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Apollo 9000 TOC Combustion Analyzer User Manual

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2. 4 Removal in IC Sparger L Liquid Sample Gaseous Sample Carrier Gas COM NO 5 VENT Sparge Gas Line NC NDIR Purge Permeation Dryer and Injection Port p WATER Lines Not Used 2 MIST TRAP During Analysis 1 TRAP IC SPARGER 4 PERMEATION NO COM DRYER Da 200 ml min ur WATER M H iRIECTION RESTRICTOR WASTE SAMPLE PORT DI WATER BOTTLE 1 i INLET HEADSPACE PURGE 5 SYRINGE CORROSIVES E DRIVER SCRUBBER OMBUSTIO TO 8 PORT COOLINGFAN 0 1 VOLT SIGNALTOP un d 200 ml min FLOW 2 VENT RESTRICTOR 2 d 200 FLOVIMETER FLOW RESTRICTOR gt ASM SPARGE 5 200 ml min 5 FLOW RESTRICTOR 2 7 50 ml min pA 9 FLOW RESTRICTOR 14 9000 074 Rev B 09 2000 SWVYDVIG apow sishjeuy DL TC and TC IC Carrier Gas NDIR Purge Permeation VENT Dryer and Injection Port Lines Not Used During Analysis p WATER TRAP IC SPARGER PERMEATION DRYER DI 200 ml min WATER FLOW RESTRICTOR INJECTION SAMPLE PORT DI WATER BOTTLE INLET HEADSPACE PURGE WASTE CORROSIVES SCRUBBER SYRINGE T DRIVER
3. Cal Curve ID CALIBRATION 5 0000 10 0000 Click on Standard Method ID TOC 0 20 ppmC TOC 0 20 ppmC TOC 0 20 ppmC Cancel Figure 4 2 5 Standard Calibration Analysis Setup without Autosampler 2 Click Sample Setup the Sample 5 Analysis screen 3 From the Sample Type list select TOC Standard 4 TheChoose Range dialog appears Select the 0 20 1 400 range Click OK Next the Select Calibrator dialog appears Select the Standard ID DI WATER you want to use by clicking its row to highlight it Click Exit You will return to the Analysis Setup screen TOC Talk automatically inserts the calibration information in the Sample ID and Method ID fields Select the Number of Reps Per Sample in the Reps column Click Save Use 4 Start Standard Calibration Analysis Run Before you begin the analysis run verify that the Sample line runs from Port D of the 8 port valve into the correct stan dard supply Acid line runs from Port A of the 8 port valve into the acid reagent supply Dl Water line runs from Port G of the 8 port valve into a fresh DI Water supply 1 Click Start in the Sample Analysis screen to begin the standard analysis run Note You must repeat the Standard Calibration Analysis Setup 3 and Start the Run 4 for the two remaining Standard IDs 5 PPM and 10 PPM in order to create a proper calibration
4. 5 4 Sample Blanks Sample Type amp Method ID Range ppmC TOC TC 0 20 TOC TCRng 1 5 4 1 Manually Set the Sample TOC TC 1 400 TOC_TCRng1 Blank 10 750 TOC_TC Rng 2 Teledyne Tekmar recommends TOC 100 4000 TOC TCRng3 setting the blank value to the raw data value of your DI water run as a sample TOC TC 1000 25000 TOC_TCRng3 IC 0 20 ICR 1 To set this up go to the Sample Blanks ids Review screen in the Results menu and 1 1 400 IC Range 1 enter the correct raw data for the 10 750 IC Range 2 desired range of analysis IC 100 4000 ICRange 3 Enter the values into Blank1 Blank2 or Blank3 or even one value into any of Table 5 4 1 Blank Ranges the 3 blank spaces Table 5 4 1 outlines the blank ranges as they correlate to the standard meth ods 5 9 SAMPLE ANALYSIS 5 4 2 Run Recirculating TOC and TC Blanks If the DI water contribution to your standards is significant to your analysis you may want to run a recirculating blank method The blanking procedure for TC and TOC analysis will recycle DI water through the furnace and then sample from the water trap to determine the sample blank value Make sure to set the number of replicates to at least 6 when running a sample blanking procedure The results for blank methods are in raw data counts and the last 3 repli cates are averaged as the sample blank Note The raw data value for the sample blank should be less than the raw data f
5. 02 oo oo 6 Hog 1825 o o Jooo OO O 5 C38 1 1 5 00000000000 019 000000000 5 OO 16 n 2 9 UM O 5 SYRINGE 85 252 C34 25 CR20 1995 2 0 8 00000 TEKMAR DOHRMANN HOST RS 232 2 ch CPU PCBA 3 14 7009 090 1 REV E 3 Figure 9 7 Apollo 9000 CPU Board 9 15 APPENDIX 1 Preventive Maintenance The Apollo 9000 Consumables Kit includes most items needed for preventive maintenance Daily Maintenance Checks The following components should be checked on a daily basis Carrier gas 500 psig from tank to run scheduled load Ample acid supply for load e Replaced and ample DI water supply for load e Check chlorine scrubber to ensure ample life for load e Carrier gas flow rate 200 cc min 1090 Make sure 8 port valve thumb screws are hand tightened Inspect and clean syringe if appropriate Load estimated amount of daily analysis Weekly Maintenance Checks The following components should be maintained on a weekly basis Daily checks plus e Clean IC sparger with soap and water if needed Change reagents if needed e Clean syringe APPENDIX A Monthly Mai
6. Outlier deletion Recalculations with different calibration curves Recalculations with different blank values Calibration Multi point and automatic blank subtraction INTRODUCTION Other Features and Options Preprogrammed point and click method setup Programmable automatic Wake up Automatic shutdown standby Selectable IC sparge methods Automatic file management Flow rate monitoring Priority samples via scheduled interrupt Online help Solids module Nearline monitoring Exceeds ISO 8245 particulate requirements with optional kit Stirring option e Automatic blanking or manual entry of blank value Typical Methods and Principal Applications EPA 415 1 and 9060A Standard Method 5310B ASTM D2579 SO Draft 8245 AOAC 973 47 e Cleaning Validation 5 643 Drinking Surface water Industrial Waste Effluent e Waste water Sea Water 1 5 INTRODUCTION Certification UL CSA and EMC EN 50081 1 EN 50082 1 Utility Requirements Power Entry Module 2IEC 5 x 20 mm fuses 100v Operation T10A 250v fast blow e 115v Operation T10A 250v fast blow 230v Operation T5A 250v fast blow Voltage 100 120 230 VAC 10 Frequency 50 60 Hz excluding NDIR Power 1200 VA Dimensions Approximate e cm40Wx61Dx53H in16 Wx23 Dx21 H 50 110 lb shipping weight G
7. Tool s Needed 10 11 12 Phillips screwdriver Slotted screwdriver Turn off power at the back of the instrument Remove plug from back of the instrument Remove both left and right side covers Locate flow meter on the plumb ing side of the instrument It will be attached to a mounting bracket that it on the lower back panel of the instrument On the electrical side of the instrument remove the power cable for the flow meter from the PCB board On the plumbing side of the instrument remove the two 2 screw and nut assemblies holding the flow meter to its mounting bracket Noting their position remove the Teflon lines and 1 4 1 8 fittings from either side of the flow meter Reattach Teflon lines and fittings to the replacement flow meter Reattach flow meter to instrument using the screws and nuts from step 5 Reattach the power cable for the flow meter to its proper position on the PCB board Reinstall both left and right covers to the instrument Plug the AC power line back into the back of the instrument and turn the power switch ON Reestablish communications with TOC Talk software MAINTENANCE AND TROUBLESHOOTING 7 2 14 Power Entry Module Tool s Needed Phillips screwdriver Turn off power at the back of the instrument Remove plug from back of the instrument The component you removed the plug from is the power entry module Remove right hand or electrical side cover by r
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9. COMBUSTION TO 8 PORT FURNACE VALVE 0 1 VOLT COOLING FAN 200 ml min FLOW RESTRICTOR 200 ml min FLOW RESTRICTOR FLOWMETER TO ASM SPARGE EALEN I E ee ee E EE 200 ml min FLOW RESTRICTOR 50 ml min FLOW RESTRICTOR 14 9000 074 Rev B 09 2000 SWVYDVIG 11 6 apow gt p WATER TRAP DI WATER WASTE SYRINGE DRIVER TO ASM SPARGE 200 ml min FLOW RESTRICTOR 5 NC NC MIST TRAP IC SPARGER 4 PERMEATION NO COM DRYER 200 ml min FLOW RESTRICTOR SAMPLE PORT DI WATER BOTTLE INLET HEADSPACE PURGE WATER TRAP CORROSIVES SCRUBBER 8 PORT is COOLINGFAN 0 1 VOLT SIGNALTO 200 ml min FLOW VENT RESTRICTOR 2 200 ml min FLOWMETER FLOW RESTRICTOR 14 9000 074 Rev B 09 2000 Liquid Sample for IC Analysis Sample Gas Carrier Gas NDIR Purge and Permeation Dryer Gas Lines Not Used During Analysis TOC FREE AIR 50 ml min FLOW RESTRICTOR SINVHDOVIG 1 6 115 VAC 60 HZ CONFIGURATION 7 ALTERNATE VOLTAGE AND FREQUENCY CONFIGURATION NOTE REPRESENTS JUMPERS LOCATED ON THE FURNACE TERMINAL BLOCK FOR VOLTAGE OPTIONS NOTE 2 EPRESENTS JUMPERS LOCATED ON THE NOR TERMINAL BLOCK FOR VOLTAGE OPTIONS NOTE 3 REPRESENTS JUMPER LOCATED ON THE BLOCK
10. In the case of the Autosampler Setup screen you must save the setup at this point which will take you back to the Run screen Select Sample Setup again and you will find the new method in the drop down list for Methods and can select it for your samples and standards It is important that you calibrate with the same method before running samples This means you must make a new calibration setup that will call out the new method Do not forget to select the new calibration in the Set Active screen for the range and mode you are running and to run new blanks SPECIAL APPLICATIONS Parameter TC TC TOC TOC Range 1 3 Range 1 3 Range 4 Range 1 3 Range 4 Injection Volume of Volume of Aliquot of Sparged Sparged Volume sample sample diluted sample sample sample delivered to IC delivered to injected to injected to injected to sparger for furnace for furnace for furnace for furnace for analysis analysis analysis analysis analysis Sparger N A Volume of Amount of Sparged Amount of Volume sample sample to be sample sample to be injected to diluted injected to diluted furnace for furnace for priming priming Dilution N A N A Amount of N A Amount of Volume water added water added to the IC to the IC sparger for sparger for dilution dilution Water DI water N A N A N A N A Volume added to IC sparger Volume of acid N A Volume of acid Volume of acid Acid added to IC added to IC added to IC Volume s
11. only one password I 4 Restricted Areas IV Inst Setup Backup System Blanks IV Diagnostics Meth Setup IV Exit Program Calibration Setup Run Screen Cal Verification Calibration Res Mult Analysis Data Editing Password Restriction Status 34j OFF I Figure 3 5 Password Setup Screen To enable password protection 1 Setup menu click Pass word 2 Check the boxes of the areas you want access restricted to in Restricted Access 3 Enter a password maximum 32 characters Passwords are case sensitive 4 Password Restriction Access click ON 5 Click OK TOC TALK Each time you or other users try to access a restricted area a window will up requesting a password If the user types in the correct password they will gain full access to that section of the program To disable password protection 1 Onthe Setup menu click Pass word 2 Enter the current password 4 n Password Restriction Access click OFF 4 Click OK Now all areas may be entered without restriction After altering configura tions calibration etc be sure to go back into the Password Setup enter a password and click ON to re enable password protection TALK 3 6 Wakeup Schedule Apollo 9000 can be scheduled to automatically wakeup when pro grammed to do so using t
12. should display the default unless another curve is set as active and in memory 5 4 7 Select 3 the Number of Repeats field Click Save Use Before you begin the analysis run verify that the a sample line runs from Port D of the 8 port valve into the correct sample vessel b acid supply line runs from Port A of the 8 port valve into the acid reagent container Dl Water line runs from Port G of the 8 port valve to a fresh DI Water supply SAMPLE ANALYSIS Start Analysis Run 1 Click Start from the Sample Analysis screen 2 The sample run will begin You will have your data in approximately 20 minutes If a printer is con nected to the computer the Detailed Report will print showing reps for each vial as well as the average standard deviation and RSD File 5 File Name Method EI Date and Time Cal Curve 2000 07 01 12 24 CALIBRATION 40815 mm 49039 i 3 39982 15981 480506 3653 3850 3875 3 9922 1 9961 479891 3677 Statistics tm Ces Std oos Asp 1 24 Figure 5 2 5 Detailed Report Example TOC Talk 9000 151 Step 1 SAMPLE LOOP START ResdyMode mW 1131 1317 1899 03 28 5 2 6 Sample Analysis Data Example 5 5 SAMPLE ANALYSIS 5 3 Tutorial TOC Resu
13. the IC sparger as in steps 1 and 2 with quantitation of the IC The IC sparger is emptied of the last rep INTRODUCTION Rinse Syringe with Sample IC Sparger Contents to Waste Wait for Endpoint Sample Gas Swept to NDIR CO Concentration is Measured Memorize Baseline Gas Off Deliver Sample to IC Sparger Rinse Syringe with DI Water Pull DI Water Sample Gas Swept Through Corrosives Scrubber Sample Gas Swept Through Moisture Control System Gas Start Integration Deliver Acid and DI Water to IC Sparger Figure 1 8 5 Analysis Process INTRODUCTION Notes SYSTEM SETUP 2 1 Before You Begin This section describes the steps neces sary to setup the Apollo 9000 TOC Analyzer Installation should be per formed in the sequence presented in this section Start up assistance is available through TeledyneTekmar or its authorized representatives When all the utilities and facilities required for start up are in place contact TeledyneTekmar or its authorized representative to schedule the installation and start up assistance Please provide adequate advance notice to avoid undue delay in processing your request IMPORTANT Please be aware that if Apollo 9000 its components and or accessories are usedina manner not specified by Teledyne Tekmar protec
14. 3 N MAINTENANCE AND TROUBLESHOOTING ASM Sparge Gas green line entering the end of the 1 Make sure the ASM sparge gas is This can be done by actuating the ASM sparge valve in the valve diagnostics screen Make sure the carrier gas source cylinder or gas generator is on Disconnect gas line to ASM needle This is the fitting entering the side of the needle Re attach the gas line to the needle Submerge the bottom end of the needle to above the second set of holes Bubbling should be vigorous If not your leak is in the connection to the ASM needle or the ASM needle itself If the needle is leaking it must be replaced Disconnect gas line to ASM needle This is the fitting entering the side of the needle Measure the flow of the gas line If it between 180 and 220 cc min then go to step 6 Otherwise go to step 8 Re attach the gas line to the needle Submerge the bottom end of the needle to above the second set of holes Bubbling should be vigorous If not your leak is in the connection to the ASM needle or the ASM needle itself If the needle is leaking it must be replaced Your leak is in the line to the ASM needle from the Clippard Valve 7 regulating ASM sparge flow If the ASM sparge gas line is 1 16 diameter remove its connection to the ASM sparge flow restrictor Verify that the tube does not contact the packing of the restrictor Check the Clippard Valve 7 connec tions for tightness
15. 3 7 2 Replacing Parts 7 4 73 Troubleshooting Apollo 9000 7 22 74 Teledyne Tekmar Customer Support 7 29 CALIBRATION STANDARD 8 1 Calibration Standard Preparation 8 3 8 2 Procedure for Making Standards 8 3 DIAGRAMS APPENDIX A INDEX INTRODUCTION 1 1 Apollo 9000 Analyzer Figure 1 1 Apollo 9000 Apollo 9000 is comprised of the following Syringe for sample and reagent introduction Sparger for inorganic analysis and sample preparation for TOC analysis Combustion Furnace Furnace Injection Port Water Trap for moisture removal Permeation Tube for moisture removal Corrosives Scrubber for halogen removal NDIR Detector for carbon dioxide detection INTRODUCTION TOC Analysis Overview Total organic carbon TOC analysis grew from the need to analyze waste water and municipal water for organic matter The need to protect it and establish criteria for screening and measuring contaminant levels was recognized when Congress enacted the Resource Conservation and Recovery Act RCRA in 1976 This act requires operators of waste disposal sites to monitor their groundwater ona quarterly basis for organic carbon levels and organic halide levels TOC analyzers are also widely used in monitoring the quality of process water in the semiconductor and pharmaceutical industries Because organic material can cause contamination TOC analysis is also performed to protect process equ
16. 7 27 MAINTENANCE AND TROUBLESHOOTING 7 3 2 1 Catalyst Efficiency Test Prepare a 20 ppm C standard of KHP Prepare a 20 ppm C standard of sodium bicarbonate Confirm that the instrument has been on with gas flowing for at least two hours Measure the gas flow from the blue tube exiting the instrument It should be 200 cc min 10 Do not change the flow at this time Renew the DI water supply Confirm that the acid supply is adequate Run the Prime System method Using TC range 0 20 ppm C analyze DI water as a sample using 6 reps Using IC range 0 20 ppm C analyze DI water as a sample using 6 reps Using TC range 0 20 ppm C analyze the KHP solution using 3 reps Using IC range 0 20 ppm C analyze the sodium bicarbonate solution Compare the TC raw data value with the IC raw data value If the TC value is lower then the IC value by more than 1096 the efficiency of the catalyst is poor and should be replaced or washed and run the Cleaning Procedure run 7 28 7 3 3 Wash the Catalyst When the Catalyst Efficiency test fails removing the catalyst from the com bustion tube and washing it may restore efficiency 1 In the Setup Menu select Instru ment and click on the large Sleep button to turn off the gas and the power to the furnace Wait until the temperature control read out indicates that the tem perature is below 50 Remove the combustion
17. 8 tubing that exits the upper chassis of Apollo to the side port of the needle 2 15 5 5 5 Install the Support Bar Rinse To install the support bar rinse station Station and Acid Vial Bracket and acid vial bracket The support bar attaches to the front 1 Attach the rinse station to the face of the autosampler rear contains mounting holes for rinse stations and its top contains mounting holes for transfer ports and filler ports Rinse Station Acid Vial Bracket Support Bar T 2 Positions 4and 5 Positions 2 11 and 12 Level sensing Rinsing Well 3 Rinsing H Well Drain Fitting 4 5 Figure 2 6 8 Rinse Station and Support Bar 6 2 16 support bar The default position for the rinse station is the left side of the support bar with the rinsing well to the left when the bar is attached to the autosampler Place the o rings supplied with the screws over the screws on the bar side of the rinsing well Attach the rinse station behind Positions 4and 5 of the support bar by tightening the set screws Attach the acid vial bracket behind Positions 11 and 12 of the support bar by securing with the two screws provided Attach the tubing to the drain by first locating the drain tubing Attach the tubing to the drain fitting Place the other end of the tubing in a drain receptacle located lower than the tray There is sufficient space behind the racks to direct the waste line to the r
18. ANALYSIS 2 Sample Setup Stn Chat 1591 Sample ID Graphs Options 1 From the menu bar of the Control screen click Run TOC Apollo 9000 Setup Results Help Click Run to Open Mode NOIA mv 1122 1303 1999 03 28 Run Screens Figure 5 2 3 TOC Talk Run Screens Figure 5 2 2 Access to Run Screens 3 Click the Sample Setup button in the Sample Analysis screen 2 Run screens are actually three Without AutoS ampler Analysis Setu separate screens that display real Sample ID SAMPLE 1 time data Sample Sample a Sample Analysis displays the as x last Sample ID Mode etc if not D running or the current Sample ate u ID etc while running The Ean Sample Setup button accesses the Sample Setup table b Strip Chart shows the detector E signal and can be changed to magnify small peaks or Figure 5 2 4 accommodate larger peaks Analysis Setup without Autosampler c Analysis Results updates 4 In the Without Autosampler analysis data at the end of Analysis Setup screen enter a each sample analysis rep name for the sample run in the Sample ID field 5 Select Sample from the Sample Type list 6 Select 0 20 ppmC from the Method ID list The analysis Mode displayed should match the Method and the Calibration Curve
19. FOR FREQUENCY OPTIONS JUMPER 8 TO 9 60 HZ NO JUMPER 8708 NOTE 4 FOR 100 VAC OPERATION INTERNAL MODIFICATIONS TO THE NOIR MUST BE MADE 0006 9 6 FLOWHETER i REMOVE THE WIRE ORIGINATING FROM THE EXTERIOR TERMINAL BLOCK PIN 7 FROM THE TRANSFORMER PNG AND REATTACH TO PNS OF THE TRANSFORVER AS SHOWIN THE uM 2 NE TES a Pi REMOVE THE WIRE ORIGINATING FROM THE EXTERIOR TERMINAL BLOCK PIN 6 FROM THE DRYER mea SPAGER NORNENT SPARGE 55 1 TRANSFORMER PIN 2 AND REATTACH PIN 1 OF THE TRANSFORMER AS SHOWN IN THE WEE wem ex 0D VAC DIAGRAM 553 1 EXTERNAL CONNECTIONS AS SHOWN THE 100 VAC DIAGRAM a 1 58 58 58 58 8 58058 d ii J 5 J J J 8 HT TOI ara On 147674201 od SEE NOTE 4 FOR INTERWAL MOCIPCATONS ina m lius
20. Fittings Nut and ferrule to connect carrier gas tubing to regulator One 1 8 Swagelok brass nut and ferrule to connect carrier gas tubing to the analyzer is supplied Power Apollo 9000 requires one 120 VAC 10 60 Hz 1200 VA 15 amp electrical outlet STS 8000 autosampler requires one 120 VAC 10 60 Hz 200 VA 15 amp electrical outlet Computer will require two electrical outlets CPU and monitor Printer will require one electrical outlet All power must be free from line spikes or interference 220 VAC 50 Hz models are available Reagents Distilled and or deionized DI laboratory grade water TOC less than 0 2 ppm 85 phosphoric acid ACS reagent grade Fora typical one month supply of 21 phosphoric acid reagent Teledyne Tekmar recommends adding 50ml of 85 phosphoric acid into 150ml of DI water 5 Apollo 9000 dimensions 16 W x 24 D x 21 H STS 8000 autosampler dimensions are 21 W x 17 D x 15 Typical computer dimensions are 18 W x 27 D x 22 H including key board Total recommended bench length is 6 1 2 feet with autosampler and computer Please allow additional space for printer if used Standards One 1000 ppm C potassium acid phthalate KHP KC H O TC TOC standard is supplied with analyzer Sodium bicarbonate ACS reagent grade will be necessary if IC calibration is desired Tools Needed 7 16 Open end wrench Phillips screwdri
21. Screens 2 The Run screen has three parts Sample Analysis Strip Chart and Analysis Result a Sample Analysis displays the last Sample ID Mode etc if not running or the current Sample ID etc while running The Sample Setup button accesses the Sample Setup table b Strip Chart shows the detector signal and can be changed to magnify small peaks or accommodate larger peaks c Analysis Results updates its analysis data at the end of each sample analysis rep 3 TOC Talk Apollo 3000 21515 eus Bun Standy Mode mV 355 1234 2000 07 01 Figure 5 3 3 TOC Talk Run Screens Click the Sample Setup button in the Sample Analysis screen Analysis Setup Rack Style 40 mL vial Sample Sample Figure 5 3 4 Analysis Setup with Autosampler In the Autosampler Analysis Setup screen select New from the File menu to open a new setup table Vial Position 1 in the table will already be assigned the Sample ID ID1 You may use the default ID or click on the cell and type a new Sample ID Select Sample from the Sample Type list Select TOC 0 20 ppmC from the Method ID list Select 3 sample repetitions from the Reps list 10 11 12 SAMPLE ANALYSIS Create two more sample analysis lines by pressing the down arrow on your keyboard twice Each new line will hav
22. Type 10 PPM the Standard ID box 14 Enter 10 in the Concentration ppm C box 15 In the Method ID list select TOC 0 20 ppmC The calculated value in the ugC column should read 5 0000 16 OntheFile menu click Save As Save this calibration setup as TOC Calibration 17 Click OK 4 12 Note After you click OK in the Calibration Setup dialog you will return to the TOC Talk Control Screen but the Setup menu and Calibration submenu will appear This is to remind you to Set Active standard calibration methods for the mode s of analysis TC IC TOC and range s you intend torun TOC Talk Apollo 9000 Setup Run Results Instrument Diagnostics Calibration Cal Verification Backup Password Wakeup Standards Exit Figure 4 3 2 Set Active Calibration Submenu CALIBRATION 2 Set Active Calibration Curve 1 From the Set Active submenu select TOC Curve TOC Mode Active Calibration Curves 0 20 1 400 10 750 default 100 4 000 default 1 000 25 000 default Aux default ues 4 3 3 Mode Active Calibration Curves In the 0 20 1 400 Range list select the TOC Calibration Curve ID TOC Calibration is the name you gave the Calibration Setup TOC Talk will use the TOC Calibration setup for the 0 20 1 400 Range data from the standards to ana
23. adjust ing the system pressure within the 30 35 psi range verifying that the pressure gauge is reading correctly If condition 1 is still not satisfied you will have to go to step 6 and or step 14 If condition 2 fails and the NDIR flow is lower than the water trap go to step 14 Leak Checking after the Water Trap If condition 2 fails and the NDIR flow is higher than the water trap then it is highly probable that the counter flow of the permeation dryer is bleeding into the sample gas flow Repair or replace the permeation dryer reconnect all lines and return to step 3 If this does not fix the leak call Teledyne Tekmar customer support for further assistance Leak Checking the IC Sparger 1 Verify that the gas supply to the IC sparger is on In the TOC Talk Control screen select Setup gt Diagnostics gt Valves Make certain that Gas to IC Sparger is turned on and Gas to the combustion furnace is turned off Locate the IC sparger Check all rubber seals to verify they are intact and securely in place Remove the red Teflon tube entering the top and measure the flow through this tube MAINTENANCE AND TROUBLESHOOTING with a hand held flowmeter If you obtain a reading of 200 cc min 10 continue to step 3 If you obtain a reading of less than 180 cc min it is likely that the IC sparger flow restrictor IC gas valve or main valve is leaking In the valve diagnostics screen set the IC
24. and then click Autosampler AutoSampler Diagnostics Rack Style 40 ml vial x Manual Movement Current Positions mm Move To Vial 1 a Y Needle Down Needle Up Update Figure 3 4 Autosampler Diagnostics Screen WARNING Do not alter this screen during an analysis Erroneous or conflicting data can damage the instrument 3 8 Rack Style Select the rack style you are using by clicking the pull down menu or the display box Manual Movement Home Click this button to home the autosampler Move To Vial Click this button to move the autosampler needle to the posi tion selected in the display box to the right of the button The posi tion number can be changed by clicking the arrow bar or the display box Note Special Position Numbers 1001 thru 1014 support bar ports 1015 Rinse Station Needle Down Moves autosampler needle down Needle Up Moves autosampler needle up Current Positions mm This section displays the current position in millimeters of the autosampler in the X Y and Z planes when the Update button is activated Communications Diagnostics On the Setup menu point to Diagnos tics and then click Communications Comm Port Selection Figure 3 3 4 Communications Diagnostics Screen The Communications Diagnostics Screen allows you to switch the communications port or re establish communicat
25. away from the syringe driver face and toward you until it is removed Turn off power at the back of the instrument Remove plug from back of the instrument Remove left hand or electrical side cover by removing seven 7 screws holding it to the chassis Locate Syringe driver Noting their position on the driver remove power and RS 232 connections Using the nutdriver remove the four 4 nuts at the corners of the syringe driver holding it to the front face of the instrument Syringe Driver 10 14 MAINTENANCE AND TROUBLESHOOTING Remove the syringe driver and replace it with the new one Using the nut driver attach the syringe driver to the front face of the instrument using the four 4 nuts from step 9 Reattach the power and RS 232 cables to the syringe driver Reattach the left hand or electrical side cover using the seven 7 screws from step 7 Reattach AC power plug to back of instrument and turn the power switch ON If you hear the syringe pumper s motors move then you know the power cable to the driver was correctly installed If not disconnect AC power reenter the electrical side of the instrument and make sure the power cable to the syringe driver is properly installed Reattach 8 port valve and syringe assembly to syringe driver making sure the pin on the inside of the 8 port valve slots into the rod from the syringe driver This may require you to initially attach the assembly
26. call Tekmar Dohrmann technical support for further assistance Your leak is before the injection port Using the valve diagnostics screen turn on the flow to the IC sparger and measure the flow of the line entering the top of the sparge tube If within the 180 to 220 cc min range then go to step 12 Otherwise go to step 13 Good IC flow implies a leak specific to the furnace carrier gas line Inspect the Clippard valve 2 the flow restrictor flow meter and connecting lines for leaks If leak is found reconnect lines and return to step 3 Otherwise call Tekmar Dohrmann technical support for further assistance 7 24 11 Bad IC flow implies a leak that will affect all carrier gas lines Look for leaks on the three way tees or other fittings and connecting lines that regulate flow to all Clippard valves and NDIR purge gas from the pressure regulator If leak is corrected reconnect lines and return to step 3 Otherwise call Teledyne Tekmar technical support for further assistance Leak Checking After the Water Trap 12 13 14 Reconnect the line to the water trap and measure the flow from the 1 8 green line entering the copper side of the corrosives scrubber If this number is within 5 cc min of the water trap go to step 15 Otherwise go to step 11 Open the right side cover and locate the permeation dryer The permeation dryer is the 1 4 tube with a white plastic tee at either end mounted beside t
27. curve see Figure 4 2 7 CALIBRATION 5 Review Analysis Results The result of each standard analysis rep appears in the Analysis Results screen 12024037 Figure 4 2 6 Analysis Results There is no calculation of PPM C during calibration The results are in area counts forthe integrated peak The Calibration Curve screen appears when the standard run ends see Figure 4 2 7 4 9 CALIBRATION Calibration r Value Curve Calibration Calibration Factor Curve ID TOC CALIBRATION ion dm Y imoret o Recalc Calibration Button Curve Results Table Figure 4 2 7 Calibration Curve The Calibration Curve table displays the standard calibration data At the begin ning of each row is a box Clicking on and off the Use box toggles X When the X is visible the calibration point repre sented by that row will be included in the calibration curve when you click Recalc Some users prefer to analyze the same standard concentration twice and then select one or both to include in the calculations Various combinations may be setup Each time you configure a new calibration set you must click Recalc The value is one way to evaluate the calibration The closer is to 1 the more precise the calibration You may delete unused lines by high lighting the row and pressing the delete key This may prevent confusion when viewing the calibration again later 4 10 CALIBRATION 4 3 StandardCa
28. mounted beside the combus tion furnace Measure the 1 8 permeation dryer nearest the front of the instrument If the number is within 5 cc min of the mist trap then replace the permeation dryer 2 reconnect removed lines and return to step 3 Otherwise go to step 13 The leak is either at valve 5 or in the lines connected to valve 5 Inspect the lines for leaks and make sure the fittings are tight Using the Diagnostic Valves screen verify that the IC sparger gas is on and the IC sparger gas output is directed to the NDIR Measure the flow from the 1 8 red tubing exiting the rear of the instrument The flow should read 0 mL min Otherwise the valve is defective Replace Valve 5 3 way Kloehn valve Reconnect all lines and return to step 3 Open the right side cover and locate the NDIR at the lower back of the instrument Measure the flow of the sample inlet line going into the detector If flow is within 5 cc min of the mist trap then go to step 15 Otherwise go to step 16 Theleak is either in the NDIR itself the connections to the NDIR or the sample outlet line Inspect these parts to find the leak If the leak is corrected reconnect all lines and return to step 3 Otherwise call Teledyne Tekmar technical 8 support for further assistance The leak is in the corrosives scrubber or the line from the scrubber to the NDIR Locate and correct the leak reconnect all lines and return to step
29. routine or troubleshoot ing procedures that may involve contact with hazard ous acids Please see Appendix A for a supply of maintenance worksheets that you can copy and fill out for your records The Consumables Kit includes most items needed for pre ventive maintenance MAINTENANCE AND TROUBLESHOOTING Daily Maintenance Checks The following components should be checked on a daily basis e Carrier gas 500 psig from tank to run scheduled load Ample acid supply for load Replaced and ample DI water supply for load e Check corrosives scrubber to ensure ample life for load Carrier gas flow rate 200 cc min 1096 Make sure 8 port valve thumb screws are hand tightened Inspect and clean syringe if appropriate Load estimated amount of daily analysis Weekly Maintenance Checks The following components should be maintained on a weekly basis Daily checks plus e Clean IC sparger with soap and water if needed Change reagents if needed e Clean syringe Monthly Maintenance Checks The following components should be maintained on a monthly basis Daily and weekly checks plus Change corrosives scrubber nspect permeation dryer for damage water accumulation Test fittings on 8 port valve injection port carrier gas and 3 way Kloehn valves Test catalyst efficiency 7 3 MAINTENANCE AND TROUBLESHOOTING 7 2 Replacing Parts Please
30. scrubber to the system if necessary Refer to Section 6 1 for discussion on effects of different acids on the analyzer 5 Introduce the sample through the automatic syringe mode Some concentrated acid will damage the stainless steel needle SPECIAL APPLICATIONS 6 2 5 Waste Water Wastewater samples vary in their carbon concentrations and chemical composition For samples containing particulates refer to Section 6 2 2 For samples containing large amounts of metal ions such as liquor bauxite and some effluents follow the directions on Section 6 2 3 6 2 6 Solids and Sludges Analysis of solids and sludges can be performed using the 183 Boat Sampler with the Apollo 9000 Refer to the manual of the boat sampler for installa tion instructions The temperature of the boat may be increased to 900 C to ensure complete oxidation of the solid sample For most applications 800 C is adequate Weighing a larger portion of the sample increases the likelihood of getting a more accurate representative aliquot of the sample However the size of the weighing boat and the total not to exceed 100ugC would limit the amount of sample analyzed An extension kit may be used to extend the range of sample analysis 6 7 SPECIAL APPLICATIONS 6 2 7 High Fraction of Inorganic Carbon For performing TOC analysis check that enough acid is added to the sample to remove all the inorganic carbon We do not recommend using TC IC
31. syringe diagnostic and verify the ports on the 8 port valve are properly aligned There is a chance that the 8 port valve is 180 off its true position Pull 1000 ul from the furnace port making sure that the DI water line can also pull liquid Dispense to waste and repeat once more with 2500 ul this time If you do not get liquid on the second pull go to step 12 If you get liquid then the 8 port valve is misaligned Perform the following steps a Make sure using the syringe diagnostic screen that the 8 port valve is in the C Furnace position b Remove 8 port thumbscrews and syringe screw and pull assembly out from driver c Inthe syringe diagnostics screen turn the valve to the DI water or port G position d Reattach 8 port valve and syringe according to step 10 12 Press the Initialize button on the right face of the syringe driver The syringe plunger will move to the predetermined position just below the top of the syringe 13 Using the thumbwheel on the bottom of the syringe move the syringe plunger to the top of the syringe Stop when you hit signifi cant resistance 14 Press the Set Home button on the right face of the syringe driver 15 Close acrylic door 16 Using TOC Talk software run 1 rep using the Prime System Method ID This method will insure that the acid and DI water lines are prop erly primed and ready for analysis Note If you accidentally hit either the Set Home or Initializ
32. syringe making sure the Teflon washer is still in the 8 port valve Do not over tighten the syringe Hand tighten 8 port valve thumb screws if necessary Using the syringe diagnostics screen in TOC Talk software set the syringe to O ul Press the Initialize button on the right face of the syringe driver The syringe plunger will move to the predetermined position just below the top of the syringe Using the thumbwheel on the bottom of the syringe move the syringe plunger to the top of the syringe Stop when you hit signifi cant resistance Press the Set Home button on the right face of the syringe driver Close the acrylic door Note If you accidentally hit either the Set Home or Initialize buttons during this procedure any errors incurred will be corrected when you initialize and home the syringe per the instruction at the end of the procedure 7 2 8 Tool s Needed 11 Slotted screwdriver Phillips screwdriver 5 16 nutdriver 12 Open acrylic door Locate 8 port valve on upper left front panel just above the 2 5 ml syringe Remove two 2 thumbscrews on 8 port valve face Gently remove the screw just below the syringe with the slotted screwdriver DO NOT force remov ing the screw If the screw is difficult to remove use the TOC Talk Syringe Diagnostics to move the plunger 5001 away from 15 the Home position Pull 8 port valve and syringe assembly
33. the SW2 selector to 10r3 1 Gentlyinserta small slotted screw driver into the SW2 selector see Figure 2 6 2 on the rear panel of the autosampler and turn gently 2 Align the white dot with 1 or 3 SYSTEM SETUP Remove the Arm Locking Screw During shipment a screw locks the horizontal arm into place Arm Locking Screw Horizontal Plastic Arm Plug Figure 2 6 4 Autosampler Arm Locking Screw To remove the arm locking screw 1 Locate and remove the black plastic plug located on the right side panel ofthe autosampler 2 With yourleft hand hold the horizontal arm in place 3 Usinga Phillips screwdriver remove the arm locking screw located inside the autosampler 4 Insert the arm locking screw into its storage location on the rear panel 5 Replace the plastic plug on the side panel 6 Ensure that the horizontal arm can move by pushing it to the left as far as it will go Before packing the autosampler for shipment always secure the horizontal arm using the arm locking screw 5 5 5 Install the Vertical Arm Before installing or changing the vertical arm check that the power is turned off the power cord is disconnected from the power socket the arm locking screw has been removed and that the horizontal arm move Horizontal Slider Plastic Control Needle Plug Rod Foot Needle 3 Bracket Horizontal Slider Needle Foot Figure 2 6 5 Autosamp
34. through the Apollo 9000 default TOC sample analysis procedure You will 1 Configure the Instrument 2 Setup the Sample 3 Start the Analysis Run SAMPLE ANALYSIS 5 2 Tutorial 1 2 3 4 5 TOC Results Made Easy Without Autosampler Configure Instrument Select Instrument from the Setup menu of the TOC Talk Control screen to open the Instrument Setup Status dialog operate one GEERT jt gt System Preferences Sample with Autosampler G Ready E Sample in i Autosampl 3 Integration Time min 40 Stabilize Baseline Time 15 Gas Flow Rates Outlier Deletions E Print data report after each sample set Auto Shutdown furnace off 0 8mm Particulate Kit Installed Halt System If Out of Calibration Over Range Options Iv Autosampler Sparge Option Figure 5 2 1 Instrument Setup Status Select Ready to wake up the instrument The gas flow will turn on and the detector signal will begin to stabilize Look for the flow rate display in the To Furnace field Select the following parameters a Select Without Autosampler from the Sample Introduction list b Check Print Data Report after Each Sample Set optional If you wish you may type in your name and give your instrument a name All other choices should remain un checked Click OK 5 3 SAMPLE
35. tion provided by the equip ment may be impaired SYSTEM SETUP Utility Requirements for Apollo 9000 Environmental Typical laboratory environment to operate the unit is 18 C 30 C 40 7096 humidity free from corrosive explosive and volatile vapors Gas Hydrocarbon and CO free air can be supplied from either cylinder or gas generator such as a Balston Whatman TOC Gas Generator Gas Consumption Instandby and sleep modes the unit will use 50 cc per minute to purge the NDIR n Ready mode Apollo will use between 450 cc to 650 cc per minute 2 3 5 5 5 Regulators Uncontaminated 2 stage regulator for above stated gas Second stage operation range should be 0 60 psi equipped with outlet for 1 8 Swagelok brass nut and ferrule When using a gas generator please check with manufacturer for recommended generator gas pressure requirements Whatman TOC gas generator Model 78 40 requires 60 psi of compressed air or better AWhatman regulator kit will be required TeledyneTekmar p n 080 021 to drop the pressure from 60 psig exiting the generator to 30 psig entering the TOC analyzer Tubing 1 8 o d x 1 16 i d PTFE tubing or 1 8 o d refrigerant grade copper tubing Lengths greater than 15 ft should be 1 4 o d or larger con nected to a short length of 1 8 tubing that connects to the analyzer Ten feet of 1 8 PTFE tubing is supplied with the instrument
36. tion standards because the carbon in the preparation water is part of the calibra tion curve Note Apollo 9000 standard calibration is performed all you have to do is assign appropri ate active calibration curves prior to sample analyses You do not need to perform the calibration procedure for each sample run Standard analyses have in general three major sources of carbon content measured carbon content added to the ultra pure water carbon from the preparation water itself and carbon associated with the reagents used to perform the relevant analysis When we calibrate the instrument to y mx b linear fit the constant carbon contribu tion of the prep water and the reagent are represented by the y intercept b y mx b b reagent rinse water CALIBRATION The slope of the curve m represents the relationship of the measured carbon in the standard to the response of the instrument since only this source of carbon changes between any set of standards Note Running your preparation water as standard can be an excellent way to cali brate the low end of the concentration range for low level methods After calibration the slope m will be used as our response factor in sample analysis However the y intercept b will not used because the carbon associated with a blank may change over time To address this issue special blank methods be run at anyti
37. tube Remove the quartz wool that is on top of the catalyst Pour the catalyst into a 100 or 250 mL beaker It may require a bit of help if there is very much solid material deposited on the catalyst Take care to not break the catalyst pieces Rinse the catalyst with approxi mately 50 mL of DI water Swirl the beaker gently Pour off the water and repeat the rinsing twice more Place the beaker with catalyst in a 100 C oven for about 1 hour Caution wear protective gloves when removing the hot beaker from the oven 7 3 4 Clean the Combustion Tube The used combustion tube will have some degree of frosting after some use The frosting is devitrified quartz and will not be removed by any common solvent It does no harm unless the devitrification is so severe that the quartz is crystallized completely through the wall Note Wear protective gloves and eyewear when handling acid Quartz chips easily Take care to not hit the ends of the combustion tube sharply on the graduated cylinder 1 Prepare some dilute nitric acid approximately 5 a 100 mL graduated cylinder 2 Carefully immerse the tube top first into the solution and allow to stand for about 30 minutes 3 Liftthe tube from the acid solu tion rinse and immerse again bottom first for the same amount of time 4 Remove the tube from the solu tion rinse thoroughly with DI water and place it in a 100 oven to dry Caution wear prote
38. when the concentration of IC is more than 50 of the total carbon The precision of the TOC analysis decreases as the amount of IC in creases For example a sample con taining TC of 20 5 0 4 ppmC and IC of 20 0 0 4 would yield a TC IC value of 0 5 0 56 ppmC From 2 rsd for TC and IC a 112 rsd is obtained for the TC IC Teledyne Tekmar has also found that the number of counts for carbonate standards 100 ppmC and up is higher when run as an IC com pared to TC This may be due to incomplete decomposition depending on concentration of carbonates at 680 C Bicarbonates HCO3 gave a better recovery 6 8 6 3 Modifying Analysis Methods The operator can modify analysis methods Pay heed to the warning message before taking up this task The analysis method contains all the parameters pertinent to an analysis such as sample volume sparge time for autosampler sparge time for IC sparger priming rep volume etc One must be sure that the IC sparger is not overfilled so that water goes to the mist trap For all of TC or TOC range 2 or 3 meth ods the maximum injection volume is 50 uL The nomenclature for the parameters is the same except for the dilution methods Table 6 3 describes what each parameter means When the new method is set up and OK is clicked a message box will instruct you to re select any samples in the Sample Setup to use the new method Click OK to return to the Sample Setup Screen
39. will appear This is to remind you to Set Active standard calibration methods for the mode s of analysis TC IC TOC and range s you intend torun TOC Talk Apollo 9000 Setup Results Help Instrument Diagnostics Calibration Cal Verification Backup Password Wakeup Standards Exit Figure 4 2 2 Set Active Calibration Submenu CALIBRATION 2 Set Active Calibration Curve 1 From the Set Active submenu select TOC Curve TOC Mode Active Calibration Curves 0 20 1 400 10 750 default 2 100 4000 default 1 000 25 000 default x Aux default Figure 4 2 3 TOC Mode Active Calibration Curves 2 Inthe 0 20 1 400 Range list select the TOC Calibration Calibration Curve ID TOC Calibration is the name you gave the Calibration Setup TOC Talk will use the Active Calibration Curve TOC Calibration setup for the 0 20 1 400 Range data from the standards to analyze calibration Note TOC Talk references the Active Calibration Curves which are files that store the information associated with a specific Calibra tion Curve ID or Method ID during sample runs If you want to analyze a standard you must first create a Calibration Setup table and then set the Active Calibra tions Curves Once you save the standard concentrations Calibra tion Curve IDs and set
40. 0 USER MANUAL TABLE CONTENTS INTRODUCTION TABLE OF CONTENTS 1 1 Apollo 9000 TOC Analyzer 1 3 1 2 Technical Specifications 1 4 1 3 Safety 1 8 1 4 Part Descriptions 1 9 1 5 Apollo 9000 Operating Modes 1 15 1 6 Sample Introduction 1 15 1 7 Prime Replicate 1 16 1 8 Analysis Process 1 16 SYSTEM SETUP 2 1 Before You Begin 2 3 2 2 Unpack and Inspect 2 6 2 3 Tools and Supplies Needed for Connections 2 7 2 4 Pneumatic Connections 2 7 2 5 Electrical Connections 2 11 2 6 Install the Autosampler Optional 2 12 2 Add Catalyst to and Install the Combustion Tube 2 18 2 8 Install TOC Talk Software 2 21 2 9 Condition Combustion Tube Catalyst 2 22 2 10 Cleaning Procedure for Conditioned Catalyst 2 23 TOCTALK 3 1 TOC Talk Control Screen 3 3 32 Instrument Setup 3 3 3 3 Instrument Diagnostics 3 6 3 4 Archive Data 3 10 3 5 Password Setup 3 11 3 6 Wakeup Schedule 3 12 CALIBRATION 4 1 System Calibration 4 3 4 2 Standard Calibration Without Autosampler Tutorial 4 4 43 Standard Calibration With Autosampler Tutorial 4 11 SAMPLE ANALYSIS 5 1 Sample Analysis 5 3 5 2 Tutorial TOC Results Made Easy Without Autosampler 5 3 5 3 Tutorial TOC Results Made Easy With Autosampler 5 6 54 Sample Blanks 5 9 SPECIAL APPLICATIONS 6 1 Sample Preservation for TOC 6 3 6 2 Applications 6 4 6 3 Modifying Analysis Methods 6 8 MAINTENANCE ANDTROUBLESHOOTING 7 1 Scheduled Maintenance Checks 7
41. 000 Maintenance Worksheet D Daily Month Year W Weekly M Monthly Notes Signature s APPENDIX A Apollo 9000 Maintenance Worksheet D Daily Month Year W Weekly M Monthly Notes Signature s APPENDIX A Apollo 9000 Maintenance Worksheet D Daily Month Year W Weekly M Monthly Notes Signature s APPENDIX A Apollo 9000 Maintenance Worksheet D Daily Month Year W Weekly M Monthly Notes Signature s APPENDIX A Apollo 9000 Maintenance Worksheet D Daily Month Year W Weekly M Monthly Notes Signature s APPENDIX A Apollo 9000 Maintenance Worksheet D Daily Month Year W Weekly M Monthly Notes Signature s INDEX Symbols ugC 4 5 4 12 7 11 7 13 7 14 7 15 Acid 2 10 5 7 7 9 Content Samples with High 6 7 reagent 5 5 supply 4 16 5 5 7 3 vial 4 16 vial bracket 2 16 Active Calibration Curve 4 4 4 6 4 13 air bubbles 1 15 Analysis 5 3 Methods modifying 6 8 range 3 5 Results 4 7 4 9 4 14 4 16 5 4 5 6 Setup 4 8 Time 1 4 Applications special 6 3 Anhydrous sodium carbonate 2 5 AOAC 973 47 1 5 Apollo 9000 1 3 dimensions 2 5 software 1 4 TOC Talk 2 21 Archive Data 3 10 Arch
42. 7 10 7 11 plunger 7 12 System 2 21 3 4 Calibration 4 3 status 3 4 T TC 1 3 1 4 1 15 methods 4 3 TC IC 1 15 TC TOC standard 2 5 Temperature Controller 1 13 2 22 Time vs Millivolts 4 7 4 14 tin 1 11 and copper granules 1 11 TOC 1 3 1 4 1 15 3 4 analysis 1 3 1 10 Analysis Time 1 5 Curve 4 6 Gas Generator 1 6 2 3 Results 5 6 sample analysis procedure 5 3 Standard 4 8 TOC Talk 1 4 2 22 3 3 3 12 7 5 TOC free carrier gas 2 7 Total Carbon 1 3 1 15 Total Carbon Minus Inorganic Carbon 1 15 Total Organic Carbon see TOC Troubleshooting 7 22 Tubing 2 4 2 8 connections 2 8 tutorial 5 3 two stage regulator 2 7 U ultra pure water 4 3 User Interface 1 4 USP 643 1 5 Utility Requirements 1 6 2 3 6 3 viii V Valves 3 6 7 24 7 27 Control 3 6 mounting plate 7 16 Vial number 2 22 Position 1 5 7 Voltage 1 6 Wakeup 3 12 Schedule 3 12 Waste bottle 2 5 water 1 3 1 5 6 7 Water accumulation 7 3 Contribution 4 4 Trap 1 3 1 11 1 12 2 22 3 6 7 24 trap flow 7 22 X XYZ robot 1 6 1 14 Y y intercept 4 3
43. ASM Sampling needle should be installed Refer to Section 7 2 16 for installation instructions SPECIAL APPLICATIONS 6 2 3 Samples with High Salt Content Analysis of samples containing high concentration of salt offers a big challenge for high temperature com bustion analyzers Metal cations such as sodium have the effect of devitrify ing the quartz combustion tube causing it to crystallize and break Salts can also deposit on the catalyst resulting in a loss of efficiency An application note Summer 99 Volume 9 14 entitled Measuring Carbon in Salty Water includes TOC analysis with seawater as samples Although the Apollo 9000 is well suited for perform ing analysis of salty waters the follow ing strategies can be used 1 Decrease Injection volume De pending on the level of carbon in the sample it is best to use as little of the sample as possible to prolong the life of the catalyst 2 Dilute the sample This can be done manually or automatically for TOC and TC analyses Samples can be diluted by using the TOC_TC Method 1 000 25 000 Method 100 5 000 for Apollo 9000 HS Refer to Section 6 3 on making new methods In addition to the directions on Section 6 3 the following should also be modified Injection volume aliquot of diluted sample injected in the combustion tube Sparger volume Amount of sample transferred into the Sparger for dilution Dilution Volume amount of DI water added to the IC s
44. Apollo 9000 Combustion Analyzer User Manual Copyright 2003 Teledyne Tekmar Co No part of this document may be copied reproduced transmitted in any form or by any means electronic or mechanical including photocopying recording or information storage and retrieval systems for any purpose other than the purchaser s personal use without the express written permission of Tekmar Company Updates Teledyne Tekmar may update the information contained in this document without notice to the purchaser The following are registered items Adobe Acrobat is a registered trademark of Adobe Systems Incorporated Intel Pentium is a registered trademark of Intel Microsoft Windows Windows Microsoft Internet Explorer and Microsoft Excel are either registered trademarks or trademarks of Microsoft Corporation in the United States and or other countries is a registered trademark of Corning Incorporated Swagelok is a registered trademark of Swagelok Companies TEFLON is a registered trademark of du Pont de Nemours amp Inc Tygon is a registered trademark of Norton Company Whatman TOC Gas Generator is a registered trademark of Whatman Inc Teledyne Tekmar Mason Ohio USA 800 543 4461 www teledynetekmar com Document Part Number 14 9000 074 Rev D Version 08 09 03 Outside the U S and Canada 513 229 7000 Service 800 874 2004 Fax 513 229 705
45. C sample If it is not Teledyne Tekmar recommends rerunning the sample blank or manually setting the sample blank To run a sample blank simply choose the appropriate sample blank type under the sample setup screen Table 5 4 3 outlines the correct blank setups for the default IC methods Sample Method ID Blank Sample ID Blank Method ID IC 0 20ppmC Blank IC Rng 1 Blank IC Rng 1 IC 1 400ppmC Blank IC Rng 1 Blank IC 1 400ppmC IC 10 750ppmC Blank IC Rng 2 Blank IC Rng 2 100 4000ppmC Blank IC Rng 3 Blank IC Rng 3 When IC Blank Range 1 is chosen IC 0 20ppmC will automatically be set as the Method ID Make sure to change this to IC 1 400 ppmC Table 5 4 3 IC Sample Blanks SAMPLE ANALYSIS Notes SPECIAL APPLICATIONS 6 1 Sample Preservation for TOC TOC methodologies vary in their requirements for the preservation of samples The addition of an inorganic acid to the sample stops the microor ganisms present in the sample from metabolizing the organics for food by The decreased pH of the sample also retards the growth of slime molds that are present as spores in the atmo sphere Sulfuric acid hydrochloric acid phosphoric acid and nitric acid can be used Since many present day TOC analyzers will automatically add an aliquot of acid to samples before sparging to remove inorga
46. E DRIVER SCRUBBER 8 5 VALVE COOLINGFAN 0 1VOLT 3 SIGNALTO mn 200 ml min FLOW VENT H RESTRICTOR 2 200 ml min FLOWMETER FLOW RESTRICTOR ASM SPARGE H 200 ml min FLOW RESTRICTOR 7 50 ml min E FLOW RESTRICTOR 14 9000 074 Rev B 09 2000 SWVYDVIG 9 6 epo abieds ajpaan DOL 26 end IC Removal with Autosampler Needle Sparge ACID p WATER TRAP DI WATER WASTE SYRINGE DRIVER EE TO ASM SPARGE 200 ml min FLOW B RESTRICTOR 14 9000 074 Rev B 09 2000 SAMPLE INLET 200 ml min FLOW RESTRICTOR IC SPARGER INJECTION PORT OMBUSTIO L Liquid Sample Line Gaseous Sample Carrier Gas COM NO IC Sparge Gas Line IC 5 VENT Removal NC NDIR Purge Permeation Dryer and Injection Port NC Lines Not Used During MISTTRAP Analysis 4 PERMEATION NO COM DRYER TOC FREE 200 ml min AIR FLOW RESTRICTOR DI WATER BOTTLE 1 HEADSPACE PURGE WATER TRAP CORROSIVES sn SCRUBBER TO 8 PORT VALVE COOLINGFAN 0 1VOLT NDIR SIGNALTO VENT 200 ml min FLOWMETER FLOW RESTRICTOR 50 ml min FLOW RESTRICTOR SINVHDOVIG 4 6 apow gt YM DOL
47. Gas to NDIR and set the Furnace Gas to vent Locate the mist trap Check all rubber seals to verify they are intact and securely in place Remove the green inlet tube at the side of the trap and measure the flow with a hand held flowmeter Again you should obtain the same reading as in step 2 If you obtain a reading of less than 9896 of step 2 remove the glass frit in the IC sparger soak the frit in basic solution of 1M NaOH rinse and then reinsert the frit into sparger Remeasure the flow entering the water trap If you obtain a reading within 9896 of step 2 entering the water trap continue to the next section Leak Checking the Combustion Furnace 7 23 MAINTENANCE AND TROUBLESHOOTING Leak Checking Before the Water Trap 6 10 Measure the flow of the 1 8 blue line entering the right side of the injection port This is the carrier gas line to the combustion furnace If flow is between 180 to 220 cc min reinstall line and go to step 7 Otherwise go to step 9 Measure the flow leaving the combustion furnace by removing stainless steel to Teflon line union If flow is good then replace your coiling coil and go back to step 3 If not go to step 8 Inspect and verify the combustion tube for cracks and tube o rings for wear Verify fittings leaving the combustion furnace for leaks If leak is identified and corrected reconnect removed lines and return to step 3 If leak problem is still present
48. Inlet Syringe Figure 1 4 4 8 Port Valve 1 9 INTRODUCTION IC Sparger The sparger is a glass vessel that holds the sample while Apollo 9000 acidifies and sparges the sample of inorganic carbon IC and purgeable organic carbon POC and prepares the sample for TOC analysis e provides the location for Range 4 sample dilution Figure 1 4 5 IC Sparger Gas flows through the sparger removing the IC from the sample The Apollo 9000 can detect IC in IC mode or send it to vent while preparing for TOC mode Combustion Furnace with Injection Port The combustion furnace provides the high temperature necessary to oxidize the carbon in the sample to CO It holds the quartz combustion tube between the bottom connector and the injection port at the top O rings provide gas tight seals at each end The combustion tube contains a bed of proprietary catalyst that promotes oxidation of organics Figure 1 4 6 Combustion Furnace with Injection Port The injection port provides the interface for the sample line and the furnace carrier gas into the combustion furnace The sample line enters from the top of the injection port and the carrier gas enters from the right of the injection port Corrosives Scrubber The detector which measures carbon dioxide can be damaged by halogen To prevent analytical errors the corrosives scrubber removes halogens from the carbon dioxide before it enters the detector The co
49. S If your results do not approximate these values and you are running samples higher than 1ppmcC it may be accept ableto run standards and samples However if you are running 1ppmC samples then repeat the conditioning procedure to lower the raw data for your DI water and background Note Some systems may not have DI water clean enough to meet these guidelines If you are running samples gt 1 ppmcC your results may be acceptable If results are not acceptable then TeledyenTekmar recommends using an improved DI water source 2 23 5 5 5 Notes 2 24 TOC TALK TALK 3 1 TOC Talk Control Screen The TOC Talk Control Screen appears when the TOC Talk software is started Menus Mode NDIR Status Output mV Current Date and Time TT Rasse a 1 TOC Talk Control Screen Figure 3 1 The Control screen contains menus with keyboard shortcuts setup options the run option results and a status bar that depicts event list items in real time along with mode status and current NDIR mV output 3 2 Instrument Setup Before you begin analyzing samples TOC Talk must be configured to run Apollo 9000 and its accessories To access the Instrument Setup Status Screen select Instrument from the Setup menu Instrument Setup Sta
50. The injection port seals to the combustion tube with an o ring Examine the o ring for any debris If necessary wipe it gently lfitis deemed necessary to remove the o ring do not attempt to pick it out with a sharp instrument Instead remove the 4 screws that hold the metal plate and spacer blockto the injection port It can now be easily removed b Anewo ring must be lubri cated with a small amount of silicone vacuum grease Withatiny amount of lubricant on the fingertips rub it on the o ring d Usealab wipe and try to wipe all the lubricant away Enough will be left to make it easy to slide the injection port onto the combustion tube Slide the injection port onto the combustion tube with gentle pressure and a slight turning movement Replace the screws Reconnectthe gas line above the right screw 2 8 Install TOC Talk Software To install the Apollo 9000 TOC Talk program on Windows 95 98 NT 1 Start Windows 2 Close any open applications 3 Place the Apollo 9000 TOC Talk CD ROM into the CD ROM drive The Apollo 9000 CD Menu will appear 4 Select the Apollo 9000 install icon 5 Follow the installation prompts Note TeledyneTekmar recommends that you accept the default installation directory on your hard drive for Apollo 9000 TOC Talk SYSTEM SETUP Configure Apollo 9000 with TOCTalk Before you begin analyzing samples TOC Talk must be configured to run Apollo 9000 and its accessor
51. afety 1 8 7 3 references 1 8 Salt Content Samples with High 6 6 Sample 1 5 4 3 5 4 5 7 Analysis 2 22 4 7 4 8 4 14 4 16 5 3 5 4 5 5 5 6 5 7 5 8 blank 4 3 concentration 1 4 Delivery 1 15 dilution 1 10 ID 4 7 4 14 5 4 inlet line 7 25 Introduction 1 5 1 15 2 21 3 4 5 6 Needle 2 15 Preservation for TOC 6 3 repetitions 5 7 run 4 3 5 5 5 8 set 3 5 Setup 2 22 4 7 4 8 4 14 5 4 5 6 5 7 Tray 2 17 Type 2 22 4 3 4 6 4 8 4 13 4 14 5 4 5 7 INDEX Scrubber 1 11 Select Calibrator 4 8 septum 7 5 piercing 1 6 Set Active Calibration Curve 4 4 4 6 4 13 Home 7 9 7 10 7 12 point 1 13 7 18 setup 2 3 Standard Calibration Analysis 4 7 4 14 Sample 5 3 Standard Calibration Analysis 4 4 Sleep Mode 2 3 3 4 Slope 4 3 4 4 Sludges 6 7 sodium hydroxide solution 2 22 Solids and Sludges 6 7 Sparge Option 3 4 Sparger 1 3 Stabilize Baseline Time sec 3 4 Standard 4 3 4 6 4 13 analysis 4 14 4 16 analysis rep 4 9 Calibration 4 3 4 4 4 6 4 10 4 12 4 14 concentration 4 10 deviation 5 5 5 8 ID 4 5 4 8 4 12 Method 5310B 1 5 run 4 9 4 16 Standards 2 5 Standby 2 3 3 4 3 5 3 12 Start 5 5 5 8 Run 4 7 4 14 5 3 Standard Calibration Analysis Run 4 4 4 16 status mode 3 4 Stirring Option 1 5 Strip Chart 4 7 4 14 5 4 5 6 STS 8000 Autosampler 1 6 2 5 1 14 vii INDEX Syringe 1 3 1 15 7 8 7 9 7 10 7 11 assembly 7 11 Diagnostics 7 8 7 10 7 11 Driver 1 5 1 9 7 8
52. ait until the furnace reaches 900 C 3 Make sure the one liter DI water supply vessel is filled 4 StartTOCTalk 5 Click Runin the main screen of the Apollo 9000 software This will bring you to the Sample Analysis screen 6 Click Sample Setup to access the Sample Setup screen 7 Whether in Autosampler or Auto matic Syringe Mode select Sample from the Sample Type list 8 Select Condition Catalyst from the Method ID list 2 22 10 11 Enter 1001 as the vial number in the Pos column if you use an autosampler Water is taken from the DI water supply rather than from avial Click Save Use Click Start in the Sample Analysis window After the system completes the conditioning process 24 reps total change the temperature setting back to 680 C and wait for the furnace to cool Reconnect the water trap tube see Step 1 After the temperature reaches 680 C a Autosampler Users Place 5 vials of freshly drawn DI water into the autosampler vial tray In Sample Setup select Sample as Sample Type TC 0 100 as the Method ID and 5 reps Click on Save Use and Startthe run b Automatic Syringe Users Place the sample tube con nected to Port D of the 8 port valve into a container of freshly drawn DI water or into the DI water supply ofthe analyzer In Sample Setup select TC 0 100 as the Method ID and 10 reps After the 10 reps finish click Start again After the second run perf
53. ake sure the carrier gas going into the instrument is on and the pressure regulator is set to 30 35 psi If not adjust the pressure within this range and recalibrate the instrument after the success ful completion of this leak check ing procedure 3 Check the flow leaving the NDIR on the 1 8 green line exiting the rear of the instrument with a manual flow meter Write down NDIR flow result MAINTENANCE AND TROUBLESHOOTING Using a manual flow meter measure the flow for the 1 8 green line entering the side of the mist trap Write down mist trap flow result The flow path is leak free if the flows measured in steps 3 and 4 will fall within a 180 to 220 cc min range Condition 1 and are within 10 cc min of each other Condition 2 Otherwise adjusting the system pressure within the 30 35 psi range verifying that the pressure gauge is reading correctly If condition 1 is still not satisfied you will have to go to step 6 and or step 11 If condition 1 fails for the mist trap go to step 6 Leak Check ing before the Mist Trap b Ifcondition 1 fails for the NDIR but not the mist trap and condition 2 passes try C If condition 2 fails and the NDIR flow is lower than the mist trap go to step 11 Leak Checking after the Mist Trap d If condition 2 fails and the NDIR flow is higher than the mist trap then it is highly probable that the counter flow of the permeation dryer is bleeding into the sample gas flow Re
54. alve at port C Make sure the fitting is finger tight but do not over tighten the nut Use the tool provided with your Apollo operating kit You may wish to remove the 8 port valve from the syringe pump to provide easier access to the ports If the valve is removed be sure to engage the nub behind port A into the syringe drive body before replacing the two valve screws After the valve is reattached use Diagnostics Syringe to turn the valve to waste and then home the syringe Reinstall the right cover to the instrument 7 9 MAINTENANCE AND TROUBLESHOOTING 7 2 7 Replace Clean Syringe Tool s Needed gt de Slotted screwdriver Teflon tape Enter Syringe Diagnostics screen in TOC Talk software Turn valve to IC sparger Port B Set syringe pull to 1000 ul Open acrylic door on instrument Locate syringe on left front of instrument Remove screw directly below the syringe DO NOT force removing the screw If removing the screw is difficult you may also need to loosen the thumbscrews on the 8 port valve face to provide more flexibility in removing the syringe screw If the screw is difficult to remove use the TOC Talk Syringe Diagnostics to move the plunger 5001 away from the Home position Remove the syringe by unscrewing it from the 8 port valve Pull plunger out of syringe Clean both plunger face and syringe with DI water until both are free of debris Reinstall the
55. as Active TOC Talk will automatically refer to the current standard calibration configuration when Standard is selected as the Sample Type for analysis CALIBRATION 3 Setup Standard Calibration 1 FromtheTOC Talk Control Screen Analysis click Run Sample Analysis displays the IMPORTANT current Sample ID information Proceed carefully Most only after a run is started Start Apollo 9000 TOC Talk stan Run button Sample Setup dard calibration errors occur button during the following steps If standard analysis setup instructions are not followed unsuccessful calibrations and reduced sample integrity can occur Strip Chart displays in real time response from the NDIR as Time vs Millivolts and refreshes atthe beginning of each sample run Analysis Results continuously displays current analysis data up to 30 rows so that you can Strip easily monitor Apollo 9000 performance Start Run Analysis Button Results Window Figure 4 2 4 TOC Talk Run Screens 4 7 CALIBRATION Without AutoS ampler Analysis Setup Select Sample ID Di water pee Sample Select Sample TET 4 Number Number of Repeats 5 BL Reps Select Method ID TOC 0 20 ppmC Mode Sample Click OK 1 Calibration Curve TOC CALIBRATION Select Calibrator 1 000 25 000
56. as Supply Hydrocarbon and CO2 free air Balston Whatman TOC Gas Generator Gas Pressure e 30to35 psi 206 7 to 241 2 kPa 1 6 STS 8000 Autosampler Sampler Changer Type XYZ robot with stationary rack design Positioning Performance e Accuracy 1mm XYZ dimensions Repeatability 0 25 mm in XYZ dimensions Septum Piercing Available with septum piercing kit Has vertical punch strength of 3 8 kg 8 38 Ibs Rinsing e Auto rinsing with sample and or rinse water via built in rinse station Rack Selection e 2 77 position trays for 25ml culture tubes 18 x 150 mm e 2 35 position trays for 40ml vials 28 X 95 mm Dimensions 53 5 43 7 Dx 37 1 H in21 1Wx17 2Dx 14 6H 17 7 kg 39 lbs INTRODUCTION Electrical e Voltage 100 120 230 VAC 10 e Frequency 50 60 Hz Power 200VA Certification UL CSA and CE e EMC EN50081 1 and EN 50082 1 INTRODUCTION 1 3 Safety Explosion The following warning illustrations describe the symbols and safety references used in this manual Hazardous Voltage Fire VAN CAUTION Hazardous situation which if not avoided will result in product or property damage and possible injury Corrosive liquid or substance High Temperature WARNING Potentially hazardous situation which if not avoided can result in death 2 a2 ME Risk of eye injury w
57. bon contri bution of particulates in the sample When using this option the appropri ate sample line furnace line and autosampler sampling needle should be installed See the Fall 1999 Volume 9 22 application note entitled TOC Analysis of Particulated Samples SPECIAL APPLICATIONS Homogenization Homogenization can be performed by using blenders ultrasonic devices or processing the sample in a homogeni zation device such as the Tissumizer from TeledyneTekmar This method is suitable when the carbon contribu tion of the particulate needs to be measured in addition to the carbon from the liquid component Filtration If only dissolved organic carbon is to be determined the sample can be filtered Use a filter that is free of compounds that contain carbon You can use the standard autosampler needle and transfer lines for filtered 0 45um samples Dilution Dilute the sample with deionized water by a factor of 10 100 Your results will need to be recalculated by multiplying the dilution factor Sample Stirring The sample particulates can be sus pended during an analysis by using a magnetic stirrer An application note Fall 1999 Issue Volume 9 22 entitled TOC Analysis of Particulated Samples is available from Teledyne Tekmar The Apollo 9000 runs a special method to include the carbon contribution of the particulates in the sample When using this option the appropriate sample line furnace line and
58. con Help Figure 3 3 1 Diagnostics Valve Control Screen A WARNING Do not alter this screen during an analysis Erroneous or conflicting data can damage the instrument Gas Input Select On or Off for each of the Apollo 9000 components you want gas carried to e Permeation Dryer turns gas on to the permeation dryer 200cc min Valve 1 Furnace turns gas on to the combustion furnace Valve 2 CSparger turns gas on to the IC sparger Valve 3 ASM Sparge turns gas on to the autosampler Valve 7 Gas Output When Valves 4 and 5 are on to direct the IC Sparger flo to the NDIR Valve 2 must off Failure to turn Valve 2 off when Valves 4 and 5 are on could result in dangerous pressurization of the combustion tube and water trap Select where you want the following combustion furnace and IC sparger output sample gases to go Furnace Gas To either Vent or NDIR Valve 4 IC Gas To either or Vent Valve 5 Auxiliary Furnace Power controls power to the combustion furnace The default setting is Off Syringe Pump and 8 port Valve Diagnostics On the Setup menu point to Diagnos tics and then click Syringe Syringe Pump amp 8 Port Valve Control x Valve Position Postion Position Position Move Home Position Syringe Volume Position pL Current Position Movei 9 0 Move Help Home Position Figure 3 3 2 Diagno
59. ctive gloves when removing the tube from the oven 5 Add Catalyst to the Combustion tube After placing new quartz wool and the catalyst into the cleaned combustion tube install it in the instrument 6 Follow the instructions in section 2 10 Cleaning Procedure for Conditioned Catalyst MAINTENANCE AND TROUBLESHOOTING 7 4 TeledyneTekmar Customer Support If you need assistance solving a prob lem please follow these steps 1 Write down the model name model number and serial number of the instrument 2 Note the type of problem you are having write down the conditions under which the problem oc curred and the display activity or result that indicated the existence of a problem 3 Place the manual near the tele phone The service representative may ask you to look at a diagram Call Teledyne Tekmar at one of the following numbers e 800 874 2004 toll free in the US and Canada 513 247 7000 outside the US and Canada gt MAINTENANCE AND TROUBLESHOOTING Notes 7 30 CALIBRATION STANDARD 8 1 Calibration Standard Preparation The objective of this section is to make accurate stock standard solutions of organic and inorganic compounds in reagent water Working standard solutions are then prepared by accu rately diluting these stock solutions with reagent water 8 1 1 Materials a
60. e and syringe per step 10 Press the Initialize button on the right face of the syringe driver The syringe plunger will move to the predetermined position just below the top of the syringe Using the thumbwheel on the bottom of the syringe move the syringe plunger to the top of the syringe Stop when you hit signifi cant resistance Press the Set Home button on the right face of the syringe driver 1 Close acrylic door 7 2 9 2 Valves Tool s Needed 1 10 11 12 Phillips screwdriver 3 8 5 16 wrenches Turn off power at the back of the instrument Remove plug from back of the instrument Remove both left and right side covers Locate the Clippard valve to be replaced on the plumbing side of the instrument On the electrical side of the instrument remove the power cable for the Clippard valve from the PCB board Remove the Clippard valve from its mounting clip With the wrenches and noting the proper line positions unscrew the lines attached to the Clippard valve Hold the small fitting stationary while loosening the large fitting Reattach these lines to the new Clippard valve Hold the small fitting to avoid loosening or overtightening it to the valve Reattach the Clippard valve to its mounting clip Plug the power cable for the Clippard valve into its proper position on the PCB board Reinstall both left and right covers to the instrum
61. e buttons during this procedure any errors incurred will be corrected when you initialize and home the syringe per the instruction at the end of the procedure 7 2 6 Furnace Injection Line 1 Remove the right cover of the instrument 2 Remove the furnace injection line from the top if the injection port 3 Remove the 1 16 diameter furnace injection line from the 8 port valve at port C and remove the line from the instrument You may wish to remove the 8 port valve from the syringe pump to provide easier access to the ports Removal of the screw holding the MAINTENANCE AND TROUBLESHOOTING plunger of the syringe is made easier by drawing the syringe down about 0 5 mL by using the Diagnostics Syringe valve DI water position and move syringe to 500 mL The screw has a very close fit tolerance It is important to not force the screw Locate the appropriate furnace injection line for your application 0 8 mm I D and 0 5 mm 1 0 lines will have tubing protruding about 1 4 from one end That end attaches to the injection port The 0 1 mm I D line will have tubing and a needle protruding from it Run the furnace injection line to the front of the instrument You may wish to remove the nut and ferrule while directing the line through the grommet When the nut and ferrule are reattached be sure that the tubing end is flush with the face of the ferrule Attach the furnace injection line to the 8 port v
62. e features of Apollo 9000 software TOC Talk Pre defined Default Methods Mutti Point Calibration Outlier Deletion e Wake up and Shut down e Plotted Calibration Curve Statistics e Multiple Method Storage Analog Display of Peaks Continuous Scrolling of Results Diagnostics 1 2 Technical Specifications Apollo 9000 TOC Analyzer Chemistry Oxidation by Combustion from 680 C to 1000 C IC by Acidification and Sparge Detector Nondispersive Infrared NDIR Measurements TOC NPOC TC IC TC IC Analytical e Range 4 ppbC to 25 000 ppmC sample volume detector and dilution dependent using only 4 selectable analytical ranges Precision Typical 0 05 of full scale RSD 396 whichever is greater over 3 replicates Injection Volume Upto2ml Analysis Time 1103 minutes typical TOC Analysis Time 15 minutes per triplicate typical Liquid Handling Syringe driver 8 port valve e Auto dilution method provided from 4000 ppmC to 25 000 ppmC and or difficult matrices e Auto rinsing with sample and rinse water Sample Introduction e Automatic syringe injection Autosampler Solids Boat ManualSyringe Controller PGInterface through Windows 95 98 or NT Password Protected Data Handling Automatic and customized Spreadsheet reports transferable to Microsoft Excel e Real time display of NDIR signal
63. e protection is recom mended 2 17 5 5 5 2 7 Add Catalyst to and Install Add Catalyst to the Combustion the Combustion Tube Tube The combustion tube is quartz and is Combustion Tube placed in the furnace 20 g Catalyst The salts from oils present on human skin if left on the tube will cause damage to the tube in the hot furnace Wear gloves while handling Quartz Wool Quartz Wool Safety Gloves the tube and wipe it clean with a damp cloth or paper towel before placing itin the furnace Tube Packing Tool Figure 2 7 1 Items Required for Combustion Tube and Catalyst Installation 1 Verifythatthe combustion tube is clean has no cracks and that neither endis chipped The narrow end is the bottom of the tube SYSTEM SETUP 2 Place a loosely wadded tuft ap proximately 1 2 thick of quartz wool through the top of the com bustion tube to just above the narrow opening To prevent catalyst from dropping through the quartz wool gently pack the top of the quartz wool so that there is no space between the perimeter of the quartz wool and the glassware Figure 2 7 3 Adding Catalyst to Combustion Tube 4 Add0 5 quartz wool on top of catalyst The added quartz wool will protect and add life to the catalyst Figure 2 7 2 Adding Quartz Wool to Combustio
64. e scrubbed from the gas stream using copper and tin but some may break through and cause the detector to be corroded Samples that contain hydrochloric acid will form gas in combustion TOC instruments Since most commer cial analyzers that are equipped with a gold lined sample cell use an NDIR to detect the corrosive nature of can damage the NDIR The Apollo 9000 copper and tin scrubber manages to scrub out some HCI but HCI break through is common and causes NDIR detector corrosion Phosphoric Acid H PO is a weaker acid compared to the others men tioned However it is not as corrosive and the combustion product is which is readily taken up water and does not stay in a gaseous state to be swept into the detector Nitric Acid HNO in combustion instruments will form N O which is a corrosive gas The copper and tin scrubber will remove some of the gas but not all and there is the potential for corrosion in the detector 6 2 Applications 6 2 1 The Apollo 9000 HS is a new genera tion combustion TOC analyzer that has the high sensitivity necessary to measure low levels of carbon When using this system or the regular Apollo 9000 several conditions must be taken into account when running samples Low level Carbon 1 Clean glassware It is recom mended that all glassware be cleaned with soap and water followed by rinsing with deionized water to eliminate any source of ca
65. e the same parameters as the first line while incrementing the vial position and the Sample ID to ID2 then 103 Click Save Use answer Yes to the Save Changes inquiry and enter TOC as the name of the Rack ID You will return to the Run screen Be sure to verify the following a That there are 3 vials of water placed on the autosampler in positions 1 2 and 3 Note Leave about one inch of headspace when sparging in the vials b Acid reagent is in the acid bottle located at Position 11 on the autosampler support bar only if you selected the Autosampler Sparge Option in Instrument Setup Status c The DI water line runs from a fresh DI water supply to Port G of the 8 port valve 5 7 SAMPLE ANALYSIS 3 Start Analysis Run 1 Click Start from the Sample Analysis screen 2 sample will begin You will have your data in approximately 45 minutes If a printer is con nected to the computer the Detailed Report will print showing reps for each vial as well as the average standard deviation and RSD TUL NOIR Output 9 6554 0 0713 4 2763 0 0835 Step 22 MEMORIZE BASELINE INDIR mV 3588 1112 2000 07 05 Figure 5 3 5 Example Please reference the TOC Talk Online Help for current comprehensive sample analysis calibration data results tutorials and ad vanced operation informa tion SAMPLE ANALYSIS
66. ear or serious injury safety glasses Hazardous or toxic substance DANGER Imminently hazardous situation which if not avoided will result in death or serious injury Moving parts can pinch and grab keep hands and clothing away while power is on 1 8 1 4 Part Descriptions Mist Trap Water Trap 8 port Valve Syringe Driver IC Sparger Temperature Controller Corrosives Scrubber Status LEDs 9 Figure 1 4 1 Apollo 9000 Front Cooling Fan Carrier Gas Inlet Waste Outlet Permeation Dryer IC Sparger Valve and NDIR Gas Outlet 1 0 Ports Power Switch Figure 1 4 2 Apollo 9000 Rear Syringe Driver and 8 port Valve The syringe driver is a precision measuring instrument that aspirates and dispenses fluid The syringe driver contains electronics a syringe 8 port Teflon valve and stepper motors The electronics control the motors and communication between the syringe driver and microcontroller The syringe driver can dispense up to 2 5 ml 196 of sample or reagent INTRODUCTION Figure 1 4 3 Syringe Driver The syringe driver turns an 8 port Teflon valve Each port on the valve is fitted with a valve washer before insertion of relevant tubing fitting to ensure airtight seal The port assignments for this valve are as follows IC Sparger DI Ay H pifj Combustion Water C a Furnace Waste LT Sample
67. ed sample is injected to the furnace as the priming rep This rep is not quanti fied 4 Successive aliquots of the sample are injected and quantified 5 ThelC sparger is emptied of excess sample 6 The water trap is emptied of condensate 1 16 Rinse Syringe with Sample Excess Water in Water Trap Emptied to Waste Deliver Sample to IC Sparger IC Sparger Contents to Deliver Acid Waste to IC Sparger Sparge Sample Rinse Syringe with Sample from IC Sparger Wait for Endpoint Sample Gas Swept to NDIR CO Concentration is Measured Memorize Baseline Combustion Furnace Gas Off Sample Gas Swept Through Corrosives Scrubber Sample Gas Swept Through Moisture Control System Deliver Sample to Combustion Furnace Start Integration Combustion Furnace Gas On Wait Time 15 Seconds Figure 1 8 1 TOC IC Removal in IC Sparger Analysis Process 1 8 2 Total Organic Carbon TOC Removal of IC with ASM Sparge Note There are rinsing steps for the syringe and other details that are not represented here 1 Autosampler ASM needle is rinsed with DI water and then the needle and transfer line is emp tied 2 ASM needle goes to the acid vial and the syringe draws the amount of acid that is prescribed by the analysis method 3 The ASM needle goes to the sample vial delivers the acid and sparge gas is started 4 After the spa
68. efore operating the autosampler you must first install fuses Figure 2 6 3 illustrates the two fuse drawers supplied with the unit the fuses are located in separately with the autosampler parts 100 120 Voltage Fuse 220240 Voltage Figure 2 6 3 Two Fuse Drawers Supplied To install fuses 1 Locate the accessory package containing the fuse drawer appro priate for your line voltage 2 Locate the accessory package containing the 2 0 amp fuses 3 Install the fuse s into the fuse drawer The fuse drawer for 100 120 V accepts one fuse The fuse drawer for 220 240 V accepts two fuses 4 Insert the fuse drawer into its receptacle in the back of the unit see Figure 2 6 2 Connect the RS 232 Interface Cable The RS 232 interface cable transfers information between the autosampler and Apollo 9000 see Figure 2 6 2 To connect the RS 232 Interface Cable 1 Locate the RS 232 cable 2 Attach the 25 pin male end of the cable to the RS 232 parallel port on the rear panel of the autosampler 3 Tighten the retaining screws 4 Attach the 9 pin end of the cable to the Com port on the rear panel of Apollo 9000 5 Tighten the retaining screws Set the Baud Rate SW2 selector sets the baud rate for the unit As a default the baud rate selector is set to 0 for identifying a baud rate of 19200 If the baud rate for your computer is 9600 complete the following steps to change the setting for
69. emoving seven 7 screws holding it to the chassis Noting their location remove all connections to the power entry module Remove power entry module by removing the two 2 mounting screws from the back of the unit Install new power entry module using screws from previous step Reconnect electrical cables to the power entry module Reinstall right hand cover Plug the AC power line back into power entry module and turn the power switch ON Reestablish communications with TOC Talk software MAINTENANCE AND TROUBLESHOOTING 7 2 15 Add Catalyst to and Replace the Combustion Tube Supplies Needed Combustion tube 20 g catalyst Quartz wool Tube packing tool not provided Safety gloves Note The salts from oils present on human skin if left on the tube will cause damage to the tube in the hot furnace Wear gloves while handling the tube and wipe it clean with a damp cloth or paper towel before placing it in the furnace Remove the Old Combustion Tube 1 Remove the right chassis cover from the Apollo 9000 2 Detach the injection port from the valve mounting plate by removing the two screws and set aside 3 Swing the locking guard at the bottom of the combustion furnace to the right until it touches the right furnace leg 4 Gently pull the combustion tube up through and out of the top of the combustion furnace and discard accordingly 5 Gently pull the bottom connector out from under
70. ent Plug the AC power line back into the back of the instrument and turn the power switch ON Reestablish communications with TOC Talk software MAINTENANCE AND TROUBLESHOOTING 7 2 10 Kloehn 3 way Valve Tool s Needed Phillips screwdriver Slotted screwdriver Turn off power at the back of the instrument Remove plug from back of the instrument Remove both left and right side covers Locate the Kloehn valve to be replaced on the plumbing side of the instrument On the electrical side of the instrument remove the power cable for the Kloehn valve from the PCB board On the electrical side of the instrument remove the two 2 screws holding the Kloehn valve to the instrument Noting their position remove the Teflon lines from the Kloehn valve Reattach Teflon lines to the re placement Kloehn valve Do not overtighten Reattach Kloehn valve to instru ment using the screws from step 5 Reattach the power cable for the Kloehn valve to its proper position on the PCB board Reinstall both left and right covers to the instrument Plug the AC power line back into the back of the instrument and turn the power switch ON Reestablish communications with TOC Talk software MAINTENANCE AND TROUBLESHOOTING 7 2 11 PCB Board Tool s Needed Phillips screwdriver Slotted screwdriver Turn off power at the back of the instrument Remove plug from back of the instrument Remove le
71. ent 5 3 5 6 Connections 2 7 2 10 Corrosives Scrubber 1 3 1 11 7 3 7 24 7 25 7 26 CPU Board 9 8 Current Positions mm 3 8 Curve 4 13 D Data Archive 3 10 files 3 10 Handling 1 5 Detailed Report 5 5 5 8 Detection and Results 1 4 Detector 1 4 7 25 Output 4 4 signal 5 3 DI Water 2 4 2 10 2 22 4 16 5 5 7 3 7 9 7 12 Diagnostics 3 6 3 8 3 9 7 6 distilled water see DI Water drain tubing 2 17 Drinking Surface water 1 5 Electrical 1 7 Connections 2 11 outlet 2 4 EPA 415 1 and 9060A 1 5 F flammable gas 2 10 flow diagram 7 22 Flow meter 3 9 7 15 path 7 22 7 25 rate 7 3 rate monitoring 1 5 restrictors 1 13 7 24 7 26 Frequency 1 6 Furnace 2 18 2 20 3 4 3 9 4 3 7 17 carrier gas 7 24 flow 7 26 Gas To either Vent NDIR 3 6 Gas to vent 7 23 Injection Port 1 3 7 8 Power 3 6 Fuses 1 6 2 12 G Gas 2 3 and water connections 2 7 flow 5 3 7 4 Flow Rate cc min 3 4 generator 2 4 In 2 10 Input 3 6 Output 3 6 permeation tube 1 12 Pressure 1 6 Supply 1 6 to IC Sparger 7 23 gas liquid separator 1 11 H halogen 1 11 removal 1 3 humidity 2 3 Hydrochloric Acid 6 4 hydrogen 2 10 IC 1 3 1 4 1 10 1 15 1 19 by Acidification and Sparge 1 4 calibration 2 5 flow 7 24 Gas 7 23 To either NDIR Vent 3 6 sparge methods 1 5 IC Sparger 1 10 1 13 3 4 3 6 7 3 7 10 7 23 7 24 7 25 7 26 Carrier Gas 7 25 7 26 output 3 6 infrared energy 1 12 Initialize 7 9 7 10 7 12 in
72. exit menu Set temperature set point to 680 by holding the SET key and pressing the Up or Down keys appropriately Release both keys MAINTENANCE AND TROUBLESHOOTING 7 2 17 Instructions for Installation of Apollo 9000 Particulate Options Parts Required For 0 5mm particulates Sample transfer line Injection line 5 filter needle attach transfer line to port D of the 8 port valve do not over tighten use the Kloehn tightening device Make sure the white Teflon washer in still in the port when installing this line Installing Injection Line Running From 8 port Valve Port C to Injection Port Over Combustion Furnace Note The sample transfer line is the regular Apollo 9000 blue transfer line For 0 8mm particulates Sample transfer line Injection line 5 filter needle Tools Required Medium size Phillips screwdriver Medium size flat blade screwdriver Installing Sample Transfer Line 1 When disconnecting or connect ing fittings of the 8 port valve it may be easier to first remove the valve syringe from the pumper by removing the two 2 thumb screws on the valve and the 4 bottom screw holding the syringe plunger This screw is easier to remove and replace if the syringe if first moved to 100mL or 500 mL via Diagnostics Syringe For 0 5mm particulates Use the standard Apollo 9000 sample transfer line For 0 8mm particu 5 lates Remove the standard A
73. ft hand or electrical side cover by removing seven 7 screws holding it to the chassis Locate PCB board It is 5 5 x 8 5 board on the middle wall to the rear of the instrument Noting their location remove all connections to the PCB board Remove board by removing the four 4 mounting screws found at its corners Replace with new PCB board using screws from previous step Reconnect electrical cables to the PCB board Reinstall left hand cover Plug the AC power line back into the back of the instrument and turn the power switch ON Reestablish communications with TOC Talk software 7 2 12 Power Supply Tool s Needed Phillips screwdriver Slotted screwdriver Turn off power at the back of the instrument Remove plug from back of the instrument Remove left hand or electrical side cover by removing seven 7 screws holding it to the chassis Locate power supply It is the 4 3 x 7 0 board on the middle wall to the front of the instrument Noting their location remove all connections to the power supply Remove board by removing the four 4 mounting screws found at its corners Install new power supply using screws from step 5 Reconnect electrical cables to the power supply Reinstall left hand cover Plug the AC power line back into the back of the instrument and turn the power switch ON Reestablish communications with TOC Talk software 7 2 13 Flow Meter
74. he TOC Talk Wakeup utility Note The unit wakeup feature is active when the following conditions are met 1 Wakeup schedule is set 2 Apollo 9000 is in Standby mode 3 TOC Talk is running Wakeup Schedule x Monday Tuesday Help Wednesday Cancel Thursday Friday Run Time hh mm Saturday 07 oo Sunday 24 Hour Clock Figure 3 6 1 Wakeup Schedule Screen 1 Onthe Setup menu select Wakeup Check all the days of the week you want the Apollo 9000 Wakeup Schedule to run Enter the time of day you want Apollo 9000 to wake up gt When satisfied with the schedule click OK A small blue clock icon will appear in the TOC Talk title bar when the Wakeup feature is activated and Apollo 9000 is in Standby mode TOC Talk Apollo 9000 Setup Run Results Help Figure 3 6 2 Wakeup Schedule Enabled Icon Please reference the TOC Talk Online Help for current comprehensive sample analysis calibration data results tutorials and ad vanced operation informa tion CALIBRATION 4 1 System Calibration Before analyses Apollo 9000 must be calibrated A response factor correlates the raw counts of the instrument to a known amount of carbon in a sample or whatis referred to as a standard Stan dards are made by adding carbon to ultra pure water to achieve determined levels of carbon It is important to use the same source of water for all calibra
75. he combus tion furnace Measure the 1 8 green line entering the end of the permeation dryer nearest the front of the instrument If the number is within 5 cc min of the water trap then replace the permeation dryer reconnect removed lines and return to step 3 Otherwise go to step 14 The leak is either at Valve 4 or in the lines connected to Valve 4 Inspect the lines for leaks and replace Valve 4 a 3 way Kloehn valve if necessary When leak is corrected reconnect all lines and return to step 3 15 Open the right side cover and locate the NDIR at the lower back of the instrument Measure the flow of the sample inlet line going into the detector If flow is within 5 cc min of the water trap then go to step 18 Otherwise go to step 17 16 The leak is either in the NDIR itself the connections to the NDIR or the sample outlet line Inspect these parts to find the leak If the leak is corrected reconnect all lines and return to step 3 Otherwise call Teledyen Tekmar technical support for further assistance 17 The leak is in the corrosives scrubber or the line from the scrubber to the NDIR Locate and correct the leak reconnect all lines and return to step 3 IC Sparger Carrier Gas Path 1 Make sure IC sparger carrier gas is on and directed through the NDIR Note Make sure that flow to the furnace is turned off These steps can be done by actuat ing the appropriate valves in the Valve Diagnostics screen 2 M
76. he nut Do not turn on the gas supply at this time Go to the next section to continue making connections before operating Apollo 9000 WARNING To avoid injury to yourself or damage to Apollo 9000 Do not exceed recommended pressure settings Observe safety regulations when handling pressurized gas For more information see Matheson Gases Data Sheets for information on specific chemicals To prevent explosion and fire Never use hydrogen or other flammable gas with Apollo 9000 Follow the manufacturers directions for safe handling of gas and chemicals Also refer to Material Safety Data Sheets for information on specific chemicals Connect Drain Line d Place a waste container of your choice not supplied to the right of theunit Route the natural colored 1 8 Teflon tube that exits the back of the unit into the waste container 5 5 5 2 5 Electrical Connections Connect the Interface Cables RS 232 straight through 9 pin cable connectors allow you to link Apollo 9000 The power requirements for Apollo to the computer and its accessories see 9000 are as follows 120 VAC 10 Figure 2 5 1 60 Hz 1200 VA 15 amp electrical outlet Itis best to use a power line dedicated 1 Locate the RS 232 cable to instrument use only Surge protection 2 Attach the male end of the cable to is highly recommended the appropriate port on the rear panel of Apollo 9000 Tighten the retai
77. he o ring should be felt When properly seated about 1 1 2 inches of tube should extend above the plate MAINTENANCE AND TROUBLESHOOTING The injection port seals to the combustion tube with an o ring Examine the o ring for any debris If necessary wipe it gently a If it is deemed necessary to remove the o ring do not attempt to pick it out with a sharp instrument Instead remove the 4 screws and spacer block that hold the metal plate to the injection port It will now be easily removed b Anew o ring must be lubri cated with a small amount of silicone vacuum grease With a tiny amount of lubri cant on the fingertips rub it on the o ring d Usealab wipe and try to wipe all the lubricant away Enough will be left to make it easy to slide the injection port onto the combustion tube e Making sure combustion tube o ring is in place attach mounting plate and spacer block to the new injection port by reattaching the four 4 screws in step 2a Slide the injection port onto the combustion tube with gentle pressure and a slight turning movement Replace the screws Reconnect the gas line above the right screw MAINTENANCE AND TROUBLESHOOTING 7 2 16 Temperature Controller Setup Set the temperature set point at or below room temperature Press and hold SET to read the set point Press Up or Down appropriately Begin software adjustments Press and hold the Up and Down keys simultaneo
78. hed into the removable boat which is readily accessible through the hatch covered port The boat is manually advanced into the furnace where the sample is combusted at 800 C Total Carbon TC is measured by direct injection of sample without pretreat ment Total Organic Carbon TOC is measured by sparging off the Inorganic Carbon IC from the acidified sample before injection using the sparging station built into the instrument IC is measured by injecting the water sample into a special vessel containing acidified water the CO produced is swept to the detector and measured 1 5 Apollo 9000 Operating Modes Apollo 9000 has four operating modes Total Organic Carbon TOC Total Carbon TC Inorganic Carbon IC and Total Carbon Minus Inorganic Carbon TC IC 1 5 1 Total Carbon TC TC is the measurement of all the carbon in the sample both organic and inor ganic as a single parameter 1 5 2 Inorganic Carbon IC Inorganic carbon consists of carbonates and bicarbonates in samples IC is analyzed in liquid samples by acidifying with an inorganic acid to pH 3 or lower and sparging with an inert gas 1 5 3 Total Organic Carbon TOC TOC analysis consists of addition of acid and sparging with an inert gas to remove IC The remaining carbon is called TOC if purgeables are less than 196 of the organic carbon 1 5 4 TC IC also called by difference requires a separate analysis for TC the
79. hlight it Click Exit You will return to the Autosampler Analysis Setup screen TOC Talk automatically inserts the calibration information in the Sample ID and Method ID fields Select the Number of Reps Per Sample in the Reps column 8 10 Press the arrow down or Insert key on your keyboard or select Insert Row from the File menu to insert another row Repeat steps 4 8 to enter the two remaining Sample IDs 5 PPM and 10 PPM Click Save Use to return to the Run screens Recalling this autosampler analysis setup will allow immediate recalibration without going through all the steps again as long as the calibration standards table is not deleted 4 15 CALIBRATION CALIBRATION 4 Start Standard Calibration Analysis Run Before you begin the analysis run make sure to do the following Place vials containing standards in their correct positions on the autosampler rack Note When sparging in the vials leave about one inch of headspace Verify that the acid supply is ample and place the acid vial in position 11 onthe autosampler support bar if you selected the Autosampler Sparge Option in Instrument Setup Status Verify that the DI Water line runs from Port G of the 8 port valve toa fresh DI Water supply 1 Click Start in the Sample Analysis screen to begin the standard analysis run 5 Review Analysis Results The result of each standard analysis rep appears in the Analy
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81. ies To configure Apollo 9000 with TOC Talk 1 Start Windows and then click the Start button Select TOC Talk from the Apollo 9000 Programs directory 2 Select Instrument from the Setup menu 3 Type a the Instrument Name box for instrument identification 4 name i e your name name of group in the Operator Name box for analysis identifcation In System select Ready mode Select relevant Options In Preferences select the Sample Introduction mode With Without Autosampler or Repetitive Sampling Note TeledyneTekmarrecommends that you use the Instrument Setup Status defaults for the remaining options until you become more comfortable with Apollo 9000 operation 8 Click OK 2 21 5 5 5 2 9 Condition Combustion Tube Catalyst Before initial Apollo 9000 operation and each time you install new catalyst you must condition the catalyst To condition the combustion tube catalyst 1 Disconnect the tube at the side port of the Water Trap a Attachalength of tubing to that tube so that the end can be submerged in a beaker of diluted sodium hydroxide solution Some noxious gases may be emitted by the catalyst upon conditioning and the water will absorb them Setthe carrier gas pressure to 30 psig 2 Elevate the temperature of the furnace to 900 C by pressing the Set button on the Temperature Control ler while pressing the Up arrow button W
82. ight or left Maintain a continuous downward slope for proper draining of the tubing Attach the support bar to the top mounting holes on the front of the autosampler using the knurled screws Install the Sample Tray The sample tray positions the racks and any accessories that fit onto the bed of the autosampler It also contains liquid spills such as those caused by overflow ing vessels Tray Mounting Brackets Position Figure 2 6 9 Sample Tray To install the tray 1 Place the tray in the lower position onthe bed of the autosampler 2 Ensure that the tray fits securely and that the drain outlet is located at the left rear of the tray 3 Attach one end of the drain tubing to the drain outlet and place the other in a drain receptacle located lower than the tray part of the drain tubing on the rinse station may be used To remove the tray 1 Lift the tray straight up and then pull it back toward you SYSTEM SETUP Install the Rack To install the autosampler rack 1 Place each rack into the tray so that the rack is perpendicular to the front panel of the autosampler Ensure that the rack handles are positioned to front of the unit Place the autosampler to the left side of Apollo 9000 Connect the Power Supply To connect the power supply 1 Locate the appropriate power cord for your line voltage Use the power cord to connect the sample changer to an AC power source Surg
83. ions when necessary COM Port Selection Select the correct Communication port from the computer to the Apollo 9000 here from list TOC Talk automatically configures the COM port a free COM port is required e OK Button Select OK to accept the port selection and re initialize the Apollo 9000 WARNING Selecting the OK button may compromise the data of the current run Cancel Button Select Cancel to exit the communi cations screen without re assign ing the port and without re initializing the Apollo 9000 TOC TALK Flowmeter Calibration Diagnostics On the Setup menu point to Diagnos tics and then click Flowmeter Calibra tion Flowmeter Calibration All values are in Calculate Calibration To Furnace Detector mmm Actual Calibrate 3 3 5 Flowmeter Calibration Diagnostic Screen The flow to the furnace can be mea sured with an independent flowmeter from the 1 8 blue gas line entering the side of the injection port over the combustion furnace the right side cover must be removed to do this Once the actual flow for the flowmeter is known type its value in units of cc min into the Actual field When the flowmeter reading is stable click the Calibrate button The ratio of Actual flow to raw flow will be displayed in the Cal Factor field 3 9 TALK 3 4 Archive Data Manual Archive You may prefer to have mo
84. ipment such as boilers turbines and purification devices Furthermore TOC levels in solids such as soils clays and sediments are of increasing interest TOC analyzers can measure total carbon TC total organic carbon TOC inorganic carbon IC purgeable organic carbon POC and nonpurgeable organic carbon NPOC If the POC is lt 1 of the TOC then NPOC is equivalent to TOC TOC measurement involves 1 Oxidizing organic carbon in a sample 2 Detecting and quantifying the oxidized product 3 Presenting the result in units of mass of carbon per volume of sample liquids or per mass of solid solids 1 3 INTRODUCTION Detection and Results Carbon in the sample is first converted to CO by the combustion furnace for TOC and TC analysis or by the IC sparger for IC analysis carrier gas then sweeps the derived CO through a nondispersive infrared NDIR detector Sensitive to the absorbtion frequency of CO the NDIR generates a non linear signal that is proportional to the instantaneous concentration of CO in the carrier gas That signal is then linearized and integrated over the sample analysis time The resulting area is then compared to stored calibration data and a sample concentration in parts per million ppm is calculated User Interface TOC Talk the Apollo 9000 software effortlessly monitors and performs calculations in a Windows 95 98 NT platform The following are some of th
85. ite line entering the water trap and using the valve diagnostics screen turn on the flow to the combustion furnace If the flow exiting the white line is within the 180 to 220 cc min range then turn off flow to the furnace and go to step 9 Otherwise turn off the furnace gas and go to step 10 Good furnace flow implies a leak specific to the IC sparger carrier gas line Open the right side cover and inspect the Clippard Valve 3 the flow restrictor and connecting lines for leaks If a leak is found reconnect lines and return to step 3 Otherwise call Tekmar Dohrmann technical support for further assistance 10 Bad furnace flow implies a leak that will affect all carrier gas lines Open the right side cover and look for leaks on the white plastic tees or other fittings and connecting lines that regulate flow to all Clippard valves and NDIR purge gas from the pressure regulator If leak is corrected reconnect lines and return to step 3 Otherwise call Teledyne Tekmar technical support for further assistance Leak Checking After the Mist Trap 11 12 Reconnect the line to the mist trap and measure the flow from the 1 8 green line entering the copper side of the corrosives scrubber If this number is within 5 cc min of the mist trap go to step 14 Other wise go to step 12 Open the right side cover and locate the permeation dryer The permeation dryer is the 1 4 tube with a white plastic tee at either end
86. ive Now 3 10 archive utility 3 5 area counts 4 9 4 16 Arm Locking Screw 2 13 ASM see Autosampler ASTM D2579 1 5 Auto Shutdown 3 5 Shutdown With Furnace Off 3 5 Auto dilution method 1 5 Auto rinsing 1 5 INDEX Automatic Archive 3 5 3 10 blank subtraction 1 5 shutdown standby 1 5 syringe injection 1 5 Wake up 1 5 Autosampler 1 5 2 12 Analysis Setup 5 7 Diagnostics 3 8 Needle 7 5 rack 2 17 sparge line 1 13 Sparge Option 3 4 4 16 5 6 5 7 vial position 4 14 Auxiliary 3 6 baseline 3 4 Baud Rate 2 13 blank 4 3 methods 4 3 values 1 5 3 9 calculated value 4 5 4 12 calculation of PPM 4 9 Calibration 1 5 3 5 3 9 4 3 4 4 4 10 blank 4 4 Curve 4 3 4 9 4 10 4 13 4 16 5 4 data 1 4 errors 3 5 factor 4 4 points 4 4 4 10 Setup 4 5 4 12 4 13 Slope 4 4 standards 4 3 verification 4 3 Carbon 1 4 content 4 3 dioxide 1 12 INDEX Carrier gas 1 4 1 11 7 22 7 25 fitting 7 6 lines 7 26 tubing 2 4 Catalyst 2 18 2 22 7 16 catalyst 1 10 2 19 7 17 Choose Range 4 8 4 14 Cleaning Validation 1 5 CO 1 3 1 4 1 10 1 12 Com 1 2 11 Com 2 2 11 Combustion Furnace 1 3 1 4 1 10 1 13 2 20 3 4 3 5 3 6 3 9 7 4 7 6 7 16 7 24 Tube 2 17 20 2 22 3 4 3 6 7 6 7 16 7 17 Communications 3 9 7 12 7 13 Diagnostics 3 9 port 3 9 compressed air 2 4 Concentration ppm C 4 5 4 12 4 13 condensor coil 1 11 Condition Catalyst 2 22 Configure Instrum
87. jection port 2 20 7 6 7 16 7 17 7 24 Injection Volume 1 4 Inorganic Carbon 1 3 1 10 1 15 1 19 High Fraction of 6 8 Instrument Diagnostics 3 6 Name 2 21 3 3 Setup 3 3 Setup Status 2 21 3 3 5 3 5 6 integrated peak 4 9 4 16 Intercept 4 4 Interface Cable 2 13 ISO 8245 1 5 K KHP KC8H504 2 5 INDEX L Leak Checking 7 22 after the Mist Trap 7 26 after the Water Trap 7 24 before the Water Trap 7 24 IC Sparger 7 23 LED display 1 13 linear equation 4 3 fit 4 3 Liquid Handling 1 5 low level Carbon 6 4 methods 4 3 M Maintenance 7 3 Checks 7 3 worksheets 7 3 Manual Archive 3 10 Movement 3 8 Syringe 1 5 Mass ugC 4 4 Max Integration Time min 3 4 measured carbon 4 3 Measurements 1 4 Memory 2 5 Method 1 5 5 4 ID 2 22 4 5 4 6 4 8 4 12 4 13 5 4 5 7 7 9 Parameters 6 9 Setup 1 5 Mist Trap 1 11 7 25 7 26 7 27 Mode 5 4 Status 3 3 Moisture Control System 1 11 removal 1 3 Move To Vial 3 8 Multi point 1 5 INDEX N NDIR 1 4 1 12 1 13 2 3 2 11 3 4 4 7 4 14 7 22 7 23 7 25 7 27 Detector 1 3 2 11 flow 7 23 mV output 3 3 purge gas 7 26 Near line monitoring 1 5 Needle 7 5 holder 2 15 Nitric Acid 6 4 non linear signal 1 4 Nondispersive Infrared see NDIR nonpurgeable organic carbon 1 3 NPOC 1 3 Operating Modes 1 15 Operator Name 2 21 3 3 Options 2 21 3 4 organic carbon levels 1 3 halide levels 1 3 Out of Calibration 3 5 Outlier 3 4 deletion 1 5 3 4 O
88. kit You may wish to remove the 8 port valve from the syringe pump to provide easier access to the ports When the valve is replaced be sure to engage the hole behind port A onto the pin extending from the syringe drive body before replac ing the two valve screws Failure to do this may result in breakage of the syringe or damage to the syringe drive 7 After the valve is reattached use Diagnostics Syringe to turn the valve to waste and then home the syringe 8 Reinstall the right cover to the instrument Installing the Autosampler ASM Filter Needle 1 Attach the sample transfer line to the vertical port at the top of the needle 2 Attach the red ASM sparge transfer line to the horizontal side port of the needle 3 Immerse the needle in a bottle of DI water 4 Using the Diagnostic screen in the Instrument setup select Valves and turn the ASM Sparge gas on Bubbling should occur from the MAINTENANCE AND TROUBLESHOOTING second stage of the needle the one with 16 small holes 5 Using the syringe diagnostic screen in the Setup pull down menu draw 2 5 mL of DI water from the sample port port D to check for a tight seal with the sample line Discard the water to waste port F Do this twice as the first time there will be some headspace in the syringe due to the dead volume of the sample transfer line and ASM needle Attaching ASM Needle to ASM ASM users only When installing adjust the positi
89. l arm s base and push the vertical arm to the back of the horizontal arm While slightly moving the needle holder bracket up and down push the control rod until it clicks into position Re insert the white plastic plug Re attach the cover plate to the front of the horizontal arm Install the Sample Needle Locate the accessory packages contain ing the needle and the needle holder guide kit Needle Holder Needle Bracket and Screw Holder zr Tubing Fitting Needle Retaining lt Needle Screw Needle Guide Figure 2 6 6 Sample Needle To install the needle guide 1 Placethe metal lock washer onto the needle guide 2 Screwthe needle guide with lock washer into place on the bottom side of the needle foot SYSTEM SETUP install the needle holder 1 Slide the needle holder into place onthe needle holder bracket and secure with the supplied screw Needle Holder Bracket Sample and Screw Needle Tubing Fitting Figure 2 6 7 Needle Holder To install the needle 1 Connect the transfer tubing to the tubing fitting Slide the needle assembly into the needle holder on the vertical arm making sure that the needle is centered over the needle guide Secure the needle by tightening the needle retaining screw Connect the 1 16 tubing attached to port D of the 8 port valve to the vertical fitting of the needle Connect the long red 1
90. lect this option to send a printout of the last sample set to your default printer Auto Shutdown Check the Auto Shutdown option box to allow the instrument to automatically run a shutdown event list and go into Standby Mode after an autosampler run This enables the automatic archive utility when ON is selected in the archive dialogue Check the Auto Shutdown With Furnace Off option box if you want the shutdown event list to include turning the combustion furnace off during unit shutdown This option is only available when Auto Shutdown is also selected TOC TALK Halt System If Out of Calibration or Over Range You can select one or both options if you want your analysis sequence halted when TOC Talk detects calibra tion or range errors Check the Out of Calibration option box if you want the sched uled analysis sequence to halt when TOC Talk detects that Apollo 9000 has slipped out of the desired calibration Check the Over Range option box if you want the scheduled analysis sequence to halt when TOC Talk detects that Apollo 9000 has detected a sample that has gone out of its analysis range TALK 3 3 Instrument Diagnostics Valves On the Setup menu point to Diagnos tics and then click Valves Gas Input Gas Output Furnace Gas NDIR COn IC Gas CNDIR Vent Sparger COn ASM Sparge con
91. ler Vertical Arm To install the vertical arm 1 Remove the cover plate from the front of the horizontal arm by removing its three screws 2 Locate the hexagonal shaped control rod and horizontal slider by looking down into the horizontal arm 3 Using your finger press on the control rod where it passes through the horizontal slider At the same time pull the needle foot toward the front of the horizontal arm This causes the white plastic plug and 2 14 4 10 11 control rod to move forward slightly When the white plastic plug is no longer flush with the front of the horizontal arm remove it and the control rod from the horizontal arm Pull the needle foot toward the front of the horizontal arm as far as it will go Position the vertical arm onto the horizontal slider When viewed from the front of the autosampler the vertical arm s needle holder bracket is on the right Use the supplied screws to secure the vertical arm to the horizontal slider The screws insert into the bottom ofthe mounting holes in the horizontal slider You may need to move the vertical arm back and forth slightly to align its mounting holes with those in the horizontal slider Re insert the control rod as far as it will go While inserting the control rod you may need to rotate it back and forth slightly to get it to pass through the gearing and motor drive socket in the horizontal slider Apply pressure at the vertica
92. librationWith 1 Define Standard Calibration Autosampler Tutorial Methods and Concentrations Note Precisely follow the steps StartTOCTalk below to achieve successful 2 OntheTOCTalk Control Screen calibration of your Apollo 9000 menu point to Setup click Calibra instrument tion and then select Standards In this exercise you will create a standard calibration for low level TOC sample analysis by setting up three calibration points Curve ID You will 1 Define the Standard Calibration L Methods and Concentrations x we 2 Set the Active Calibration Curve Figure 4 3 1 TOC Calibration Setup Setup the Standard Calibration Analysis 4 Start the Standard Calibration 3 On the File menu click New Analysis Run 4 4 Highlight the first row Line 1 to 5 Review the Analysis Results select it 5 DI Water in the Standard ID box 6 Enter zero 0 inthe Concentration ppm C box 7 Inthe Method ID list select TOC 0 20 ppmC The calculated value in the ugC column should read 0 0000 8 Pressthearrow down key on your keyboard to insert a new row Line 2 9 5 the Standard ID box 10 Enter 5 in the Concentration ppm C box CALIBRATION 11 Inthe Method ID list select TOC 0 20 ppmC The calculated value in the ugC column should read 2 5000 12 Pressthe arrow down key on your keyboard to insert a new row Line 3 13
93. lts Made Easy With Autosampler 1 Configure Instrument 1 Select Instrument from the Setup menu to open the Instrument Setup Status dialog Operator Name USERT Help Preferences 3 Sample with Autosampler G Ready mm Sample ion Mih Autosamp Standby Max Integration Time 40 Stabilize Baseline Time 15 Gas Flow Rates To Furnace Outlier Deletions E Print data report after each sample set Auto Shutdown furnoce off Halt System If Out of Calibration Over Range 7 Iv Autosampier Sparge Option Figure 5 3 1 Instrument Setup Status 2 Select Ready to wake up the instrument 3 The gas flow will turn on and the detector signal will begin to stabilize Look for the flow rate display in the To Furnace field 4 Select the following parameters a Select With Autosampler from the Sample Introduction List b Select Autosampler Sparge Option Check Print Data Report after Each Sample Set optional d If you wish you may type in your name and give your instrument a name All other choices should remain un checked 5 Click OK 5 6 42 Sample Setup 1 From the menu bar of the Control screen click Run Jl TOC Talk 9000 Setup Run Results Help Click Run to Open Run Screens Figure 5 3 2 Access to Run
94. lyze calibration Note TOC Talk references the Active Calibration Curves which are files that store the information associated with a specific Calibration Curve ID or Method ID during sample runs If you want to analyze a standard you must first create a Calibration Setup table and then set the Active Calibrations Curves Once you save the standard concentrations Calibration Curve IDs and set as Active TOC Talk will automatically refer to the current standard calibration configuration when Standard is selected as the Sample Type for analysis 4 13 CALIBRATION 3 Setup Standard Calibration 1 FromtheTOC Talk Control Screen Analysis click Run Note Proceed carefully Most Apollo 9000 TOC Talk standard calibra tion errors occur during the following steps If standard analysis setup instructions are not followed unsuccessful calibrations and reduced sample integrity can occur Sample Sample Strip Setup Analysis Chart Window Sample Analysis displays the current Sample ID information only after a run is started Start Run button Sample Setup button Strip Chart displays in real time response from the NDIR as Time vs Millivolts and refreshes atthe beginning of each sample run Analysis Results continuously displays current analysis data up to 30 rows so that you can easily monitor Apollo 9000 performance 2 ClickSample Setup in the Sa
95. me The linear equation for samples is simply b ew For 0 20 1 400 ppm TOC and TC methods the carbon contribution from the preparation water that is presentin standards but not samples may be significant The blank method in this range uses rinse water from the rinse water bottle continuously recycles it through the furnace for a period of time and then measures the water derived as the sample blank To run check stan dard against the calibration curve you mustthen run the standard as a calibra tion verification instead of a sample This calibration verification sample type will apply the correct blank the y intercept or b totheanalysis cal CALIBRATION 4 Calibration Points 25 50 75 and 100 ppm Water Contribution gt 5 gt fo 5 5 x gt gt Reagent Contribution Mass ugC Slope calibration factor Intercept calibration blank Figure 4 1 Calibration Slope 4 4 4 2 Standard Calibration Without Autosampler Tutorial IMPORTANT Precisely follow the steps below to achieve successful calibration of your Apollo 9000 instrument In this exercise you will create a stan dard calibration for low level TOC sample analysis by setting up three calibration points You will 1 Define the Standard Calibration Methods and Concentrations Set the Active Calibration Curve Setup the Standard Calibration Analysis Start the Sta
96. mple Analysis screen 4 3 Enter the autosampler vial position ete te in the Pos column see Figure 0 12 48 60 4 3 5 Sample 10 Mea 5 Message 4 Fromthe Sample Type list select TOC Standard _ BundyMode _ 040 1559 0375 Start Run Analysis Note You must physically select a Button Results Window Sample Type from the list Figure 4 3 4 TOC Talk Run Screens although the one you want may already be displayed for each line you set up 5 TheChooseRange dialog appears Select the 0 20 1 400 range Click OK 4 14 AutoSampler Analysis Setup Click TEE Save Enter Rack Style 40 EZ Use Exit Sample Vial 1 Di water Position 1 ppt 513 incon i Select Sample Select EMEND 5 Number d _ Choose CON 0 20 1 400 Range p Click OK C10 750 1 100 4 000 Cal Curve ID 1 000 25 000 CALIBRATION Select Standard 5 0000 10 0000 ppm TOC 0 20 ppmC TOC 0 20 ppmC 4 Calibration Line Click Exit Cancel Figure 4 3 5 Standard Calibration Analysis Setup with Autosampler Next the Select Calibrator dialog appears Select the Standard ID DI Water you want to use by clicking row to hig
97. n IC If present purgeable organic carbon POC will be included in the TC mea surement INTRODUCTION 1 6 Sample Introduction Before introducing a sample Apollo 9000 automatically rinses the syringe to eliminate any contaminants that may interfere with the testing process This rinsing occurs through a loop sequence where the syringe is filled and dis carded with DI water Because air bubbles in the syringe can affect test results Apollo 9000 auto matically discards sample from the top and bottom portion of the sample regardless of your sample size 200 ul to Waste Deliver 1 ml Sample 50 ul to Waste Figure 1 5 1 Syringe Drive Sample Delivery INTRODUCTION 1 7 Prime Replicate All methods use a priming replicate before sample analysis It is typically half the standard injection volume and it will not be quantified The amount of sample used for the priming replicate is a method parameter The peak can be seen on the NDIR strip chart in the Run Screen of TOC Talk software 1 8 Analysis Process Please refer to the flow diagrams in section 8 for the following mode descriptions 1 8 1 Total Organic Carbon IC Removal in IC Sparger Note There are rinsing steps for the syringe and IC sparger and other details that are not described here 1 Sample acid are delivered to the IC sparger 2 Sample is sparged and IC is vented POC if present also vents 3 Analiquot of the sparg
98. n Tube 3 Thecatalyst 20 grams is in a small vial Pourthe entire 20 grams into the combustion tube 5 5 5 Install the Combustion Tube 1 Remove the right chassis cover from the Apollo 9000 Detach the injection port from the valve mounting plate by removing the two screws and set aside Remove the blue tube on the right side for easier access to that screw Swing the locking guard at the bottom of the combustion furnace to the right until it touches the right furnace leg Gently pull the bottom connector out from under the furnace Examine the bottom connector for any debris on the black o ring that seals to the combustion tube If necessary remove the connector at the stainless steel union and rinse it under clean running water Shake out the excess water and gently wipe the o ring with a lint free cloth Install the Combustion Tube by gently lowering it into the furnace until the bottom end protrudes from the furnace Hold the combustion tube in place until the bottom connector is resecured a Replace the bottom connector and secure it in place by swinging the locking guard to the left until it touches or nearly touches the left furnace leg 2 20 b Contact with the o ring will be felt Push down firmly while turning the tube slightly The movement of the tube through the o ring should be felt When properly seated about 1 1 2 inches of tube should extend above the plate
99. nd Reagents 1 Reagent Water The reagent water used must be of the highest quality deionized distilled or reverse osmosis water available and contain the least amount of carbon in water 2 Potassium Hydrogen Phthalate KHP ACS Acidimetric Standard 99 95 100 05 1 000 ppmC and 2 000 ppmC KHP certified standards are available from Teledyne Tekmar 3 Sodium Bicarbonate ACS Reagent Grade CALIBRATION STANDARD 8 2 Procedure for Making Standards 1 Preparation of Stock Standard Solution One L of 1000 ppmC KHP Stock Calibration Solutions crystals must be dry and stored in a dessicator Other wise dry by placing in the oven at 105 C for 2 hours prior to preparation of the stock solution e Accurately weigh 2125 mg of KHP Transfer the KHP to 1 01 volumetric flask which is a half full of reagent water e Swirl the flask to dissolve the Fill the flask to the 1 0 L mark with reagent water nvert the flask 5 times to equilibrate the solution For other standards use the equation below to determine the weight needed to prepare the stock standard solution Weight of standard mg stock standard concentration mgC L final volume L 96 C wheremgC L ppmC decimal fraction of carbon in the reference material ex KHP 0 4705 NaHCO 0 1428 8 3 CALIBRATION STANDARD 2 Preparation of Working Standard Solutions 500 mL of 10 ppmC KHP W
100. ndard Calibration Analysis Run Review the Analysis Results CALIBRATION 1 Define Standard Calibration Methods and Concentrations 1 StartTOCTalk 2 OntheTOCTalk Control Screen menu point to Setup click Calibra tion and then select Standards Curve 0 Figure 4 2 1 TOC Calibration Setup 3 On the File menu click New 4 Highlight the first row Line 1 to select it 5 DI Water in the Standard ID box 6 Enter zero 0 inthe Concentration ppm C box 7 Inthe Method ID list select 0 20 ppmC The calculated value in the ugC column should read 0 0000 8 Press the arrow down key on your keyboard to insert a new row Line 2 9 Type5PPMin the Standard ID box 10 Enter 5 the Concentration ppm C box 11 In the Method ID list select 0 20 ppmC The calculated value in the ugC column should read 2 5000 12 Pressthe arrow down key on your keyboard to insert a new row Line 3 13 Type 10 PPM in the Standard ID box 14 Enter 10 the Concentration ppm C box 15 In the Method ID list select TOC 0 20 ppmC The calculated value in the ugC column should read 5 0000 16 OntheFile menu click Save As Save this calibration setup as TOC Calibration 17 Click OK Note After you click OK in the Calibration Setup dialog you will return to the TOC Talk Control Screen but the Setup menu and Calibration submenu
101. nic carbon IC problems can arise from adding acid to the already acidified samples collected in the field In the case of pre acidified samples additional acid should not be used You must consider the possible effects of these acids on the system used to determine the TOC of the samples Sulfuric acid H SO in combustion TOC instruments will form SO gas It has been observed that the SO can be absorbed to some extent by the catalyst in the combustion tube After some amount has been absorbed the catalyst becomes saturated and then with each ensuing injection of water some of the SO is released and will cause a response in the NDIR detector It is also affects the corrosives scrubber used to protect the detector causing additional maintenance SPECIAL APPLICATIONS An additional scrubbing device can be used ahead of the corrosives scrubber that will remove the SO from the gas going to the detector without remov ing CO Teledyen Tekmar recommends installing the SO Mist Scrubber when running sample that contain sulfuric acid Please contact Teledyen Tekmar Customer Support for additional information or to order the SO Mist Scrubber 6 3 SPECIAL APPLICATIONS Hydrochloric Acid in combustion TOC instruments will form gas Since most commercial analyzers use a NDIR to detect CO and they have a gold lined sample cell the corrosive nature of HCl is a problem Some of the b
102. ning screws VAN WARNING Do not plug Apollo 9000 into 4 Attachtheotherend ofthe cable to anextension cord An a serial port Com 1 or Com 2 only extension cord may overheat onthe rear panel of the computer and cause a fire 5 Tightenthe retaining screws Please note that the NDIR detector requires approximately two hours to warm up before operating To Surge protected Power Source c RS 232 1 0 Cable a 9 pin 8 to Apollo 9000 Monitor Power Unit ID Fuse Mouse Switch Selector Drawer Keyboard Baud Rate Power Selector Switch Figure 2 5 1 Apollo 9000 System Electrical Connections 5 5 5 2 6 Autosampler Optional The following instructions are Apollo 9000 specific Please refer to the Gilson 223 Sample Changer User s Guide for further autosampler information Vertical Status Sample Needle Arm LED Support Horizontal Station Rack Tray Figure 2 6 1 Optional Apollo 9000 Autosampler Unit ID Selector Baud Rate RS 232 1 0 Port Selector to Apollo 9000 use Receptacle Switch Drawer Figure 2 6 2 Autosampler Rear Panel 2 12 Tools and Supplies Needed Before you begin assembling the autosampler gather the following tools and supplies Slotted screwdriver Phillips screwdriver e Accessory packages shipped with unit Install Fuses B
103. ntenance Checks The following components should be maintained on a monthly basis Daily and weekly checks plus Change corrosives scrubber nspect permeation dryer for damage water accumulation Copy and use the following Apollo 9000 Maintenance Worksheets as a checklist in your daily analysis plans APPENDIX A Apollo 9000 Maintenance Worksheet D Daily Month Year W Weekly M Monthly Notes Signature s APPENDIX A Apollo 9000 Maintenance Worksheet D Daily Month Year W Weekly M Monthly Notes Signature s APPENDIX A Apollo 9000 Maintenance Worksheet D Daily Month Year W Weekly M Monthly Notes Signature s APPENDIX A Apollo 9000 Maintenance Worksheet D Daily Month Year W Weekly M Monthly Notes Signature s APPENDIX A Apollo 9000 Maintenance Worksheet D Daily Month Year W Weekly M Monthly Notes Signature s APPENDIX A Apollo 9000 Maintenance Worksheet D Daily Month Year W Weekly M Monthly Notes Signature s APPENDIX A Apollo 9000 Maintenance Worksheet D Daily Month Year W Weekly M Monthly Notes Signature s APPENDIX A Apollo 9
104. ntroller The set point for the combustion furnace is controlled by a temperature controller found on the front face of the Apollo 9000 instrument just below the syringe driver The temperature con troller LED displays the actual tempera ture of the combustion furnace The blue button Set displays the set point for the combustion furnace when pressed By holding down the Set button and pressing the appropriate gray Up and Down buttons the set point for the combustion furnace can be adjusted as needed Figure 1 4 13 Temperature Controller INTRODUCTION Optional STS 8000 Autosampler The optional autosampler is an XYZ robot that automates sample handling procedures It allows the user to increase throughput and operate the analyzer unattended for many hours The autosampler tray holds 2 racks each rack can hold up to 77 25ml culture tubes or 35 40ml VOA vials Vials may be fitted with pierceable Teflon backed septum caps The autosampler rinses the inside and outside of the needle via a dedicated rinse station XYZ Arm Sample Needle Sample Vials Vial Racks Figure 1 4 14 Optional STS 8000 Autosampler Optional 183 Boat Sampler The 183 Boat Sampler is ideal for soils sediments sludges and particle laden liquids Syringeable samples are injected directly into the platinum sample boat through a septum minimizing contami nation of the combustion stream by ambient air Solid samples are weig
105. olutions away from direct sunlight use the phosphoric acid reagent within one month and change DI water daily 2 9 5 5 5 Connect Reagents Organic free deionized or distilled water 50 ppb C or lower is required for trace analysis is recommended for proper operation of Apollo 9000 Note For best results change water on a daily basis 1 Locatethe DI water bottle and place itto the left of the unit 2 Place the end ofthe 1 16 tube connected to Port G of the 8 port valve into the DI water supply 3 Insert this tubing to the bottom of the water container Be sure that the tube does not hit the bottom of the bottle and curl back up and out of the water 4 Insert the tube from Port A of the 8 port valve into Automatic Syringe Users a con tainer of phosphoric acid reagent Autosampler Users a40 ml VOA vial at Position 11 onthe autosampler support bar see Figure 2 5 7 CAUTION Acid will burn eyes and skin To prevent injury wear safety glasses and skin protection when using these chemicals Refer to Material Safety Data Sheets for detailed informa tion Connect Gas Supply 1 Turn the pressure on the two stage gas regulator to zero psi This prevents a sudden burst of pressure from damaging parts Locate the fitting labeled Gas In on the back of the unit Using a nut and ferrule connect your tubing from the gas supply tank to this fitting Do not overtighten t
106. on of the ASM needle to allow the stir bars in the vials to rotate unimpeded using the needle retaining screw This is typically 0 5 up from the normal needle position Make sure that bottom of the needle is within the blue needle guide but not protruding below the guide If the needle does not reach the blue needle guide you may need to attach the guide from the top of the needle foot instead of the bottom In some cases you may need to replace the blue needle guide with a 10 24 thread 1 8 nut Verifying Complete Assembly 1 Make sure that the particulate option is chosen in the Setup Instrument window 2 Checkthe configuration with 10 100 ppmC standards An RSD of 196 396 should be ob tained MAINTENANCE AND TROUBLESHOOTING 7 3 Troubleshooting Apollo 9000 Please review the Safety information in Chapters 1 and 2 before performing any troubleshooting procedures 7 3 1 Leak Checking Leak checking the Apollo 9000 is a simple process of checking the flows at various points in the flow path to identify potential leaks Please refer to the flow diagram when leak checking You will compare flows from different points on the flow path so it is impor tant that the flow meter used be the same to achieve accurate results For this reason using the flow meter provided on the Apollo 9000 in follow ing these steps is not recommended Tools required Flow meter electronic calibrated or bubble
107. ons that follow Sample Gas Inlet Waste Outlet Figure 2 4 1 Pneumatic Connections Rear 2 7 5 5 5 Swage Nuts and Ferrules onto Plastic Ferrules Tubing 1 Slide the nut onto the tubing To connect Apollo 9000 to gas supplies you must swage nuts and ferrules onto tubing then connect the tubing to Apollo 9000 This section instructs you how to complete this task correctly If the nuts and ferrules are the wrong sizes or are not properly swaged leaks can 3 Insert the tubing into the desig occur nated connector on Apollo 9000 2 Formostconnections allow 3mm 1 8 of tubing to extend past the end of the ferrule For 8 port valve fittings make sure tubing is flush with the end of the ferrule Tubing connections must be made with 4 Tighten the nut with your fingers either a one piece plastic ferrule or a being careful not to over tighten two piece metal ferrule CAUTION To prevent damaging the metal nuts and ferrules do nottighten them over 3 4 turn 270 Once swaged onto tubing you may need to tighten a nut only slightly to eliminate a leak If leaking persists look for other causes of the leak Swagelok Two piece Metal Ferrule esir To check if a nut and ferrule have been properly swaged loosen the nut and pull on the ferrule The ferrule should not slide Figure 2 4 2 Nuts Ferrules 2 8 Swagelok Ferrules 1 Slide
108. opposite directions Reattach permeation dryer to 1 black clasps Reinstall right cover to instrument 7 2 2 Copper Cu and Sn Corrosives Scrubber Tool s Needed Septum puller or pointed tweezer 1 Push open acrylic door and locate the corrosives scrubber on bottom right center of instrument face It is a U tube with Cu on one side and Sn on the other 2 Noting their position remove the green lines entering and leaving the corrosives scrubber 3 With septum puller or pointed tweezer remove gray septum from the Cu scrubber end 4 With septum puller or pointed tweezer remove Pyrex wool from Cu scrubber end 5 Empty old Cu from scrubber Use septum puller or pointed tweezer if necessary 6 Add new Cu to scrubber 7 Replace or add new Pyrex wool to Cu scrubber end 8 Reinsert gray septum 9 Perform steps 3 8 again for Sn scrubber end if necessary 10 Reattach green lines to corrosives scrubber 11 Reattach corrosives scrubber to front of instrument and close acrylic door MAINTENANCE AND TROUBLESHOOTING 7 2 3 Autosampler Needle Tool s Needed None 1 Home the autosampler by using the autosampler diagnostics screen in TOC Talk software 2 Locate the autosampler needle on autosampler 3 Loosen hand screw on upper needle holder and remove autosampler needle from autosampler 4 Noting their position unscrew both sparge gas and sample line fit
109. or your DI water run as a TOC sample If it is not Teledyne Tekmar recommends rerunning the sample blank or manually setting the sample blank To run a sample blank select the appropriate sample blank type under the sample setup screen Table 5 4 2 outlines the correct blank setups for the default TOC and TC methods Sample Method ID Blank Sample ID Blank Method ID TOC TC 0 20ppmC Blank TOC_TC Rng 1 Blank TOC_TC Rng 1 TOC TC 1 400ppmC Blank TOC_TC Rng 1 Blank TC 1 400ppmC TOC TC 10 750ppmC Blank TOC TC Rng 2 Blank TOC TC Rng 2 TOC TC 100 4000ppmC Blank TOC TC Rng 3 Blank TOC TC Rng 3 TOC TC 1000 25000ppmC Blank TOC TC Rng 3 Blank TOC TC Rng 3 When TC Blank Range 1 is chosen TC 0 20ppmC will automatically be set as the Method ID Make sure to change this to TOC TC 1 400 ppmC Table 5 4 2 TOC TC Sample Blanks 5 4 3 Run an IC Blank The blanking procedure for IC analysis will measure the background of the DI water and acid used in an IC measure ment to determine the sample blank value Make sure to set the number of replicates to at least 6 when running a sample blanking procedure The results for blank methods are in raw data counts and the last 3 replicates are averaged as the sample blank SAMPLE ANALYSIS Note The raw data value for the sample blank should be less than the raw data for your DI water run as an I
110. orking Standard Solutions Fill a 500mL volumetric flask 1 2 full with reagent water Transfer 5 mL of the 1 000 ppmc KHP stock solutions into the flask using a pipette Swirl the flask for 10 seconds to mix Fill the flask to the 500 mL mark with reagent water e nvert the flask 5 times to equilibrate the solution For other standards use the equation below to determine the volume of stock standard solution to use Transfer volume mL working standard concentration mgC L final volume of working standard mL stock standard concentration mgC L 3 Cap and store the stock and working calibration standards 2 C to 8 C refrigerator However they need to be brought to room temperature to use them 4 The typical shelf life for the work ing standard solutions containing less than 20 ppmC is less than 1 week while the higher concentra tion stock solutions have a shelf life of at least 1 month DIAGRAMS 6 16 4 Spo Apeay Ready Mode TOC TC Carrier Gas Ready Mode NDIR Purge and 5 VENT Permeation Dryer NC Lines Not Used During Ready Mode ACID NC p WATER MIST TRAP 3 TRAP IC SPARGER 4 PERMEATION NO COM DRYER DI 200 ml min AIR WATER INJECTION RESTRICTOR WASTE SAMPLE PORT DI WATER BOTTLE 1 1 R INLET HEADSPACE PURGE WATER TRAP SYRINGE CORROSIVES E
111. orm 5 more reps Theraw data count should finally be less than 30 000 counts for the standard Apollo and Less than 375 000 counts for the Apollo HS If the raw counts are greatly higher then proceed to section 2 10 2 10 Cleaning Procedure for Conditioned Catalyst Fresh catalyst background might be too high for most applications Before initial Apollo 9000 operation and each time the catalyst is replaced the catalyst conditioning procedure must be per formed To condition the combustion tube catalyst 1 Make sure DI water vessel contains minimum 1 liter supply 2 Setthe combustion furnace tem perature to 900 C Do not use this temperature with old catalyst unless it has been washed Press and hold the Set button onthe Temperature Controller and then press the Up arrow button until the display reads 900 C e Release both buttons and wait until the furnace reaches 900 C 3 Run the TOC Talk Cleaning Proce dure Method as a sample for 10 replicates overnight in repetitive sampling mode every 5 minutes the minimum time allowed 4 The next day exit the repetitive sampling procedure return the combustion furnace temperature to 680 C and run DI water as a TOC Sample SYSTEM SETUP For applications measuring 1 ppmC samples or less the raw data for this sample should be e Less than 30000 area counts for the standard Apollo 9000 Less than 375000 area counts for the Apollo 9000 H
112. output 2 function Press SET to display none If display does not read none press the Up or Down keys appropriately until the display does read none Release both keys Ot2 still appears on the screen Press the Down key to display disp display default Press SET to display Ac If display does not read Ac press the Up or Down keys appropriately until the display does read Ac Release both keys disp still appears on the screen Press the Down key to display FAIL failure mode Press SET to display bPLS If display does not read bPLS press the Up or down keys appropriately until the display does read bPLS Release both keys FAIL still appears on the screen Press the Down key to display SLOC set point lock Press SET to display no If display does not read no press the Up or Down keys appropriately until the display does read no Release both keys SLOC still appears on the screen Press the Down key to display tag lockout tag Press SET to display P Press the Up or Down keys appropriately until the display is blank Release both keys tag still appears on the screen The configuration menu is now set appropriately Press and hold the Up and Down keys simulta neously for three seconds to exit menu To begin editing PID settings enter software menu by holding the Up and Down keys simultaneously for three seconds Press the down key until
113. pair or replace the permeation dryer reconnect all lines and return to step 3 If this does not fix the leak call Teledyne Tekmar technical support for further assistance 7 25 MAINTENANCE AND TROUBLESHOOTING Leak Checking the Moisture Control System 1 Locate the corrosives scrubber Check all rubber seals to verify they are intact Remove the green tube entering the side of the scrubber with copper granules and measure the flow If you obtain a reading of less than 200 cc min check the rubber seal on the water trap outlet and the seal in the bottom of the water trap If you still obtain a reading of less than 200 cc min the problem may be a leak in the permeation tube connections f you obtain a reading of more than 200 cc min at the scrub ber inlet the problem is most likely a break inside the permeation tube which should be replaced Leak Checking Before the Mist Trap 6 You have a leak before the mist trap Measure the flow on the 1 8 red line entering the sparge tube at the top of the IC sparger If flow is between 180 and 220 cc min go to step 7 Otherwise go to step 8 Inspect the IC sparger tube IC sparger and line running between IC sparger and mist trap for leaks Replace defective parts if neces sary Reconnect all lines and return to step 3 Otherwise call Tekmar Dohrmann technical support for further assistance If your leak is before the IC sparger Remove the 1 8 wh
114. parger to dilute the sample 6 6 Example sample containing 1 salt and 20 ppmC can be automatically diluted by a factor of 10 So the method setup should be changed to Injection volume 0 1 mL Sparger volume 0 5 mL Dilution volume 4 5 mL A total amount of 5 mL for the sparger and dilution volume is recommended to make sure that there is enough liquid for efficient mixing and enough sample for the analysis If the sample foams a lot a higher dilution should be used 3 Clean the combustion tube and catalyst Refer to Section 7 3 3 and 7 3 4 for maintaining the catalyst and combustion tube To minimize downtime prepare a second combustion tube assembly 6 2 4 Samples with High Acid Content Samples containing 5096 or more acid present a challenge for a combustion instrument The introduction of large amount of acid results in decrease in efficiency of the combustion catalyst If it is necessary to run these types of samples the following measures must be taken 1 Decrease Injection volume De pending on the level of carbon in the sample it is best to use as little of the sample as possible to prolong the life of the catalyst 2 Do not add more acid to the sample Make a new method by following the instructions on Section 6 3 Under acid volume type 0 mL 3 Dilute the sample This can be done manually or automatically for and TC analyses See the discussion on Section 7 4 4 Attach a
115. parger to sparger to sparger to convert IC to remove IC remove IC co ASM N A N A Volume of Volume of acid Volume of Acid sample added to ASM sample Volume delivered to to remove IC delivered to furnace for furnace for priming priming Internal Internal Internal Internal Internal Pre Parameter Do Parameter Do Parameter Do Parameter Do Parameter Do sparge Not Change Not Change Not Change Not Change Not Change Ic N A N A Mixing time of Sparging time Sparging Sparge diluted sample sparger Mixing time in in the IC to remove IC IC sparger to sparger remove IC ASM N A N A N A Sparging time N A Sparge in ASM to remove IC Table 6 3 Method Parameter Definitions SPECIAL APPLICATIONS Notes MAINTENANCE AND TROUBLESHOOTING 7 1 Scheduled Maintenance Checks VAN CAUTION Please review the Safety information in Chapters 1 and 2 before performing any maintenance procedures WARNING Do not operate Apollo 9000 without the cover Operating Apollo 9000 without the cover properly attached may result in an electrical shock hazard To avoid electrical shock disconnect the power supply to Apollo 9000 and any accessories before servicing interior components Moving parts can grab and pinch Keep hands and cloth ing away from moving parts while power is on Use caution when performing any
116. pollo sample transfer line attached to the 8 port valve at port D and 7 20 1 Remove the right cover of the instrument Remove the furnace injection line from the top if the injection port Remove the 1 16 diameter furnace injection line from the 8 port valve at port C and remove the line from the instrument You may wish to remove the 8 port valve from the syringe pump to provide easier access to the ports Removal of the screw holding the plunger of the syringe is made easier by drawing the syringe down about 0 5 mL by using the Diagnostics Syringe turn the valve to the DI water position and move the syringe to 500 mL The screw has a very close fit tolerance It is important to not force the screw Locate the appropriate furnace injection line for your application The 0 8 mm I D and 0 5 mm 1 0 lines will have tubing protruding about 1 4 from one end That end attaches to the injection port The 0 1 mm I D line will have tubing and a needle protruding from it Run the furnace injection line to the front of the instrument You may wish to remove the nut and ferrule while directing the line through the grommet When the nut and ferrule are reattached be sure that the tubing end is flush with the face of the ferrule 6 Attach the furnace injection line to the 8 port valve at port C Make sure the fitting is finger tight but do not over tighten the nut Use the tool provided with your Apollo operating
117. r left front panel just above the 2 5 ml syringe Remove two 2 thumbscrews on 8 port valve face Gently remove the screw just below the syringe with the flat head screwdriver DO NOT force removing the screw e If the screw is difficult to remove use the TOC Talk Syringe Diagnostics to move the plunger 5001 away from the Home position Pull 8 port valve and syringe assembly away from the syringe driver face and toward you until it is removed Unscrew syringe from 8 port valve Noting their position unscrew the Teflon nuts 7 total from around the 8 port valve Reattach Teflon nuts from previous step to new 8 port valve making sure each port has a white washer spares come with the 8 port valve in it beforehand Reattach syringe Make sure white washer is in place and the threads on the syringe are covered with 1 2 turns of Teflon tape Reattach 8 port valve and syringe assembly to syringe driver making sure the pin on the inside of the 8 port valve slots into the rod from the syringe driver This may require you to initially attach the assembly with the syringe out of position Attach anyway and then turn the assembly until the hole on 8 port valve behind port A aligns over the gray circular protrusion on the syringe driver When properly aligned reattach assem bly using thumbscrews and syringe screw in steps 3 and 4 DO NOT force the syringe screw Using TOC Talk software go into the
118. rbon contamination 2 Check the system blank Low level analyses are especially sensitive to effects of system blanks because of the lower amounts of carbon measured Run the blank method using fresh deionized or ultra pure water The raw data obtained should be Less than 30 000 counts for the standard Apollo 9000 Less than 300 000 counts for the Apollo 9000 HS If your results do not approximate these values perform the catalyst maintenance instruction in Section 3 Increase injection volume Use Method 0 20 ppmC when per forming low level analysis A new method may also be created to inject volumes of 0 6 2 0 mL to increase the number of counts measured If the analysis volume has been changed we strongly recommend making a new method for the blank and perform ing calibrations using the new injection volume See Section 6 3 on modifying analysis methods 6 2 2 Particulated Samples When analyzing samples containing high levels of particulate matter like wastewater effluents Tekmar Dohrmann recommends pretreating the sample to break up the particulate matter Reproducibility of the analysis will be dependent upon the degree of sample homogeneity It is important to use as large a volume of the sample as possible to get a good representative sample You can pretreat samples in several ways Homogenization Filtration Dilution and Sample Stirring Note Apollo 9000 runs a special method to include the car
119. re control over archival of your data files On the Setup menu click Archive B e i 1 Specify a file path for the archive files to be created under or accept the default C APOLLO ARCHIVE Archive old data files every 15 days to t path Automatic Archive Utility Status 2 Click Archive Now A dialogue will OFF appear on your screen indicating that the archive was successful x ne 3 Click OK Figure 3 4 Archive Settings Screen Automatic Archive TOCTalk automates the process of data archive with its Archive utility When enabled TOCTalk creates a new direc tory tree copies all files to the new location and deletes them from their original location while leaving the original directory structure intact Archival occurs up to the present day when the interval in days has been reached the system mode is in Standby and the TOC Talk software is on 1 Enter an interval number of days value in the first field 2 Either type in a new file path for the backup files to be created under or accept the default C APOLLO ARCHIVE path 3 Select On in the Automatic Archive Utility Status 4 Click OK 3 5 Password Setup The Password Setup utility is designed to enforce limited access to control lable features within TOC Talk This is beneficial if you want to limit access to method setups calibration setups and data archival Each system may have
120. red to the IC sparger 5 sparge gas is turned on and the IC is quantified 6 The IC sparger is emptied of sample 7 Steps 3 through 6 repeat until all reps are completed 8 The water trap is emptied of condensate 1 18 1 8 4 Total Carbon TC 1 Sample is drawn into the syringe 2 The priming rep aliquot is injected into the furnace This rep is not quantified 3 Successive analysis reps are injected into the furnace and quantified 4 Condensate is removed from the water trap Rinse Syringe with Sample Excess Water in Water Trap Emptied to Waste Memorize Baseline Combustion Furnace Gas Off Wait for Endpoint Deliver Sample to Combustion Furnace Start Integration Sample Gas Swept to NDIR CO Concentration is Measured Wait Time 15 Seconds Sample Gas Swept Through Combustion Corrosives Furnace Scrubber Gas On Sample Gas Swept Through Moisture Control System Figure 1 8 4 TC Analysis Process 1 8 5 Inorganic Carbon Note There are rinsing steps for the syringe and IC sparger and other details that are not represented here Sample is delivered to the IC sparger DI water and acid are delivered to the IC sparger The sparge gas is turned on but this rep is not quantified The IC sparger is emptied of the sparged sample Successive aliquots of the sample acid and DI water are delivered to
121. review the Safety information in Chapters 1 and 2 before replacing or installing any Apollo 9000 parts 7 2 1 Permeation Dryer Tool s Needed e Phillips screwdriver 1 Remove right hand or plumbing side cover by removing seven 7 screws holding it to the chassis 2 Locate the old permeation dryer It should be in front of the combus tion furnace when looking at the instrument from the right side 3 Remove the permeation dryer from 1 black clasps found near each end of the dryer 4 Youcan now change out the permeation dryer in two ways Disengage green and yellow tubing both entering and leaving the permeation dryer by unscrewing the appropri ate fittings Make sure that you keep the Tygon tubing overlay on the yellow tubes intact for the new permeation dryer Attach these four 4 lines on the new permeation dryer by inserting them into the appropriate fittings Make sure that the sample gas green lines flows in the opposite direction of the drying gas yellow lines Disengage the four 4 fittings holding the green and yellow tubes entering and leaving the permeation dryer Remove the same fittings from the new permeation dryer Attach the old permeation dryer s fittings to the new permeation dryer in the proper order This will be easier to do but incurs the minimal risk of reusing a cracked fitting Verify that sample and drying gas flows are at 200 cc min 10 96 and are flowing in
122. rge time is completed and aliquot of the sparged sample is injected to the furnace as the priming rep This rep is not quanti fied 5 Successive aliquots of the sample are injected and quantified 6 After the final rep of a vial is injected the ASM needle is rinsed with DI water and then the se quence begins for the next sample vial 7 The water trap is emptied of condensate INTRODUCTION Deliver Acid to Sample Vial Excess Water in Water Trap Emptied to Waste Sparge Sample Vial Rinse Syringe NDIR Signal with Sample Linearized and Sent to Computer for Analysis Memorize Baseline Combustion Furnace Sample Gas Gas Off Swept to NDIR CO Concentration is Measured Deliver Sample to Combustion Furnace Sample Gas Swept Through Corrosives Scrubber Wait Time 15 Seconds Sample Gas Swept Through Moisture Control System Combustion furnace gas on Figure 1 8 2 TOC IC Removal with ASM Sparge Analysis Process 1 17 INTRODUCTION Total Carbon Minus Inorganic Carbon TC IC 1 8 3 Note There are rinsing steps for the syringe and IC sparger and other details that are not represented here 1 Sample is drawn into the syringe 2 The priming rep aliquot is injected into the furnace This rep is not quantified 3 The analysis rep is injected to the furnace and quantified 4 Sample DI water and acid are delive
123. rrosives scrubber is a glass tube filled with Pyrex wool and tin and copper granules Figure 1 4 7 Corrosives Scrubber INTRODUCTION Moisture Control System Moisture is removed from the gas going to the detector to prevent condensation in the detector The Apollo 9000 moisture control system consists of a condensor coil cooling fan water trap and permeation dryer The combustion furnace where carbon in the sample is converted to carbon dioxide generates high heat Carrier gas sweeps CO and water vapor out of the combustion furnace The sample then travels through tubing cooled by a fan to condense water vapor FX 9 KOS Figure 1 4 8 Cooling Fan INTRODUCTION Next the carbon dioxide travels through the water trap where water is collected to Permeation Dryer to 8 port Figure 1 4 9 Water Trap Then the carbon dioxide passes through a semi permiable Nafion tube to further remove moisture This tube is sealed into an impermeable shell which has openings adjacent to the sample inlet and outlet When a wet gas stream flows through the tube and a countercurrent dry gas stream purges the shell water molecules diffuse through the walls of the tubing Purge Gas Out L lt 91 1 Purge Gas In Figure 1 4 10 Permeation Tube 1 12 Nondispersive Infrared Detector Apollo 9000 converts carbon in the sample to carbon dioxide The nondi
124. s on either side of the injection port Be careful when removing the injection port from the combustion tube to avoid breakage Remove mounting plate and spacer block by removing the four 4 screws attaching them to the injection port Making sure combustion tube o ring is in place attach mounting plate and spacer block to the new injection port by reattaching the four 4 screws in step 8 Reattach injection port to the combustion furnace with the two 2 screws used in step 7 Be careful when sliding injection port over the combustion tube to avoid breakage Make sure that 1 8 blue furnace carrier gas fitting is oriented to the right Reattach the 1 8 blue furnace carrier gas fitting to right of injection port Reattach the 1 16 furnace line to the injection port Make sure fitting is hand tight but DO NOT over tighten Using TOC Talk software turn on gas flow to the combustion furnace and make sure the furnace gas goes to the NDIR Verify 200 cc min 10 through the furnace using the To Furnace or manual flowmeter If leak is present tighten 1 8 blue line fitting and sample injection line fitting until proper flow is achieved If there is no leak replace right cover to instrument MAINTENANCE AND TROUBLESHOOTING MAINTENANCE AND TROUBLESHOOTING 7 2 5 8 port Valve Tool s Needed 7 8 Slotted screwdriver Teflon tape Open acrylic door Locate 8 port valve on uppe
125. sis Results screen Figure 4 3 6 Analysis Results There is no calculation of PPM C during calibration The results are in area counts forthe integrated peak The Calibration Curve screen appears when the standard run ends see Figure 4 3 7 Calibration r Value Curve Graph TOC CALIBRATION gt Cabra Cocker ml teen Yee Recalc Calibration Button Curve Results Table Figure 4 3 7 Calibration Curve The Calibration Curve table displays the standard calibration data At the begin ning of each row is a box Clicking on and offthe Use box toggles X When the X is visible the calibration point repre sented by that row will be included in the calibration curve when you click Recalc Some users prefer to analyze the same standard concentration twice and then select one or both to include in the calculations Various combinations may be setup Each time you configure new calibration set you must click Recalc The value is one way to evaluate the calibration The closer is to 1 the more precise the calibration You may delete unused lines by high lighting the row and pressing the delete key This may prevent confusion when viewing the calibration again later CALIBRATION 4 17 CALIBRATION Notes SAMPLE ANALYSIS 5 1 Sample Analysis The following tutorials will guide you
126. spersive single beam infrared detector uses electromagnetic radia tion or infrared energy to measure this carbon dioxide This measurement is proportional to the carbon in the sample Inside the detector a beam of infrared energy is directed through a sample cell to the detecting apparatus This apparatus consists of two chambers which are filled with CO and con nected by a flow sensing device The unobstructed infrared energy absorbed by this CO causes the pressure to increase in the forward chamber and equilibrate between the two chambers When CO is then introduced to the sample cell some of the infrared energy is absorbed Therefore the pressure in the forward chamber decreases and CO flows to equilibrate the pressure This flow causes a voltage output from the flow sensor which is proportional to the concentration of CO in the sample cell Figure 1 4 11 Nondispersive Infrared Detector NDIR Flow Restrictors Five flow restrictors maintain the flow rate of the supply gas as follows 1 200 ml min to the combustion furnace 2 200 ml min to the IC sparger 3 200 ml min to the autosampler sparge line 4 200 ml min to the permeation tube 5 50 ml min to purge the Figure 1 4 12 Flow Restrictor When you turn off the gas valve 1 50 ml min of carrier gas continues to purge the NDIR INTRODUCTION Temperature Co
127. stics Syringe Pump amp 8 port Valve Control Screen WARNING Do not alter this screen during an analysis Erroneous or conflicting data can damage the instrument Valve Position Current Position Displays current position of the outer port of the 8 port valve The common port is always connected to the syringe Move To Position You can choose the outer port position here by clicking on the pull down window or the display box and then clicking on the Move button TOC TALK Acid Not Used Reactor F Waste C Furnace G DI Water D Sample H Water Trap e Home Position Button Automatically switches the outer port of the 8 port valve to position A Acid Syringe Volume Position pL Current Position Displays current position of the syringe in microliters Move To Volume You can move the syringe by entering the absolute position of the syringe in microliters and clicking the Move button Example If you want to pull 1000 uL from a syringe already located at 200 uL enter 120091 in the Move to Volume field and click the Move button Home Position Button Automatically moves the syringe to 0 uL and the valve to the waste position while discarding syringe contents Note Updating the current position during analysis may result in communication and data loss 3 7 TALK Autosampler Diagnostics On the Setup menu point to Diagnos tics
128. tartup Tekmar Dohrmann recommends that Apollo 9000 remain in Standby Mode when not in use Sleep sends the instrument to Standby Mode and turns off the combustion furnace but maintains power to the NDIR Gas Flow Rate cc min Furnace detects flow of carrier gas to the combustion tube Options 0 8 mm Particulate Kit Installed Select this option only if you have the 0 8 mm Particulated Sample Kit installed Autosampler Sparge Option Select this option only if you want the autosampler to sparge the sample for TOC analysis before transferring the sample to the Apollo 9000 3 4 Preferences Select from the following options to configure the instrument specific to your sample analysis requirements Sample Introduction e Without Autosampler With Autosampler Repetitive Sampling Max Integration Time min Time in minutes allotted for the reaction portion of an analysis to take place Default is set to 4 minutes Stabilize Baseline Time sec Some analysis modes may require added wait between analyses to allow proper return of the baseline to a stable value 15 seconds is recommended Outlier Deletions Select the Outlier Deletion check box if you want to delete a certain number of outliers maximum is 4 per sample analyzed 1 1 2 3 4 3 4 5 6 7 Table 3 2 Maximum Outlier Deletions for Sample Rep Count Print Data Report after Each Sample Set Se
129. terial With the exception of the combustion tube and reagent bottles all glassware is installed at the TeledyneTekmar factory Open the door of the Apollo 9000 by gently pulling the right front side of the door It will swing open to the left Carefully remove the foam packing that protects the installed glassware during shipment Verify that the 1 16 OD tube at the bottom of the water trap extends into the larger diameter portion of the trap about 1 4 to 1 2 Bench Placement Arrange Apollo 9000 on the laboratory bench with the computer and optional autosampler The autosampler should be placed to the left of Apollo 9000 as it needs to be near the syringe You may also wish to place a local or networked printer near the computer for printing data reports Allow for generous workspace around and above the analyzer 2 3 Tools and Supplies Needed for Connections Before you begin making connections gather the following tools and supplies nuts and ferrules supplied with unit 1 1 8 open end wrench 7 16 open end wrench tank of TOC free carrier gas equipped with a two stage regula tor for steady delivery of gas at 30 to 35 psi 206 7 to 241 2 kPa large bottle or beaker to collect waste SYSTEM SETUP 2 4 Pneumatic Connections Figure 2 4 1 illustrates the gas and water connections that need to be made atthe back before operating Apollo 9000 Specific instructions for each connection are given in the secti
130. the furnace a Examine the bottom connec tor for any debris on the black o ring that seals to the com bustion tube If necessary remove the connector at the stainless steel union and rinse it under clean running water Shake out the excess water and gently wipe the o ring with a lint free cloth b Replace the bottom connector and secure it in place by swinging the locking guard to the left until it touches or nearly touches the left furnace leg Add Catalyst to the Combustion Tube 1 Verify that the combustion tube is clean has no cracks and that neither end is chipped The narrow end is the bottom of the tube 2 Place a loosely wadded tuft approximately 1 2 thick of quartz wool through the top of the combustion tube to just above the narrow opening To prevent catalyst from dropping through the quartz wool gently pack the top of the quartz wool so that there is no space between the perimeter of the quartz wool and the glassware 3 The catalyst 20 grams is in a small vial Pour the entire 20 grams into the combustion tube 4 Before the tube is installed into the furnace the injection port and old combustion tube must be re moved from the furnace and its bottom connector must be examined see previous section Install the New Combustion Tube 1 Gently insert the combustion tube into the top of the furnace and push down firmly while turning the tube slightly The movement of the tube through t
131. the nut onto the tubing with the wide opening toward the end of the tubing 2 Slide the small back ferrule onto the tubing with the flat side toward the nut 3 Slide the front ferrule onto the tubing with the narrow end toward the end of the tubing 4 Tighten the nut with your fingers 5 For metal ferrules such as to the gas supply use a wrench to tighten the nut further Turning the nut 1 4 turn 90 to 1 2 turn 180 is usually adequate However the amount of force you need to apply can vary depending on the friction between the nut and threads as well as the composition and thickness of the tubing or line SYSTEM SETUP Prepare Reagents WARNING Acid will burn eyes and skin To prevent injury wear safety glasses and skin protection when using these chemicals Refer to Material Safety Data Sheets for detailed informa tion Put on safety glasses and protective clothing before proceeding to the next step To prepare reagents gather the follow ing supplies e 250ml bottle for acid supplied 1000 ml bottle for DI H O ultra pure water e phosphoric acid H PO 85 To prevent organic contamination wash bottles thoroughly with hot soapy water and rinse at least three times with ultra pure water before using To Prepare Acid Reagent 1 Measure 150 ml of ultra pure water into a rinsed 250 ml bottle 2 Add50mlof8596 phosphoric acid H PO For best results store prepared s
132. the screen displays Pid Press SET to display NO While still holding SET press the Up or Down key until YES appears on the screen Release both keys to display Pbh proportional band heat Press SET to display a number While still holding SET press the Up or Down keys appropriately until 75 appears on the screen Release both keys Pbh still appears the Screen 19 20 21 22 23 24 MAINTENANCE AND TROUBLESHOOTING Press the Down key to display Cth cycle time heat Press SET to display a number Press the Up or Down keys appropriately until the display read 2 0 Release both keys Cth still appears on the screen Press the Down key to display It integral function Press SET to display a number Press the Up or Down keys appropriately until the display reads 10 0 Release both keys It still appears on the screen Press the Down key to display de derivative function Press SET to display a number Press the Up or Down keys appropriately until the display reads 0 25 Release both keys de still appears on the screen Press the Down key to display CAL calibration Press SET to display a number Press the Up or Down keys appropriately until the display reads 0 Release both keys CAL still appears on the screen The PID menu is now set appropri ately Press and hold the Up and Down keys simultaneously for three seconds to
133. tings from the autosampler needle 5 Verify flow of 200 cc min 10 from 1 8 tubing by turning on the Sparge Gas in the Diagnostics Valves menu 6 Attach gas line 1 8 tubing to side port and sample line to vertical fitting on the new autosampler needle Verify vigor ous flow through second from bottom set of holes in needle MAINTENANCE AND TROUBLESHOOTING 7 6 Place the needle in small beaker of rinsing water and using the Diagnostics screen in TOC Talk software verify that sample is being effectively pulled into the syringe Remember that your first pull could have dead volume from the sample line By dispensing syringe pulls to the waste port F and pulling again from the sample port D you should be able to verify proper performance Reattach the autosampler needle to autosampler Make sure bottom of needle is level with the bottom needle guide blue fitting Hand tighten the upper needle fitting to lock the autosampler needle in place 7 2 4 Injection Port Tool s Needed Phillips screwdriver Slotted screwdriver Remove right hand or plumbing side cover by removing seven 7 screws holding it to the chassis Locate Teflon injection port above the combustion furnace Remove the 1 16 furnace line from the top of the injection port Remove Tygon waste line from the right rear of the injection port Remove injection port from the combustion furnace by removing the flat head screw
134. tus gt Instrument Name Apollo 3000 Operator Name USERT zi Help System oo Preferences Sample it losampler G Ready P ith Autosampl Standby Max Integration Time 40 Gas Flow Rates cc min Stabilize Baseline Time 15 To Furnace L Outlier Deletions Print data report after each sample set Auto Shutdown w Options 0 8mm Particulate Kit Installed Hak Syetan if i Out of Calibration Over Range IV Butosampies Option Figure 3 2 Instrument Setup Status Screen The Instrument Setup Status Screen is the main system configuration inter face this screen you will configure TOC Talk to recognize your Apollo 9000 system options Instrument Name Type a name in this text box to identify the Apollo system Operator Name Enter a name i e your name name of group in this text box for analysis identifcation 3 3 TALK System Select a system status mode for the Apollo 9000 from the following Ready turns on the permeation dryer gas and the combustion furnace gas and then routes carrier gas from the IC sparger to vent and from the combustion furnace to the NDIR In order to execute a sample run the instru ment must be in Ready Mode Standby turns the gas valves off The NDIR and furnace remain on Shutting off the NDIR will incur a minimum two hour stabilization delay upon s
135. type Phillips screwdriver 7 16 wrench To remove the right cover first move reagents DI water and waste contain ers away from the unit Remove the seven screws that hold the cover and lift it off the unit Furnace Carrier Gas Flow Path 1 Make sure combustion furnace carrier gas is on and directed through the NDIR This can be accomplished by setting the instrument to Standby and then Ready in the instrument setup screen This can also be done by actuating the appropriate valves in Valve Diagnostics 2 Make sure the carrier gas going into the instrument is on and the pressure regulator is set to 30 35 psi If not adjust the pressure within this range and recalibrate the instrument after the successful completion of this leak checking procedure 3 Checkthe flow leaving the NDIR on the 1 8 green line exiting the rear of the instrument with a manual flow meter Write down NDIR flow result 4 Using a manual flow meter mea sure the flow for the 1 8 white line entering the side of the water trap Write down water trap flow result 5 Theflow path is leak free if the flows measured in steps 3 and 4 will fall within a 180 to 220 cc min range Condition 1 and are within 10 cc min of each other Condition 2 Otherwise a If condition 1 fails for the water trap go to step 6 Leak Checking before the Water Trap b If condition 1 fails for the but not the water trap and condition 2 passes try
136. usly for three seconds to enter the software menu Once in the software menu the word AUT will appear on the screen Press the Up or Down keys until the word CNFG appears on the screen Press SET to display NO While still holding SET press the Up or Down key until YES appears on the screen Release both keys to display In input type Press SET to display J While still holding SET press the up or Down key until 5 appears on the screen Release both keys In still appears on the screen Press the Down key to display C_F Celsius Fahrenheit Press SET to display F While still holding SET press the Up or Down key until C appears on the screen Press the Down key to display rL input range low Press SET to display O If display does not read 0 press the Up or Down keys appropriately until the display does read 0 Release both keys rL still appears on the screen Press the Down key to display rh 12 input range high Press SET to display 1450 While still holding SET press the Down key until 1000 appears on the screen Release both keys rh still appears on the screen Press the Down key to display Ot1 output 1 function Press SET to display heat If display does not read heat press the Up or Down keys appropriately until the display does read heat Re lease both keys Ot1 still appears on the screen Press the Down key to display Ot2
137. ver Range 3 5 Oxidation by Combustion 1 4 Particulate Kit 3 4 particulate requirements 1 5 Particulated Samples 6 5 parts per million ppm 1 4 Password 3 11 Restriction Access 3 11 Setup 3 11 PCB board 7 13 7 14 7 15 Permeation Dryer 1 11 7 3 7 23 7 24 Tube 1 3 1 11 1 13 Phosphoric Acid 2 4 2 10 6 4 Pneumatic Connections 2 7 vi POC 1 3 1 10 Port A 2 10 5 5 B 7 10 D 2 22 5 5 G 2 10 4 16 5 5 7 8 Pos 2 22 4 14 Position 4 and 5 2 16 11 2 10 4 16 5 7 11 and 12 2 16 potassium acid phthalate 2 5 Power 1 6 2 4 Entry Module 7 15 requirements 2 11 Supply 2 17 7 14 Preferences 2 21 3 4 pressure 2 4 3 6 regulator 7 26 preventive maintenance 7 3 Print Data Report 3 5 Data Report after Each Sample Set 3 5 5 6 Priority samples 1 5 purge 1 13 purgeable organic carbon 1 3 1 10 Q quartz 2 18 combustion tube 1 10 wool 7 16 R r 4 10 rack 2 17 3 8 Selection 1 6 Style 3 8 Range 1 4 4 3 errors 3 5 Raw counts 4 3 Data 4 4 Ready 2 21 5 3 5 6 Mode 3 4 Reagent 2 4 4 3 7 3 Contribution 4 4 1 5 4 10 Recalculation see Recalc Repetitive Sampling 3 4 Reps 4 8 5 5 5 7 response factor 4 3 Restricted Access 3 11 result 4 9 Review Analysis Results 4 4 4 9 4 16 Rinse 1 6 Station 2 16 2 17 Water 4 3 RS 232 2 11 2 13 7 11 connections 7 11 Interface Cable 2 13 7 11 RSD 1 4 5 5 5 8 Run 4 7 4 14 5 4 5 6 Screens 4 7 4 14 5 S
138. ver set Slotted screwdriver set Small needle nose pliers Other Waste bottle 4 liter for sample rinse Vials for appropriate autosampler rack i e 40 ml vials SYSTEM SETUP PC Requirements Processor Minimum 486DX 66 MHz or better e Recommended Intel Pentium or compatible processor Memory Minimum 16 MB e Recommended 64 Hard disk Minimum 150 MB free hard disk space e Recommended 500 MB free hard disk space Display Minimum or higher resolution Recommended VGA or higher resolution Drive e Minimum 3 5 floppy drive e Recommended 4X CD ROM and 3 5 floppy drive Input Output Devices Minimum Mouse Windows 95 98 NT compatible speakers and sound card 2 5 5 5 5 2 2 Unpack and Inspect Apollo 9000 must only be lifted and positioned from beneath its base The Apollo 9000 front cover glassware or any other external compo nents should never be used for lifting or positioning support Bodily injury or damage to Apollo 9000 may occur if Apollo 9000 is not lifted and or positioned properly The Apollo 9000 TOC analyzer associ ated glassware and accessories should be carefully unpacked and immediately inspected for damage Claims for loss or shipping damage should be promptly filed with the carrier Notify the Tekmar Dohrmann Customer Support Center directly for any shortages or packing errors 2 6 Remove Packing Ma
139. with the syringe out of position Attach anyway and then turn the assembly until the hole on 8 port valve behind port A aligns over the gray circular protrusion on the syringe driver When properly aligned reattach assem bly using thumbscrews and syringe screw in steps 3 and 4 Do not force the syringe screw MAINTENANCE AND TROUBLESHOOTING 16 Reestablish communications with TOC Talk software by using the Setup diagnostics Communica tions Screen The Syringe driver should initialize If not disconnect AC power reenter the electrical side of the instrument and make sure the RS 232 cable to the syringe driver is properly installed Using TOC Talk software go into the syringe diagnostic and verify the ports on the 8 port valve are properly aligned There is a chance that the 8 port valve is 180 off its true position Pull 1000 ul from the furnace port making sure that the DI water line can also pull liquid Dispense to waste and repeat once more with 2500 ul this time If you do not get liquid on the second pull go to step 12 If you get liquid then the 8 port valve is misaligned Perform the following steps a Using the syringe diagnostic screen make sure that the 8 port valve is in the C Furnace position b Remove 8 port thumbscrews and syringe screw and pull assembly out from driver c Inthe syringe diagnostics screen turn the valve to the DI water or port G position d Reattach 8 port valv

Apollo 9000 TOC Combustion Analyzer User Manual

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