TitraLab Karl Fischer
Contents
1. n 17 3 4 3 4 Connection of tubes for waste bottle 18 3 44 Electrode i emeret tet pe ue eet a e ERE ers 19 3 4 5 Power supply external nennen nene nnne nnne nennen nnns nennen nnne 20 3 5 Keypad seren ore A IR IO HR 21 36 R8eage tS uuu PE E end tnd e lata ua La tena Nao tat aaa tds aoaaa a aie 23 3 6 1 Chemical reactions eee E A nnn nennen nennen ns IS nnne 23 3 6 2 Titrant and solvents eire da usa AUR 23 3 6 2 1 One comporient reagents cond doi io Rias 23 3 6 2 2 Two componenireagents iosa lella inci a Es 23 Section 4 Operationhi e IER ee eir RR In ER IN EM ia 25 4 1 Switch on the instrument nennen eee u sn eee en sense nnne nne nen 25 Ay 2 I da 25 4 2 1 Language and data output setting leale 25 4 2 1 1 Change the language setting a A A 25 4 2 1 2 Change the data output setting erica leia los Pie te Pas 25 4 2 2 First steps after installation rr rsrsssssssssssssssssssa 25 4 3Menu structure Ln 25 Table of contents 4 4 General information on KF titration rra 29 4 4 1 Individual titration StepS nennen nnne nnne nnne Ennan ennenen eent 29 5 S ANIM m 29 4 4 3 SUMING Speed u ususln A Riario 29 4 4 4 Removal of bUbbIES nono nnnnnnnnnnnnnnnnnnnn2. 4 1 Switch on the instrument Become familiar with the instrument functions before operation Learn how to navigate through the menu and perform the relevant functions 1 Connect the input connector of the power supply to the POWER IN port on the back of the TitraLab 2 Connect the power supply to a power socket 3 Press ON OFF below the display to switch on the instrument 4 The instrument performs a self test upon each activation Note Wait approximately 20 seconds before switching on again so as not to damage the electronics and mechanics of the instrument 4 2 Startup 4 2 1 Language and data output setting The titrator software supports multiple languages The first time the instrument is switched on a language selection list is displayed automatically upon completion of the self test 1 Select the required language 2 Press OK to confirm the selection 3 Select the type of data output deactivated printer computer and confirm with OK 4 2 1 1 Change the language setting The instrument functions in the selected language until the option is changed 1 Turn the instrument on 2 Select SYSTEM gt LANGUAGE 3 Select the required language 4 Press OK to confirm the selection 4 2 1 2 Change the data output setting The instrument functions in the selected data output until the option is changed 1 Turn the instrument on 2 Select SYSTEM gt DATA OUTPUT 3 Select the required setting 4 Press OK to co
3. 4 8 page 33 KF Standard with automatic drift control unit Program Program status Activated Active Deactivated Inactive Type Type of titration Classic For titration with standard reagents Special For titration with special reagents Extraction Type of water extraction Previous to titrat Time between dispensing of sample and start of titration During Titration Minimum duration of titration No Start of titration directly after addition of sample Std V Standard volume in mL EP Delay End point delay time during which the end point of the reaction must remain stable Max Vol Maximum volumes of the titration cell Drift C Drift control Automatic Automatic maximum drift limit 30 uL min Manual Manual sample can be added at any time Units Unit of the result mL mg ppm 96 A U volume A U weight L Comment Comment lines No No Yes Yes up to 8 lines P2 KF 1 Titration program for very low water content P3 KF 1096 P4 KF Standard KF Standardization Titration program for high water content KF Standard unit mg mL Calibration program Type Type of titration Classic For titration with standard reagents Special For titration with special reagents Standard Type of standard solution Standard G Standard solution water concentration in g Standard V Standard so
4. LANGE NV SA Motstraat 54 B 2800 Mechelen Tel 32 0 15 42 35 00 Fax 32 0 15 41 61 20 info hach lange be www hach lange be HACH LANGE S R L Via Rossini 1 A 1 20020 Lainate MI Tel 39 02 93 575 400 Fax 39 02 93 575 401 info hach lange it www hach lange it HACH LANGE S R O Zastrcen 1278 8 CZ 141 00 Praha 4 Chodov Tel 420 272 12 45 45 Fax 420 272 12 45 46 info hach lange cz www hach lange cz HACH LANGE 8 Kr Sarafov str BG 1164 Sofia Tel 359 0 2 963 44 54 Fax 359 0 2 866 15 26 info hach lange bg www hach lange bg Repair Service in Latin America the Caribbean the Far East Indian Subcontinent Africa Europe or the Middle East Hach Company World Headquarters P O Box 389 Loveland Colorado 80539 0389 U S A Tel 001 970 669 3050 Fax 001 970 669 2932 intl hach com HACH LANGE GMBH Hutteldorfer Str 299 Top 6 A 1140 Wien Tel 43 0 1 912 16 92 Fax 43 0 1 912 16 92 99 info hach lange at www hach lange at DR LANGE NEDERLAND B V Laan van Westroijen 2a NL 4003 AZ Tiel Tel 31 0 344 63 11 30 Fax 31 0 344 63 11 50 info hach lange nl www hach lange nl HACH LANGE S L U Edificio Seminario C Larrauri 1C 2 Pl E 48160 Derio Vizcaya Tel 34 94 657 33 88 Fax 34 94 657 33 97 info hach lange es www hach lange es HACH LANGE S R O Roln cka 21 SK 831 07 Bratislava Vajnory Tel 421 0 2 4820 9091 Fax 421 0 2 4820 9093 info hach lange sk www h
5. RNH SO3CH Il H20 l gt RNH SO3CH3 RN RNH SO CHg 2 RNH I III RN denotes the employed base 3 6 2 Titrant and solvents TitraLab is suitable for all KF solvents and reagents whereby both one component and two component reagents can be used 3 6 2 1 One component reagents The titrant contains all required chemical compounds such as iodine sulfur and the base as a single reagent The common titer value is 5 mg of water per mL of titrant Any solvent can be used to dissolve the sample provided it has a methanol content of at least 25 One component reagents have the following advantages e Unlimited water capacity e Allows specific solvent matrix composition to test difficult to dissolve samples 3 6 2 2 Two component reagents The titrant contains iodine dissolved in methanol Titer values of 1 2 and 5 mg of water per mL of titrant are commonly used The titrant of the titer should be chosen on the basis of the expected water concentration so that the titration can be performed with a single burette filling The solvent contains sulfur dioxide a base and methanol Two component reagents have the following advantages Rapid titration due to high reaction kinetics Improved reproducibility due to stable reaction environment with constant pH value and unchanging sulfur dioxide concentration e Higher buffer capacity Higher titrant titer stability 23 Installation 24 Section4 Operation
6. in the display Note Need for entering weight depends on the result unit selected Enter the weight of the new sample via the keypad and press OK to confirm the entry Press OK to confirm the result Further samples with emptying of titration cell If the titration cell is too full the pH value is incorrect or the methanol content drops below 25 the titration cell must be emptied before any further analyses can be performed 1 Press the Navigation key RETURN to access the manual activation menu 2 Select EMPTY VESSEL and press OK to confirm The titration cell is emptied into the waste bottle via pump 2 3 Select DISPENSE SOLVENT and confirm with OK The solvent is dispensed into the titration cell 4 Select CONTINUE and press OK to confirm Once the pre titration has been completed and the titration cell conditioned the text CONTINUE is shown in the display Press OK to confirm Dispense the sample into the titration cell Select START TITRATION and press OK to confirm During the titration WEIGHT ENTRANCE is shown in the display 8 Enter the weight of the sample via the keypad and press OK to confirm the entry 9 Press OK to confirm the result 10 Press the Navigation key RETURN to end the titration sequence select QUIT Operation 4 7 Manual component activation 4 7 4 Burette 4 7 2 Pumps 4 7 3 Stirrer Select MANUAL ACTIVATION gt BURETTE and press OK to confirm Select FILL with the DOWN
7. lange hu Repair Service in the United States HACH Company Ames Service 100 Dayton Avenue Ames lowa 50010 Tel 800 227 4224 U S A only Fax 515 232 3835 HACH LANGE LTD Pacific Way Salford GB Manchester M50 1DL Tel 44 0 161 872 14 87 Fax 44 0 161 848 73 24 info hach lange co uk www hach lange co uk HACH LANGE FRANCE S A S 8 mail Barth l my Thimonnier Lognes F 77437 Marne La Vall e cedex 2 T l 33 0 820 20 14 14 Fax 33 0 1 69 67 34 99 info hach lange fr www hach lange fr HACH LANGE AB Vinthundsvagen 159A SE 128 62 Sk ndal Tel 46 0 8 7 98 05 00 Fax 46 0 8 7 98 05 30 info hach lange se www hach lange se HACH LANGE SP ZO O ul Krakowska 119 PL 50 428 Wroclaw Tel 48 801 022 442 Zam wienia 48 717 177 707 Doradztwo 48 717 177 777 Fax 48 717 177 778 info hach lange pl www hach lange pl HACH LANGE S R L Str Caminului nr 3 et 1 ap 1 Sector 2 RO 021741 Bucuresti Tel 40 0 21 205 30 03 Fax 40 0 21 205 30 17 info hach lange ro www hach lange ro Contact information Repair Service in Canada Hach Sales amp Service Canada Ltd 1313 Border Street Unit 34 Winnipeg Manitoba R3H 0X4 Tel 800 665 7635 Canada only Tel 204 632 5598 Fax 204 694 5134 canada hach com HACH LANGE LTD Unit 1 Chestnut Road Western Industrial Estate IRL Dublin 12 Tel 353 0 1 460 2522 Fax 353 0 1 450 9337 info hach lange ie www hach lange ie HACH
8. loop control Navigation key LEFT Moves the cursor backward for entry of numeric values e Scrolls up in menus e Empties the syringe through the feed tube during manual open loop control Navigation key RIGHT e Moves the cursor forward for entry of numeric values e Scrolls down in menus 21 Installation RETURN key e Scrolls back in menus e Cancels a manual control e Cancels a titration e Shows the most recent calibration data in calibration mode OK key Check mark Confirms the gray highlighted menu items and scrolls forward in the menu e Shows the first data record in the data log Figure 13 Keypad 1 Navigation key UP 5 Navigation key DOWN 2 ON OFF key 6 Navigation key LEFT 3 Navigation key RIGHT 7 RETURN key 4 OK key Check mark 22 Installation 3 6 Reagents 3 6 1 Chemical reactions Karl Fischer titration is based on the principle of oxidation of sulfur dioxide by iodine in the presence of water It is the same principle as for the iodometric titration of sulfur dioxide in water lo SO 2H50 2HI H2SO I However a shift in equilibrium in the above reaction I to the right requires the neutralization of the formed hydriodic or sulfuric acid In many cases imidazole is used as a buffer for this purpose The solvent methanol is also involved in the reaction The Karl Fischer reaction can be described by the following reactions CH30H SO RN
9. navigation key to fill the burette Select EMPTY with the UP navigation key to empty the burette into the titration cell B O de S Select RETURN with the LEFT navigation key to empty the burette back into the titrant bottle Note Repeat this procedure multiple times to make sure that the dispensing process functions correctly 1 Select MANUAL ACTIVATION PUMPS and press OK to confirm 2 EMPTY VESSEL activates pump 2 to empty the titration cell into the waste bottle 3 DISP SOLVENT activates pump 1 to dispense the solvent into the titration cell 4 Select QUIT with OK to exit the menu Note Repeat this procedure multiple times to make sure that the dispensing process functions correctly 1 Select MANUAL ACTIVATION gt STIRRER and press OK to confirm 2 Press OK to switch the stirrer on or off 3 Use the navigation keys UP and DOWN to select the stirring speed The stirring speed can be modified during the vessel conditioning pre titration and titration Once the stirring speed has been selected it is recommended to maintain it constant during the analysis 4 8 Programming 4 8 4 Configuration of the calibration program The function can be used to adapt the calibration program to specific requirements 1 Select PROGRAMMING gt KF STANDARDIZATION and press OK to confirm 2 Select TYPE and press OK to confirm CLASSIC is suitable for titration with standard reagents SPECIAL is suitable for titration with specia
10. serviced by the manufacturer s service department at the prescribed intervals 3 4 Installation 3 4 1 Installation of the burette The burette dispenses the titrant that is the one or two component reagent The burette comprises the syringe stepper motor and valve The stepper motor and valve are already installed in the TitraLab the syringe must be installed by the user Risk of injury to pinch points and cuts Make sure that the titrator is never used operated without the syringe cover Make sure that the system is only assembled by qualified and trained personnel Warning against system damage Make sure that the syringe is never operated without the attachment sleeve Only use genuine replacement parts and accessories The instrument must be serviced by the manufacturer s service department at the prescribed intervals Note Make sure that you do not misplace the attachment sleeve for the syringe It is not provided with a new syringe 1 Push the syringe piston into the syringe body Slide the attachment sleeve fully onto the syringe so that the narrow end points toward the piston 2 Remove the syringe cover by unscrewing it 13 Installation 3 Point the syringe tip upward place the syringe into the bracket such that the attachment sleeve is above the bracket 4 With the narrow side facing down carefully press the attachment sleeve into the bracket Hold the attachment sleeve in the bracket and screw t
11. stirrer onto the base of the titration stand so that it locks into place 2 Place a magnetic stirring bar into the titration cell glass Press the titration cell glass into the lid from below so that it locks into place 3 Lower the titration cell onto the magnetic stirrer Place a desiccant cartridge into the designated opening in the titration cell lid 14 Installation Figure 5 Installation of the titration stand Lower the titration cell onto the magnetic stirrer 1 Lock the magnetic stirrer into place on the titration stand 3 Place a desiccant cartridge into the titration cell lid base 2 Place a magnetic stirring rod in the titration cell glass Attach the titration cell glass to the lid 3 4 2 1 Electrical connection of the magnetic stirrer 1 Connect the cable of the magnetic stirrer to the STIRRER port on the back of the TitraLab The power is supplied via the TitraLab Figure 6 Electrical connection of the magnetic stirrer 1 Connect the cable of the magnetic stirrer to the STIRRER port Installation 3 4 3 Installation of tubes Risk of injury to eyes skin and respiratory During the first days of system use check the screw joint between the syringe and valve to avoid leaks and the potential escape of reagents When working with chemicals and or solvents always observe the relevant accident prevention reg
12. the sample into the titration cell 4 Place the empty syringe or weighing boat back onto the balance to obtain the weight difference of the sample as a negative number 5 Enter this figure into the titrator as the sample weight Weigh the sample 47 48 Appendix B Volume test The volume test calibrates and checks the burette Different volumes are dispensed from the burette into a vessel on high precision analytical balance Based on the weights measured by the balance the instrument automatically calculates the volume dispensed by the burette The difference between the actual volume and nominal volume of the syringe is used to determine a correction factor to be used in the subsequent calculation If the instrument is connected to a printer a report detailing the established data is provided The procedure and maximum acceptable error are based on standard UNE EN ISO 8655 The test is performed with doses equivalent to 10 20 30 50 70 80 90 and 100 of the entire syringe volume The syringe is fully filled before each dose The titrator calculates a correction factor after each dose 8 1 Required equipment Figure 16 Analytical balance resolution 0 0001 g with RS 232 C output Thermometer with resolution of 0 1 C Protective cover for analytical balance Cat No LZW8721 99 Cable for connection between titrator and balance Liquid to be dispensed distilled water at room temperature Vessel on bala
13. up or put into operation Pay attention to all danger and warning statements Failure to do so could result in serious injury to the operator or damage to the equipment To make sure that the protection provided by this instrument is not impaired do not use or install this instrument in any manner other than that specified in these operating instructions ADANGER Indicates a potentially or imminently hazardous situation that if not avoided results in death or serious injury Indicates a potentially or imminently hazardous situation that if not avoided could result in death or serious injury Indicates a potentially hazardous situation that may result in minor or moderate injury Indicates a situation that if not avoided could result in damage to the instrument Information that requires special emphasis Note Information that supplements points in the main text Warning labels Read all labels and tags attached to the instrument Personal injury or damage to the instrument could occur if not observed For symbols applied to the instrument corresponding warnings are provided in the user manual This symbol if noted on the instrument references the instruction manual for operation and or safety information This symbol may be found on an enclosure or barrier within the product and indicates a risk of electrical shock and or death by electrocution Ri P P Electrical equipment mark
14. x 0 1 in conical adapter FZW87 10 99 Pump cassette with neoprene tube internal diameter 3 2 mm flow rate 170 mL min LZW9082 99 Desiccant cartridge LZW9200 99 Screw cap DIN 45 LZW8729 99 KF Glass vessel 120 mL Thermostated for TitraLab KF LZW9139 99 Electro valve for Burette LZW9249 99 AS7 cable 1M BNC For instruments with BNC connector LZW9055 99 7 2 Accessories Description Cat No Standard PC keyboard mini DIN connector LZW9013 99 LZW9135USB 99 LZW87XX 99 43 Replacement parts and accessories 44 Section 8 HACH Company World Headquarters P O Box 389 Loveland Colorado 80539 0389 U S A Tel 800 227 HACH 800 227 4224 U S A only Fax 970 669 2932 orders hach com www hach com HACH LANGE GMBH WillstatterstraRe 11 D 40549 Dusseldorf Tel 49 0 2 11 52 88 320 Fax 49 0 2 11 52 88 210 info hach lange de www hach lange de HACH LANGE GMBH Rorschacherstrasse 30a CH 9424 Rheineck Tel 41 0 848 55 66 99 Fax 41 0 71 886 91 66 info hach lange ch www hach lange ch HACH LANGE APS Akandevej 21 DK 2700 Br nsh j Tel 45 36 77 29 11 Fax 45 36 77 49 11 info hach lange dk www hach lange dk HACH LANGE LDA Av do Forte n 8 Frac o M P 2790 072 Carnaxide Tel 351 214 253 420 Fax 351 214 253 429 info hach lange pt www hach lange pt HACH LANGE KFT V r skereszt utca 8 10 H 1222 Budapest XXII ker Tel 36 1 225 7783 Fax 36 1 225 7784 info hach lange hu www hach
15. Figure 2 Back view 1 PS 2 connector for keyboard 4 Electrode connector 2 RS 232 C for external scales 5 Connector for power supply 3 RS 232 C for printer or computer 6 Connector for magnetic stirrer 10 Section3 Installation Risk of injury to eyes skin and respiratory When working with chemicals and or solvents always observe the relevant accident prevention regulations and wear appropriate personal protective clothing for eye face hand body and or respiratory protection Make sure that the system is only unpacked assembled connected and operated by qualified and trained personnel 3 1 Unpack the instrument Unpack all supplied parts carefully as they are highly sensitive in part to shock and impact Read the user manual prior to installation and proceed exactly as described 3 2 Scope of delivery Please check that the order is complete If anything is missing or damaged please contact the manufacturer or retailer 11 Installation Figure 3 Scope of delivery 210 10x 8 Wk O Titrator TitraLab Karl Fischer 152B 10 Titration cell 2 Burette titrant suction tube with bottle closure DIN 45 11 Electrode cable with BNC connector thread black 12 Double platinum electrode 3 2x Solvent or waste bottle tube with bottle closure 13 Power supply external DIN 45 thread 4 Burette titrant additio
16. LD DOC022 52 90357 Karl Fischer Titrator USER MANUAL 01 2013 Edition 2A Hach Company 2011 2013 All rights reserved Printed in Germany Table of contents Section 1 Specifications a 5 Section 2 General information nono n 7 2L Sae SITO UO ss u n SS uuu n disonore lath d ia aa A Sin eat aati Mate geri 7 2 1 1 Warning labels ias 7 2 1 2 Chemical and biological safety coi A u ee eee 8 2 2 Overview OT product ee E HERE RR OE E E RA Saa TER YU e RE Dea d E Per EE RR TED TRE 8 2 3 Front and back VI W ce tese et rn 9 Section 3 Installation de ion ai 11 3 1 Unpack the instrumenter o e e e ao eee tane ein e ioa dtr a RP pe e Ens 11 As eco e tret le vec eh pa I rid t Mastery 11 3 3 Operating environment geo is 13 3 4 InistallatiOn ix ot ttt a E ba e t b M RR EA ian 13 3 4 1 Installation of the burette mme rennen nenne 13 3 4 2 Installation of the titration stand Hmmm rennen 14 3 4 2 1 Electrical connection of the magnetic stirrer 15 3 4 3 Installation of tubes mem QI nennen nennen nenne 16 3 4 3 1 Removal of protective stickers r 16 3 4 3 2 Connection of tubes for KF titrant Y 16 3 4 3 3 Connection of tubes for solvent
17. ach lange sk HACH LANGE SU ANALIZ SISTEMLERI LTD T Ilkbahar mah Galip Erdem Cad 616 Sok No 9 TR Oran ankaya ANKARA Tel 90312 490 83 00 Fax 90312 491 99 03 bilgi hach lange com tr www hach lange com tr 45 Contact information HACH LANGE D O O HACH LANGE E N E Fajfarjeva 15 AUidog 27 SI 1230 Dom ale GR 115 27 A8rlva Tel 386 0 59 051 000 TnA 30 210 7777038 Fax 386 0 59 051 010 Fax 30 210 7777976 info hach lange si info hach lange gr www hach lange si www hach lange gr HACH LANGE OOO Finlyandsky prospekt 4A Business Zentrum Petrovsky fort R 803 RU 194044 Sankt Petersburg Tel 7 812 458 56 00 Fax 7 812 458 56 00 info russia hach lange com www hach lange com 46 HACH LANGE D O O Ivana Severa bb HR 42 000 Varazdin Tel 385 0 42 305 086 Fax 385 0 42 305 087 info hach lange hr www hach lange hr HACH LANGE MAROC SARLAU Villa 14 Rue 2 Casa Plaisance Quartier Racine Extension MA Casablanca 20000 T l 212 0 522 97 95 75 Fax 212 0 522 36 89 34 info maroc hach lange com www hach lange ma Appendix A Weigh the sample Figure 15 Precise sample and standard weights are absolutely essential for the calculation of correct results 1 Weigh liquid or viscous samples with a syringe and solid samples with a weighing boat 2 Place the filled syringe or weighing boat onto the analytical balance and set the balance to zero via the tare function 3 Dispense
18. burette volume 4 4 7 Empty the titration cell Note The discharge tube must reach to the bottom of the titration cell during emptying The tube must then be pulled back up to allow the magnetic stirring bar to move freely If a sample fails to dissolve in the titration cell it is better to remove and empty the titration cell manually to prevent pump blockage The tubes should not touch the liquid in the titration cell during a titration or calibration process The titration cell should be emptied at the end of the working day refer to section 5 2 page 37 4 5 Calibration Before a sample can be analyzed a calibration is performed to determine the exact titer of the titrant This requires a standard solution with a known water content 1 Select STANDARDIZATION and press OK to confirm 2 Select STATISTICS gt NO or YES to perform a statistical analysis If YES is selected enter the number of analyses used to determine the factor The absolute and relative standard deviation is shown Enter the water content of the employed standard solution in mg mL 4 Select CONTINUE and press OK to confirm 30 4 6 Titration 10 11 12 13 Operation Select DISPENSE SOLVENT and press OK to dispense the solvent into the titration cell Select CONTINUE and press OK to confirm The pre titration starts automatically The water content of the solvent and the drift are determined WAIT is shown in the display Adjust the s
19. e electrode is contaminated and must be cleaned or the electrode is broken cracked at platinum wire level and need to be replaced 42 Section 7 7 1 Replacement parts Replacement parts and accessories Description Cat No TitraLab KF 1S 2B Karl Fischer Titrator with 1x 5 mL syringe and 2 pumps Included accessories electrode holder with magnetic stirrer electrode 52 64 cable for electrode and special KF titration cell Double platinum electrode Pt 0 80 C For KF and SO titrations LLV8671 97 1202 LZW5264 97 0002 RS 232 C cable for connection between titrator and PC with 9 pin and USB connectors Cable for connection between scales and titrator Cable made on demand depending balance model please contact your local distributor Titration stand with magnetic stirrer and titration cell for KF LZW9160 99 Teflon coated stirring bar 20 x 6 mm 10 units LZW9339 99 KF Glass vessel 120 mL for TitraLab KF LZW9142 99 O ring for titration cell Viton LZW2 145V 99 Borosilicate glass syringe for burette TLL SL 5 mL LZW9228 99 Hardware sleeve for 5 mL syringe LZW8741 99 White O rings x 10 LZW8734 99 Inlet tube set for burette L 65 cm 2 13 ft d 1 5 x 2 5 mm 0 06 x 0 1 in black sheath ii Outlet tube set L 46 cm 1 51 ft d 2 x 1 mm 2 x 0 04 in black sheath antidiffuser conical LZW8708 99 adapter Tube for emptying dispensing pump L 65 cm 2 13 ft d 1 5 x 2 5 mm 0 06
20. e tip of the electrode Place the electrode into the designated opening on the lid of the titration cell Connect the electrode cable to the ELECTRODE port on the back of the TitraLab 19 Installation Figure 11 Connection of the electrode E SE 3 4 5 Power supply external ADANGER Make sure the AC supply voltage is suitable for the power supply and the mains plug style is suitable for the type of outlet socket Only use the original power supply and plug connectors Risk of electric shock The power supply is provided with different plug connectors The correct plug connector must be attached to the power supply before first use 20 Installation Figure 12 Plug connector attachment 1 Slide the plug connector into the power supply 2 Click the plug connector into place 3 5 Keypad Note To change the plug connector press in the catch and slide the plug connector upward ON OFF key Navigation key UP Used to select between different options on the display Increases numeric values Shows the previous data record in the data log menu e Empties the syringe through the discharge tube during manual open loop control Navigation key DOWN Used to select between different options on the display Reduces numeric values Shows the next data record in the data log menu Fils the syringe through the feed tube during manual open
21. ed into the titration cell default setting 13 s DATE HOUR entry of date and time DISPLAY CONTRAST increases or decreases the display contrast LANGUAGE English Spanish Italian French 4 12 Default settings The instrument features four titration programs and one calibration program The default settings are as follows Program 1 KF Standard activated Titration type classic Drift control automatic maximum drift 30 uL min Unit 96 Program 2 KF lt 1 H20 deactivated Program 3 KF gt 10 H20 deactivated Program 4 KF Standard deactivated Calibration program classic Water standard water standard in volume mg H5O mL The following overview indicates the recommended program for various sample types quantities and reagents Mii RN Sample quantity Titer Titrant consumption Program number o g mL 100 0 1 5 20 P3 10 0 1 0 2 5 2 4 P1 1 1 5 2 P1 0 1 1000 ppm 5 10 5 1 2 P2 0 01 100 ppm n x ai P2 0 011 10 ppm 20 30 2 0 125 0 150 P2 36 Section5 Maintenance NOTICE Warning against system damage Before maintenance or repair work is conducted thoroughly rinse the instrument with methanol and make sure that there are no residual chemicals in the tubes and pumps Only use genuine replacement parts and accessories The instrument must be serviced by the manufacturer s service department at the prescribed intervals 5 1 Maintenance schedu
22. ed with this symbol may not be disposed of in European domestic or public disposal systems after August 12 2005 In conformity with European local and national regulations European electrical equipment users must now return old or end of life equipment to the manufacturer for disposal at no charge to the user Note For return for recycling please contact the equipment manufacturer or supplier for instructions on how to return end of life equipment manufacturer supplied electrical accessories and all auxiliary items for correct disposal General information 2 1 2 Chemical and biological safety ADANGER Potential danger in the event of contact with chemical biological materials Handling chemical samples standards and reagents can be dangerous Familiarize yourself with the necessary safety procedures and the correct handling of the chemicals before the work and read and follow all relevant safety data sheets Normal operation of this instrument may involve the use of hazardous chemicals or biologically harmful samples Observe all cautionary information printed on the original solution containers and safety data sheet prior to their use Dispose of all consumed solutions in accordance with national regulations and laws Select the type of protective equipment suitable to the concentration and quantity of the dangerous material at the respective work place 2 2 Overview of product Volumetric titration accord
23. ess OK to confirm 4 10 Printer computer 4 11 System This function is only displayed if a printer or computer is connected and activated for data output Programs settings and results can be printed or transferred Following a titration or calibration the following data is printed or transferred e Header line 2 lines of 20 characters each date and time reagent factor drift sample ID titration result final volume duration of titration and operator ID 1 Select SYSTEM gt DATA OUTPUT 2 Select FOR PRINTER followed by the relevant printer model such as thermal or dot matrix Confirm with OK 3 Select FOR COMPUTER followed by either CAPTURE or TICOM Confirm with OK This function can be used to adapt the titrator to specific requirements REAGENT NAME entry of a reagent name via an external PC keyboard The reagent name is printed maximum of 10 characters OPERATOR NAME up to four operator names can be defined via an external PC keyboard The operator name is printed maximum of 17 characters DATA OUTPUT deactivates or activates data output on the printer or computer VOLUME TEST program for burette calibration ENTRY OF WEIGHTS manual entry or automatic if scales are connected The communication is defined via a protocol baud rate word length parity stop bits STANDBY CYCLE entry of standby interval default setting 15 min 35 Operation TIME D SOLVENT time in which the solvent is dispens
24. fault program settings are detailed in section 4 4 1 Select PROGRAMMING gt P1 KF STANDARD or another of the four available titration programs Press OK to confirm Select PROGRAM gt ACTIVATED or DEACTIVATED to show hide the program in the titration menu Press OK to confirm Select TYPE and press OK to confirm CLASSIC is suitable for titration with standard reagents SPECIAL is suitable for titration with special reagents such as aldehyde and ketone An end point of 200 mV is recommended for this setting Select EXTRACTION and press OK to confirm PREVIOUS TO TITRAT is used to program a time prior to titration at which the sample is to be dispensed into the titration cell This setting is particularly useful for samples that release water at a slow rate DURING TITRATION is used to program a minimum titration period required to make sure that all of the water contained in the sample is released If NO is selected the titration will start immediately after the sample has been added to the titration cell Select EP DELAY to define a time in seconds during which the end point of the reaction must remain stable Press OK to confirm Select MAX VOL to define the maximum volume of the titration cell The default setting is 10 mL If the maximum volume is reached the titration stops and the following error message is displayed MAXIMUM VOLUME REACHED Press OK to confirm Select DRIFT C gt AUTOMATIC or MANUAL Press OK
25. he bottles 37 Maintenance 5 3 Clean the burette Make sure that there are no crystals or other sediments inside the syringe If such deposits are discovered clean the syringe immediately as this will otherwise damage the plunger The temperature of the liquid inside the syringe must be between 15 and 40 C 5 4 Clean the electrode The double platinum electrode does not require any special maintenance Simply rinse with ethanol if required Remove any sticky materials with solvent and soft tissue Pay attention not to twist or bend the platinum wires 5 5 Replace pump tubes 1 o va m 38 Remove the screws on the right and left of the housing cover refer to point 1 in Figure 14 Remove the housing cover Press the ends of the gripper clamps together with pliers for example and slide the clamps down and off the connectors Remove the tubes from the connectors Press in the catches on the right and left of the pump cassette Remove the pump cassette from the shaft Slide the gripper clamps onto the tubes of a new pump cassette Slide the new pump cassette onto the shaft until the catches engage Slide the tubes onto the connectors Press the ends of the gripper clamps together with pliers for example and slide the clamps up onto the connectors Put the housing cover back on and tighten the screws Maintenance Figure 14 Replace pump cassette 1 Remove the screws
26. he syringe onto the valve from below 5 Withdraw the piston from the syringe and place it onto the screw in the dosage arm Hold the syringe piston and turn the attachment screw on the dosage arm into the thread in the piston 6 Fix the syringe cover with six screws Risk of injury to eyes skin and respiratory During the first days of system use check the screw joint between the syringe and valve to avoid leaks and the potential escape of reagents When working with chemicals and or solvents always observe the relevant accident prevention regulations and wear appropriate personal protective clothing for eye face hand body and or respiratory protection Figure 4 Installation of the burette 1 Push the piston into the syringe body 4 Place the attachment sleeve into the bracket Slide the attachment sleeve onto the syringe Screw the syringe tip onto the valve 2 Unscrew the six screws and remove the syringe cover 5 Screw the piston onto the dosage arm 3 Insertthe syringe into the bracket 6 Fix the syringe cover with six screws 3 4 2 Installation of the titration stand The titration stand consists of a holder onto which the titration cell and magnetic stirrer are attached The actual KF titration is performed in the titration cell Since air humidity disturbs the titration process the titration cell is hermetically sealed by means of an airtight lid 1 Place the magnetic
27. ing to the Karl Fischer KF method is an important method used to determine water content The method is routinely applied in many fields including the chemical petrochemical pharmaceutical and food industries The method is also prescribed by a number of ASTM ISO and DIN standards as well as in regulations from European and US pharmacopeias USP TitraLab is suitable for all KF solvents and reagents whereby both one and two component reagents can be used The instrument covers a measuring range from 100 ppm to 100 water Most applications are served by the four pre programmed titration programs though individual programs are also possible The clearly structured user interface enables quick and simple navigation TitraLab features two RS 232 C interfaces to enable communication with a computer printer or external scales for automatic weight transfer A PS 2 interface is also provided to allow the connection of a PC keyboard for entering alphanumeric sample names A convenient titration stand is also integrated and equipped with stirrers and pumps to add and extract the KF reagents 2 3 Front and back view Figure 1 Front view General information 1 TitraLab Karl Fischer 1S2B 7 Titrant 2 Keypad 8 Titration stand 3 Waste container 9 Magnetic stirring bar 4 Display 10 Titration cell 5 Solvent 11 Syringe cover 6 Desiccant cartridges 12 Burette General information
28. itration or calibration is started the titrator empties the contents of the burette into the titrant bottle The burette is then filled which removes any bubbles from the syringe and tube 29 Operation 4 4 5 Standby cycle If the titrator remains in drift control for more than 15 minutes the standby cycle is activated automatically The contents of the burette are pumped back into the titrant bottle e The magnetic stirrer is switched off To exit the standby cycle select START TITRATION e The burette is filled The pre titration is started and the titration cell is conditioned e Drift control checks whether the calculated drift values match the programmed thresholds Sample can be dispensed 44 6 Standard water solutions STANDARD V a standard solution with a known water quantity per mL of standard The default setting is 5 00 mg H O mL this value can be changed but should be between 1 and 5 mL of standard STANDARD G a standard solution with a known quantity of water per g of standard The default setting is 10 00 mg H O g this value can be changed but should be between 0 5 and 2 g of standard H20 distilled water The recommended quantity to be used is 10 to 25 mg of water TARTRATE sodium tartrate 2 hydrate A primary standard with a water content of 15 66 The recommended quantity to be used is 0 1 to 0 15 g of standard Recommended titrant consumption volumes are between 20 and 100 of the
29. l reagents such as aldehyde and ketone An end point of 200 mV is recommended for this setting 3 Select STANDARD and press OK to confirm STANDARD G is used for a standard solution with a known water concentration specified in grams g STANDARD V is used for a standard solution with a known water concentration specified in milliliters mL H20 is selected when distilled water is used as the standard 33 Operation 4 8 2 34 TARTRATE is selected when sodium tartrate 2 hydrate is used as a primary standard with a water content of 15 66 Select STD V to enter the volume of the employed standard solution in mL Press OK to confirm Select EP DELAY to define a time in seconds during which the end point of the reaction must remain stable Press OK to confirm Select DRIFT L to define a maximum drift limit in uL min Press OK to confirm Select MAX VOL to define the maximum volume of the titration cell The default setting is 10 mL If the maximum volume is reached the titration stops and the following error message is displayed MAXIMUM VOLUME REACHED Press OK to confirm Select L COMMENT gt NO or YES to enter comments Press OK to confirm If YES is selected up to eight comment lines can be entered using a standard keyboard This text is displayed in printouts Configuration of the titration programs The titrator features four titration programs which can be adapted to specific requirements The de
30. le Maintenance task every week or more 6 months 12 months Replace syringe x Replace valve block x Check burette feed tube replace if damaged Check burette discharge tube replace if x damaged Peristaltic pump pump cassette x1 x Check pump feed tube replace if damaged Check pump discharge tube replace if x damaged Check bottle closure set replace if damaged x Replace dry desiccant cartridges every week or x more frequently upon ambient humidity Check all tube connections for leaks and x damage KF titration cell Viton O ring x 1 When using Chloroform in solvent it is recommended to replace the pump cassette every 6 months 5 2 Poweroffthe instrument Never clean the tubes pumps and burette with distilled water At the end of the working day deactivate the instrument as follows Empty the contents of the burette into the titrant bottle refer to section 4 7 1 page 33 Empty the titration cell refer to section 4 7 2 page 33 When the instrument is to be deactivated for multiple days or extended periods perform the following steps Clean the burette and pump with methanol refer to section 4 7 page 33 Seal the reagent bottles with the original bottle closures Empty and clean the titration cell Store the desiccant cartridges in an exsiccator for example To avoid sediment intake make sure that the feed tubes do not touch the bottom of t
31. lution water concentration in mL H20 Distilled water is standard solution Tartrate Sodium tartrate 2 hydrate Std V Standard volume in mL EP Delay End point delay time during which the end point of the reaction must remain stable Drift L Maximum drift limit Max Vol Maximum volumes of the titration cell L Comment Comment lines No No Yes Yes up to 8 lines 27 Operation MAIN MENU 28 DISPLAY DATA Data log with up to 55 results refer to section 4 9 page 35 Empty Data Logger Empties the data log Display Data Display results with search filters By Date Display results by date By Sample ID Display results by sample ID By User Display results by user By Type Display results by titration or calibration Continue Display all results SYSTEM System settings refer to section 4 11 page 35 Reagent s Name Reagent name entry of no more than 10 characters Operator s Name Up to four operator names can be defined Operator 1 Operator name entry of no more than 17 characters Data Output Define the data output refer to section 4 10 page 35 Deactivated Deactivates the data output For Printer Activates data output on the printer For Computer Activates data output on the computer Volume Test Program for bure
32. n tube with antidiffuser unit black 14 Adapter for power supply 5 2xSolvent addition or suction tube with conical adapter 15 Hardware sleeve 6 Titration stand holder 16 Syringe plunger 7 Magnetic stirrer 17 Syringe body 8 10xwhite O rings for burette and pump threads 18 4xdesiccant cartridge 9 10x Teflon magnetic stirring bars 12 mm x 6 mm 12 Installation 3 3 Operating environment Note the following points so that the instrument will operate correctly and have a long service life Place the instrument firmly on an even surface Do not push any objects under the instrument e The ambient temperature must be 15 to 40 C 60 to 104 F The relative humidity should be less than 80 moisture should not condense on the instrument e A minimum clearance of 15 cm 5 9 in must be ensured above and on all sides of the device this allows the air to circulate and prevents overheating of the electric parts The dosage arm of the stepper motor operating the syringe piston must be able to move freely Do not operate or store the instrument in extremely dusty humid or wet locations Make sure that no liquids enter the instrument and immediately wipe away any liquids that contact the instrument Protect the instrument against vibrations direct sunlight corrosive gases as well as strong magnetic and or electric fields Only use genuine replacement parts and accessories e The instrument must be
33. nce to hold the liquid during the tests Printer for example CITIZEN CBM 270 connected to the titrator Volume test SF IW lp a mmr a 4 i Le 49 8 2 Execution Position the titrator next to the balance Clean the burette to remove any previously used reagents Make sure that the syringe and tubes are in perfect condition Fill the syringe with distilled water Fill a vessel with a little distilled water and place it onto the balance u Pe ee Ku Place the protective cover over the balance The burette discharge tube must extend into the vessel via a cannula 7 Select SYSTEM gt VOLUME TEST and follow the instructions on the titrator Enter the temperature and air pressure Note It is essential that all the dispensed water is transferred to the vessel on the balance Therefore the tip of the cannula must be lowered to the liquid surface after each dose The cannula is then withdrawn and the weight is read from the balance 8 Ifthe displayed results correction factors and standard deviations are within the permitted limits the titrator will function correctly Note Clean the burette with ethanol after the volume test Figure 17 Immerse the cannula O 2 50 Index B Burette tu io Di ea ne 13 D Data log civic 35 Data l6gg6ru one eee 5 E Empty obtenir iet ata 30 Error messages sss 41 F Flange tube connectio
34. nfirm the setting 4 2 2 First steps after installation 1 Prime the burette with titrant section 4 7 1 2 Prime the pump solvent to add the reagent section 4 7 2 3 Check the stirring speed section 4 7 3 4 Prime the pump waste to dispose the reagent section 4 7 2 4 3 Menu structure Note Section 6 Troubleshooting provides a list of all error and warning messages and also describes all necessary countermeasures 25 Operation MAIN MENU TITRATE Titration program to determine water content refer to section 4 6 page 31 P1 KF Standard Default setting of activated titration program Select Prg Changes the default setting P1 KF Standard KF Standard with automatic drift control unit P2 KF lt 1 H20 Titration program for very low water content P3 KF gt 10 H20 Titration program for high water content P4 KF Standard KF Standard unit mg mL Statistics Statistical calculation of results No No Yes Yes No of results Number of analyses Continue Preparation of titration cell Disp Solvent Dispenses new solvent into the titration cell Continue Starts the pre titration Continue Pre titration completed successfully the titration cell has been conditioned Start Titration Dispense the sample into
35. nnnnnnnnnnnnnnnnnnnnnnnnnnneninenss 29 445 Standby tino AR Re 30 4 4 6 Standard water SOlUtions nennen nnne nnne nenne nennen nnns 30 447 Empty the Uta bell cita tI ele ZR Shu oer tuus sa etai Does it 30 4 5 Cali rationed a sys 30 A doi 31 4 7 Manual component activation nennen nennen nennen nn nen nnne n nnne 33 47 1 BUT Eee etr ve ATA aie ene P meta ee AE dT YEN Ts 33 4 7 2 PUmps iste e ire eR AS qun daa e aan vane utet emat onu ade alare 33 ATS EA AA inue TL oU INI NEN 33 4 5 Programming qm artioli e etas ON elogio 33 4 8 1 Configuration of the calibration program u 33 4 8 2 Configuration of the titration programs 34 4 9 Data log m 35 AOA Printer COMpUlO EEEE T u u te E E sai tn 35 4 a ESAE EA PTT E EV E AE ES 35 4 12 Default Settings e c t 36 Section 5 Maintenance perde ALA e aa 37 5 1 Maintenance schedule een r 37 5 2 Power off the instrument cnn enn nennen nnne nsn nnn ener RR RR nnne nein nsns nnne 37 5 3 Clean the b rette i rr e Ever iaia iaa 38 5 4 Clean the electrode nara nennen 38 5 5 Replace PUMP tubes u uu e tete ee en pr convey e EI a A EX RR CR EA E GR Ra NUR RR NR S de ERR HEURE d 38 Section 6 Troubleshooting siinon A cut rte ep ue depu eec ante eu cade dua d a 41 OD Er
36. ns societies ipio bite e gie 16 K Karl Fischer titration 8 23 Keypad vic tg eui d deeds 21 M Magnetic Stitren u toit e t e Rog thin ext 15 Maintenance schedule ne 37 O One component reagent 23 P Peristaltic pump u aii adei iaaa 5 Power supply external 20 s Safety information UU R u a aD Iska 7 Scope of delivery u 11 Specifications seria date 5 T Titration Cell 2 32 id a 15 30 Titration program ne 8 Titration Stand comidas eere reete ornat 14 Two component reagent_ 23 W Warming labels ici iii alii 7 Vamings ata iaia cer nia 41 51 Index 52
37. on cell Titrate the water content of the sample Enter the sample amount Calculation of result The titrator calculates the water content of the sample with consideration of the measured drift factor and blank value Replace the solvent Multiple titrations can be performed with the same filling of the titration cell However a minimum methanol content of 25 and pH value between 5 and 7 is essential Karl Fischer titration is more complex than most other volumetric titration methods Note the following points in particular 4 4 3 Stirring speed Water is everywhere even in the air and unwanted water ingress will distort the results The pump controlled filling and emptying of the titration cell allows solutions to be replaced and dispensed without the need to open the titration cell The titration cell only needs to be opened briefly in order to dispense the sample The desiccant in the cartridges must also be replaced at regular intervals Select a stirring speed that ensures maximum mixing of the solutions without adding excessive amounts of air If the stirring speed is too slow this can distort the results overly fast stirring on the other hand can disrupt the actuation of the electrodes Set the required stirring speed during pre titration do not change it again during an analysis 1 Adjust the stirring speed by pressing the Navigation keys UP DOWN during the pre titration 444 Removal of bubbles Before t
38. on the right and left of the housing 3 Press the ends of the gripper clamps together with cover pliers for example and slide the clamps down and off the connectors Remove the tubes from the connectors 2 Remove the housing cover 4 Press in the catches on the right and left of the pump cassette Remove the pump cassette from the shaft 39 Maintenance 40 Section 6 6 1 Error messages Troubleshooting Error displayed Cause Resolution Factor value higher than 10 mg H20 mL The factor of the reagents varies between 1 and 5 mg mL Excessively high values indicate an anomaly of the sample or an error in the standard weight input Check the sample for side reactions Check the weight input High drift Drift higher than 30 uL min Tubes and burette are moist Sample displays interfering side reactions Sample only releases water slowly Titration cell is not closed correctly Drift too high Drift higher than 60 uL min Tubes and burette are moist Sample displays interfering side reactions Sample only releases water slowly Titration cell is not closed correctly Conditioning not possible If the message Drift too high is displayed for more than five minutes the process is cancelled Upon start up rinse all tubes using KF reagent Following titration of a sample use a special KF reagent that does cause any interfering side reactions with the sample Increa
39. own in the display Once the pre titration has been completed and the titration cell conditioned the text CONTINUE is shown in the display Press OK to confirm Dispense the sample into the titration cell Use a pipette to dispense liquid samples Viscous samples are dispensed with a syringe and solid samples with a weighing boat funnel Open the filler inlet in the titration cell lid and add the sample The filler inlet must then be closed immediately to avoid the ingress of air humidity which would distort the results 31 Operation 32 9 Select START TITRATION and press OK to confirm The titration begins in accordance with the selected program The titrator continuously determines the optimum rate of titrant addition After the titration WEIGHT ENTRANCE is shown in the display Note Need for entering weight depends on the result unit selected 10 Enter the weight of the sample via the keypad and press OK to confirm the entry Drift control is activated automatically the result is shown in the display and sent to the printer or computer if applicable 11 Press OK to confirm the result Further samples without emptying of titration cell Multiple samples can be analyzed with the same titration cell filling 1 To do so select CONTINUE and press OK to confirm 2 Dispense the new sample into the titration cell 3 Select START TITRATION and press OK to confirm After the titration WEIGHT ENTRANCE is shown
40. ration Sample has very low water content In the case of samples with a very low water content reproducibility greatly depends on prior handling preparation and addition of the sample Increase the sample quantity Water capacity of solvent exhausted Empty the titration cell and add new solvent Poor reproducibility of results Very small size of control sample Increase the control sample size Sample not homogeneous Homogenize the sample and increase the control sample size Sample has very low water content In the case of samples with a very low water content reproducibility greatly depends on prior handling preparation and addition of the sample Increase the sample quantity Very slow titration Sample only releases water slowly Increase the interval between dispensing of the sample and the start of titration Factor not reproducible or too high The employed standard is water The use of water as a standard requires extensive practical experience use a standard solution The employed standard is sodium tartrate 2 hydrate The reagent does not immediately dissolve in the solvent Increase the interval between dispensing of the sample and the start of titration The employed standard is a normal standard solution Make sure that the correct standard concentration has been entered Solution in titration cell turns brown Over titration Th
41. rew the bottle closure onto the solvent bottle bottle 2 Figure 9 Place the desiccant cartridge into the designated opening in the bottle closure Pick up a white tube with conical adapter Screw the tube into the OUT socket on pump 1 Insert the conical adapter into the designated opening in the lid of the titration cell The tube extends approximately 3 cm 1 2 in into the titration cell 17 Installation Figure 9 3 4 3 4 18 Connection of tubes for solvent 1 LA JA Connection of tubes for waste bottle 1 2 3 4 o mw A a Pick up a white tube with conical adapter Screw the tube into the IN socket on pump 2 Insert the conical adapter into the designated opening in the lid of the titration cell The tube extends to the bottom of the titration cell Note Make sure that the tube end doesn t hit the magnetic bar while stirring Pick up a white tube with bottle closure Screw the tube into the OUT socket on pump 2 Screw the bottle closure onto the waste bottle bottle 3 Figure 10 Place the desiccant cartridge into the designated opening in the bottle closure Figure 10 3 4 4 Electrode ue e IN em Installation Connection of tubes for waste bottle N 7 WE sw N r_T lt 2a_N Remove the red cap from the electrode connector Screw the electrode cable onto the electrode Remove the white cap from th
42. ror Mess ads s oem a uite eU ute o C wang apakuna Dc 41 O 2 Incorrect results anime sos 42 Section 7 Replacement parts and accessories 1 11 1 sss 43 TA Replacement parts cuiii iere teta i a ela EO EET LU aes 43 T2 CCOSSOFLIBS n seite O edes Fonte gau eeu Fas 43 Section 8 Contact information eee enne en hern nen n nennen nnn 45 Appendix A Weigh the sample a a rsarssssssss 47 Appendix B Volume testi Ac 49 Sc Required equipe nre t eee eb ep i E in ad d e RE C ERE EY 49 t 2 E Xr tne I IA sha Aa ua ua ANI 50 AE O O 51 Section1 Specifications These are subject to change without notice Performance specifications Measuring principle Volumetric titration according to Karl Fischer method for water content determination Measuring range Water content between 100 ppm or 0 01 and 100 H20 Factor 0 to 99 999 Resolution 0 10 H20 0 001 Resolution 10 100 H20 0 01 Programs 4 KF titration programs and 1 calibration program Languages English Spanish French and Italian Data logger Last 50 data records Date time DD MM YYYY Header text 2 lines of 40 characters each Memory Users Names of 4 users Comment text 8 lines of 40 characters each RS 232 C interface Communication parameters for scales Display 128 x 64 pt backlit liquid crystal display Keypad 7 membrane keys splash proof PET gt 6 million key pre
43. se the interval between dispensing of the sample and the start of titration Check that the titration cell is correctly positioned grease the filler inlets for the sample addition Check the O ring of the titration cell Check the desiccant cartridges Maximum volume reached The maximum volume is reached before the titration is completed The titration is cancelled automatically Empty the titration cell and restart the titration Value not calculable The result is outside the accepted limits Repeat the titration Data logger empty No results are stored or no results match the search filter Change the search filter function All data will be erased All data in the data log will be erased Printing error Printer is connected but not activated Switch on the printer PC not connected Computer is activated but not connected Check the computer connection 41 Troubleshooting 6 2 Incorrect results Incorrect results Cause Resolution The result differs from the expected value The sample reacts with the titration medium Check whether the sample contains interfering ions that react with the reagents Use a different reagent Sample only releases water slowly Increase the interval between dispensing of the sample and the start of titration The reagent factor is incorrect or has not yet been calibrated Perform a calib
44. sses Burette Resolution 1 40 000 of nominal syringe value at least 0 001 mL Dosing accuracy lt 0 2 if volume gt 10 of syringe volume Reproducibility of dosing 10 1 if volume gt 10 96 of syringe volume Material of syringe Borosilicate glass and PTFE 5 mL Material of electrovalve Material with liquid contact PTFE and KEL F Material of tubes Black tubes PTFE Reagent tubes White tubes PTFE Peristaltic pump Volumetric flow 170 mL min 15 Tube Novoprene internal diameter 3 2 mm Inputs and outputs Measuring electrode BNC connector Magnetic stirrer RCA connector cinch External keypad Mini DIN connector RS232 for computer or printer Telephone connector RJ9 RS232 for scales Telephone connector RJ9 Power supply external 24 VAC 1 25 A 30 VA Specifications Dimensions of measuring instrument and environmental conditions Enclosure material ABS and enameled steel Mass approximately 4 kg Dimensions 130 x 160 x 300 mm Working temperature 15 to 40 C 60 to 104 F Storage temperature 10 to 50 C 14 to 122 F Air humidity lt 80 relative humidity non condensing Warranty Warranty 2 years Section 2 General information 2 1 Safety information 2 1 1 Please read the entire user manual carefully before the equipment is unpacked set
45. the titration cell and start the titration Weight Entrance Enter the weight of the sample Result Displays the result STANDARDIZATION a program for exact titer determination of titrant refer to section 4 5 Statistic Statistical calculation of results No No Yes Yes H20 mg mL Entry of water content of standard Continue Preparation of titration cell Disp Solvent Dispenses new solvent into the titration cell Continue Starts the pre titration sion Dispense the standard into the titration cell and start the titration Result Displays the result Accept Result Saves the factor for all titration programs Repeat Sample Starts another calibration MANUAL ACTIVATION Select which element is to be controlled manually refer to section 4 9 page 35 Burette Manual control of burette Return Empties the burette into the titrant bottle navigation key LEFT Empty Empties the burette into the titration cell navigation key UP Fill Fills the burette with titrant navigation key DOWN Pumps Manual pump open loop control Empty Vessel Activates pump 2 empties the titration cell into the waste bottle Dispense Solvent Activates pump 1 dispenses solvent into the titration cell Start Actuation Exit the menu Sets the stirring speed Stirrer Select ON OFF with OK Select the stirring speed with UP DOWN 26 Operation MAIN MENU PROGRAMMING P1 KF Standard Individual adjustment of saved programs refer to section
46. tirring speed by pressing the Navigation keys UP DOWN If required Once the pre titration has been completed and the titration cell conditioned the text CONTINUE is shown in the display Press OK to confirm Dispense the standard solution into the titration cell and press OK to confirm The titration begins the titrator continuously determines the optimum rate of titration addition Once the titration has been completed the drift control is activated The result is shown in the display and sent to the printer or computer if applicable Press OK to confirm the result To save the factor for all titration programs including inactive programs select ACCEPT RESULT and press OK to confirm A new calibration can be started with REPEAT SAMPLE Following successful calibration the titration cell is ready for sample analysis Select TITRATE and press OK to confirm Select the titration program if more than one program is activated Select STATISTICS gt NO or YES to perform a statistical analysis If YES is selected enter the number of analyses The absolute and relative standard deviation is shown Select CONTINUE and press OK to confirm If you require a new solvent filling select DISPENSE SOLVENT and confirm with OK The solvent is dispensed into the titration cell Select CONTINUE and press OK to confirm The pre titration starts automatically The water content of the solvent and the drift are determined WAIT is sh
47. to confirm AUTOMATIC a maximum drift limit of 30 uL min must not be exceeded A sample cannot be added before the drift limit is met The drift limit can be changed MANUAL a sample can be added at any time If the drift control takes more than 15 minutes the process is stopped automatically and the titrator switches to the standby cycle 4 9 Data log Operation 8 Select UNIT to define the results output The following units are available for selection mL mg ppm A U volume and A U weight Press OK to confirm 9 Select L COMMENT gt NO or YES to enter comments Press OK to confirm If YES is selected up to eight comment lines can be defined using a standard keyboard This text is displayed in printouts This section describes the functions of the data log e Up to 55 titration or calibration results are stored e The results can be displayed printed or sent to a computer When the data log is full the oldest result is overwritten automatically 1 Select DISPLAY DATA gt DISPLAY DATA and press OK to confirm A range of search filters can be used to display the results X all BY DATE displays the results for a specific date BY SAMPLE ID displays the results for a specific sample BY USER displays the results obtained by a specific user BY TYPE displays either titration or calibration results CONTINUE displays all results 2 To empty the data log select DISPLAY DATA gt EMPTY DATA LOGGER and pr
48. tte calibration and control Temperature Entry of temperature Pressure Entry of air pressure Weights E Entry of weight Manual Manual weight entry Automatic Automatic weight entry via scales connection Operator Operator name entry of no more than 17 characters Start Test Starts the volume test Entry of weights Type of weight entry Weights E Entry of weight Manual Manual weight entry Automatic Automatic weight entry via scales connection Baud Rate Entry of baud rate 1200 2400 4800 9600 19200 Word Length Entry of word length 8 or 7 Parity Selection of parity none even odd Stop Bits Number of stop bits 1 or 2 Continue Return to system menu Standby Cycle Entry of standby interval Time D Solvent Time during which the solvent is dispensed into the titration cell Date Hour Entry of date and time Display Contrast Selection of display contrast Language Selection of operating language SPANISH ENGLISH ITALIAN FRENCH Operation 44 General information on KF titration 4 4 1 Individual titration steps Regardless of whether a one or two component reagent is used the titration process involves the following steps 1 2 1 o Aa a 4 4 2 Titration cell Fill the burette with titrant Fill the titration cell with solvent Pre titration Water traces added via the solvent are removed The titration cell is conditioned Dispense the sample into the titrati
49. ulations and wear appropriate personal protective clothing for eye face hand body and or respiratory protection Make sure that the tubes are never kinked Regularly check the system as well as all tubes and connections for leaks condition and cleanliness To prevent twisting of the tubes you should always connect flange tube connections before those with grommets 3 4 3 1 Removal of protective stickers 1 Remove the protective stickers on the burette valve and the four pump connections 2 Make sure that the pre installed white O rings are not removed 3 Check that the O rings are in a horizontal position inside the thread Figure 7 Position of protective stickers 3 4 3 2 Connection of tubes for KF titrant 1 Screw the black burette feed tube onto the valve 2 Screw the bottle closure of the feed tube onto the titrant bottle for the KF reagent bottle 1 Figure 8 Place the desiccant cartridge into the designated opening in the bottle closure 4 Screw the black burette discharge tube onto the valve Insert the conical adapter with the antidiffuser unit of the discharge tube into the designated opening in the lid of the titration cell 16 Installation Figure 8 Connection of tubes for KF titrant 3 4 3 3 Connection of tubes for solvent A OO P I Pick up a white tube with bottle closure Screw the tube into the IN socket on pump 1 Sc
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