample then open the Sample Window The Sample Window is divided into 3 sections the Graph the Parameter Table and the Injection Table Note that the sections can be resized by dragging the dividers between sections 7 Sample Name Standard _ 4 Sample ID Tutorial Analysis TC TN q Dilution 1 0000 Result TC 50 00ppm TN 10 0 isl j Figure 4 123 Sample Window Graph The upper left section of the Sample Window displays the peak profile graph Change the graph type by choosing from the options on the drop down list Setting Items Description Current Peak Displays the peak profile of the highlighted injection All Peaks Displays all injection peaks for the selected sample Calibration curve Displays calibration curves for calibration standards only This function is not available during real time analysis Note To view the peak profile of the measurement in progress click the row with the asterisk in the Sample No column To view a previous measurement click the desired row Parameter Table The upper right section of the Sample Window displays sample parameters Setting Item Description Sample Name Displays the name of highlighted sample Sample ID Displays the sample identification from the Sample Table Analysis Displays the analysis method used for the sa
348. rent option from the drop down list Two calculation methods are available point to point and linear regression For both types a curve represent ing the relationship between detector response and concentration is displayed The point to point curve fit draws a straight line between adjacent data points and considers each line segment to be a separate calibration line governed by its own equation A linear regression statistically determines the line that best fits the pat tern of all data points The number used to describe the agreement between the calculated line and the data points is called the Coefficient of Determination a A coefficient of 1 indicates that the line fits the data points perfectly The general equation for a straight line is Y mX b where Y Y axis data point X X axis data point m slope of line b Y axis intercept point TOC VCPH CPN 171 Setting Item Description Zero Shift Multiple Injections Calibration Curve File Analysis Tab Select Zero Shift to shift the regression curve through the origin Note that this option does not change the slope of the line Use this option as a correction when the TC content in the Zero water used to prepare the calibration standards is too large to ignore Select to enable the syringe to draw up a single aliquot with a volume equal to that required for all injections of the standard When this option is not selected the syringe will draw up a separate aliq
349. report i Page setup MDate of creation CComments Figure 4 107 Page Setup Window Header Tab LLL TOC fy 753 Miscellaneous Tab The Miscellaneous tab displays a list of format items for the report as described below Page setup x Instrument Calibrations Samples Header Miscellaneous Date Time M User IV Document name Figure 4 108 Page Setup Window Miscellaneous Tab Setting Item Description Margins Use the spin controls to enter the page margins in mm Footer Page No Select this option to print the page number in the footer of each page Header Organization Select this option and enter the name of the organization in the text box to print the organization name in the page header Logo Select this option to print a bitmap in the page header Use the Browse button to select the bitmap file Date Time Select this option to print the current system date and time in the page header User Select this option to print the current user name in the page header Document name Select this option to print the document file name in the page header LSA QQ ON PN 4 4 2 16 Exit The Exit command is used to exit the Sample Table Editor If the active file has been modified but not saved and the Exit command is selected a dialog box is displayed as shown below Click the Yes button to save the file before exiting Click the No button to exit without saving the modified information Cli
350. ric furnace lt Prevents the floating of high sensitivity catalyst gt e Allow the electric furnace to cool to room temperature before removing or exchanging the combustion tube Burns may result if this procedure is attempted when the furnace is at a high temperature lt Burn prevention gt e Do not heat the electric furnace without the combustion tube installed Parts employed by the TC injection port slider block assembly will be exposed to radiant heat from the center of the electric furnace and may be deformed If the furnace must be heated with out a combustion tube installed first remove the TC injection port parts to prevent deformation or close off the furnace core opening with a heat insulating material such as quartz wool lt Part damage prevention gt To reduce back pressure verify that the external drain tubing connected to the waste port on the right side of the instrument does not touch the surface of the liquid in the waste container The height of the external tube must always be lower than the height of the drain port Excessive back pressure will result in insufficient drainage and waste will overflow inside the instrument lt Part corrosion prevention gt Drain tubing Tubing placement should be as indicated by the solid line Drain container Supplied by user Figure 1 1 External Drain Tubing e Hand tighten the various connectors to the 8 port valve Use of a tool may cause deformation and leakage i
351. rnative means of operation or useful advice Reference Indicates a reference location in the manual where more detailed information can be found vi TOC VCPH CPN Warning Labels Used on this Instrument Warning Labels Used on this Instrument High Temperature Warning When the electric furnace is heating up or is at its operational temperature 680 C or 720 C the central portion of the electric furnace is extremely hot To prevent burns NEVER touch the electric furnace area with bare hands Allow the furnace to cool before performing any maintenance on the combustion tube or catalyst A CAUTION HOT SURFACE Burn Risk Cool sufficiently before performing maintenance The internal temperature of the ozone treatment unit reaches 50 C while the instrument is running To prevent burns switch off the TN unit and wait at least 2 hours for the unit to cool sufficiently before performing any maintenance ACAUTION HOT SURFACE Avoid touching when at higher temperatures YA A oye A Olz o Le o E lHo TOC VCPH CPN vii viii Warning Labels Used on this Instrument Electric Shock Warning Do not remove this panel as there is danger of electric shock 2 OTS 2 o RISK OF ELECTRIC SHOCK DO NOT open this cover o o oToToTo AL
352. rols to enter the page margins in mm Footer Page No Select this option to print the page number in the footer of each page Header Organization Select this option and enter the name of the organization in the text box to print the organization name in the page header Logo Select this option to print a bitmap in the page header Use the Browse button to select the bitmap file Date Time Select this option to print the current system date and time in the page header Operator Select this option to print the current user name in the page header B 1 11 Exit Select Exit to close the Control Chart application Control Charts Edit Menu B 2 Edit Menu Copy Cree a Recalculate Exclude Figure B 12 Edit Menu Copy Use the Copy command to copy the selected range from the data table to the clipboard Recalculate Use the Recalculate command to recalculate the limits of the control chart This function should be performed after one or more control samples have been excluded or added to the control chart Exclude Use the Exclude command to exclude a selected range of control samples from the control chart calculations When Exclude is selected the Exclude dialog box is displayed Enter a comment describing the reason for excluding the sample The Exclude function is only available when one or more control samples are selected A dialog box displays a message requesting confirmation that the sample be excl
353. rows or cells and stores it on the clipboard Note that the Cut command cannot be used to delete entire samples after measurement is completed The Copy command copies selected data from rows or cells and stores it on the clipboard The Paste command copies the contents of the clipboard to the selected cells or rows of the table When pasting an entire row click the destination row number to highlight the entire destination row then execute the Paste command Note When pasting do not select a destination row that currently contains data The data will be overwritten e The Cut Copy and Paste commands can also be accessed by clicking the icons on the Toolbar TOC VCPH CPN 4 4 Sample Table Editor 4 4 3 Edit Menu 4 4 3 3 Replace 4 4 3 4 Find The Replace function is used to replace text in Sample Table cells with specified text Select the Replace function to open the Replace dialog box The Replace command can be used to replace data in the Sample Name Sample ID Dilution and Comment fields of the Sample Table The command cannot be used to replace data for samples after measurement is complete Replace 2 x Find what fT C Replace with Replace Replace All Cancel I Match case Figure 4 112 Replace Dialog Box Setting Item Description Find what Enter the text to be searched for Replace with Enter the text that the searched for text should be replaced with Match case Select to perform a case sensitiv
354. rposes TOC VCPH CPN 339 340 6 9 Material Safety Data Sheets 6 9 8 Normal Sensitivity Catalyst 6 9 8 Normal Sensitivity Catalyst Shimadzu Scientific Instruments Inc 7102 Riverwood Drive Columbia MD 21046 Control No Tel 1 800 477 1227 Date MATERIAL SAFETY DATA SHEET SECTION I PRODUCT IDENTIFICATION CAT NO 017 42801 00 and 017 42801 01 CAS NO 7440 06 4 Platinum and 1344 28 1 Alumina NAME Regular Sensitivity Catalyst OTHER NAME Platinum on 1 8 Alumina Pellets SECTION IT PRDUCT USE This product is specifically for use as a catalyst in the TOC 500 TOC 5000 and TOC 4000 series of TOC analyzers Refer to the appropriate instruction manual for directions on proper use SECTION II PHYSICAL DATA Melt Boil Density Vapor Vapor Evaporation Odor Color Phase Water Point Point Pressure Density Rate Solubility N A N A N A N A N A N A N A Grey Solid Pellets N A SECTION IV HAZARDS IDENTIFICATION FLAMMABLE Possible sensitizer keep away from sources of ignition no smoking Take precautionary measures against static discharges Keep container tightly closed and in a well ventilated place Harmful by inhalation Irritating to respiratory system TARGET ORGAN S Lungs bones do not breathe dust In case of insufficient ventilation wear suitable respiratory equipment Wear suitable protective clothing SECTION V TOXICITY DATA ACUTE EFFECTS May be harmful by inhalation or ingestion May caus
355. rs to the total volume of sample that can be injected into the combustion tube before catalyst and combustion tube mainte nance is required e Dilution Water Refers to dilution water volume Total Acid Volume Refers to the total volume of acid used Syringe Stroke Refers to the number of syringe operations e UV Lamp Refers to time of operation of UV lamp IC Unit Pump Tubing Refers to time of IC unit pump tubing use The recommended warning value is 300 hours ASI Rinse Pump Refers to time of ASI rinse pump tubing use The recommended warning value is 300 hours Procedure 7 From the Instrument menu in the Sample Table Editor window select Maintenance gt History The Maintenance History dialog box is displayed Maintenance History Dig E x Total operation time hour 0 Preset Limit Current Total TC InjVol m 0 f Rese Dilution water ml po 0 Reset Total Acid voljo Reset Syringe Stroke no fo 0 Reset UY Lamp hou if Ozone Generator hour fe UY Oxid Vol ul Poo IC Unit Pump hour pooo ASI Rinse Pump hour po Cancel Figure 4 29 Maintenance History Dialog Box 2 Enter warning limits by placing the cursor in the appropriate fields and entering numeric values 3 Click the OK button TIP Measurement will be interrupted if the dilution water or acid reservoirs run dry during analysis To prevent measurement interruption set the dilution water and total acid volume
356. rt data Select to enable export of the selected data options This option is selected by default Miscellaneous Tab ASCII Export Options T abulator J M Figure 4 98 ASCII Export Options Window Miscellaneous Tab The Miscellaneous tab contains additional options for the format of exported data To change data format open a Sample Table select File gt ASCH Export Options then select the file to which changes should be made On the Miscellaneous tab select the desired type of Separator from the drop down list The Separator is the type of delimiter that will be used to separate items of data Select the Export strings in quotation marks option to enclose all of the character string items in quotation marks 4 4 2 9 Database Export The Database Export command is used to enable automatic export of data to an external Microsoft Access database during analysis Selecting the command displays the Database Options window Database Options Figure 4 99 Database Options Window Setting Item Description Enable automatic database Select this option to enable the database export function export Database Enter the name and filepath of the database or click the Browse button to select the database using the File gt Open dialog box LS QQ VON APN LS 4 4 2 10 Print gt Table The Print gt Table command is used to print the active Sample Table in a table format Select this command to open the Print dialog bo
357. rument and communication errors are displayed in the Notification Bar The Background Monitor window cannot be open during measurement TOC Tab c und Monitor Toc tN Jasi Fumace SEED Dehumidifier EE NDIR Baseline Pos K Baseline Fluc Baseline Noise NDIR Figure 4 161 Background Monitor Window TOC Tab Parameter Description Furnace Displays the temperature of the TC furnace Dehumidifier Displays the temperature of the dehumidifier NDIR Baseline Pos Displays the status of the NDIR detector baseline position Baseline Fluc Displays the status of the NDIR detector baseline fluctuation Baseline Noise Displays the status of the NDIR detector baseline noise The bottom portion of the TOC tab window displays a graph of the selected items TOC VcPHICPN 203 TN Tab Background Monitor Signal m Time min Figure 4 162 Background Monitor Window TN Tab Parameter Description TN Reactor Displays the temperature of the TN reactor Chemiluminescence Baseline Pos Displays the status of the chemiluminescence detector baseline position Baseline Fluc Displays the status of the chemiluminescence detector baseline fluctuation Baseline Noise Displays the status of the chemiluminescence detector baseline noise The bottom portion of the TN tab window displays a graph of the selected items ASI Tab The ASI tab is available only if the ASI is connected
358. s eee 71 41 16 Sample Preparation hao enn nn RENEK R E ER A eh 72 AVVO 1 C Vital Bry pests 2ecce cases A E tober ets taaes codes nhgee oot 72 4 1 16 2 Filling Vials with Sample cccccecescesseesseeeecsseeseeseceeeeeeneesseeeeeees 72 4 1 16 3 Placing Vials in the Vial Rack c ce ceccecseesseesecseeesececeeeeteeereneeaes 74 4 1 16 4 High Sensitivity Autosampler Analysis cc seseseeseeceeceeereeeeeees 75 4 1 16 5 Acid Addition in NPOC Analysis 0 ccccsceeseeseeseseceeceseeteeeeeeteeaes 76 4 1 16 6 Sparging in NPOC AnalySis ccccsesessesecseceeeseeeeeeseeeeeeseeneeeaes By A1167 Stirrer Preparation 43 30 taei een ain Ra awe wan iawn 78 xiv TOC VCPH CPN Table Of Contents 4 1 17 8 Port Sampler Measurement cccsceccessesscesceeeceeceseeesecaeeeaeeeeeaeensenseens 80 4 1 17 1 Type of Sampler Container ccccecccesceseesceeeeeeceseeseeeseeeeeeeeneeenees 80 4 1 17 2 High Sensitivity Using the 8 Port Sampler eee eeeeeeeteeeeeeeees 82 4 2 Setting General Measurement Parameters ccceseesceceseeeeeneeeeeeteeaeenee 83 4 2 TOC Parameter Settings enner en a taco ene A eee 83 4 2 2 AST Parameter Settings 2 0 ccceesecscceseeseceeceeeeescesceeeceseeeeecaeeeecaeenaeeeeeeeeeees 84 4 2 3 Setting Default Measurement Parameters c cecceeseesceeseeseeeseeeeneeeteerens 87 4 2 4 Maintenance History Settings cccecceccsssesscesceesceeceeeeeseeeecaeeeececneee
359. s from the air If a compressor is used install the air filter equipped with drain separation and discharge branch close to the tubing connection at the instrument e Ifa compressor is used select an oil less type air compressor The oil less air compres sor SLP 5D 2 SVF P N 638 59203 01 is available as an option Using a High Purity Air Filled Cylinder Via Branch Tubing from Carrier Gas High purity air is synthesized air using pure nitrogen and pure oxygen Ensure that contaminants including carbon dioxide carbon monoxide and total hydrocarbons are guaranteed not to exceed Ippm each Install a pressure regulator on the gas cylinder and supply gas to the instrument so that the pressure is 300kPa at the instrument gas connection port Note If there are excessive contaminants in the carrier gas measurement results will be adversely affected due to low measurement reproducibility etc TOC VCPH CPN 329 6 8 Installation 6 8 6 Installing the TN Unit AN Precautions in Handling Gas Cylinders The handling and safety management of high pressure gases is strictly regulated by high pressure gas control laws general high pressure gas safety codes and fire laws The gas used in this instrument itself is not dangerous but mistakes in the handling of high pressure gas cylinders can be extremely hazardous Carefully read and obey the following precautions e Place gas cylinders in a well ventilated location out of direct sunlight
360. s appropriate Select the desired options on pages 6 and 7 of the Calibration Curve Wizard which list peak time parameter and history settings respectively Click the Finish button to create the new calibration curve Note Select the settings described in Section 4 2 Setting General Mea surement Parameters Create a Sample Table for the calibration curve From the Insert menu select Calibration Curve Select the newly created calibration curve from the list of files in the Open dialog box Connect the instrument by selecting Connect from the Instrument menu Then select Start from the Instrument menu The Manual Injection Parameter dialog box is displayed Draw an appropriate amount of sample into the syringe Note Draw in and discharge the sample 3 or 4 times before filling the syringe for measurement Enter the injection volume in the Manual Injection Parameter dialog box and click the Set button Verify that the instrument is ready for measurement and click the Start button For TC or TN measurement open the injection port valve and insert the syringe needle into the injection port For IC measurement insert the syringe needle into the injection port septum Note Insert the syringe needle as far as possible into the injection port e To obtain reproducible results perform all injections at the same speed Withdraw the syringe from the injection port For TC or TN measurement close the injection port valve Th
361. s are shown below 1 2 3 4 If the measured value is less than the concentration of Calibration Curve and greater than the concentration of Calibration Curve 2 and Calibration Curve 3 Calibration Curve is used Conc of Calibration Curve 1 gt Measured Value gt Conc of Calibration Curves 2 and 3 gt Calibration Curve 1 is used If the measured value is less than the concentrations of Calibration Curve 1 and Calibration Curve 2 and if the concentration of Calibration Curve 2 is less than that of Calibration Curve 1 Calibration Curve 2 is used Conc of Calibration Curve 1 gt Conc of Calibration Curve 2 gt Measured Value gt Calibration Curve 2 is used If three calibration curves are specified the calibration curve that is greater than and closest to the measured value is used Conc of Calibration Curve 1 gt Conc of Calibration Curve 3 gt Measured Value gt Conc of Calibration Curve 2 gt Calibration Curve 3 is used If the measured value is greater than the concentration of all curves and the concentration of Calibration Curve is greater than the concentration of Calibration Curves 2 and 3 Calibration Curve 1 is used Measured Value gt Conc of Calibration Curve 1 gt Conc of Calibration Curve 2 gt Conc of Calibration Curve 3 gt Calibration Curve 1 is used Note By setting the concentration ratio between calibration curves to a factor of approximately 10 the automatic selection f
362. s containing the data to be tested From the View menu select Outlier Test The Outlier Test window is displayed Select either Conc or Area CNV for the data source Exclude the injection that is suspected of being an outlier then select OK to close the dialog box If the sample does not contain enough injections for the test to be performed an error message is displayed and the Outlier Test window will not open The Outlier Test window contains the parameters listed below Setting Items Description Result List Displays the result of the Outlier Test Conc radio button Select to indicate that test calculations are to be performed based on the concentration data Area CNV radio button Select to indicate that test calculations are to be performed based on the area data Result Displays the result of the test Exclude button Click this button to exclude a suspect sample and recalculate the test result Suspicious inj Indicates the injection suspected of being an outlier which is identified as the sample with the highest deviation from the mean value SD Displays the standard deviation for all of the injections CV Displays the coefficient of variation for all of the injections Grubb Value Displays the corresponding value from the Grubb table Test Value Displays the calculated Outlier Test value TOC VCPH CPN 169 4 4 Sample Table Editor 4 4 4 View Menu 4 4 4 5 Properties The View gt Properties function display
363. s gt Notification Bar Settings The Display Settings gt Notification Bar Settings function is used to set options for the Notification Bar where error messages and other notices are displayed The Notification Bar is located at the bottom of the Sample Table Editor window Four folders can be displayed in the Notification Bar Notifications System Folders Errors and Events When a folder is selected for display a tab appears for that folder in the Notification Bar When more than one folder is selected for display the contents of a specific folder can be displayed by clicking the appropriate tab Notification Bar Settings x T Display Folder System Folder Max Number of Displayed Lines Figure 4 178 Notification Bar Settings Window Setting Item Description Folder List Lists the folders that can be displayed in the Notification Bar Display Folder Place a check in this box to display the folder Max Number of Displayed Enter the maximum number of lines to be displayed in the Lines Notification Bar Acceptable values range from 0 to 200 Font Displays the selected font Modify the font by selecting the Browse button to open the Font dialog box To select a folder for display in the Notification Bar click the folder in the Folder List then select the Display Folder option Set the Max Number of Displayed Lines field to a value greater than 0 To change the color or appearance of the text displayed in the fold
364. s of Analysis 6 1 2 Principles of IC Inorganic Carbon Analysis 6 1 2 Principles of IC Inorganic Carbon Analysis Two methods for measuring IC using the TOC V are available analysis within the injection syringe and analysis using the optional IC reactor In both methods the measured IC consists of carbon derived from carbonates hydrogen carbonates and dissolved carbon dioxide Defining IC The IC measured by TOC analysis consists of the carbon contained in carbonates and in carbon dioxide dissolved in water By acidifying the sample with a small amount of hydrochloric acid to obtain a pH less than 3 all carbonates are converted to carbon dioxide CO3 by the following reactions Me CO3 2HCI gt CO 2MeCl H2O MeHCO HCI gt CO MeCl H2O Carbon dioxide and dissolved carbon dioxide in the sample are volatilized by bubbling sparging air or nitrogen gas that does not contain carbon dioxide through the sample Analysis Using the IC Reaction Vessel H Type Instrument The TOC V IC reactor kit is used to sparge the IC reaction solution acidified reaction liquid with carrier gas Sample is injected into the IC reaction vessel and the IC in the sample is converted to carbon dioxide which is volatilized by the sparging process and detected by the NDIR Analysis Within the Syringe N Type Instrument The sample is acidified to pH 3 or lower in the syringe using hydrochloric acid The sample is sparged with carrier gas
365. s s ated nineio iie Gas Flow Rate Wet Chemical Gas ValVescscscsesineioatinaches NPOC Analysis 0 cceecesesscsseeeecreeeceeceeeeeneeeeees Time Settings onere tibet escent Sparging Acid Addition Window esses Special Accessories Specifications Autosampler eeee Carrier Gas Purifier Kit Gas Sample Injection Kit eeeeeeeees Manual Injection Kit eee eeceeeeeeeeeee POG Kitee rte EAEE s Manual Injection Kit POC Kit aaa ete TN eae ea E A dis uel E AE E E TOG V CPH CPN onina nine naa 298 TC Analysis New Catalyst cecsseceecresecteeeeees 36 Blank Check 0 66 269 Principles 4 1 284 Standard Solution ccccccccesessceseesseeeeesseees 60 TC TN Standard Solution ccccccescesessecereesseeees 61 IRES L AAE E EN ENEN SETANE a ee 288 Technical Information ccccscecereesseeeee 289 293 Time Sparte lasno a e E ee 139 Standard Solution Analysis 0 0 High Sensitivity o enee aaa es 64 Preparing nana aE EE E OES 60 Spar Sines enea a A RE EA ET 292 StOPING senesenca aiii iaia 62 Standby Window 120 206 Starting The Instrument 0 0 0 eee eee seeeeeeeeeeees 207 Starting the Instrument ee ceeeeseeeceeeeeeeeteeeeees 89 Status Bare csdcscccssscccsess ces seadescecgeccudde cevecseasects 124 178 DUMPED oss E a E aE E E ni 78 86 Stopping the Instrument Halt e T 207 Stop Finish Current
366. s specifications standard and optional accessories and specialized terms associated with this instrument This chapter also includes the installation procedure for use in the event that instrument is moved to another site Appendix A Method Validation This appendix describes the software s Method Validation tool which is used to test the variance and linearity of a data set Appendix B Control Charts This appendix describes the software s Control Charts tool which is used to monitor the precision and accuracy of a data set TOC VCPH CPN Notation Conventions Notation Conventions Precautionary Conventions Used in this Manual The following precautionary conventions are used in this manual Convention Description CAUTION Indicates the possibility of slight to moderate injury or equipment dam age Note Provides additional information to ensure the correct use of the instru ment Other Conventions Used in this Manual Instrument Model Names Descriptions in this documentation pertain to two models of the TOC V Total Organic Carbon Analyzer namely the TOC VcPH and TOC VCPN These models will be referred to in relevant descriptions as the H Type and N Type respectively Supplementary Conventions In addition to the precautionary conventions the Tips and Reference conventions are used to supply additional information Convention Description TIP Indicates a particular technique alte
367. s various windows The display depends on the content of the cell selected in the Sample Table If a range of cells is selected the upper left cell is considered the active cell The table below shows the possible selections and the corresponding Properties windows Table 4 4 Properties Windows Content of Active Cell Properties Window Calibration Curve Calibration Curve Properties window Method Sample Method Properties window Any other cell for a sample Sample Method Properties window Any other cell of a control Control Sample Properties window sample The Properties window contains options for viewing and modifying the method calibration curve and sample properties Each Properties window consists of several tabs The Calibration Curve Properties window tabs are shown and described below Calibration Curve Properties Window x Common Parameter Analysis Data Graph History System Our OC User J2 stem Administrator Date of Creation 1 Comment l Figure 4 125 Calibration Curve Properties Window The Common Tab Common Tab The Common tab of the Calibration Curve properties window contains the following information about the calibration curve Setting Item Description System Displays the system used to create the calibration curve This field cannot be edited User Displays the name of the user who created the calibration curve Date of Creation Displays the date and ti
368. same measurement parameters as those in the specified method or calibration file Some of the source parameters can be edited in subsequent pages of the Control Sample Wizard Note that a control sample can also be added to the Sample Table without specifying a source an option that is desirable when a control sample is to be analyzed using different parameters than those specified in the method or calibration files In this case unique measurement parameters for the sample will be entered on subsequent pages of the Control Sample Wizard Control Sample Wizard Page 3 Parameter Source x Create the sample by using parameters from C Edit parameters manually Skip remaining Wizard pages and use measurement parameters from the source Enter the parameter source for the sample lt Back Next gt Cancel Figure 4 153 Control Sample Wizard Page 3 Parameter Source Parameter Description Method radio button Select this option to use the measurement parameters from a specified method Enter the method name in the text field or use the Browse button to select the file using the File gt Open dialog box This is the default option Calibration Curve radio but Select this option to use the measurement parameters from a ton specified calibration curve Enter the calibration curve name in the text field or use the Browse button to select the file using the File gt Open dialog box Edit parameters manually Sele
369. se the Print gt Graph command to print data in graphical format For more information on the Print function refer to Section 4 4 2 10 Print gt Table B 1 8 Print Preview gt Data Print Preview gt Graph Use the Print Preview gt Data function to display a preview of the data to be printed Use the Print Preview gt Graph function to display a preview of the graph to be printed For more information on the Print Preview function refer to Section 4 4 2 12 Print Preview gt Table TOC VCPH CPN 373 B 1 9 Print Setup Use the Print Setup command to select the printing parameters AutoSelect Tray Figure B 8 Print Setup Dialog Box The print options available vary based on the printer installed Select the paper size and source from the drop down lists and select Portrait or Landscape to change the orientation of the printed file Select OK to save the selections or Cancel to close the dialog box without saving changes B 1 10 Page Setup Use the Page Setup command to select items to be printed and to select options for printing format such as margins headers and footers Page Setup pa e E Figure B 9 Page Setup Window Data Tab The Page Setup window consists of several tabs Use the OK button to save changes and exit the Page Setup window Click the Cancel button to exit the Page Setup window without saving changes Click the Apply button to update the parameters without closing the Page Setup
370. seens 88 4 3 Measurement Procedures and Tutorial 0 cccecscecseesceesseeteceeeeeeeeseennees 89 4 3 1 Starting Up the Instrument secs ccecechecv ee Meee acess ree i eaten were 89 4 3 1 1 Turning on the Power ccccccccesesseesecesceseeesceseeeeceseeeeecaeeeeeeaeeeeenees 89 43 1 2 Carrier Gas Press re moenia neta een aie at ae alain 89 4 3 1 3 Carrier Gas Flow Rate cccceccesessceseeesceeceeeeeeeeeeeeneeseecseceeeaeeneeaees 90 4 3 1 4 Electric Purmace eee i EE deen cach reese E GNERE 90 LI TN U e ee stecs a e teabecbadaneie ibaa tous E 91 4 3 1 6 Ozone Source Airflow Rate for the TN Unit esesseeesseeeeserseeeesseee 91 4 3 2 Tutoria e Sieveves teen A O E A a ec 92 4 3 3 Ending Measurement sssssessseseesesseeesstesseeesetstsresteressesessestesessesesstereseesee 120 4 4 Sample Table Editor cecceccesceesseesseeseceseceseeeseeesecnseceeeeeeeseeeneeeeeees 122 4 4 1 Sample Table Window Overview ceccesceesseseeescesceeseeseeeeeeaeeaeenaeeeensees 122 4 4 1 1 Toolbar Functions 0 ccccececscceseeseseeceseeeseeeceeeceeceneecsecseecaecsseeeeensens 122 4 4 1 2 Status Bar and Notification Bat ce ceeeceeeeeessesceeseesseeseeneeeseens 124 AAD File Menun E a A hee ee a eh 125 AAD NO Wich E E E A N R 125 4 4 2 2 Calibration Curve ccccscescceccesesssceseeesceseessessceceeeneeseeeaeceenseeneeeseens 126 4 4 2 3 Method Wizard a a a are ane aast 135 AA DA OE E E AS AN 143 Ah ASD S s E E T A
371. ses 159 4 4 3 10 Importen riin ja E RE E E iis 159 AAA View Menisin AEE eR a Re a 160 4441 Calibration Curve caeeaaeo eanit ia as 160 ARFA 2 Method erae eee ARRENE 161 4 4 4 3 Sample WindoW ss sessssesessseesssessssrsssessesessesessesrsseeneserseseseeeessese 167 A444 Outlier Testei neren e n A tees 169 AAAS O Properties ss e a aie a aa a ae eni se 170 4 44 6 Customize noria E E EAE deceased eve dee eae 177 AAAS Toolbar esni ee a Gal aiid BR OR AE OE 178 AAAS StAtUs Bat eenn eeen arn E EAER TAE TRTI OA RN PRATA ESTEAR 178 4 4 4 9 ASI 8 Port Sampler Vials s ssneeessensesseseesessesersrsresreessersesseseesessee 179 4 44 10 Data Profile zrnin e tees E eee 180 AAS Inserts Men eivesecatecies EE REEE EEN N E ca Cebes ice REE 181 AA SAY AUTO Generates sr sys asvachasivesstuncs a buness E aE ates 181 AA SD catnple rec cosets oi gcse ck achatteie iad ceteehepadiebenk high ae A 185 AAS Control r a eileen Nn E AS Rika Aas 193 446 Instrument Menu eiroet sscsesesdasssta se ceceasscediencscdh eitcuse cdesesgudecsdeseuntes 203 4 4 6 1 Background Monitor c ceccceccesseescesseesceseeeseceecsececsaecssenteeeeneeees 203 A462 CONNECE n ntoniien io eo nth aa en eee Meine ats 205 4 4 6 3 Standbysesccecicecd eann nn R eden E ER 206 44 64 Measurement Start vcsee ccvcesceveseiesives cseeccs caver coociavecsecesevsdeverecoeeteviges 207 4 4 6 5 Stop Peak Stop mee eaea e EE E E E EE E O 207 4 4 6 6 Stop gt Finish Current Sample
372. seseeeseeseeeeereeeerereesee Reaction Solution Pump ccceseseseeeeeee 250 Reaction Solution Regeneration 27 84 262 Removal Pretreatment Standard Solution oo cece sees cseeereeeeeenes Injection Parameters Control Sample ec eeeeseeeeteteeseteeeeeeenees Method ssc css rr A enters Mas ocnsteetietins Samples hyny ia E tensthes Injection Volume Setting Injury Warning i ts 2 sepe santitestcade lie steliee itee evi sescoves Inorganic Carbon See IC Insert Menu Sample Table Editor eee 181 Inside Front View TNs E E A tae 17 TOC V ena e N 10 Inside Top View TOCG V aee a EA S 11 Inspection Dailyo paepae ees 236 237 Periodic i sn naonana iiA 238 251 Front View 8 Port Sampler esssesseosrssesesesereseseseseseressssssese 15 Autosampl tsisasran san onn bathe 14 TOG V apaia E EE A 8 BURN ACC sea nenarera raa i OTE 90 PO WEDS aoda i n E E 90 Temperaire ionaire sri 27 84 Ground Connecting cccceesesceseeeeeeeeeeeeeeeeeeeeees 312 GrOUndIN Gs sinen debe cseeena Meese 312 328 Grubb Test See Outlier Test History Log Calibrations o nec dina kan p n ke Control Sample noinein Instrument ne nehan Meth d seinar History Settings Maintenance Humidifier Checking Water Level 0 cceccceseeeeeeeeeeeeee 237 Filling with Water 0 eeseeeeeeereeeceeeeeees 49 Hydrochloric acid ccecesessesseeseeseeseeeeeseeseeeeeeeeeees 333 Installation 8 Port Sampler Autosamp
373. sesseseesecseereereeeeees 114 Measurement 2 cccscesswcsresnis cncetserversernerrerrentens 112 Printing Report eceeeeeeeeseneeeeeseeeecnetees 117 Unknown Run cceeesceecseseseecseeeceeeeeeeens 108 USP EP aende Se Beene em a 141 192 View Menu Sample Table Editor eee 160 Viewing Measurement Data in Real Time 167 Water VA A OEE RAE AEE EAEE dei 60 Zero W Aber a EEA EE E ria 60
374. shes Rinse Rinse after acid addition Stirrer ON Setting Procedure 1 In the TOC Control V main window double click the icon for the desired instrument The Instrument Properties dialog box is displayed TOC VCPH CPN 4 2 Setting General Measurement Parameters 4 2 2 ASI Parameter Settings 2 Click the ASI tab xi System Options TOC ASI ssm Communication History Tray Type 24ml Vial Needle No of Needle Washes 2 a No of Flow Line Washes 2 IV Rinse IV Rinse after acid addition D Stirer On Notice If tray type is 125ml vial needle type should be Single or Coaxial Combustion Figure 4 27 Instrument Properties Dialog Box ASI Tab 3 Enter the parameters as described below Tray Type Specifies the size of the vials used in the ASI rack Select the vial size from the drop down list Available options are 24mL Vial and 40mL Vial Needle Specifies the type of needle used for analysis Select the needle type from the drop down list Options are e Sample for analysis using only a sample needle e Sample Sparge for analysis using both a sample needle and a sparge needle e Coaxial for analysis using an integrated sample and sparge needle e Coaxial Sparge for analysis using both the coaxial needle and a sparge needle which allows a sample to be measured while the next sample is sparged e The instrument does not automatically recognize the type of needle installed Be sure to se
375. sidered a non regulated product but may react vigorously with some specific materials Avoid contact with all materials until investigation shows substance is compatible SECTION VII EXPOSURE CONTROLS PERSONAL PROTECTION AIRBORNE EXPOSURE LIMITS Not applicable VENTILATION SYSTEM Not applicable PERSONAL RESPIRATORS NIOSH APPROVED Not applicable SKIN PROTECTION None required EYE PROTECTION None required SECTION VIII PHYSICAL AND CHEMICAL PROPERTIES Melt Boil Specific Vapor Vapor Evaporation pH Color Phase Water Point Point Gravity Pressure Density Rate Solubility 0 C 100 C 1 00 17 5 20 C N A N A 7 0 Clear Liquid Complete Colorless SECTION IX STABILITY AND REACTIVITY STABILITY Stable under ordinary conditions of use and storage HAZARDOUS DECOMPOSITION PRODUCTS Not applicable HAZARDOUS POLYMERIZATION Will not occur INCOMPATIBILITIES Strong reducing agents acid chlorides phosphorus trichloride phosphorus pentachloride phosphorus oxychloride SECTION X ECOLOGICAL INFORMATION ENVIRONMENTAL FATE Not applicable ENVIRONMENTAL TOXICITY Not applicable SECTION XI DISPOSAL CONSIDERATIONS Whatever cannot be saved for recovery or recycling should be flushed to sewer If material becomes contaminated during use dispose of accordingly Dispose of container and unused contents in accordance with federal state and local requirements SECTION XII TRANSPORT INFORM
376. site of the plunger tip and plunger becomes loose causing a slight backlash with vertical movement of the plunger As the above conditions start to occur repeatability of sample injection volume decreases resulting in diminished analysis reproducibility Item 2 above rapidly leads to decreased reproducibility Since it is very difficult to determine backlash by inspecting movement of the plunger tip inspect as follows Before sample injection observe the wash injection used to replace the previous sample in the syringe and flow line with the new sample After injection if a droplet forms at the tip of the injection tubing and increases in size there is a strong possibility that backlash has increased The corrective action in this case is to replace the plunger tip Note The effect of backlash increases with smaller sample injection volumes Poor results might be obtained with a sample injection volume of 10uL while the effect might be negligible with a 100uL sample injection volume TOC VCPH CPN 281 282 E TOC VcPHICPN iin Reference Information This chapter describes the principles of analysis and lists instrument specifications accessories and parts This chapter also includes installation procedures for use in the event that the instrument is relocated 6 1 6 2 6 3 6 4 6 5 6 6 6 7 6 8 6 9 Principles of Analysis The principles for TC IC POC NPOC TOC and TN analysis are described in
377. small the size of the acid droplet on the tip of the needle will not be large enough to drop from the needle Visually observe the process through the glass vial to determine if the acid droplet is actually added to the sample The needle will be rinsed following each acid addition by selecting the Rinse after acid addition option in the Instrument Properties Dialog Box gt ASI Window To save time during the analysis sequence rinsing of the needle is unnecessary if the variation in NPOC concentration among the samples is not large TOC VCPH CPN 4 1 Analysis Preparation 4 1 16 Sample Preparation 4 1 16 6 Sparging in NPOC Analysis Samples placed in the autosampler can be sparged by setting a sparge time if the optional external sparge kit is installed If the coaxial needle is used 24mL or 40mL vials sparging can be performed for the specified time followed immediately by drawing sample into the syringe and then by analysis If the coaxial sparge needle is used 24mL and 40mL vials the next sample to be measured can be sparged while the sample vial in the sampling position is being measured In this case sparging is not performed again on the sample when it reaches the sampling position which does not pose a problem for ppm level NPOC When measuring NPOC at the ug L level use the coaxial needle This will prevent atmospheric CO and other contaminants from entering the vial If the sparge gas flow rate is set too high
378. stal is found in both anhydrous and hydrated forms Because the carbon dioxide gas absorbance properties of the hydrated form are slightly inferior to those of the anhydrous form use anhydrous lithium hydroxide to fill the CO absorber e The life of the CO absorber will be shortened by performing POC analysis on samples with high concentrations of IC TOC VCPH CPN 231 232 5 3 Autosampler ASI V Maintenance 5 3 1 Rinse Bottle Inspection 5 3 Autosampler ASI V Maintenance Maintenance of the autosampler includes periodic inspection of the rinse bottle sample catcher and rinse pump 5 3 1 Rinse Bottle Inspection Perform the following inspections before conducting analysis with the autosampler If the following inspections are not properly conducted air will be drawn into the autosampler injection pump preventing the delivery of rinse water e Check the rinse water level Verify that the water in the rinse bottle is above the 2 liter level mark Add water if nec essary e Check the rinse tubing Verify that the tip of the rinse tubing reaches nearly to the bottom of the rinse bottle Adjust the tubing position if necessary Wi Rinse Tubing CEA Rinse Bottle ae Figure 5 13 Rinse Bottle Inspection 5 3 2 Sample Catcher Inspection Examine the turntable black plate and the sample catcher tray below the turntable when installing or removing the autosampler vial rack If they are wet or dirty wipe them clean
379. strial waste The properties and handling guidelines for lithtum hydroxide are described in the mate rial safety data sheets MSDS in Section 6 9 Material Safety Data Sheets To clean the instrument wipe the surface with a soft cloth moistened with water Do not use chemicals Repairs to the inside of the instrument can be dangerous Contact your Shimadzu representative to have a trained service engineer perform repairs Do not disassemble or modify the instrument beyond the scope of the maintenance procedures described in this manual as safety may be compromised The construction of the instrument is not explosion proof It must not be used in dangerous areas Use the instrument with a power supply of AC 100 127V 10 100V systems or AC 220 240V 10 200V systems The instrument backup battery will last for approximately one year Connection to a PC may not be possible if the instrument has been idle for more than one year If this is the case turn the instrument power ON for at least 30 seconds then turn the instrument power OFF for 10 seconds and back ON again If the instrument usually remains idle for extended periods turn the instrument power ON for 24 hours once every six months Do not use the following characters when naming files or systems to be saved back slash these are all normal width characters space normal width em width Turn OFF the Power Management function of the PC to prevent shutdown
380. strument Note To connect the nylon tubing firmly insert it into the half union To disconnect the tubing pull the tubing off while pushing down firmly on the blue ring of the half union with a screwdriver Verify that there are no gas leaks N caution Do not allow acute bends in the tubing Clean the tubing and connectors to remove any oils or other contaminants on their inner surfaces Copper tubing or stainless steel tubing may also be used TOC VCPH CPN 315 6 8 Installation 6 8 3 Installation Procedure 6 8 3 4 Connecting the Drain Tubing Drain tubing is connected to provide for external discharge of measured samples and other liquid waste If a nearby drainage pit is not available use a 10 to 20 liter polypropylene container as the drain receptacle Figure 6 7 Connect the Drain Tubing The drain tubing from the dehumidifier drain port is located inside the right panel Connect it to the external drain tubing using two of the provided wiring bands so that there are no leaks caution e Drainage occurs on a gravity basis Keep resistance to a minimum Ensure that the drain tubing is never higher than the drain discharge port Do not allow the tip of the drain tubing to come in contact with the surface of the liquid in the container If resistance is high insufficient drainage could cause the drainage liq uid to overflow inside the instrument e Corrosive substances such as acids may be present in the dra
381. strument Corrosion Warning Acid and other corrosive substances are present in the liquid waste drained from this instrument Be careful not to touch or spill the liquid waste OD O CAUTION Leil O O ngi fe CORROSIVE The waste liquid may contain acid DO NOT spill or touch The soda lime in the CO absorber of the carrier gas purifier is a corrosive chemical substance Be careful not to touch or spill this substance CORROSION Soda lime is corrosive Be careful not to touch or spill it TOC VCPH CPN Warning Labels Used on this Instrument The liquid discharged from the drain tube connected to the TC injector contains acid and other corrosive substances Verify that the tip of the drain tube is securely inserted into the Y shaped fitting when connecting the combustion tube and sample injector AL A CAUTION Danger of corrosive substance leakage Securely connect the Y shaped fitting to the tip of the tubing 4 iF Sea E BI The IC reaction solution is acidic Be careful not to touch or spill the IC reaction solution TOC VCPH CPN xi Hydrochloric acid is a corrosive chemical substance Be careful not to touch or spill the hydrochloric acid n HA AN xii E 10C Vcrich i TT Ti Table Of Contents introducti
382. sure gauge 5 Carrier gas flow adjustment knob 6 Carrier gas flowmeter 7 Carrier gas pressure adjustment knob 8 Sparge gas flowmeter option 9 Sparge gas flow adjustment knob option 10 Halogen scrubber 11 Humidifier 12 Pump for IC reagent supply H Type only 13 Syringe pump cover 14 SmL syringe 15 8 port valve 16 3 way valve TOC VCPH CPN 2 1 TOC VcPH CPN Construction 2 1 6 Inside Top View 2 1 6 Inside Top View Slide Motor Cooling Fan for Sample Injection Block Slider Sample Injection Tubing Sample Injection Block Figure 2 6 Inside Top View 2 1 7 Flow Diagrams Backflow IC Reagent i Vessel P IC Reagent Diluent Supply Pump Acid Drain ASI Phosphoric Acid Sample Light Source Backflow Slide TC Sparge Prevention Valve Sample Solenoid Q Injector CO Absorber NDIR Tandem Cell Halogen Scrubber Sample Cell 5mL Syringe g Flow Control n Membrane Capillary eee Filter Detector i Combustion Carrier Gas Tube TC Flowmeter ji Pressure NN SEIS JJ Drain Pot Solenoid Cooling Tubing D gt Carrier Pressure Gas Inlet Valve Humidifier TOC VcCPH Figure 2 7 Flow Diagram TOC Vcpx TOC VCPH CPN lI 2 1 2 1 7 Flow Diagrams TOC VcPH CPN Construction
383. sured in samples will be biased high by the amount of TC in the system blank In most cases with the exception of high sensitivity analysis this bias is not significant Measurement error resulting from the TC or TN content in the water used to prepare standard solutions is typically much greater than measurement error resulting from the system blank value Correcting the calibration curve based on the TC or TN content in the standard solution preparation water will produce satisfactory analyses Using this correction method the value obtained for a system blank would be greater than zero by the amount of the blank value The instrument allows shifting of calibration curves only to the extent of the system blank value The system blank peak height varies with such factors as the system configuration and the type of catalyst used Shift to Blank Point The shift to blank point procedure is performed for high sensitivity analyses when the system blank value could have a significant effect on the measurement value By selecting the shift to blank point option a TC blank check analysis is performed using the same injection volume that will be used for sample measurement The calibration curve zero point is shifted to the TC blank check value Peak Area Value 0 TC Concentration mg L 10 0 5 10 0 5 Figure 6 2 Shifting of Calibration Curve TOC VCPHI CPN 291 292 6 2 Analysis Related Technical Information 6 2
384. switch the instrument back ON and follow the correct shutdown procedure Reference For the correct shutdown procedure refer to Section 4 3 3 Ending Measurement 3 Remove the nut using the provided wrench Figure 5 9 Removing the Nut 4 Pull up to remove the rotor drive component Hang it on the screw on the right side of the plunger 246 TOC VCPH CPN 5 2 Periodic Inspections 5 2 10 Replacing the Syringe Pump 8 port Valve Rotor 5 Loosen the retaining nut using the provided wrench Spring equipped Rod Retaining Nut Figure 5 10 Removing the Retaining Nut 6 Note the orientation toward port No 1 of the flat surface of the spring equipped rod Remove the spring equipped rod and retaining nut 7 Note the orientation of the rotor hole position Grasp the rotor with forceps and remove by pulling up Figure 5 11 Removing the Rotor amp Insert a new rotor taking care that the rotor hole matches original orientation 9 Reinsert the retaining nut and spring equipped rod with the flat surface directed toward port No 1 Tighten the retaining nut 70 Replace the rotor drive component and tighten the nut 77 Switch the instrument ON Note Perform the syringe pump zero detection procedure before analysis Refer to Section 4 1 3 1 Syringe Pump Zero Point Detection TOC VCPH CPN 247 248 5 2 Periodic Inspections Replacing the CO Absorber for the Optional Carrier Gas Purifier 5 2 11 Repla
385. system administration are described in detail in the TOC V Administrator s Manual Be sure to read this documentation carefully before using the instrument for the first time Read the Operational Precautions before operating the instrument Follow the procedures in the manual to avoid compromising user or instrument safety L caution e Do not operate this instrument before understanding the contents of this manual If this manual or the warning labels on the instrument become lost or damaged promptly obtain replacements from your Shimadzu representative To ensure safe operation read and follow the procedures in Section 1 2 Opera tional Precautions before operating the instrument iv Product Warranty and Post Sale Service Product Warranty and Post Sale Service Product Warranty The warranty does not cover malfunctions that result from misuse repairs or modifications made by any company other than the manufacturer or a manufacturer approved company external factors operation in environments with severe conditions such as high temperature high humidity corrosive gas or vibration fire earthquake or other forces of nature moving or transporting the unit after its initial installation the consumption of items or parts that can be regarded as consumable For example the service life of an LCD display panel depends on actual operating conditions Post Sale Service If any problems occur with
386. t Lists the reason for the modification TOC VCPH CPN 4 4 4 6 Customize The View gt Customize window contains two tabs one that displays or hides the toolbars and one that customizes the toolbar content Toolbars Tab Customize MMenu bar ioobarnane Figure 4 131 Customize Window Toolbars Tab Select the desired toolbars from the list All items are selected by default Option Description Show Tooltips Cool Look Large Buttons New button Reset Delete button Displays tooltips when the mouse cursor is positioned over the toolbar button Select this option to display the toolbar buttons as flat but tons This item is selected by default Select this option to display the toolbar buttons in a larger size Click this button to create a user defined toolbar button Click this button to reset the toolbar display to its original state or delete a user defined toolbar button LLL TOC my 777 Command Tab Customize Default Figure 4 132 Customize Window Command Tab Option Description Categories Displays the available toolbars Buttons Displays the buttons in the selected toolbar The buttons can be moved by dragging them to another toolbar Description Displays a description of the selected button 4 4 4 7 Toolbar The View gt Toolbar function is used to select or deselect individual toolbars for display Toolbar display options such as button size or appear
387. t Parameter Window This window is only displayed if the Recovery Control Chart is selected in the Control Chart Wizard and Automatic calculation of the control chart limits is not selected Control Chart Wizard Page 4 Recovery Control Chart Parameter Figure B 5 Control Chart Wizard Recovery Control Chart Parameter Window Setting Item Description Use of certified standard Select this option to use a certified sample as a control sam ple Fixed theoretical concentra Select this option if the standard has a fixed concentration tion Enter the concentration in the text box Use of real sample Select this option if the control sample is a real sample Fixed concentration of the Select this option if the spiked component has a fixed con spiked component centration Enter the concentration in the text box Control Chart Wizard Spanwidth Control Chart Options Window This window is only displayed if the Spanwidth Control Chart is selected in the Control Chart Wizard Control Chart Wizard Page 5 Spanwidth Control Chart Options Figure B 6 Control Chart Wizard Spanwidth Control Chart Options Window Setting Item Description No of inj per sample Enter the number of injections for a sample used in the con trol chart The default value is 3 and the range is 3 25 Refuse control samples with Select this option to exclude from the control chart samples different inj no whose number of injections differs from
388. t control chart data to an ASCII formatted file ASCII Export Options xi M Header M Data Cancel I Limits Separator Tabulator T Export strings in quotation marks Figure B 19 ASCII Export Options Dialog Box Setting Item Description Header Select this option to export control chart file header Data Select this option to export control chart data Limits Select this option to export control chart limits Separator Select the type of separator to be used between items in the ASCII file Export strings in quotation Select this option to add quotation marks to all exported marks strings To export a file create or open a control chart Select the desired options from the ASCII Export Options dialog box and select OK The File gt Save As dialog box is displayed Enter a file name for the ASCII file and select the txt file type B 4 5 Enable Exclusion Use the Enable Exclusion command to exclude a selected range of control samples from the control chart calculations When the Enable Exclusion command is executed the Exclude dialog box is displayed Enter a comment describing the reason for excluding the sample This option is only available when one or more control samples are selected A dialog box displays a message requesting confirmation that the sample be excluded Select Yes to confirm and recalculate the control limits or No to abort the process TOC VCPH CPN 383 B
389. t diluted standard solution Note In the case of the TOC VcpN dilution measurement cannot be performed for IC measurement Therefore since the dilution function will not work even if Use Source Dilution Function or Dilution Factor Manual Setting are selected select Dilution Factor Automatic Setting In IC measurement using the TOC VCPH the dilution function can be used The Analysis Information window is used to specify the type of analysis and the standard name for the calibration curve Calibration Curve Wizard Page 3 Analysis Information Cal Pts Analysis Figure 4 78 Calibration Curve Wizard Page 3 Analysis Information Parameter Description Analysis Select the analysis type Default Sample Name Enter the sample name for the calibration standards 64 char acters maximum Default Sample ID Enter the default sample identification for the calibration standards 64 characters maximum Calculation Method Select the calculation method to be used for the calibration from the drop down list Available calculation methods are point to point and linear regression Refer to Section 4 4 4 5 for detailed descriptions of the calibration methods Zero Shift Select this option to shift the calibration curve through the origin Refer to Section 4 4 4 5 for a detailed description of the Zero Shift option Multiple Injections Select to enable the syringe to draw up a single aliquot with a volume equal to that required
390. t the sample tubing directly into the volumetric flask until it reaches the bottom of the flask Perform analyses quickly Four to five repeated analyses can be made with almost no effects from the absorption of atmospheric carbon dioxide Cover the opening of the volumetric flask with sealing film or paraffin to prevent contamination Use this method when the IC value of the purified water used for standard solution preparation specifically Oug L standard solution is about 50ug L or less 2 Sparging the standard solution To sparge in the sample injection syringe set the acid addition ratio to 0 5 and the sparge time to 2 minutes To sparge using the optional external sparge kit transfer about 60mL of the standard solution to a clean sample container add 1 2 drops of 2M hydrochloric acid sparge for 10 minutes and analyze Cover the sample container with paraffin or sealing film to prevent contamination A glass container with an external diameter of 24 25mm and a height of 200 250mm is appropriate Test tubes stopper equipped test tubes and chromatography tubes of suitable size are available commercially If the outer diameter of the container is too large the air to water contact efficiency is decreased requiring a longer sparge time Ensuring that the tip of the sparge tube is near the bottom of the container will improve the sparging efficiency Reference Refer to Section 4 3 2 Tutorial and Section 4 4 2 2 Calibration Curve for det
391. t the tip of the sample needle Is there a leak at the connection of sample needle and ASI YES Air is drawn in at the connection Properly reconnect the tubing Poor reproducibility due to a problem with the TOC V Refer to Troubleshooting 1 TOC V item 5 5 7 2 3 8 Port Sampler OCT 1 1 8 Port Sampler does not operate Are the signal and power cables properly connected Cables are not properly connected Connect the cables properly Electrical system is defective Contact your Shimadzu representative TOC VcPHICPN 279 5 7 Troubleshooting 5 7 2 Troubleshooting 2 Reproducibility is poor Is any foreign material adhering to the sample tubing YES Reduced reproducibility due to Eliminate blockage at the tip of the Is the leakage present at the 8 port valv and sample tubing connection Connection is leaking Connect the tubing properly Poor reproducibility is due to the TOC V unit Refer to the TOC V User Manual 5 7 2 4 Corrective Actions for Poor Reproducibility Corrective Action for Poor Sample Injection The manner in which sample is discharged from the TC or IC sample injection tubing has a large influence on reproducibility The sample should be injected as vertically as possible onto the TC catalyst or into the IC reaction vessel If the sample is scattered or injected obliquely detach the sample injection tubin
392. tains unsaved information a prompt to save changes is displayed Select Yes or No or select Cancel to abort the exit function Figure A 12 Prompt to Save Data Changes LLL TOC fy 355 356 Method Validation Edit Menu A 3 Edit Menu Options such as Cut Copy and Paste are available only if content is selected Undo Cells amp Cut Ctx Copy Ctr C EA Faste j Insert Row Delete Row Insert Col Delete Col FY Recalculate Figure A 13 Edit Menu A 3 1 Undo Use the Undo function to reverse the last change made in the data table This function is available only in documents that can be manually edited and when the user changes the content of a cell in the data table A 3 2 Cut Copy Paste Use the Cut Copy and Paste commands to edit highlighted table cells and rows The Cut command deletes information in rows or cells and stores it on the clipboard The Copy command copies data from rows or cells to the clipboard The Paste command copies the contents of the clipboard to the current row of the table When pasting a whole row select the entire destination row first by clicking the row number Note Do not select a row for pasting that currently contains data The data will be over written TIP The Cut Copy and Paste commands have shortcut buttons on the toolbar A 3 3 Insert Row Use the Insert Row command to add an additional row to the data table This command is available
393. tart measurement can be performed immediately at the specified startup time Refer to Section 4 4 6 3 Standby for detailed descriptions of the available instrument shutdown options TOC VCPH CPN 2l 122 4 4 Sample Table Editor 4 4 1 Sample Table Window Overview 4 4 Sample Table Editor The TOC Control V Sample Table Editor menus and commands are described in this section 4 4 1 Sample Table Window Overview 4 4 1 1 Toolbar Functions If the Toolbar is not visible select Toolbar from the View menu then specify the desired Toolbar options Note Many of the Toolbar functions are disabled until a Sample Table is opened or communication is established with an instrument A description of each Toolbar button 5 function appears when the mouse pointer is positioned over the button a 5 All of the Toolbar commands are also accessible through the Sample Table Editor menus New File Opens a new blank Sample Table Open File Opens a saved Sample Table Clicking the button displays the Open dialog box in which a t32 file can be selected Save File Saves the data in the open Sample Table If the open Sample Table is new and has not yet been saved the Save As dialog box is displayed Cut Removes data from highlighted cells in a table and saves them to the clipboard Copy Copies data from highlighted cells in a table and saves them to the clipboard Paste Copies the contents of the clipboard to a
394. tas cal tat TN A E echt 218 4 5 Application Operations ccceccecsseessesteceseceeceeseeesecsecnseseeceeeeeseeeaeeseenes 219 4 5 1 Manual Injection Analysis ccccccscessecsecsseeseeeeceseeeeceeceeeeeeeaeeeeeeneeeneenees 219 4 5 1 1 Analysis Preparation cceccesesscescesseescesceesecseeeseceesseceeceseeneeeseens 219 A cMeasurementsiis act iste nna need ee ii es 221 4 5 1 3 Measurement Precautions for Low Concentration Samples 225 45 14 Maintenancesiish siceisG Ahi tetciein ss eat T ES 226 45 2 Gas Sample Analysis cvctiics eee Res Se RA 227 4 5 2 1 Analysis Preparation c cceccesesscesceeseescesceesecseeesecaeesaeceesseeeeeseens 228 A522 Measurement i aroi o aE EAE ies ie eee 229 M intenante eenaa n e a ea e E a DOD 5 1 Daily Inspection cee eececsseessesseceneceeeeseeeesecsaecsseseeseeeeseeeseecseeneeseeenes 236 5 1 1 Checking Dilution Wat r sesmarias sesti nnt i 236 si PVA Checking Acid E E A E EA 236 5 1 3 Checking Drain Vessel Water Level ceccceccesseescesceeeceseeeseensenseeeensees 236 5 1 4 Checking Humidifier Water Level s nessesesssesessesesseeeeserseseesreressesesresesees 237 5 2 Periodic Inspections cccecccecseesseesseeseceseceseeesecsseceaeseeeseeeeseecsaeeneeseeeaes 238 52 1 Catalyst Regeneration ceina agi kent aa oii E 238 5 2 2 Washing or Replacing Catalyst cccccecsessessecseceeceteceeceeeeeeeeseeneeeeeeneeenees 239 S221 Washing
395. ted If the History Log was enabled during setup edits to the Communication tab will be tracked and listed in the History tab 32 TOC VCPH CPN 3 2 Instrument Setup and System Properties 3 2 9 Removing a Configured System SSM Tab The SSM tab is identical to the SSM window in the Instrument Setup Wizard Some fields on the SSM tab can be edited If the History Log was enabled during setup edits to the SSM tab will be tracked and listed in the History tab History Tab If the History Log was not enabled during setup the History tab is identical to the History Function window in the Instrument Setup Wizard Use this screen to enable the History log If the History Log was enabled during setup the History tab lists all changes made to the system parameters The log lists modifications chronologically with the most recent modification at the top If the mandatory comment option was selected during setup all modifications listed in the History tab window contain a comment describing the reason for the change View or edit previously entered comments by selecting the modification from the list and clicking the Edit Comment button If the History Log is not required it need not be enabled as the software operates properly without it Item Catabst Type Comment the modification Figure 3 14 Comment Dialog Box Note that if the mandatory comment option was selected in the History Function window during instrument setup the Comment
396. ter File as shown in the figure below and described in the text following the figure Sample Run Calibration ve a ee Method Control Sample Template Co ea Figure 4 74 New Dialog Box A new file can also be created by clicking the New File button on the Toolbar and typing in the new file name Sample Run Displays the General Information window which can also be accessed by select ing General Information from the Options menu Refer to Section 4 4 9 1 Gen eral Information for a detailed description of the General Information window Calibration Curve Opens the Calibration Curve Wizard which can also be accessed by selecting Calibration Curve from the Insert menu Refer to Section 4 4 2 2 Calibration Curve for a detailed description of the Calibration Curve Wizard LLL TOC Vco mm 125 4 4 Sample Table Editor 4 4 2 File Menu Method Opens the Method Wizard Refer to Section 4 4 2 3 Method Wizard for a detailed description of the Method Wizard Control Sample Template Opens the Control Sample Wizard Refer to Section 4 4 5 3 Control for a detailed description of the Control Sample Wizard Refer to Appendix B for a description of the Control Charts function Parameter File Displays the Save As dialog box which can be used to save a parameter file OK Button Opens a new file for the selected icon and closes the New dialog box Cancel Button Press the Cancel button to close the
397. th the 0 8mm diameter sample injection tubing provided in the kit 4 Reinstall the sliders on the sample injection blocks 5 Connect the TC injection tubing and the IC injection tubing to port 7 and port 5 respectively Note During analysis verify that the sample flow is normal Refer to Section 5 7 2 4 Corrective Actions for Poor Reproducibility If the sample stream is not normal the tip of the Teflon tube may be deformed or scratched Use a knife to cut off a portion of the tube 54 TOC VCPH CPN 4 1 Analysis Preparation 4 1 10 Installing the Suspended Solids Kit Replacing Sample Tubing For TOC V TOC V main unit only 7 Remove the bushing from port 1 of the 8 port syringe pump valve and replace the sample tubing with the 0 8mm diameter tubing provided in the kit 2 Connect the new sample tubing to the 8 port valve in the original position For TOC V ASI V TOC V and autosampler Refer to Section 6 8 4 Installing the Autosampler to remove the autosampler sample needle and sample tubing Replace these with the sample needle and tubing provided in the Suspended Solids Kit Ner for Measuring Suspended Solids When performing measurement of solid samples using the Suspended Solids Measurement kit follow the precautions below to ensure the best possible conditions for measurement Refer to Section 4 1 15 4 Analysis of Samples Containing Suspended Solids e Before measurement use a homogenizer etc to make the sa
398. than the NPOC analysis because IC often accounts for a significant portion of the TC and the errors in the two values are additive which significantly affects TOC analysis To generate a calibration curve fill well washed vials with standard solutions to about 5 10mm from the top of the vial and immediately seal each vial Use a cap that has been washed with purified water prior to use When placing the vial in the rack handle the vial carefully to avoid contact between the standard solution and the cap Low concentration standard solutions must be prepared each time they are used To stabilize the peaks perform 4 to 5 injections using the same analysis parameters prior to analyzing the calibration standard solutions For example to generate a 400ug L calibration curve place a Oug L standard solution in vial position 1 and measure it 4 to 5 times using the same analysis parameters that were selected for the calibration curve Refer to Section 4 4 4 1 Calibration Curve The objective at this point is not to generate a calibration curve but to inject water using the same injection volume used for the calibration curve that is to be generated This not only stabilizes peaks but also thoroughly washes the sample needle and sparge needle with purified water After the stabilizing injections are complete place the Oug L and 400ug L calibration standard solutions in vial positions 2 and 3 insert the calibration standards into the Sample Tab
399. the Background Monitor window It cannot be open during analysis 5 Place the cursor in the first row of the Sample Table this allows the measurement sequence to begin with the TC calibration From the Instrument menu select Start or click the Start button on the toolbar The Standby window is displayed 112 TOC VCPH CPN 6 The Standby window displays 3 options e Keep running Shut down instrument e Auto restart Figure 4 62 Standby Window Reference Refer to Section 4 4 6 3 Standby for detailed descriptions of the Standby window options 7 Click the Keep Running radio button Then Click the Standby button The Sparging Acid Addition window is displayed 8 Verify the vial positions then click the OK button 9 The Start ASI measurement window is displayed Click the Start button to begin the analysis 10 The status of the measurements can be monitored during analysis by viewing the Sample Window To open the Sample Window either select Sample Window from the Figure 4 63 Sample Window LLL TOC VcH me 7 73 114 4 3 Measurement Procedures and Tutorial 4 3 2 Tutorial Reference Note The Sample Window is divided into 3 sections as shown in the above figure The Graph is in the upper left corner the Parameter Table is in the upper right corner and the Injection Table is the bottom half of the window The current injection is displayed with asterisks in the Injection Table As each
400. the Viton tubing to the 2 rigid tubes as follows Tubing labeled L Connect to tube labeled L on the CO absorber Tubing labeled S Connect to tube labeled S on the CO absorber 3 Place the NO absorber behind the instrument Viton Tubing TN Unit Rigid Tubing Figure 4 21 Connecting the NOx Absorber TOC VCPH CPN 59 60 4 1 Analysis Preparation 4 1 14 Preparation and Storage of Standard Solutions 4 1 14 Preparation and Storage of Standard Solutions 4 1 14 1 Preparation of Standard Solutions Zero water refers to a standard solution with zero concentration of TC IC or TN zero water also refers to the water used to prepare these standard solutions Water that is in theory absolutely free of carbon TC or nitrogen TN is used as zero water In practice it is difficult to obtain this type of water Even ultra pure water obtained using a high performance membrane technique and water that has been repeatedly distilled will have a TC content of about 10ug L This value is measured directly after manufacture and increases when the water is stored in a container Carbon dioxide is contained in the atmosphere at concentrations ranging from 300 to 500mg L The CO content of ambient air is higher in a room with many people or where combustion equipment is used Carbon dioxide in ambient air dissolves in stored water taking the form of IC The dissolved amount is generally about 0 2mg L but dep
401. the drain container on the floor 3 To minimize resistance keep the tip of the drain tubing above the surface of the drain liquid and as close to the instrument as possible N caution Do not allow any slack or bends in the tubing that could cause a buildup of water pressure Before Starting Analysis Check the following before starting analysis e The rinse water bottle is filled to above the 2 L mark The tip of the rinse tubing reaches nearly to the bottom of the rinse water bottle TOC VCPH CPN N caution Perform the checks described above to ensure that rinse water will be delivered and air will not be taken into the TOC V injection pump 6 8 Installation 6 8 5 OCT 1 8 Port Sampler Installation 6 8 5 OCT 1 8 Port Sampler Installation The OCT 1 8 port sampler is installed as described below 6 8 5 1 Installation Procedure y This section describes the procedure for installing the OCT 1 8 Port Sampler The unit is set up to the left of the TOC V main body as shown in Figure 6 15 Installation of the 8 Port Sampler When 2 OCT 1 8 Port Samplers are to be used place both units to the left of the TOC V main unit as shown in the overhead view of Figure 6 4 External Dimensions of Instrument with OCT 1 8 Port Sampler 8 Port Sampler TOC V Main Unit Figure 6 15 Installation of the 8 Port Sampler Cab
402. the instrument A confirmation request dialog box is displayed when the command is selected as shown below Disconnect x Are you sure you want to disconnect the instrument I Abort Communication Cancel Figure 4 165 Disconnect Confirmation Request Dialog Box Click the OK button to disconnect the instrument or the Cancel button to abort the operation TOC VcPHICPN 205 4 4 Sample Table Editor 4 4 6 Instrument Menu 4 4 6 3 Standby The Standby function is used to shut down the instrument To access the Standby function open a Sample Table then select Standby from the Instrument menu The Standby window which lists options for the shut down operation is displayed Select the desired options and click the Standby button Click the Escape button to abort the Standby operation and maintain the instrument in Ready mode Reference To end measurement refer to Section 4 3 3 Ending Measurement N caution Do not turn off the TOC V main instrument switch for at least 30 minutes after initiating the shut down procedure Standby x System TC TN Shut down instrument C Auto restart Auto start time 2 7 01 Select the standby mode and press Standby Standby mse Escape Figure 4 166 Standby Window Setting Item Description Shut down instrument Select this option to begin a 30 minute countdown to instru ment shutdown During the shutdown process the carrier gas is turne
403. the sample group The templates specify measurement parameters evaluation criteria and failure actions for the control samples This table is empty by default Use the options listed below to revise the list of control sample templates associated with the sample group Option Description Add Select this option to add a control template to the sample group Delete Select this option to delete a highlighted control template from the list After all four pages of the Sample Group Wizard are complete click the Finish button to save changes and add the sample group to the Sample Table If invalid parameter values were entered an error message will be displayed and the sample group will not be inserted into the Sample Table until after the error is corrected TOC VCPH CPN 4 4 5 2 Sample 4 4 Sample Table Editor 4 4 5 Insert Menu The Sample command opens the Sample Wizard which is used to insert sample measurement parameters into an existing Sample Table The Sample Wizard is not accessible during an analysis Sample Wizard Page 1 Parameter Source The Parameter Source window is used to specify the source of the sample measurement parameters The source can either be a method file or a calibration file When one of these sources is selected the sample will be analyzed using the same measurement parameters as those in the specified method or calibration file Some of the source parameters can be edited in subsequent pages of the S
404. this instrument inspect it and take appropriate corrective action as described in Section 5 7 Troubleshooting If the problem persists or symptoms not covered in the Troubleshooting section occur contact your Shimadzu representative TOC VCPH CPN Contents of This Manual Contents of This Manual Chapter 1 Overview This chapter provides an overview of the instrument and operational precautions for its use Chapter 2 System Description This chapter describes the TOC V system components and optional accessories Chapter 3 Software Overview Administration and Setup This chapter provides an overview of the TOC Control V software and describes the software s Administration and Instrument Setup Wizard tools which are used to manage user accounts and configure new systems Chapter 4 Operation This chapter describes pre analysis preparations and instrument and software functions such as setting measurement parameters starting up the instrument generating calibration curves and conducting sample analysis This chapter also includes a tutorial that covers setup and measurement procedures Chapter 5 Maintenance This chapter describes maintenance procedures and periodic checks required to ensure that the instrument provides consistently high accuracy analyses Troubleshooting procedures and error messages are also included in this chapter Chapter 6 Reference Information This chapter describes principles of analysis and list
405. tific Instruments Inc 7102 Riverwood Drive Columbia MD 21046 Control No Tel 1 800 477 1227 Date MATERIAL SAFETY DATA SHEET SECTION I PRODUCT IDENTIFICATION CAT NO CAS NO 7157 79 1 NAME Potassium Nitrate OTHER NAME Nitric Acid Potassium Salt Saltpeter PRODUCT USE This product is for specific use with TOC instruments SECTION IT PHYSICAL DATA Melt Boil Specific Vapor Vapor Evaporation Odor Color Phase Water Point Point Gravity Pressure Density Rate Solubility 334 C N A 2 11 N A 3 0 N A Odorless White Crystalline Pow Appreciable der gt 10 SECTION HMI HAZARDS IDENTIFICATION Possible eye and skin irritation Avoid contact SECTION IV HEALTH HAZARD DATA TARGET ORGANS Blood Central Nervous System SIGNS SYMPTOMS OF OVEREXP Chronic exposure can cause anemia nephritis and methemoglobinemia SECTION V FIRST AID MEASURES INGESTION If conscious induce vomiting and call a physician SKIN Flush with water EYES Flush with water for 15 minutes and call a physician SECTION VI FIRE FIGHTING MEASURES EXTUNGUISHING MEDIA Carbon dioxide dry chemical or appropriate foam SPECIAL Use NIOSH MSHA approved SCBA amp full protective equipment Move containers from fire area if it can be done without risk Use water to keep fire exposed containers cool UNUSUAL FIRE AND EXPLOSIONS HAZARDS Strong oxidizer Contact with other materials may cause fire When exposed to
406. time in the Maintenance His tory Settings TOC VCPH CPN Table 5 2 Error Message List 2 5 7 Troubleshooting 5 7 1 Error Messages Error Message Description Corrective Action Information entered is incorrect Re enter user name and password The user name and password entered are not valid Enter the correct user name and password These fields are case sensitive If the user account has not been set up contact the system administrator Database path not found The specified file does not exist in the specified path Check the file name and path Check if the specified file has been deleted or moved or if the system used for the file has been deleted Opening of communication port has timed out Check instrument connection and transmission set tings The process of opening the communication port has timed out Verify that the instrument is switched on and that the instru ment connection and communica tion port settings are correct Closing of communication port has timed out Transmission will be ended The process of closing the communication port has timed out Verify that the instrument is switched on and that the instru ment connection and communica tion port settings are correct Communication is automatically closed in that condition Instrument initialization has timed out The process of initializing the instrument has timed out Ch
407. tion The 8 port valve is not operating nor mally due to clogging inside of the sam ple injector 8 port valve Switch off the instrument and remove the rotor from the 8 port valve Remove any particles found in the 8 port valve and wash valve ERROR TC Slider The TC slider is not operating normally due to particles wedged between the moving parts ERROR IC Slider The IC slider is not operating normally due to particles wedged between the moving parts Switch off the instrument inspect the slider and remove any foreign particles from the slider mechanism Then switch on the power again ERROR ASI Arm Verti cal Position Detection The ASI V arm is not operating nor mally in the vertical direction ERROR ASI Arm Verti cal Movement The ASI V arm is not operating nor mally in the vertical direction ERROR ASI Arm Hori zontal Position Detection The ASI V arm is not operating nor mally in the horizontal direction ERROR ASI Arm Hori zontal Movement The ASI V arm is not operating nor mally in the horizontal direction Switch off power to the TOC V main instrument After switching on the power and running the instrument again see if the same error is generated Since the problem is unrelated to the TOC V main unit disconnect the ASI V from the main unit and perform operations using the TOC V main unit alone until nor mal operation of the ASI V is restored
408. tions File Name Enter the name of the new method Click the Browse button to save the file in a directory other than the default directory 136 W TOC VcpmcPn eee Method Wizard Page 3 Calibration Curves The Calibration Curves window is used to specify the calibration curves that will be used to calculate results for samples analyzed by the method Up to 3 calibration curves can be entered and during analysis the system automatically determines which curve is most suitable for the sample Refer to Section 6 2 5 Automatic Selection of Optimum Calibration Curve Method Wizard Page 3 Calibration Curves ra Parameters Cal Curve Gen Info Corporation T 003201 CalCurves tctutorial cal C Program Files Shimadzu Corporation TOC3 System Figure 4 86 Method Wizard Page 3 Calibration Curves Setting Item Description Analysis Displays the previously selected analysis type Calibration Curve 1 2 3 Enter the name of the calibration curve or click the Browse button to select a file using the File gt Open dialog box Skip the injection parameter Select this item to skip the Injection Parameters window of pages of the wizard the Method Wizard Use this option when the sample injec tion parameters will be the same as those used for calibration curve measurements LLL
409. tive External conditions are aaverse Eliminate the adverse condition TOC VCPH CPN 275 276 5 7 Troubleshooting 5 7 2 Troubleshooting 5 Poor reproducibility with standard solution TOC VCPH CPN Is the standard solution normal NO YES sample injected normally from injection tube NO YES Do bubbles remain in syringe especially in dilution analysis YES NO Was plunger tip NO replaced recently YES Does carrier gas sometimes leak from the drain bottle YES NO Does the poor reproducibility occur in the TC or IC circuit TC Was the NO TC catalyst regenerated YES TC catalyst deteriorated Replace the TC catalyst Bad standard solution Prepare new standard solution Poor injection condition Adjust injector Poor injection volume repeatability Eliminate bubbles Backlash of plunger tip Replace plunger tip Low water level Replenish the water IC reaction solution has deteriorated Regenerate the IC reaction solution Insufficient regeneration of theTC catalyst Regenerate the TC catalyst 5 7 Troubleshooting 5 7 2 Troubleshooting 6 No peaks appear after sample injection Is sample injected into TC combustion tube or IC reaction vessel confirm visually NO YES Correct the injection condition Is carrier gas always flowing
410. to cut off 2 3mm from the tip of the currently used sample injection tubing Tube Bushing Packing spacer washer gasket Approximately 2 2 5mm Figure 5 39 Slider Assembly Corrective Action to Eliminate Bubbles Inside the Syringe Small bubbles that adhere to the inside of the syringe by the plunger tip will have little effect on analysis values Larger bubbles inside the syringe will affect values and result in poor reproducibility Large bubbles form easily inside a dirty syringe This is evident when sample is mixed with dilution water in the syringe and when sparging with carrier gas inside the syringe for IC removal pretreatment for NPOC analysis In this case detach the syringe from the syringe pump Repeatedly draw in and discharge laboratory glassware detergent to wash the inside of the syringe Then draw in a full stroke volume of the cleaning agent and let it sit for about 20 minutes or overnight if the syringe is extremely dirty Thoroughly rinse away all of the detergent and reattach the syringe to the syringe pump Decreased Reproducibility Due to Plunger Tip Backlash The plunger tip is a consumable item and as it is used wears in the following ways 1 The surface of the plunger tip becomes worn and the seal between the plunger tip and the inside of the glass syringe barrel deteriorates allowing slight amounts of water to leak out with vertical movements of the plunger 2 The contact
411. to enable automatic calculation of the control chart control chart limits limits The upper and lower warning and control limits are calculated after the control samples for the preparation period are added to the control chart No of samples in the pre Enter the number of samples in the preparation period The period default value is 12 This option is disabled if the Automatic calculation of the control chart limits option is not selected No of samples in the control Enter the number of samples in the control period The period default value is 50 LLL TOC Vcc fm 369 Setting Item Description Working range Enter the upper and lower limits of the working range Match the range with the concentration of samples used for control tracking and the concentration range of the selected calibra tion curve Use the drop down list to select the units Rated Value Enter the rated value of the working range This option is dis abled if the Automatic calculation of the control chart limits option is not selected Control Limits Enter the upper and lower control limits This option is dis abled if the Automatic calculation of the control chart limits option is not selected Warning Limits Enter the upper and lower warning limits This option is dis abled if the Automatic calculation of the control chart limits option is not selected Exclusion Limits Enter the upper and lower exclusion limits Control Chart Wizard Recovery Control Char
412. to the container through this opening Note In either case wash the container with a laboratory detergent and rinse it thor oughly with water before use TOC VCPH CPN Sealing the Container with Parafilm 7 Cut a piece of Parafilm to size according to the size of the sample vessel opening 2 Insert the tip of the sampling tube into the vessel cover the opening with the prepared Parafilm and seal the opening of the vessel stretching the Parafilm over the edges Be sure that a very small gap in the seal is formed to prevent creation of negative pressure inside the vessel 3 Press the overlapping portions of the Parafilm around the neck of the opening Parafilm Figure 4 25 Sealing the Container LLL TOC fm 87 8 amp 2 4 1 Analysis Preparation 4 1 17 8 Port Sampler Measurement 4 1 17 2 High Sensitivity Using the 8 Port Sampler If samples such as purified water or ultra pure water having a TOC concentration of 100ppb or less are to be measured using the 8 Port Sampler it is necessary to consider the following precautions associated with high sensitivity analysis Refer to Section 3 3 1 4 High Sensitivity Autosampler Analysis in the TOC VCSH CSN User Manual for more information TOC VCPH CPN 1 2 3 NPOC analysis is recommended because TOC TC IC analysis tends to have a greater variation in measured values than NPOC This is because IC often accounts for a significant portion of the TC and the err
413. to the instrument The ASI Power indicator displays the power status of the ASI The ASI Cover indicator displays the status of the ASI cover Background Monitor T amp T a Ll Time min Figure 4 163 Background Monitor Window ASI Tab 204 OC VM RN ae 4 4 Sample Table Editor 4 4 6 Instrument Menu 4 4 6 2 Connect The Connect command is used to connect or disconnect the instrument and the software If the instrument is not connected selecting the Connect command opens the communication port initializes the instrument and downloads and checks the instrument parameters During this process the Sequence window displays the progress of the connection To abort the Connect operation while it is in progress click the Cancel button Sequence xj Sequence in progress Connect instrument TOC Initialize now Initializing Figure 4 164 Sequence Window The bottom portion of the Sequence window displays a list of tasks that are performed during the Connect process The progress of each task and the result after completing the task are shown in columns to the right of the task list The Sequence window closes when the connection process is complete If an error occurs during the Connect process an error message is displayed in the Notification Bar and the result column and the Sequence window remains open If the instrument is already connected to the software the Connect command is used to disconnect
414. top of the vessel Add water until the level reaches the Hi mark LLL TOC fm 237 238 5 2 Periodic Inspections 5 2 1 Catalyst Regeneration 5 2 Periodic Inspections Periodically inspect the items listed in this section to maintain instrument performance quality 5 2 1 Catalyst Regeneration Inorganic substances contained in the samples accumulate in the catalyst as salts and oxides Buildup of these residues decreases the sensitivity and reproducibility of analyses Catalyst performance can be checked by measuring a standard solution This type of catalyst contamination occurs when measuring alkaline samples and samples that contain high concentrations of IC compounds When catalyst contamination occurs performance can be restored by regenerating the catalyst Catalyst regeneration is also an effective means of reducing the system blank peaks that are present when using new catalyst or catalyst that has not been used for a long time The catalyst regeneration procedure has little effect on TN analysis Catalyst is regenerated by injecting dilute hydrochloric acid onto the catalyst The acid used in the procedure is 2M hydrochloric acid obtained from the instrument reservoir acid used during IC and NPOC analysis The catalyst regeneration process is the same for both TOC standard catalyst and TOC high sensitivity catalyst If performance is not restored after the regeneration process has been conducted replace the catalyst Re
415. torial one unknown sample will be analyzed The unknown sample is actually the mid level calibration standard SOppm TC 10ppm TN Creating a Method File 1 Open the Sample Table From the File menu select New 2 The New dialog box is displayed Click the Method icon and then click the OK button The Method Wizard opens 3 Select the system to be used for the analysis from the drop down list on page 1 of the Method Wizard Click the Next button Page 2 of the Method Wizard lists options for the analysis 4 Select TC TN from the Analysis drop down menu Enter Sample in the Default Sample Name field and Tutorial in the Default Sample ID field In the File Name field enter Tutorial met as the name of the Method File l Analysis TC TN i Parameters Cal Curve Gen Info System Default Sample Name fStendad Default Sample ID Tutoria Dilution fioo No of Determinations mz File Name Tutorial met ae ES the analysis type the default sample nang and ID and the dilution factor for the metho lt Back Cance Figure 4 57 Method Wizard Page 2 Analysis Information 108 TOC VcPHI CPN 5 Click the Next button Page 3 of the Method Wizard specifies the calibration curves to be used to calculate unknown sample results Note Itis possible to enter the calibration curve file in this screen since it contains the data that needs to be entered on this page 6 Place the
416. tory Settings Replenish the water in the dilution water con tainer Then reset the Dilution Water amount in the Maintenance History Settings WARNING Acid depleted Actual amount of hydrochloric acid used exceeds value set in the Mainte nance History Settings Replenish the hydrochloric acid in the acid con tainer Then reset the Total Acid Volume in the Maintenance History Settings ERROR Combustion tube sample injections exceeded Actual volume of sample injected into combustion tube exceeds value set in the Maintenance History Settings Either regenerate the catalyst or replace the cata lyst and combustion tube Then reset the Total TC Injection Volume in the Maintenance History Settings ERROR Syringe stroke num ber exceeded Actual number of syringe strokes per formed exceeds value set in the Mainte nance History Settings Replace the plunger tip Then reset the Syringe Stroke value in the Maintenance History Set tings WARNING IC pump tube operating hours exceeded Actual IC pump tubing operation time exceeds value set in the Maintenance History Settings Replace the IC pump tubing Then reset the IC Unit Pump time in the Maintenance History Set tings WARNING ASI pump tube operating hours exceeded Actual ASI pump tubing operation time exceeds value set in the Maintenance History Settings Replace the ASI pump tubing Then reset the ASI Rinse Pump
417. ttings respectively Click the Finish button to create the new method Note Select the settings described in Section 4 2 Setting General Mea surement Parameters From the Insert menu select Sample to open the Sample Wizard Select the newly created method from the list of files in the Open dialog box Complete the remaining wizard pages From the Instrument menu select Start The Manual Injection Parameter dialog box is displayed Draw an appropriate amount of sample into the syringe Draw in and discharge the sample 3 or 4 times before filling the syringe for measurement Enter the injection volume in the Manual Injection Parameter dialog box and click the Set button Verify that the instrument is ready for measurement and click the Start button For TC or TN measurement open the injection port valve and insert the syringe needle into the injection port For IC measurement insert the syringe needle into the injection port septum Note Insert the syringe needle as far as possible into the injection port e To obtain reproducible results perform all injections at the same speed Remove the syringe from the injection port For TC or TN measurement close the injection port valve Click Additional Measurements to perform repeat measurements Repeat the procedure Click the Finish button when all measurements are complete 4 5 Application Operations 4 5 1 Manual Injection Analysis 4 5 1 3 Measurement Precautions f
418. tton to display the next page of the report Click the Previous page button to display the previous page of the report Note that the Next Page button is disabled when the last page of the report is displayed and the Previous Page button is disabled when the first page of the report is displayed Click the One Page button to display one page at a time in the Print Preview window After selection the button toggles to the Two Page button Click the Two Page button to display two pages side by side Click the Zoom In and Zoom Out buttons to change the mag nification of the displayed pages Three different zoom fac tors are available Repeated selection of either option will continue to increase or decrease the magnification as appli cable Click the Close button to close the Print Preview window and return to the previous window Note that the Print Preview window must be closed to edit the report Click the Print button to print the report 4 4 2 13 Print Preview gt Sample Report The Print Preview gt Sample Report option is used to display the sample report before printing Use the buttons at the top of the Print Preview window to change the display or print the report as described in Section 4 4 2 12 Print Preview gt Table Leg TOC Control Sample Table Tutorial t32 _ x Rey age zoom out 10 0 6 12 20 Timefnin Area 0 842453 j i o 110 Cone ppm qole HE BEE Braet tba Simal 200 purren
419. uced with fluctuating baseline to obtain the correct peak area Figure 6 1 Determining Peak Area 6 2 2 Peak Shape Multiple peaks are especially prominent when using the high sensitivity catalyst with sample injections greater than 100uL As sample is injected onto the catalyst the easily volatilized organic substances and the crystalline organic substances are combusted at different rates As a result carbon dioxide is generated multiple times resulting in the formation of multiple peaks Easily volatilized organic substances are organic compounds that are volatilized with water when an aqueous solution of the compounds is heated ethanol is one example of such a compound Crystalline organic compounds remain in a solid form following the heating of an aqueous solution of the compound glucose is one example of such a compound The manner in which the sample is injected also has an effect on peak shape Ifa portion of the sample is injected into the center of the combustion tube while another portion is injected at the periphery combustion may occur at different times resulting in multiple peaks Peak shape does not affect the analysis results Even if multiple peaks occur due to the type of organic substance or injection manner described above the TOC Control V calculates the total area of the peaks generated to determine the TOC or TC accordingly TOC VcPHICPN 289 290 6 2 Analysis Related Technical Information 6 2 3 Calibratio
420. uch as in high sensitivity analysis of ultra pure water samples for this type of analysis the blank peaks must be small and stable To check and correct for the magnitude of the system blank peaks use the TOC Control V Blank Check procedure described below Note The Blank Check procedure is available only when the high sensitivity catalyst is used The Blank Check procedure takes approximately 8 hours to complete and does not require continuous monitoring by the user As a result performing the procedure overnight is recommended e Blank values measured during the Blank Check procedure should rapidly decrease in magnitude and stabilize If the instrument flow lines syringe pump interior or catalyst have been contaminated the blank values will not rapidly decrease In such instances the Blank Check procedure should be repeated Blank peaks are negligible in the IC analysis flow line The IC value will be zero if the water is acidified and sparged This can easily be confirmed by conducting analysis using the IC flow line however this is not normally necessary Consequently there are no special IC flow line check procedures as with the TC blank check TOC VCPH CPN Blank Check Procedure 1 Open the TOC Control V Sample Table Editor and create a blank Sample Table for the high sensitivity system Note Do not insert a sample into the Sample Table The Blank Check procedure only works in an empty Sample Table 2 Con
421. uded Select Yes to confirm and recalculate the control limits or No to abort recalculation TOC VCPH CPN 377 B 3 View Menu Figure B 13 View Menu B 3 1 Statistics The Statistics command displays the Statistics window Setting Item Statistics Mean Contr Lower Contr Upper Contr Lower Warmi Upper Warni Lower Exclu Upper Exclu Average Co Standard De Coefficient Figure B 14 Statistics Window Description Type No of samples pre period Total no of samples Control limits Data from the control period Displays the type of control chart Displays the number of samples in the preparation period This value was entered in the Control Chart Wizard Displays the total number of samples in the control chart Excluded samples are not included in the total number Displays the control limits Displays the Average Control Value which is the mean value of the samples in the control period Also displays the calcu lated standard deviation and coefficient of variation B 3 2 Comparison After a control chart is completed the results from the control period must be compared with the results from the preparation period For control charts without a preparation period the current values must be compared with the results of the preparation period or the control period from the previous control chart The View gt Comparison command displays the
422. ults by scrolling to the Result column in the Sample Window Note The results should be close to 50ppm for the TC analysis and 10ppm for the TN analysis Current Peak z Sample Name Standard Sample ID Tutorial Analysis TC TN Dilution 0000 Result TC 50 00ppm TN 10 1 Mean Conc 50 00 50 00 18357 18357 ne An j ig Figure 4 65 View Sample Results TIP Use the TC and TN tabs at the bottom of the Sample Information table to view the results for both analyses 3 Close the Sample Window when the evaluation is complete 116 TOC VcCPHI CPN 4 3 Measurement Procedures and Tutorial 4 3 2 Tutorial Outlier Test The Outlier Test is used to provide additional information about the measurement result 7 Place the cursor in the third row of the Sample Table which contains analysis information for the unknown sample 2 From the View menu select Outlier Test Note The Outlier Test is conducted to identify suspect results The test statistically compares all unknown samples that have the same sample name Because this tutorial includes only one measurement of the unknown sample the outlier test calculation is not meaningful Printing a Report Step 8 Print a report after measurement is complete and the results have been evaluated Selecting the Report Items 7 From the File menu select Page Setup 2 The Page Setup window is displayed Each tab in the windo
423. unction can be effectively utilized for analyses covering a wide range of concentrations For example use a concentra tion of 10ppm for Calibration Curve 1 100ppm for Calibration Curve 2 and 1000ppm for Calibration Curve 3 Considerations for the Automatic Selection Function The automatic selection process rules do not change when multi point calibration curves are included When more than one injection is performed the calibration curve is selected based on the measured value of the first injection Because the measured value is always calculated first using Calibration Curve 1 specify the most commonly used calibration curve in this field The priority of the second and third calibration curves is determined based on the calibration curve concentrations and the sample concentration TOC VcPHICPN 293 6 3 Specifications 6 3 1 TOC VcPH CPN 6 3 Specifications 6 3 1 TOC VCPH CPN Analyte TC IC TOC TC IC NPOC Measurement principle 680 C catalytically aided combustion oxidation non dispersive infrared detection NDIR Measuring range TC 0 25000mg L IC e TOC VCPH 0 30000mg L e TOC VCPN 0 3000mg L Detection limits TC e TOC VCPH 4ug L e TOC VcPN TC 50ug L IC 4ug L Measurement time TC Approx 3min IC e TOC VCPH Approx 3min e TOC VCPN Approx 4min Repeatability CV within 1 5 Sample introduction Auto injection using syringe pump slider
424. unger tip straight into the plunger tip seat as shown in Figure 5 7 Installing the New Plunger Tip cross section Save the syringe for future use since the plunger tip seat is enclosed inside the syringe Plunger Tip Plunger Tip Seat Figure 5 7 Installing the New Plunger Tip cross section Note Do not scratch the perimeter of the plunger tip This could cause leaks e Use only Shimadzu specified plunger tips Use of unspecified parts may result in malfunction and or diminished performance 5 2 Periodic Inspections 5 2 8 Replacing Ferrules at the Combustion Tube Outlet Connection 5 2 8 Replacing Ferrules at the Combustion Tube Outlet Connection For High Sensitivity Analysis Kit The front and rear Teflon ferrules used in the compression fitting connections at the combustion tube outlet gradually become deformed and scratched with repeated use and may cause gas leakage When this occurs replace them with new ferrules Keep a 6F T Sleeve set on hand as replacement parts Reference For details on the replacement procedure refer to Section 4 1 2 Connecting the Combustion Tube 5 2 9 Replacing the Sliding Sample Injector O rings Two types of O rings are stacked between the injection block and the slider of the sample injector If a gas leak develops in this area replace both O rings e White Upper O ring O ring Teflon P10 P N 036 11408 84 e Black Lower O ring O ring 4DP10A P N 0936 11209 84 White O ring
425. uot for each injection as a result selecting this option reduces analysis time Displays the file name of the calibration curve This field cannot be changed The Analysis tab displays additional analysis parameters Figure 4 127 Calibration Curve Properties Window Analysis Analysis Parameters Setting Item Description No of Washes Acid Addition Sparge Time Density By Weight Volume 172 WE TOC VcPmcPn E Displays the number of times 0 10 the syringe is washed with standard prior to the first injection Note that if the Auto Dilution option was selected the standard will be diluted and the syringe will then be washed with the diluted standard This option is not available for SSM This field can be edited Displays the quantity of acid to be added to each standard prior to injec tion This value is expressed as a percent of the sample volume and is available only for NPOC or related analyses This field can be edited Displays the pre sparge time 0 20 minutes This option is only avail able when the external sparge kit is installed and the analysis type is NPOC This field can be edited Displays the sample density This option is available only for SSM Displays the basis Weight or Volume for sample calculations This option is available only for SSM Peak Time Parameters Setting Item Description Use default settings This option is selected if the default settings are used for peak int
426. ure 4 15 Acid Preparation TOC VCPH CPN 5 4 1 Analysis Preparation 4 1 8 Installation of the CO Absorber 4 1 8 Installation of the CO Absorber A CO absorber is used to remove CO from the carrier gas that purges the optical system of the detector The CO absorber is installed using the following procedure Procedure 7 Cut the tips of the 2 rigid tubes in the lid of the CO absorber with a knife 2 Connect the flexible tubing that exits the rear panel of the instrument near the top as follows Tubing labeled L Connect to tube labeled L on CO absorber Tubing labeled S Connect to tube labeled S on CO absorber Note The flexible tubing should not be bent 3 Place CO absorber in the holder behind the instrument Flexible Tubing Rigid Tubes CO Absorber Figure 4 16 Installation of the CO Absorber 52 TOC VCPH CPN 4 1 Analysis Preparation 4 1 9 Adjusting Sparge Gas Flow Rate 4 1 9 Adjusting Sparge Gas Flow Rate The sparge gas flow rate should be adjusted before sparging is performed using the optional external sparge kit The procedure for adjusting the sparge gas flow rate is described below Procedure 7 Open the TOC Control V Sample Table Editor and connect the instrument 2 From the Instrument menu select Maintenance gt Sparge Gas Valve The sparge gas solenoid valve opens and sparge gas begins to flow 3 Open the front door of the instrument 4 A
427. urport to be all inclusive and shall be used only as a guide SHIMADZU shall not be held liable for any damage resulting from handling or from contact with the above product Users should make their own investigations to determine the suitability of the infor mation for their particular purposes TOC VCPH CPN 333 334 6 9 Material Safety Data Sheets 6 9 2 Phosphoric Acid 6 9 2 Phosphoric Acid Shimadzu Scientific Instruments Inc 957006 7102 Riverwood Drive Columbia MD 21046 Control No Tel 1 800 477 1227 November 1995 MATERIAL SAFETY DATA SHEET SECTION I PRODUCT IDENTIFICATION CAT NO 630 00710 00 CAS NO 07664 38 2 NAME Phosphoric Acid 25 Ultrapure SYNONYM Phosphoric Acid IC Reaction Liquid SECTION II PRDUCT USE This product is specifically for use in the IC channel of the TOC 500 TOC 5000 and TOC 4000 series of TOC analyzers Refer to the appropriate instruction man ual for directions on proper use Keep tightly sealed in a cool dry well ventilated place Store separate form flammable and combustible materials Wear appropri ate protective clothing and eye protection SECTION III PHYSICAL DATA Melt Point Boil Point Density Vapor Pressure Color Phase Water Solubility N A N A N A N A Colorless Clear Liquid Completly Soluble SECTION IV HAZARDS IDENTIFICATION Corrosive causes burns Harmful if swallowed Target organ s liver blood In case of contact with eyes rinse immediately with plenty of
428. urve and one unknown sample will be measured Pure water and the following calibration standards are needed for the tutorial A calibration standard mixture of Oppm potassium hydrogen phthalate and Oppm ammonium chloride A calibration standard mixture of 50ppm potassium hydrogen phthalate and 10ppm ammonium chloride A calibration standard mixture of 100ppm potassium hydrogen phthalate and 20ppm ammonium chloride Reference Prepare calibration standards as described in Section 4 1 14 1 Preparation of Standard Solutions The following topics are covered in the tutorial Step 1 Configuring the instrument Step 2 Connecting the instrument Step 3 Creating a sample table Step 4 Setting up the calibration standard runs Step 5 Setting up an unknown sample run Step 6 Performing measurement Step 7 Evaluating the results Step 8 Printing a report TOC VCPH CPN Configuring the Instrument Step 1 SOHSSHSHSHSSHSHSHSHSHSHSSHSHSHOHSHSSHSSHSSHSSHSSHSHSHSSHSSHSSHSSHHSHSSSHSHSHSHSHSHSHSSSSHHSHSSHECHSESEE Procedure 7 Start the TOC Control V software by double clicking the icon or selecting it from the Start gt Programs list The TOC Control V main window is displayed LT x OurTOC 2 DIN 38402 Control Charts History Data Profile Part 51 Database Figure 4 32 TOC Control V Main Window 2 The instrument configuration must be specified in the software before the instrument can be connected to the P
429. us Bar commands show and hide the Toolbar and Status Bar respectively 380 E TOC Vcecen nen Control Charts Options Menu B 4 Options Menu Control Chart Options A Font T Floating point numbering format ASCII Export Options v Enable Exclusion Figure B 17 Options Menu B 4 1 Control Chart Options Use the Control Chart Options command to view and edit the control chart parameters entered in the various pages of the Control Chart Wizard Refer to Section B 1 1 New Note Some options within the Control Chart Options tabs such as control chart type or sample concentrations may be disabled if the control chart contains data The disabled parameters are options that cannot be modified once data is entered B 4 2 Font The Font command opens the standard Font dialog box Refer to Section 4 4 9 3 Display Settings gt Display Font for detailed information about font options TOC VCPH CPN 38 Control Charts Options Menu B 4 3 Floating Point Numbering Format The Floating Point Numbering Format command is used to select display options for numeric results in the control charts These options apply only to the manner in which numbers are displayed internal data retain their original values Floating Point Format x Display floating point numbers in the following format m Common Floating Point Numbers 2 Cancel C Number of significant digits 1 012 2
430. ust tubing to the instrument and discharge the exhaust gas to the outdoors or an exhaust pit e Ifthe gas exhaust tubing is not connected ozone and NO gas may be exhausted from the instrument causing harm to the respiratory organs of individuals in the vicinity 332 TOC VcPHICPN 6 9 Material Safety Data Sheets 6 9 1 Hydrochloric Acid HCl 6 9 Material Safety Data Sheets 6 9 1 Hydrochloric Acid HCI Shimadzu Scientific Instruments Inc 957006 7102 Riverwood Drive Columbia MD 21046 Control No Tel 1 800 477 1227 November 1995 MATERIAL SAFETY DATA SHEET SECTION I PRODUCT IDENTIFICATION CAT NO 630 00998 00 CAS NO Hydrochloric Acid 7647 01 0 NAME Hydrochloric Acid OTHER NAME Muriatic Acid Regeneration Liquid PRODUCT USE This product is for specific use in the regeneration of the catalysts of the Shimadzu TOC Refer to the Instruction Manual of the unit for proper use SECTION II PRECAUTIONS TO BE TAKEN IN HANDLING Do not get in eyes on skin or on clothing Wear rubber or neoprene gloves and impervious boots apron or coveralls as needed to prevent skin contact Avoid breathing mist Use only with adequate ventilation local and or general exhaust is recommended to keep employee exposure below the Airborne Exposure Limits If TLV is exceeded a full face piece chemical cartridge respirator may be worn in general up to 100 times the TLV or the maximum use concentration specified by the respirator supplier whi
431. w represents a section of the report and contains several items Selections will be made on each tab to print a typical report for the calibration standards and unknown sample Reference Refer to Section 4 4 2 15 Page Setup for detailed descriptions of the Page Setup options 3 On the Instrument tab ensure that the Print system information check box is selected then select the options shown in the figure below Instrument Calibrations Samples Header Grid Miscellaneous System Used options Detector Syringe V Catalyst Syringe wash vol ASI Tray Type No of needle washes No of flow line washes Cell length ly Preview Select All Select None Default Cancel Figure 4 66 Page Setup Instrument Tab TOC VCPH CPN 117 4 Click the Calibrations tab and select the options shown in the figure below Page setup Weight Volum Ru Figure 4 67 Page Setup Calibrations Tab 5 Click the Samples tab and select the options shown in the figure below Mlini Yol Notes R MExcluded Modified Cal Curve Figure 4 68 Page Setup Samples Tab Note Use the default selections on the Header and Grid tabs 6 Click the Miscellaneous tab and enter Tutorial in the Organization name field Select the Footer check box to include page numbers on the report TIP 4 company logo can be added to the report header by selecting the Logo check box and specifying the log
432. water and seek medical advice Take off immediately all contaminated clothing Wear suitable protective clothing gloves and eye face protection SECTION V TOXICITY DATA UNR MAN LDLO 220mg kg ORL RAT LDS50 1530mg kg IHL RAT LC50 gt 850mg m3 1h SKN RBT LD50 2740mg kg SECTION VI HEALTH HAZARD DATA Acute Effects Harmful if swallowed May be harmful if inhaled May be harmful if absorbed through the skin Material is extremely destructive to tissue of the mucous membranes and upper respiratory tract eyes and skin Inhalation may result in spasm inflammation and edema of the larynx and bronchi chemical pneumonitis and pulmonary edema Symptoms of exposure may include burning sensation coughing wheezing laryngitis shortness of breath headache nausea and vomiting May cause cyanosis Chronic Effects Target organ s liver blood bone marrow To the best of our knowledge the chemical physical and toxicological properties have not been thoroughly investigated SECTION VII FIRST AID MEASURES In case of contact immediately flush eyes or skin with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes Assure adequate flushing of the eyes by separating the eyelids with fingers If inhaled remove to fresh air If not breathing give artificial respiration If breathing is diffi cult give oxygen If swallowed wash out mouth with water provided person is conscious C
433. x which contains several tabs is displayed Each tab contains a list of export options as shown in the figures below Note that on each tab certain items are selected by default Individual options can be selected or deselected by clicking in the check box Use the Select All and Select None buttons to quickly select and deselect all options on a tab Use the Default button to select the default options on a tab Click the Cancel button to exit the ASCII Export Options dialog box without saving changes Click the OK button to save changes and exit the ASCII Export Options window Header Tab Header System Data Misc l IV Export header information V File version User MDate of creation V Comment Default Figure 4 95 ASCII Export Options Window Header Tab Setting Item Description Export header information Select to enable export of the selected header options This option is selected by default TOC VCPH CPN System Tab ASCII Export Options Figure 4 96 ASCII Export Options Window System Tab Setting Item Description Export system information Select to enable export of the selected system options This option is selected by default Data Tab ASCII Export Options Mean Result Notes Vv Sample Name OSD Area MSample ID CCV Area igi SD Cone OCY Cone Vial MeExcluded Modified Figure 4 97 ASCII Export Options Window Data Tab Setting Item Description Expo
434. x which may have a variable display depending on the installed printer driver Specify items to be included in the printout by using the Page Setup command Refer to Section 4 4 2 15 Page Setup for more information Figure 4 100 Print Dialog Box The Name text field identifies the printer that will be used to print the table Specify a different printer by selecting it from the Name drop down list Setting Item Description Properties Modify the printer settings using standard Windows proce dures Print range Click the All radio button to print all pages of the table Click the Pages radio button and enter the page numbers to be printed if all pages are not desired Number of copies Enter the number of copies to be printed LLL TOC my 149 4 4 2 11 Print gt Sample Report The Print gt Sample Report command is used to open the Print dialog box to print the Sample Table in report format The print dialog box is the same as that described in Section 4 4 2 10 Print gt Table 4 4 2 12 Print Preview gt Table The Print Preview gt Table option is used to display the sample table before printing Use the buttons at the top of the Print Preview window to change the display or print the table as described below Button Figure 4 101 Print Dialog Box Description Next Page and Previous Page One Page Two Page Zoom In and Zoom Out Close Print 150 WE TOC VcPmcPn ieee Click the Next Page bu
435. xcept when they are extremely easy to crush Pretreatment of samples that contain suspended solids should include sample homogenization to a point where the particles are distributed uniformly in as small a particle size as possible Well homogenized samples can be measured with good reproducibility Stirring a non homogeneous suspension will not provide a uniform suspension resulting in poor measurement reproducibility First apply a powerful enough homogenization process ultrasonic waves etc to crush every particle in the sample as much as possible and then perform the TOC measurement e The ASI V stirrer bar may not be able to sufficiently agitate and mix the sample because of the wide variety of characteristics of suspended particles such as shape specific gravity size strength degree of cohesion etc For example solid particles with a high specific gravity sink to the bottom and prevent formation of a good mixture 78 TOC VCPH CPN Note 4 1 Analysis Preparation 4 1 16 Sample Preparation Operation of the Optional ASI V Magnetic Stirrer Two types of magnetic stirrers available one for the 24mL and one for the 40mL size vials All of the vial positions may be used with 40mL vials All positions except the innermost row can be used with 24mL vials The magnetic stirrer will only properly agitate vials in the sampling position and the position just in front of the sampling position advance processing position For exa
436. ximum number of injections specified for the calibration points The Delete Column function is not available if the number of columns is 3 or less Once a column is deleted the format of the remaining columns is updated A confirmation dialog box opens asking you to confirm the deletion A 3 7 Recalculate Use the Recalculate command to recalculate all method validation data The results and calibration curve sections of the Method Validation window are also updated when the Recalculate command is selected Errors that occur during the recalculation process are displayed in message boxes For example an error message may be displayed if the data in the table does not contain sufficient information if there are not enough data points defined in the table if less than 3 injections are available and if numeric data is incorrect and results in an illegal mathematical operation such as division by zero TIP The Recalculate command has a shortcut button on the toolbar TOC VCPH CPN 357 A 3 4 View Menu Figure A 15 View Menu Toolbar The Toolbar function displays or hides the toolbar Status Bar The Status Bar function displays or hides the status bar 358 E TOC Vcecen ieee A 5 Options Menu Figure A 16 Options Menu A 5 1 General Parameter Select the General Parameter command to display the General Information dialog box General Information Figure A 17 General Information Dialog Box
437. zation normally occurs within one hour Used halogen scrubbers should be disposed of according to local industrial waste disposal regulations It must be clearly disclosed using an industrial waste manifest that the halogen scrubber contains copper Clamps Clips Viton Connectors Figure 5 5 Halogen Scrubber Replacement TOC VcPHICPN 243 244 5 2 Periodic Inspections 5 2 7 Replacing the Syringe Plunger Tip 5 2 7 Replacing the Syringe Plunger Tip The syringe plunger tip is constructed of fluororesin and wears with use Gaps will eventually form between the plunger and the inner wall of the syringe barrel glass tube causing leaks When leaks occurs bubbles are produced near the syringe tip when sample is drawn into the syringe or sample may leak from the bottom of the barrel when the sample is discharged When these problems are observed replace the plunger tip Replacement Procedure 1 Z TOC VCPH CPN Remove the syringe referring to Section 4 1 3 Installing the Syringe Use a sharp knife to make two or three incisions at the bottom of the plunger tip as shown in Figure 5 6 Removing the Old Plunger Tip Grasp the plunger tip with a pair of pliers and remove it from the plunger The O ring that is held in place by the plunger tip also comes off DO NOT reuse this O ring Figure 5 6 Removing the Old Plunger Tip Pushing down on the plunger press the leading edge of the new pl

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