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TitraLab 550 Volumetric Karl Fischer Titrator

1. 34 Accessing KF cell functions during a UMN OM e 35 4 Programming and running eese ee eere AY SUS 37 Programming the KF reagent library seeeeneene 37 Programming a KF Titration seem 43 Performing a titration unco aee t rere rr tere tha riget kx d 51 Pre programmed methods sssseeeenn 59 Contents 1 ROJO CUING P 61 ACCO UNO TE 61 EEE E e T E T E a Ea uA R ER ea Eos 62 TOGON nir cneeiaacae uence see sbeteenaaidentexetus subtecsvaneceiatberveneernaes 63 SUCCESSIVE TATIONS wise uscito ton tex Eee Re lett pha Eee dae aaa a 65 GLP fable vesn ative tae einer tities ict ane a aae n aE E aE 66 PATOU C 71 6 Connection of peripherals e eeeeee eene 77 Connection of PG et tt th eura te uae v tue xe esu do 77 Connection of a printer ssssssssssseseeeeeenenenen nnn 79 Connection of a balance sssssssssseeeeeee eene 80 Connection of keyboard and bar code reader suusss 84 Keyboard functions sess 85 7 Troubleshooting oett notante n sasdo tanken noraen 67 Changing the battery ssssssssssssssseeeeen nennen 87 Replacing the fuses ssssssssesssssseseeeeeeennnene enne 88 Dismounting the pump module seseeeenns
2. Edit Method 10 Method 10 Copy from Reset Copy from TONOO2 445 Confirm lt Yes gt No Method ID ABCDEFGH Use Oven Yes lt No gt s Autostart Yes lt No gt The table on page 44 gives the definition Blank of each parameter Yes No Uncert calc Yes lt No gt gt If Uncertainty calc Yes Reproducibility 10 Edit Edit Edit lt Parameters gt lt Sample gt lt Blank gt Enter titration method data in each menu At the end of each menu press V to return to the start Programming and running analysis 4 3 Definition of parameters Parameter Range available Default value Description Autostart Yes or No No The Autostart function enables the TIM550 to automatically detect the addition of sample to the KF Cell The titration will start as soon as the water is detected in the sample whichever option is selected Yes or No When No is selected and water is not detected after sample injection slow release of water then titration can be started manually by pressing v Blank Yes or No No Set to yes to create a titration method using a blank Method ID A to Z 0 to 9 blank space Use A Z to enter the ID Reproducibility 0 to 999 99 10 Appears if Uncert calc Yes in the method If you are to perform only one titration enter the reproducibility of the resu
3. 9999 999 mg ml This is a Quality control parameter setting Quality control Yes Set the maximum acceptance range for results An alarm message will apear if the result lies above this value Minimum blank 0 001 to maximum blank 0 001 mg ml This is a Quality control parameter setting Quality control Yes Set the minimum acceptance range for results An alarm message will apear if the result lies below this value 50 Chapter 4 Performing a titration Procedure 1 oa F wo LW Setup up the titration system as described in the Installation Sheet part no D26T019 Prepare the burette refer to chapter 3 Add solvent to the fill mark on the KF cell refer to chapter 3 Prepare your sample refer to page 52 Press the Method key and select the method using the arrow keys Press Run to start the method To perform a calibration refer to page 55 To perform a blank titration refer to page 56 To perform a KF titration refer to page 57 To perform a KF titration using an oven refer to page 58 To perform one of the 10 pre programmed methods refer to page 59 Programming and running analysis 5 1 Weighing the sample For the connection of a balance refer to chapter 6 Liquid samples using the weight by difference method Liquid samples can be injected into the KF cell with a syringe through the exchangeable septum stopper 1 2 Fill the syringe with s
4. Thecell volume is above the maximum authorised level to avoid overflowing 34 Chapter3 Accessing KF cell functions during a titration It is possible to access the following functions during a titration i e before introducing the sample to the KF cell or before confirming a repeat analysis Use Pump v i Mol Sieve gt W Press Cell and select the required function lt Pump gt lt Stirrer gt or lt Mol Sieve gt You can then empty the KF cell add solvent and or change the stirring speed Select Return titr gt to return to the ongoing titration Manualfunctions 3 5 36 Chapter 3 4 Programming and running analysis Programming the KF reagent library Press for 3 seconds Burette Enter Code Enter the protection code if the edit mode has been protected Refer to page 18 KF reagent no Select the reagent no 1 to 20 Edit an existing reagent Copy an existing reagent Reset selected reagent Reagent 2 Reagent 42 Edit Copy from gt Copy from COMP 2 4 Confirm Yes No Reagent lt 2 gt lt Reset gt KF reagent ID ABCDEFGH Program a calibration procedure Enter the titre manually KF reagent titre KF reagent titre lt Calibrate gt lt Enter gt 2 ese SO Definition of parameters page 39 Cal every 7 days z Reproducibility Available when Uncert calc yes 10 Edit Edit lt Parameters gt lt Standard gt Enter KF reagent dat
5. 89 Error and warning messages ssssseseeeenn 90 8 M241P12 8 Double Platinum Electrode 97 9 General information ioosenienucssnn antenas nao nip nana oon cane 99 SPSCIICAL OMS eveisis 99 Transporting the TIM550 ssseen enn 103 Sp M 103 Disposal of Karl Fischer reagents sss 103 Cleaning the TIM550 ssssssssssssseeeneneen nennen 104 Regenerating the molecular sieve sesseeese 104 International Standards sssssssssseeeeeeennns 105 2 Contents 1 Introduction The TIM550 Volumetric Karl Fischer Titrator from Radiometer Analytical is especially designed for water analysis in many sectors including the pharmaceutical oil and food industries On the TIM550 Volumetric Karl Fischer Titrator burette pump for safe solvent handling titration stand and keyboard are all integrated in one compact unit To speed up maintenance and guarantee reproducible titrations the TIM550 is equipped with the new Bayonet cell This is designed with a special L shaped slot so that electrodes fit into place in a single easy movement The Bayonet concept keeps all parts completely moisture tight during use with no risk of leakage or water entering the cell The TIM550 increases analysis throughput by keeping your cell ready for immediate use An automat
6. SA Press V to view Press v to end statistics cycle 9 runs mg mL 10 runs mg mL 10 runs mg ml 4 006 0 002 A 4 006 40 002 A 4 006 0 002 Accept result No Accept result Yes The titration has been performed 10 times The mean result is displayed See chapter 5 Programming and running analysis 5 7 KF titration with oven Run method Oven 5 wv Preliminary titration User ID ABCDEFG v Sample ID ABCDEFGH P4 Sample no 5 v Advised amount 1 000 g v Introduce sample into cold zone Vv Sample amount 1 000 g Drift ST 59 9 ug min Addition of sample Introduce sample into warm zone Titration 2 254 mg ml 500 ug min 00 10 Calculate result ABCDEFG 1 3 554 mg ml W Press VW Accept result Accept result Yes No WV Yes No WV T 1 i i TE Press to reject ___ the result Press W to view statistics 9 runs mg mL 10 runs mg ml 4 006 20 002 A 4 006 0 002 A Accept result No Accept result Yes 5 8 Chapter 4 Select method no 1 to 50 Press Run to start the titration Appears when selected in setup menu Appears when selected in the Edit lt Sample gt menu The TIM550 indicates the sample amount required for the titration Weigh approximately this amount into the boat Introduce the sample into the oven Enter the exact amount of sample Range available 0 001 to 9999 999 Drift display Introduce the sample into the oven Analysis cycle Live measuring
7. lt Blank gt v Accepted result 10 Blank no Press gt 12 Mean result Press for date and time 10 Blank mg ml 4 325 0 001 all cases Time 15 20 10 Date 3FEB1999 10 Mean 4 522 mg ml 0 003 10 Mean 10 runs Rejected result 10 10 Reject mg ml 8 732 0 004 Blank no kkkkk 68 Chapter 5 KF reagent GLP Run method Select method no 1 to 50 B222 4 w Press GLP Method no 4 Press V to view results KF reagent V Calibration procedure Accepted result 9 ID Std no Pres gt f 9 cal mg ml Press for date and time KF002 5 5 002 20 002 Mean result all cases 9 Date Time 10FEB1999 09 12 9 Mean mg mL 5 154 0 003 9 ID Mean KF002 6 runs t expanded uncertain Rejected result P y 9 9 Reject mg ml 3 001 0 003 ID Std no KF002 kkk kk Manual entry 12 Enter mg ml 12 Date Time 4 989 0 002 16MAR1999 12 17 If the titre is entered manually the uncertainty values which appear in the GLP table are double those entered during programming This can be explained by the fact that the uncertainty entered is the standard uncertainty u whereas the uncertainty displayed in the GLP table is the expanded uncertainty U U uxk k coverage factor Refer to Guide to Uncertainty Calculations R31T009 Resultsand archives 6 9 Resetting the GLP table F
8. programming on the balance please refer to balance operating instructions The following balances can be connected to the TIM550 Balance Type Cable Cable part no length Mettler PE option 016 A95Z201 1m AE option 012 or 011 A95Z205 2m AM PM SM AT MT UMT PJ AJ A95Z206 1m Sartorius MasterPro A95Z202 1m QC MP8 4 A95Z204 2m See page 82 for the pin layouts of the cables 80 Chapter 6 Note cables can be made to your desired specifications Please contact our sales representative if you require information regarding the type of cable to use with your balance Format of messages accepted by the TIM550 Messages end LF or CR LF Units g mg kg The character g of the unit is required to mark the end of the data recognised by the instrument Spaces are ignored The number of characters situated between the first character in the message and the g in the unit must not be more than 30 spaces not included The number of characters received after the g and before the end of the message LF is insignificant The numeric data corresponding to the weight must be transmit ted before the unit Example of a message transferred from a balance type Mettler S I 1 2 3 4 5 6 g CR LF data received 12 3456 g IMPORTANT The units selected in the TIM550 must be identical to the units used by the balance Con
9. the date 1 Using A Z enter the day Press W to move to the month 2 Using the arrow keys enter the month Jan Feb Mar Apr May etc Press W to move to the year 3 Using A Z enter the year Choosing the language Choose your language for displays and printouts from the list available Use the arrow keys to select the language desired Choosing the keyboard type An external PC keyboard can be connected to the 6 pin mini DIN socket situated on the right hand side of the TIM550 Using the arrow keys select your keyboard type Refer to Chapter 6 for information on keyboard functions Selecting printer type and printout format Select 80 columns printer gives a detailed printout of results Select 40 columns printer gives a condensed printout of results Select No if a printer is not connected Refer to Chapter 5 Getting started 1 9 Keyboard beep Select Yes the TIM550 will emit 3 beeps when a result is obtained and 1 beep when the cell is ready to receive the sample Select No to cancel all beeps Entering Instrument Electrode and Burette ID Instrument ID A XXXR123N456 v The instrument ID is defined during manufacturing therefore it cannot be changed Electrode ID A XXX YY ZZZ VW For Radiometer Analytical electrodes the ID is given as follows XXX month YY batch number ZZZ electrode number Burette ID A XXXR125N456 W Use A Z to enter the i
10. the maximum titration time titration time setting in the time entered in the edit method menu or the KF menu edit has elapsed reagent library Alarm Tmax before the titration has ended Press Run to perform au new titration A result is obtained with the alarm message Tmax Alarm low This message is displayed if If necessary check the the Quality Control option has mininum and maximum Alarm high been selected in the edit values entered in the edit menus For a reagent calibration refer to page 41 For a KF titration refer to page 48 Press W to accept or reject the result The use of this instrument may jeopardise the security of all living beings uses that may for example cause burns and electric shocks These are considered as being improper and are there fore forbidden Troubleshooting 9 5 96 Chapter 7 8 M241Pt2 8 Double Platinum Electrode The M241Pt2 8 Double Platinum Electrode is specially designed for use with the TIM550 Volumetric KF Titrator Preparing for measurement 1 Remove the protection cap from the electrode 2 Before starting a measurement rinse the electrode with a suitable solvent 3 Check that the electrode body and sensing elementare not damaged 4 Place the electrode in the KF cell 5 When stirring make sure that the platinum wires are covered by the solvent Cleaning and maintenance Platinum wires In order to have reproducible and accurate results wi
11. 0 001 to 1 000 The sample factor is used when 9999 999 it is necessary to correct a result Example 10 g of sample containing two components 5 g A 4 5 g B are added to the KF cell A contains no water B water content unknown In order to calculate the water content of B enter a sample factor of 0 5 Result unit If sample g mg ug g The result unit will appear with unit ul ml mg ml g l the result at the end of titrations ug ml Result unit If sample g mg ug g The result unit will appear unit mg g g kg with the result at the end of mg g ug g titrations ppm mg kg Number of digits 3106 5 Select the number of digits to be displayed in the result at the end of the titration Quality control Yes or No Yes This is the quality control option It will help you determine whether or not you should accept or reject a result Select Yes to enter an acceptance range See minimum and maximum values on next page Programming and running analysis 4 7 to 9999 999 Parameter Range Default Description available value Minimum value 0 001 to 0 001 ml This is a Quality control maximum value parameter setting Quality control Yes Set the minimum acceptance range for results An alarm message will appear if the result lies below this value Refer to chapter 7 Maximum value minimum value 9999 999 ml This is a Quality control parameter setting Quality control Yes S
12. 019 and start mounting your system If you intend to work with a method which is already stored in the TIM550 you may immediately proceed to chapter 5 page 51 Getting started 5 Rear panel Figure 1 rear panel of the TIM550 1 Check that the voltage selection switch setting 115 V 230 V corresponds to the mains voltage If not use a suitable tool to move the required voltage to the arrow 2 Connect the mains socket of the TIM550 to the mains supply using the line cord 230 V Euro or 115 V If the TIM550 is to be used in the USA with a 230 V supply the tandem blade attachment plug cap must be used part no 615 405 3 When setting up the instrument for the first time it is necessary to install the battery delivered with the system refer to chapter 7 4 Connect the M241Pt2 8 Double Platinum Electrode to the socket marked ELECTRODE INPUT 5 RS232C PC PRINTER port for connection of printer or a personal computer 6 RS232C port for TIM550 interconnection 7 A balance can be connected to the TIM550 via the RS232C BALANCE port Refer to chapter 6 Note an external keyboard or bar code reader can be connected to the TIM550 via the 6 pin mini DIN socket situated on the right hand side of the instrument refer to chapter 6 6 Chapter 2 Adjusting the contrast The contrast of the TIM550 s display can be adjusted by means of a screw located on the bottom of the TIM550 By turning the screw clock wise or anticlockw
13. 5 Programming and running analysis 5 5 Blank titration Run method A B222 4 v Run blank B222 4 A Preliminary titration User ID ABCDEFG v Blank no 1 v Drift ST 59 9 ug min Addition of blank Introduce blank 1 000 mL P4 Blank amount 1 000 mL P4 Titration 3 001 mg ml 500 ug min 00 10 Calculate result ABCDEFG 1 4 005 mg m L WV Select method no 1 to 50 Press if the option Blank Yes is selected Press Run to start the blank determination Appears when selected in setup menu The TIM550 automatically increments the blank no each time a new blank analysis is performed Drift display Introduce an approximate amount of blank into the KF cell If the lt Autostart gt function has been selected the TIM550 will immediately start the titration Enter the exact amount of blank Range available 0 001 to 9999 999 Live measuring display showing the volume of titrant delivered titration speed and time from the start of the titration 3 result beeps are sounded as soon as the end point is reached if Beep is selected in the setup menu The name of the method blank no result and units are displayed Follow the procedure given on page 55 To repeat an analysis cycle To accept reject a result To view statistics 5 6 Chapter 4 KF titration Run method A Select method no 1 to 50 Fuel oil 41 w Press Run to start the titration Preliminary titration
14. 550 returns to the burette menu display Manualfunctions 2 7 Dismounting the burette IMPORTANT prior to dismounting the burette from the burette stand the burette must be rinsed using the Rinse procedure from the burette menu 1 If necessary press the Burette key and select Fill The Fill procedure ensures that the piston is in its lowest position 2 Run Burette exc procedure when prompted to do so see below Turn the burette a 1 4 of a turn anti clockwise Slide the burette off the stand in order to free the piston shaft Warning The calibration certificate supplied with a calibrated burette will no longer be valid if the burette stand is replaced or any parts dismounted Please contact your Radiometer Analytical representative to recalibrate the burette Burette exchange procedure If the burette stand has been replaced or dismounted the calibration data is no longer valid This procedure allows you to reset the calibration parameters of the burette stand if it has been replaced or dismounted The TIM550 will therefore use the default parameters Burette Press V to start the procedure The Stand by is deactivated Burette exch gt y The burette starts emptying into the Burette busy contents of the KF cell into the waste bottle When the emptying is over the y to stop burette is filled with air and the piston returns to its lowest position Replace burette Press V after burette replaceme
15. A new calibration is required The delay entered in the Cal every display has elapsed see page 39 Select lt New Cal gt and press V to start the calibration procedure Select lt Continue gt and press v to continue the titration using the current reagent titre Note this choice is not available if the user has entered a protection code in the setup menu The user is therefore forced to perform a new calibration by pressing Vv Check solvent level There is no solvent in the KF cell Press Cell and add solvent Select Return titr gt to continue the titration Enter titre Yes No This message appears when the option KF reagent titre Entered Either the KF reagent GLP is empty or the titre stored in the GLP was determined using the calibration procedure Select lt Yes gt and press V to enter KF titre manually Select No and press v to return to the method menu H20 displayed in the drift display Excess water in KF cell The TIM550 will add reagent until the drift reading is stable One beep is sounded to indicate that the cell is ready for titration Troubleshooting 9 3 Message Problem Action I2 displayed in the drift display Excess iodine in KF cell This generally indicates that the maximum burette speed is too high If conditioning of the KF cell takes some time 1 Inject a few ul of water into the cell 2
16. A or Z to change the alpha numeric data The left and right arrow keys are used to 1 Move the cursor left or right 2 Selectanoption which appears within the arrows on the display Note if a chain of characters has already been entered pressing the right arrow key will position the cursor at the end of the chain pressing the left arrow key will position the cursor at the beginning of the chain The up and down arrow keys are used to move up and down in the edit mode displays IMPORTANT the down arrow key can be used to accept a non stable drift reading thus continue to the next step if the reading is inferieur to drift threshold parameterentered during programming Getting started 1 3 Check mark The Check Mark V is used to Start a direct access function i e Burette Fill To confirm a display during sample analysis thus continue to the next step To accept a result during reagent calibration and sample analysis Printout data results and GLP tables 14 Chapter2 Entering alphanumeric characters Using the TIM550 keypad For example enter the name of a method Method ID OIL432 4 1 Use the right and left arrow keys to position the cursor in the text 2 Use A Z to enter the alphanumeric characters Note 16 characters can be stored to identify the method the last 8 characters are displayed The method ID is longer than 8 characters Arrows at the beginning and end of t
17. Dimensions H x W x D 380 x 230 x 450 mm excluding tubings Languages English French German Danish Spanish and Italian 100 Chapter9 KF cell lt 178 ml overflow level 140 ml of titrant max allowable level 120 ml normal maximum level WARNING 40 ml fill mark 40 ml mpm m 85 ml min immersion level 35 n Pneumatic module Approximate filling time Working cell volume 35 ml approximately 5 seconds Approximate emptying time Total cell volume 140 ml approximately 10 seconds Minimum needle length required 115 mm Functions Solventaddition Moisture protected by dessicant cartridge Protected against KF corrosive vapours Solvent waste push button commands Timer on cell emptying function Generalinformation 101 Burette Syringe volume 10 ml Resolution over 18 330 steps Trueness lt 20 ul Trueness the closeness of agreement between the average value obtained from a large series of test results and an accepted reference value Precision 7 ul Precision the closeness of agreement between independent test results obtained under stipulated conditions Maximum filling time Total burette volume 20 seconds Maximum empting time Total burette volume 30 seconds Functions Flush Fill Empty Rinse Titrant exchange procedure Glass syringe with plastic cover UV protected PTFE piston According to ISO 5725 1 1994 edition and IS
18. O 3534 1 1993 edition 102 Chapter9 Transporting the TIM550 Always use the packaging supplied by the manufacturer IMPORTANT Remove the metal rod before transporting the TIM550 Never pick up or carry the TIM550 by the metal rod Servicing DO NOT ATTEMPT TO SERVICE THIS PRODUCT YOURSELF except as noted in this manual For servicing please contact your Radiometer Analytical representative at the address given below or Or Radiometer Analytical SAS 72 rue d Alsace 69627 Villeurbanne Cedex France Tel 33 0 4 78 03 38 38 Fax 33 0 4 78 68 88 12 E mail radiometer nalytical com Warning we accept no responsibility when using the TIM550 and its peripheral devices under conditions that are not specified in this User s Manual Disposal of Karl Fischer reagents Dispose of Karl Fischer reagent and cleaning solutions in a proper manner Refer to the saftey data sheets for the reagents to identify chemical hazards Follow all local regulations regarding the disposal of chemical wastes Generalinformation 103 Cleaning the TIM550 The exterior surface of the TIM550 can be cleaned with a soft cloth and tepid water In the case of spillages from the titration cell or waste bottle itis recommended to clean the surface with the KF solvent e g Hydranal solvent Regenerating the molecular sieve If you are using a one component reagent itis necessary to regenerate the molecular sieve once a week For two compo
19. Press Cell and add some solvent to the cell Select Return titr gt to continue the titration 3 Decrease the burette speed see page 45 Perform Cal Yes No This message appears when the option KF reagent titre Calibrated Either the KF reagent GLP is empty or the titre stored in the GLP was entered manually Select lt Yes gt and press V to start to the calibration procedure Select No and press v to return to the method menu Cell not available This message is displayed at the start of a titration if the KF cell is in the process of emptying Wait until the KF cell has finished emptying Press Run to start the titration Printer not available This message is displayed if the printer is off line Turn the printer on line and press V to continue 94 Chapter 7 Titration end errors Message Problem Action Maximum volume reached This message is displayed if thec maximum volume of titrant is delivered before the end point is reached No result obtained Change the Maximum volume setting in the edit method menu or the KF reagent library or decrease the sample amount Press Run to perform a new titration Maximum time This message is displayed Change the Maximum menus for a titration or a calibration The final result is above Alarm high or below Alarm low the QC parameter setting reached if
20. TR 4 8 CTS GND 5 5 GND DSR 6 7 RTS RTS 7 gt 6 DSR CTS 8 4 DTR 9 9 DTE Female 9 pin Female 9 pin 78 Chapter 6 Connection of a printer For the connection of a printer use the cable 9 25 pin part no A95P201 The printer must have the following characteristics for connection to the TIM550 Printer 40 or 80 characters e RS232C interface 9600 baud no parity 8 data bits 1 stop bit e Flux control via the DTR line pin 20 on the 25 pin plug e Printout of tables IBM Fonts character sets ma jf gt 2m A95P201 Printer TIM550 1 1 RxD 2 e 2 TxD TxD 3 3 RxD DTR 4 5 CTS GND 5 7 GND DSR 6 4 4 4 RTS RTS 7 6 DSR CTS 8e 20 DTR 9 DTE DTE Female 9 pin Male 25 pin Note to connect the Kyoline MTP640 Thermal Pocket Printer part no A70P020 230 V A7OP021 115 V use the cable 5 9 pin part no A95X506 Connection of Peripherals 7 9 Connection of a balance RS232C specifications 9 pin sub D connector 2400 baud even parity 7 data bits 1 stop bit Pin connections 1 5 1 No connection 2 Receiving Data input RxD 3 Transmitted Data output TxD 6 9 4 Data Terminal Ready output DTR 5 Ground GND 6 No connection DSR 7 Request to Send output RTS 8 Clear to Send input CTS 9 No connection Balanceconfiguration automatic transmission autosend or autotransmit Communication may need some
21. TitraLab TIM 550 Volumetric Karl Fischer Titrator User s M anual D21T028 D21T028 Printed by Radiometer Analytical SAS France 2004 071 All rights reserved Approved Quality System RADIOMETER ANALYTICAL SAS 72 rue d Alsace 69627 Villeurbanne Cedex France E mail radiometer nalytical com Web www radiometer analytical com Tel 33 0 4 78 03 38 38 Fax 33 0 4 78 68 88 12 Contents DN EPOGUCUION T 3 PAPE Ell M A 5 ROOM PANG sses eE 6 Adjusting the contrast eesseseenne nnn 7 Changing the selected source voltage ssessssssss 7 Setting up the Bayonet KF Cell with accessories X91T003 8 TIMS50 front panel 2 ci aee e reete eee tae ranae 11 Description of keys esses eene nnne 12 Entering alphanumeric characters sssseees 15 Deleting alphanumeric characters sseeeeene 15 The Setup menu sssssssssssssssesesenee ener nnns 16 Programming the Setup menu sssssssseeeeeennnne 18 Uncertainty calculations sssssseeeeeennnn n 21 3 Manual functions iosuisiiiin onsite auno tana staat sa ua nnn a Rana nur udn 23 B rette fUfictlOris essiri bte te ER acta rere teda xerit 23 KF cell f lctlons siano coercere hes pete test iineee ds ees 30 PUMP TUMCUONS RD 31 Automatic moisture drift compensation Stand by
22. User ID Appears when selected in the setup menu ACO v Sample ID Appears when selected in the Edit lt Sample gt menu ABCDEFGH v Sample no The TIM550 automatically increments the lt 3 gt v sample no each time a new sample analysis is performed Drift The moisture drift compensation can be followed by ST 59 9 ug min means of the drift reading and the STABility indicator When STAB is displayed one beep is sounded to indicate that the cell is ready Addition of sample Introduce sample Introduce an approximate amount of sample into the KF cell 1 000 mL y If the lt Autostart gt function has been selected the TIM550 will immediately start the titration Sample amount Enter the exact amount of sample Analysis cycle 1 000 mt Range available 0 001 to 9999 999 Titration Calculate result 3 001 mg ml Live measuring display showing the volume of titrant 500 ug mn 00 10 delivereg titration speed and the time from the start of the titration 3 result beeps are sounded as soon as the end point is reached if Beep is selected in the setup menu The name of the method sample no result and units are displayed ABCDEFG 3 4 005 mg ml WV Press V to accept the result The result is automatically transferred to GLP Sample Press V Accept result Accept result Repeat analysis Yes No Wv Yes No Wv Yes No Vv Press v i NE Press v to reject Repeat analysis the result Ves
23. YDRANAL Solvent Acetic acid HYDRANAL Titrant 5 40 ml HYDRANAL Solvent Cetone HYDRANAL Composite 5K 40 ml HYDRANAL Working Medium K Mayonnaise HYDRANAL Titrant 5 40 ml HYDRANAL Solvent CM or 15 ml HYDRANAL Solvent 30 ml chloroform Cereals HYDRANAL Titrant 5 40 ml HYDRANAL Solvent Programming and running analysis 5 9 60 Chapter4 5 Results and archives The TIM550 automatically calculates the water content of the sample in the chosen units The drift measured from the start of the titration the quantity of water introduced by the solvent and the dilution parameters are also taken into account during calculations If a series of measure ments is performed the TIM550 will calculate the mean value the standard deviation and the uncertainty on the mean value The user is able to accept or refuse the last result obtained and check the impact it might have on the mean result Accepting Press V The result is automatically transferred to the GLP table OIL 432 2 12 34 mg ml W Rejecting From the result display at the end of the titration OLL 432 2 Press V 12 354 mg ml W Accept result Select No and press v The rejected result is automatically Yes No vv transferred to the GLP table for consultation Resultsa nd archives 6 1 Viewing statistics From the result display at the end of the titration OIL 422 Pres
24. a in each menu At the end of each menu press V to return to the start Programming and running analysis 3 7 KF reagent library The KF reagent library has the possibility to store calibration data for up to 20 different Karl Fischer reagents Important whichever titrant is selected is used for all methods To change titrant refer to the KF titrant replacement chapter 4 Do not forget to select your titrant from the reagent library no 1 to 20 and if necessary determine the titre You have two possible ways to introduce the titre 1 Performa calibration Select lt Calibrate gt when programming the KF reagent library Start the calibration procedure in the burette menu refer to page 55 2 Enter the titre manually Select lt Enter gt when programming the KF reagent library Enter the KF reagent titre in the burette menu refer to chapter 3 As the KF reagent quickly deteriorates with time Radiometer Analytical recommend frequent calibrations to ensure optimal accuracy 3 8 Chapter 4 Definition of parameters Parameter Calibration Range Default Description type available value Autostart Calibrate Yes No No When activated the Autostart function enables the TIM550 to automatically detect the addition of sample to the KF Cell The titration will start as soon as the water in the sample is detected Cal every Calibrate 1 to 99 7 days Enter a calibration reminder The TIM550 will prompt you
25. al no b Electrode serial no C KF reagent titre d Blank Resultsa nd archives 7 5 Edit method data 1 Select the Method 1 to 50 2 Press Method for 3 seconds to enter the edit mode 3 Press Print You will obtain a printout of the method menu parameters Edit KF reagent calibration data 1 Press Burette for 3 seconds to enter the edit mode 2 Select the KF reagent titre 1 to 20 3 Press Print You will obtain a printout of the parameters used for the calibration procedure 76 Chapter 5 6 Connection of peripherals The TIM550 Volumetric KF Titrator is equipped with terminals for connec tion of Printer PC balance PC keyboard bar code reader and platinum electrode The terminals in the rear panel are illustrated in chapter 2 Connection of PC RS232C specifications 9 pin sub D connector 1 5 Pin connections 1 No connection 2 Receiving Data input 6 9 3 Transmitted Data output 4 Data Terminal Ready output 5 Ground 6 No connection 7 Requestto Send output 8 Clear to Send input 9 No connection RxD TxD DTR GND DSR RTS CTS For the connection of a personal computer use the cable 9 9 pin part no A95X501 See page 78 for the pin layouts of the cables Connection of Peripherals 7 7 Pin layout of the A95X501 cable ma jf gt 2m A95X501 TIM550 PC 9 pin 1 1 RxD 2 4 3 TxD TxD 3 2 RxD D
26. alibration results are stored in chronological order for each reagent When the GLP key is pressed followed by the Print key a summary of either the sample blank or KF reagent data is printed out refer to Printouts The GLP data are accessible in the following way 1 Press Method and select a method using the arrow keys 2 Press GLP 3 Using the arrow keys select Sample Blank or KF reagent 4 Press to view the GLP data 6 6 Chapter 5 Sample GLP Run method Select method no 1 to 50 B222 4 Ww Press GLP Method no 4 Press to view results Sample v 1 st and rd display display 3 display Accepted single result If Uncert calc No 101 ID Smp no Press gt OIL 154 1 mp no 1 If Uncert calc Yes 101 ID S 101 Result mg ml OIL 154 5 002 0 002 Mean result Press for date and time 101 Result mg ml expanded uncertainty If Uncert calc No all cases 100 Mean mg mL 5 154 s0 038 Time 10 34 100 Date 2FEB1999 100 ID OIL 154 Mean 4 runs s Standard deviation of the mean If Uncert calc Yes 100 ID Mean 100 Mean mg ml OIL 154 4 runs 5 154 0 040 Rejected result 100 ID Smp no OIL 154 KKKKK 100 Reject mg ml 7 532 0 003 Resultsand archives 6 7 Blank GLP Only available when Blank Yes Run method Select method no 1 to 50 B222 4 w Press GLP Method no 4 Press to view results
27. ample Place the syringe onto the balance and set the balance to zero tare When the message Introduce sample appears on the display inject the contents of the syringe It is recommended to inject your sample as soon as the message appears on the display If the auto detection function is activated the titration will start immediately on detection of the sample injection If this is not the case press V to start the titration Weigh the syringe The value shown on the TIM550 s display has been sent from the balance Sample amount 0 0159 g v This weight is expressed as an absolute value for calculation purposes Press V to accept the sample amount indicated on the stable balance reading and continue the titration 52 Chapter 4 Solid samples A special sample container with funnel part no 923 174 is available for weighing solid samples plastic ring funnel sample sample container Weigh the sample in the sample container and fit the funnel Bend the funnel and secure into place with the plastic ring Put back on the balance and set the balance to zero tare B ge ee When the message Introduce sample appears on the display remove the septum stopper from the electrode head and introduce the sample into the cell It is recommended to inject your sample as soon as the message appears on the display If the auto detection function is activated the titration will start immediately on dete
28. ction of the sample If this is not the case press v to start the titration 5 Weigh the empty sample container and funnel The value shown on the TIM550 s display has been sent from the balance Sample amount 0 0159 g v 6 Press V to accept the sample amount and continue the titration Programming and running analysis 5 3 Blank samples Remove an aliquot of solvent to be used for the dilution of the sample Follow steps 1 to 5 on page 52 The blank titration procedure is described on page 56 How to use the dilution volume Dissolve the sample in the appropriate KF solvent When throughly dissolved remove an aliquot quantity of sample for analysis The dilution volume and dilution uncertainty is entered in the edit sample menu when programming a titration using a blank Example 2 g of sample 1 ml of aliquot 10 ml of solvent KF Cell 1 Dissolve 2 g of sample in 10 ml of solvent 2 1 mlofthe diluted sample aliquot is added to the KF cell for titration Enter a dilution volume 10 ml For uncertatinty calculations enter the standard uncertainty of the dilution volume aliquot and sample amount 54 Chapter 4 Reagent calibration Burette Press Burette Reagent cal Use arrows to select Reagent cal Press v to start the procedure Preliminary titration User ID Appears if selected in the setup menu ACO s Standard ID Appears if selected in th
29. d time In the method display press A to display the date and time 01 Jan 1999 09 17 34 v A v Run method A OIL12 lt 50 gt v A v Run blank OIL12 50 A Running a blank titration If you have selected the option Blank Yes in the edit method menu Press W then the Run key to start the blank titration Gettingstarted 1 7 Programming the Setup menu The TIM550 will perform an autotest as soon as it has been switched on After 3 seconds press v to gain access to the setup menu TIM550 xyyww v v Setup 4 Entering a protection code Enter code A m v Use A Z to enter a four character code to lock the TIM550 Code A Yes No Neu V Select New to enter a new user defined code Select Yes the user defined code entered above is maintained The TIM550 will prompt you to enter this code in the Enter code display each time you enter the Edit mode Select No your method will remain unprotected Entering a User ID User ID A Yes No wv Select Yes to enter a User ID at the start of each method i e after pressing Run 18 Chapter2 Setting the time The TIM550 is fitted with an internal clock It is possible to visualise the date and time by pressing Method then A The actual date and time are entered in the following displays Current time A 12 37 v Use the arrow keys to position the cursor and A Z to enter the hour and minutes Current date A 4 Mar 1999 v Setting
30. d to the 6 pin female socket on the bar code reader Keyboard type PCT or compatible with a 6 pin mini DIN connector Radiometer Analytical offers two types of keyboards The Notebook Keyboard used for alphanumeric entry Is a full 83 key layout with 101 key functionality available in various languages The Numeric Keypad used for numeric entry only allows you to pro gram 4 keys for a dedicated function e g Run Cell A Notebook Keyboard Mask part no X31T108 indicating keyboard functions see next page is available for use with the mini keyboards 84 Chapter 6 Keyboard functions In combination with the TIM550 the keys of the PC keyboard perform predefined functions Referto table below Keyboard TIM550 TIM550 command key action operation F1 Run Starts the displayed method lt F4 gt lt Enter titre gt Manual entry of KF titre lt F5 gt Method Display method lt F6 gt Cell Operate cell functions lt F7 gt Burette Operate burette functions lt F8 gt GLP Access GLP table lt F9 gt Press v during autotest Edit Setup menu lt F10 gt Method key 3 seconds Edit method F11 Burette key 3 seconds _ Edit burette lt F12 gt GLP key 3 seconds Edit GLP lt Enter gt Check mark Print Confirmation of the input lt Esc gt Method key Stop titration lt Pause gt Press and release v key Stop solvent addition Up arrow Up arrow Within
31. dentification This identification will appear at the top of all detailed printouts 20 Chapter 2 Uncertainty calculations The results obtained at the end of a titration can be displayed directly associated to their corresponding expanded uncertainty The uncertain ties given for your Karl Fischer reagent titre burette and instruments usedto prepare sample balance pipette are programmed based on standard manufacturer specifications These calculations comply with the following standard EN 13005 GUM Radiometer Analytical has developed an Uncertainty Plug in R31T009 so that the TIM550 can give results with their expanded uncertainty Follow the procedure given below to unlock the uncertainty calculations 1 Select lt Yes gt Uncert calc A lt Yes gt No wv 2 Use A Z to enter the 6 digit access key from the product package Enter access A If the correct access key has been entered the uncertainty calcula tions are unlocked Press to return to the start of the Setup menu Note you can select No to re lock the uncertainty calculation option w GUM Guide for the Expression of Uncertainty in Measurement published by ISO 1993 Getting started 2 1 22 Chapter2 3 Manual functions Burette functions The following burette functions can be controlled by the TIM550 by means of the Burette key Use the arrow keys to select the burette function and press V to start Note stand by s
32. display showing the volume of titrant delivered titration speed and the time from the start of the titration 3 result beeps are sounded as soon as the end point is reached if Beep is selected in the setup menu The name of the method sample no result and units are displayed Press v to accept the result Remove Take sample Press sample v out of oven r Repeat analysis _ Press v d Yes No v Repeat analysis Yes lt No gt Vv Press V to end cycle 10 runs mg ml 4 006 0 002 The titration has been performed 10 times The mean result is displayed See chapter 5 Pre programmed methods The TIM550 offers the following pre programmed methods Simply select the method number press Run and inject the sample when the message telling you to do so appears on the display The TIM550 will take care of the rest These methods are pre programmed but can be modified to suit your specific needs Method no Method ID Titrant Solvent 41 KNO 3 HYDRANAL Composite 2 Mixture of 30 ml HYDRANAL Solvent 15 ml formamide Salicylic acid HYDRANAL Composite 2 HYDRANAL Solvent Melamin HYDRANAL Titrant 5 40 ml HYDRANAL Solvent 10 g Salicylic acid at 50 C EDTA HYDRANAL Titrant 5 mixture of 30 ml HYDRANAL Solvent 15 ml formamide Toothpaste HYDRANAL Composite 5 40 ml methanol Skin cream HYDRANAL Titrant 5 40 ml H
33. e Edit lt Standard gt menu COMP2 v Standard no The TIM550 automatically increments the 1 v standard no each time a new sample analysis is performed Drift Drift display ST 59 9 ug min Addition of standard IEDEETUCENEDIT Introduce an approximate amount of standard into the KF cell 1 000 g z If the lt Autostart gt function has been selected the TIM550 will immediately start the titration Std amount Enter the exact amount of standard 0 592 g v This can be entered even when the titration has ended Range available 0 001 to 9999 999 Titration nu f Analysis cycle 3 001 mg ml Live measuring display showing the volume of titrant 500ug min 00 10 delivered titration speed and the time from the start of the titration Calculate result 3 result beeps are sounded as soon as the end point is reached if Beep is selected in the setup menu COMP2 1 5 2 mg ml WV Press v to accept the result The result is automatically transferred to GLP KF reagent Repeat analysis Accept result Press Yes No v Press V Yes lt No gt WV Accept result lt Yes gt No Vy RES Press to reject Repeat analysis the result Yes Nor V Press Y to view Press V to end statistics cycle 4 runs mg ml 5 runs mg ml 5 runs mg ml 5 003 0 001 A 5 002 0 001 A 5 0026 0 001 Accept result No Accept result Yes The calibration has been performed 5 times The mean result is displayed See chapter
34. e KF cell during the titration The value will appear on the Introduce standard display in the calibration procedure If standard unit volume H 0 in std 0 001 to 5 000 mg ml Enter the amount of water the 9999 999 standard contains This data is given on the standard bottle H 0 in std 0 to 0 02 mg ml Enter the standard uncertainty 9999 999 u on the amount of water in the standard The value given on the bottle corresponds to the tolerance T Use the following equation to calculate the uncertainty u TA 3 For additional information refer to Uncertainty Plug in R31T009 If standard unit weight H20 in std 0 to 100 15 66 see above H20 in std 0 to 100 0 05 see above Standard ID Yes or No No When selected this option allows you to identify the standard during the calibration Standard unit ul ml ug mg g ml The unit used for the standard Uncertainty 0 001 to 0 01 ml Enter the standard uncertainty u 9999 999 of the standard used for the calibration u UK or u TN 3 U expanded uncertainty k coverage factor 42 Chapter 4 Programming a KF Titration Creating or editing a titration method Run method Select method no 1 to 50 TIPO02 lt 10 gt Press Method 3 seconds Enter Code Enter the protection code if the edit mode has been protected Refer to chapter 3 Create a new method or Copy an existing method Reset selected method edit an existing one Method 10
35. eagent library is displayed Mount new bottle If necessary enter a new KF titre see below If KF reagent titre calibrate If KF reagent titre enter Run calibration KF titre Yes lt No gt Vv 5 005 mg ml V Press V to start the calibration Enter KF titre Refer to procedure Refer to page 55 page 57 The new KF titre will now be stored in the KF reagent GLP table Atthe end of the procedure the TIM550 returns to the burette menu display 26 Chapter3 KF titrant replacement procedure This procedure allows you to change the titrant in use with a titrant of a differenttype Press V to start the procedure Burette New titrant gt Vv Burette busy The contents of the KF cell are emp E t tied into the waste bottle The burette DUE starts emptying into the KF cell Using the arrow keys select the new KF reagent from the reagent library COMP 5 3 v numbers 1 to 20 refer to chapter 4 KF reagent no Place the new titrant bottle into the bottle holder optional Screw the COMP 5 y bottle stopper onto the bottle Mount new bottle Enter a new KF titre see below If KF reagent titre calibrate If KF reagent titre enter Run calibration KF titre Yes lt No gt V V 5 005 mg ml Press V to start the calibration Enter KF titre Refer to procedure Refer to page 55 page 57 The new KF titre will now be stored in the KF reagent GLP table At the end of the procedure the TIM
36. ee page 34 is set to off when a burette function is activated except when performing a reagent calibration Burette Fill V I FIRE Burette exch gt J One of the following displays will appear depending on the choice made in the Edit Burette menu Calibrate or Enter Method ID Burette Burette Enter titre v Reagent cal y The following display appears when a burette function is running Press 4 to stop the function and return to the previous display Burette busy V to stop Manualfunctions 2 3 Fill procedure This procedure is used to fill the burette with titrant IMPORTANT prior to dismounting the burette the piston should be taken to its lowest position Perform a Fill to do so Empty procedure This procedure allows you to empty the contents of the glass cylinder into the cell Flush procedure This procedure ensures complete rinsing of the system and expulsion of air bubbles from the burette delivery tube etc It is recommended to carry outthis procedure whenever titrant reagent has been changed or when ever it is suspected that air bubbles have been drawn into the burette The flush procedure lasts for approximately 2 minutes Within this period the burette will be flushed with titrant reagent The flush procedure leaves the burette filled and ready for use Note that the length of the flush programme has been adapted to delivery tubes of standard length 90 cm If a
37. et the maximum acceptance range for results An alarm message will appear if the result lies above this value Refer to chapter 7 Sample menu Blank No Parameter Range Default Description available value Advised amount 0 001 to 1 000 ml Enter the recommended sample 9999 999 amount to be added to the KF cell during the titration The value will appear on the Introduce sample display in the run procedure Uncertainty 0 to 0 01 ml Enter the standard uncertainty of 9999 999 the sample This parameter comprises different components for example the uncertainty of the syringe and or balance For additional information refer to Uncertainty Plug in R31T009 48 Chapter 4 Sample menu Blank Yes Parameter Range Default Description available value Sample amount 0 001 to 1 000 ml This is the amount of sample that 9999 999 has been added to the solvent Refer to Blank samples Sample uncert 0 to 9999 999 0 01 ul Appears if Uncert calc Yes Enter the standard uncertainty of the sample amount entered Dilution volume 0 001 to 10 ml Enter the volume of solvent used 9999 999 to dissolve the sample Refer to Blank samples Dilution uncertainty 0 001 to 0 2 ml Appears if Uncert calc Yes 9999 999 has been selected in the setup menu Enter the standard uncertainty of the dilution volume Advised aliquot 0 001 to 1 000 ml Enter the recommended amount 9999 999 o
38. eys Run Press to start the method indicated on the TIM550 display method no 1 to 50 Press to activate the cell s functions refer to chapter 3 Pump empty cell add solvent Standby activate deactivate Stirrer set the stirrer On Off and select the stirring speed from 100 to 1100 rpm Molecular sieve replace molecular sieve Burette Press to select burette s functions Fill Empty Flush Rinse Bottle exch New titrant Calibrate or Enter titre Hold down the key for 3 seconds to enter the burette edit mode The user can now perform the following 1 Select Enter for manual entry of the KF reagent titre Select Calibrateto determine the KF reagent titre using a calibration procedure GLP The GLP key gives access to the following 1 Last200 sample results stored in chronological order Last blank result stored for each method last 10 blank results in chronological order Last 10 KF titre results are stored in chronological order for each KF reagent 12 Chapter 2 Method This key is used to select one of the 40 programmable methods and one of the 10 pre programmed methods Hold down for 3 seconds to enter the Edit mode and edit a method to fit your particular requirements IMPORTANT the Method key is used to stop a titration Use these keys to enter the following alphanumeric characters ABC YZ0123456789 and blank space 1 Pressthe arrow keys to move the cursor 2 Press the
39. f sample to be added to the KF cell during the titration The value will appear on the Introduce sample display in the run titration procedure Aliquot uncertainty 0 001 to 0 01 ml Appears if Uncert calc Yes 9999 999 has been selected in the setup menu Enter the standard uncertainty of the recommended amount of sample aliquot to be added to the KF cell during the titration Programming and running analysis 4 9 Edit Blank menu Parameter Range available Default value Description Advised amount 0 001 to 9999 999 1 000 ml The recommended blank amount to be added to the KF cell during the titration The value will appear on the Introduce blank display in the run procedure Uncertainty 0 to 9999 999 0 01 ml Enter the standard uncertainty of the blank This parameter comprises in general different components for example the uncertainty of the syringe and or balance For additional information refer to Uncertainty Plug in R31T009 Blank res unit mg ml or pg ml mg ml The blank result unit will appear with the blank result at the end of titrations Quality control Yes or No Yes This is the quality control option It will help you determine whether or not you should accept or reject a blank result Select Yes to enter an acceptance range See minimum and maximum blank Maximum blank minimum blank to 9999 999
40. f tests are automatically performed when the TIM550 is switched on during calibration and during titration If a problem is de tected an error warning message will appear on the display The mes sages are listed below By pressing V the TIM550 will normally return to the operational state in which the error was detected This makes it possible to correct the error andimmediately resume operation If any of the error messages cannot be cleared by actions listed contact your Radiometer Analytical representative at the adress given on page 103 Message Problem Action Battery low The battery is run down Replace the battery and must be replaced as described on page 87 Press V to continue Wrong access key This message is displayed when an incorrect access key has been entered to unlock the uncertainty calculations Enter the correct code and press to continue Invalid entry This message appears when an entry is made which lies outside the available range The entry is replaced by the previous value Memory error This message is displayed at power on if the TIM550 detects an error in the data stored in the non volatile memory This message is generally displayed after a battery failure Press v Default values are used instead of the erroneous data If this error remains on the display after the battery has been changed contact your Radiometer Analytical representative Wr
41. he chain indicate that there is hidden text Use the right and left arrow keys to move along the chain Method ID Deleting alphanumeric characters Deleting an entire chain of characters 1 Use the arrow keys to position the cursor on the first letter in the chain 2 Press Z to delete the chain Deleting certain characters in the chain 1 Use the arrow keys to position the cursor on the first letter in the chain 2 Press A and select the blank space Please note that spaces will now replace text Please note that a PC keyboard and or bar code reader can also be used to enter alphanumeric data Getting started 1 5 The Setup menu 1 Switch on the TIM550 using the on off switch situated on the rear panel 2 The first display you will see will remain for a few seconds and shows that the TIM550 is performing an autotest 3 Press V to enter the setup menu when setup appears on the display Refer to page 18 for details on how to program the setup menu 4 f no keys are pressed the TIM550 switches to the method Run method A 1 display Press Run to start the titration or use the arrow keys to select another method from 1 to 50 To activate the Stand by refer to chapter 3 The method display will now show the live drift value 50 ug min A Milk 50 v Refer to chapter 4 to calibrate your KF reagent titrant and create your KF titration method 16 Chapter2 Displaying the date an
42. ic conditioning function avoids long cell reconditioning and continuous cell volume monitoring avoids overflowing During the conditioning the moisture drift is measured and automatically taken into account in calculations for faster more accurate analyses To comply with quality control requirements the TIM550 includes specific QC parameter setting together with High Low alarms to help operators make the right choice in reviewing results The results obtained at the end of a titration can be given directly associated to their uncertainty Radiometer Analytical offers an Uncertainty Plug in to allow the uncertainty given for your Karl Fischer reagent titre burette and instruments used to prepare sample balance pipette to be programmed based on standard manufacturer specifica tions Introduction 3 4 Chapter 1 2 Getting started This instrument has been developed to meet the requirements of electrochemical applications It is aimed at experienced users who have the knowledge required to operate the instrument and implement the security instructions enclosed Please remember that this system must not under any circumstances be used to perform tests on living beings Make sure that the TIM550 mains socket is within easy access for quick disconnection purposes Radiometer Analytical SAS have developed installation kits to make setting up the TitraLab 55 Titration Workstation easy refer to the Installation Sheet part no D26T
43. ise the display will turn darker or brighter respectively Changing the selected source voltage The TIM550 is designed to operate at 115 V and 230 V depending on the setting of the voltage selection switch located on the back of the instru ment When changing the input voltage the fuse has to be changed Refer to the table chapter 7 To change the voltage first unplug the power cord Pull out the fuse cover and compare the fuse ratings with the desired voltage setting Using a suitable tool move the required voltage to the white arrow Getting tarted 7 Setting up the Bayonet KF Cell with accessories X91T003 X31T038 10 pcs r1 X31T036 X31T040 X51T013 X31T037 A90A410 O O X31T033 O X31T032 Q X31T051 C t y C YC 923 174 5 pcs 10 pcs OOC IL C90 X41T006 10 pcs 8 Chapter 2 X31T069 1 X31T033 X31T061 X31T048 X31T036 X51T013 Getting started 9 Mounting the titration vessel Place the magnet bar A90A41 0 into the titration vessel X51T013 Screw the titration vessel clockwise onto the electrode head Mounting the KF cell onto the TIM550 Press the two clips situated on both sides of the electrode head and slide the head on
44. lar sieve Use the arrow keys to select one of the cell functions Press W to continue to the next level of displays Once the pump has been activated use this key to add solvent to the cell Once the pump has been activated use this a key to empty the cell 30 Chapter 3 Pump functions Emptying the KF cell Pump Press V to activate the pump Empty cell Vv The stirrer starts at medium speed Press to empty the cell re ppl aoa The pump will automatically stop after pume alae 60 seconds This message will appear when the Cell full maximum level in the cell is reached empty cell Vv Press V to activate the pump and the Waste key to start emptying the cell Refer to chapter 7 section error messages Manualfunctions 3 1 Adding solvent to the KF cell eT dtr Press to add approximately Add L t gt iad CO Radiometer Analytical have marked the KF cell to indicate the minimum level to which solvent must be added Refer to chapter 9 n Once the fill mark is reached release To stop the pump the solvent button to stop the pump press v The pump will automatically stop after 60 seconds 32 Chapter3 Stirrer functions Stirring speed A Select a stirring speed from one of the 11 available speeds 100 200 300 lt 500 gt rpm 400 500 default value 600 700 800 900 1000 1100 rpm Press to valid the stirring speed and continue to the next step Press V to start
45. ld be used as a stop criterion corresponding to the maximum volume of titrant to be added during the titration The titration will stop when the volume reaches the entered value Quality control Yes or No Yes This is the quality control option It will help you determine whether or not you should accept or reject a result Select Yes to enter an acceptance range See the minimum and maximum titre values on the next page Programming and running analysis 4 5 maximum titer Parameter Range Default Description available value Minimum titre 0 001 to 0 001 mg ml This is a Quality control parameter setting Quality control Yes Set the minimum acceptance value for the KF reagent titer An alarm message will appear if the titre lies below this value Refer to chapter 7 Maximum titre minimum titer to 9999 999 9999 999 mg ml This is a Quality control parameter setting Quality control Yes Set the maximum acceptance value for the KF reagent titre An alarm message will appear if the titre lies above this value Refer to chapter 7 46 Chapter 4 Edit Sample menu general parameters Parameter Range Default Description available value Sample ID Yes or No Yes When selected this option allows you to identify the sample during the titration Sample unit ul ml ug mg g ml Unit used for the sample Sample factor
46. longer delivery tube is used start out with the flush programme 24 Chapter3 Rinse procedure For safe reagent handling use this procedure each time the burette is to be replaced It makes sure the delivery tubes are titrant free Press V to start the procedure Burette busy The contents of the KF cell are emp tied into the waste bottle and the y to stop burette starts emptying into the KF cell Remove the bottle stopper from the Remove TIERE titrant bottle bottle 4 Mount rinse sol Mount the rinse solution bottle Screw the bottle stopper onto the bottle bottle v The burette starts the flush procedure Remove the bottle stopper from the Remove rinse rinse solution bottle sol bottle 4 Replace the titrant bottle and screw the bottle stopper into place At the end of the rinse procedure the TIM550 returns to the burette menu display Manualfunctions 2 5 Bottle exchange procedure This procedure allows you to remove the empty titrant bottle and replace it with a new one Press V to start the procedure Burette Bottle exch gt J Burette busy The contents of the KF cell are emp Js tied into the waste bottle The burette anal starts emptying into the KF cell Remove the bottle stopper from the titrant bottle Remove titrant bottle Place the new titrant bottle into the bottle holder optional and screw the COMP 2 4 bottle stopper into place The KF reagent ID entered in the r
47. lt estimated from a previous series of measurements refer to chapter 5 Uncert calc Yes or No No This option appears if the uncertainty calculations have been unlocked in the setup menu Select Yes results will be given directly associated to their related uncertainty The calculations will also take into account all the parameters involved in your analyses Select No results for a series of measurements will be given with their standard deviation Use Oven Yes or No No Set to yes if you are working with an oven 44 Chapter 4 Method menu parameters The following general parameters are available when you press Method for 3 seconds Edit Parameters menu Parameter Range Default Description available value Drift Threshold 0 to 999 g min 50 g min This is the maximum drift allowed to start the titration Max burette 1 to 200 150 min The maximum speed at which speed the burette will deliver KF reagent Min titr time 00 01 to 00 30 min s This is the minimum time the max titr time titration will take The timer will start as soon as the sample is introduced into the KF cell if autostart otherwise as Soon as V has been pressed Max titr time Min titr time 00 05 h min This is the maximum time the to 99 59 titration will take This parameter is used to avoid never ending titrations Max volume 1 to 99 10 ml This setting shou
48. must empty empty the cell before continuing the titration Continue empty the cell or continue titration the titration Cell full This message appears Press v to empty the cell empty cell when the contents of the Select Return titr to continue the titration KF cell reach maximum level The user must empty empty the cell before continuing the titration After a manual key press e g add solvent Message Problem Action Cell full This message appears Press v to empty the cell empty cell when the contents of the Molecular sieve saturated This message appears when the Empty cell function is activated and the number of empty cells is greater than 50 or the molecular sieve replacement date is greater than 7 days It is time to replace the molecular sieve Replace molecular sieve and press V to reset the empty cell and replacement date counters 92 Chapter 7 Titration start errors Message Problem Action Blank titration Yes BIk 0 This message appears at the start of a sample titration A blank value is not available for the titration i e Blank GLP is empty Select Yes and press V key to start the blank procedure Select lt Blk 0 gt to perform the titration using a blank value 0 Cal time elapsed lt New Cal gt Cal time elapsed lt Continue gt This message appears when the option KF reagent titre Calibrated
49. nection of Peripherals 8 1 Pin layout of the A95Z201 cable DTE Female 9 pin Pin layout of the A95Z202 cable ma gt 1m I L i TIM550 A95Z201 Balance BALANCE socket Bd METTLER ia 1 1 RxD 2r 3 TxD TxD 3 2 RxD DTR 4 5 CTS GND 5 7 GND DSR 6 44 4 RTS RTS 7 9 6 DSR CTS 8 4 20 DTR 9 DCE Male 25 pin ma jf gt 1m A952202 TR ey ONC SARTORIUS 1 1 RxD 2 p 4 2 TxD TxD 3 m3 RxD DTR 4 4 Gnd Return GND 5 5 CTS DSR 6 4 e 7 GND RTS 7 20 DTR CTS 8 4 25 9 Female 9 pin 82 Chapter 6 DTE Male 25 pin Pin layout of the A95Z206 cable ka e 1m A95Z206 BALANCE TIMS50 oO METTLER RxD 2 4 12 TxD TxD 3 2 RxD DTR 4 3 CTS GND 5 e 13 GND DSR 6 44 4 RTS 7 gt o CTS 8 9 DTE METTLER PLUG Female 9 pin 15 pin Connection of Peripherals 8 3 Connection of keyboard and bar code reader A keyboard and or a bar code reader can be connected to the TIM550 via the 6 pin mini DIN port situated on the right hand side of the instrument Note you can also connect the keyboar
50. nent reagents regener ate the molecular seive after having performed 50 fill empty cycles with the KF cell The regeneration procedure takes place in two stages 1 Wash with deionised water to eliminate SO 2 Place in an oven temp 250 to 300 C to eliminate the water Procedure 1 Empty the molecular sieve into a tall beaker 2 Slowly pour deionised water over the molecular seive until fully immersed WARNING risk of splashing due to the release of SO Shake the beaker Pour off the water Repeat steps 2 to 4 four to five times Dab the molecular sieve with an absorbent paper towel Place the molecular sieve in a crystallising dish oN Oa Rh o Place the crystallising dish in a hot oven temp 250 to 300 C for at least one night o Place the molecular sieve in an airtight flask ready to be re used 10 Activate the Molecular Sieve function in the Cell menu refer to page chapter 3 104 Chapter9 International Standards EMC Directive 89 336 EEC The TIM550 complies with the following standards Emission EN 55022 Class B for conducted emission EN 55011 Class A for radiated emission Immunity EN 61000 4 2 level 2 for contact discharge and level 3 for air discharge EN 61000 4 3 level 2 EN 61000 4 4 level 2 EN 61000 4 5 level 2 EN 61000 4 6 level 2 EN 61000 4 11 Low Voltage Directive 73 23 EEC The TIM550 complies with the following standard Reference standard EN 6101 0 1 Gene
51. new battery should be positioned with the sign facing towards the sign on the inside of the cap WARNING only replace with a battery of the same type and rating Troubleshooting 8 7 Replacing the fuses NE tet 1 Disconnect the TIM550 The fuse is positioned just above the power Socket on the rear panel 2 When the two vertical flaps on the cover are gently squeezed together the cover can be pulled out and the old fuse changed WARNING for continued protection only replace the fuse with one of the same type and rating see table below 3 HRe insert the cover with the new fuse Voltage rating Fusedescription Part no 115 Vac 2 x fuses slow blow 0 4 A 450 016 230 Vac 2 x fuses slow blow 0 2 A 450 013 Note a secondary fuse is mounted on the printed circuit board If necessary contact a Radiometer Analytical service representative for replacement of the 2 A picofuse UL recognised 4 Put the cap back in place 8 8 Chapter 7 Dismounting the pump module 1 Remove the transparent tubes from the outlets O 2 Unscrew the screws on the pump 3 Lift out the pump see figure 1 below 4 Insert the new module into place and tighten the screws Refer to the Pneumatic Module Operating Instructions D26T021 for further information regarding the dismounting and installation Figure 1 Dismounting the pump module Troubleshooting 8 9 Error and warning messages A number o
52. nt The default parameters are restored Burette lt Flush gt Return to the burette menu 28 Chapter3 Manual entry of KF titre Available if KF reagent titre Enter is selected in the KF reagent library Refer to chapter 4 Press V to continue Burette Enter titre Vv KF titre Enter the KF titre Range available 0 001 to 9999 999 5 005 mg mL If Uncertainty calc Yes Enter the standard uncertainty of the 0 002 mg ml titre Refer to bottle indications or titrantcertificate R31T009 Range available 0 to 9999 999 Uncertainty The entered KF titre will be automatically stored in the KF reagent GLP table Reagent calibration procedure This procedure allows you to determine the Karl Fischer reagent titre Available if KF reagent titre Calibrate is selected in the KF reagent library Refer to chapter 4 page 38 Press V to start the calibration Burette Reagent cal v The titre determined at the end of the calibration procedure is automati cally transferred to the KF reagent GLP table An overview of the calibration procedure is given in chapter 4 page 55 Manualfunctions 2 9 KF cell functions The following functions are controlled by the TIM550 by means of the Cell key Use A Pump v EU Mol Sieve gt VW Pump functions empty cell and add solvent Stand by on off Stirrer functions stirrer on off set stirring speed Molecular sieve replace molecu
53. ollow the procedure given below to delete results stored in the Sample Blank and or KF reagent menus of your selected method Run method Select the method no 1 to 50 Press GLP 3 seconds Enter code Enter your protection code if the edit mode has been protected Refer to chapter 2 Reset method 4 Use arrow keys to select the menu in which Sample v you wish to delete the results sme Press W to continue lt KF reagent gt W Select yes Confirm Press W to confirm Yes No 70 Chapter 5 Printouts An explanation is given here of the printouts available when a printer is connected to the TIM550 Specific information can be found on the following pages and in the order shown concerning KF titration results Blank titration results KF reagent titration results GLP data Edit menu data How to obtain printouts Use this key in association with other keys to obtain your printouts When Method is pressed followed by Print method menu Method parameters are printed out Burett When Burette is pressed for 3 seconds followed by Print KF reagent parameters are printed out When GLP is pressed followed by Print the results stored in the GLP table are printed out Two types of printout formats exist You can select 80 columns detailed or 40 columns condensed in the setup menu refer to Chapter 3 KF titration calibration and blank results are printed automatically when a printer i
54. olumns x TIM550 10 May1999 16 46 Burette xxxROOONOO Electrode DOUBLE Pt okkck kk kk kkkk SAMPLE KEXKKKKKKKEKEK Method 7 VINC KF reagent titre 0 040 mg ml Sample ID AQUA no Sample result Time mg g h min 12 4 186420 957 16 49 as a 4257 0 1007 16 52 ERIS 4 1099 0 0955 3 9432 0 0941 Mean 4 1851 0 3430 mg g R Rejected L Alarm Low H Alarm high kkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkxkk Resultsand archives 7 3 Blank titration printouts The following information is obtained at the end of a blank titration Blank no Blank result QC messages OK Rej rejected Low High Time h min Blank amount ml Volume ml of titrant used Drift ug min Dur min s Mean result KF reagent calibration printouts The following information is obtained at the end of a calibration proce dure Standard no KF titre mg ml QC messages OK Rej rejected Low High Time h min Std amount ml Volume ml Drift ug min Dur min s 74 Chapter 5 GLP Printouts To obtain the printout 1 Press Method and select a method from 1 to 50 2 Press GLP 3 Select Sample lt Blank gt KF reagent 4 Press Print The following information is obtained GLP no Sample ID Sample no Sample result QC messages Date Time h min Note If any of the following data for the selected method change then a new table will be printed out a Burette seri
55. ong code This message is displayed when an incorrect protection code has been entered Enter the correct code in the Enter code display Press to continue 90 Chapter 7 Burette errors Message Problem Action Burette not This message is displayed Press V to continue available if a burette function Fill Empty Flush Rinse Bottle exchange or New titrant is requested after pressing the Run key or when the Stand by is activated BURETTE These errors may occur when If any of the following ERROR 2 the burette is performing a Fill error messages occur Empty Flush Rinse Bottle contact your Radiometer BURETTE exchange or New titrant Analytical representative ERROR 3 procedure and an operational or Radiometer Analytical error has occured to the burette at the address given on BURETTE 2 Stopcock sensor page 103 ERROR 4 ON position not found Please remember state 3 Stopcock sensor the error number 2 3 4 BURETTE OFF position not found or 5 ERROR 5 4 Piston sensor ON position not found 5 Piston sensor OFF position not found Troubleshooting 9 1 Cell errors During a titration cycle Message Problem Action Cell almost full Empty cell This messages warns the user that it is time to empty the cell Press V to empty the cell Cell almost full The user can either Press V to continue the KF cell reach maximum level The user
56. pA 5 Voltage range 2000 mV Resolution 0 1 mV Uncertainty lt 4 mV Resistance 71 5 KQ 2 RS232C serial ports for Printer PC and additional TIM550 connections 1 serial port for balance 1 Mini DIN port for PC keyboard and or bar code reader Volumetric KF titration KF reagent standardisation Blank determination 50 user programmable methods with alphanu meric name and protection facility including 10 pre programmed applications TIM550 storage capacity for 20 KF standards 20 KF titrants 20 titrant standardisation 200 results 10 blank determinations 11 reproducible speeds 100 200 300 400 500 600 700 800 900 1000 and 1100 rpm 2 to 5 minutes Condensed and detailed GLP result bulletins Printout of methods GLP tables 5 to 40 C Metrological characteristics guaranteed be tween 15 and 30 C 99 Generalinformation Relative humidity 20 to 8096 Fuserequirements Powerrequirements Main fuses slow blow 0 2 A 230 V Secondary fuse 2 A picofuse UL recognised 47 5 63 Hz 115 230 Vac 15 18 Position of Mains supply voltage range Typical current Max selector 18 15 to 15 current switch 115 V 94 V 133 V 200 mA 400 mA 230 V 188 V 265 V 100 mA 200 mA Level of pollution 2 Transitory overvoltage level II Display 2 x 16 character alphanumeric LCD display Finish chemical resistant splashproof cabinet Weight 5 kg excluding bottles
57. ralinformation 105 106 Chapter9
58. s V 12 54 mg ml W Accept result Press V Yes No The mean result is given with the corresponding units 0 010 AJ Depending on whether Yes or No is selected above the mean is displayed for n or n 1 results Press A to return to accept result display 4 runs mg ml The following results are possible for a series of titrations no of runs 1 1 If Uncert calc Yes 3 runs mg ml 5 003 0 020 a 2 If Uncert calc No indicates that this is the expanded uncertainty 3 runs mg ml s indicates that this is 5 005 A the standard deviation of the mean Sm 62 Chapter 5 Theory Let R be the concentration to be found during the titration The distribution of R estimated as normal has the following characteris tics u mean value of the distribution of R o standard deviation of the distribution of R By definition these characteristics are limits of mathematical functions and correspond to an infinite number of determinations of R Their estimations m and S respectively are determined by population sampling i e from n titrations with results R1 R2 Rn The estimations of the characteristics of the distribution of u mean of R are m mean value of the distribution of u s Sas m m S standard deviation of the mean of u where For a series of n titrations where the mean m is expressed the standard deviation of the mean s_ is used to represent the di
59. s connected Resultsand archives 7 1 KF titration results The following printout is obtained during a KF titration Each line in the table is printed as soon as the result is obtained Detailed 80 columns TIM550 Volumetric Karl Fischer Titrator 679ROONOO7 10May 1999 16 35 xxx Burette xxxROOONOOO Electrode 768 11 008 kkkkkkkkkkkkkkkkkkkkkkkkkkkkk SAMPLE KKK KKK KKK KKK KKK KKK KERR KK KKK KKK KER KKK ke e Method 7 VINC KF reagent titre 2 000 0 040 mg ml KF Reagent 5 Date O7MAY1999 Sample ID AQUA no Sample result ac Time Sample amount Volume Drift Dur mg g h min g mL ug min min s 8 4 36894 0 0992 High 16 37 1 015 0 001 2 21740 012 17 3 01 07 9 3 8848 0 0903 Low 16 40 1 032 0 001 2 00540 012 15 3 01 07 10 4 06294 0 0938 OK 16 43 1 028 0 001 2 088 0 012 46 4 01 12 13 63644 0 0862 Rej 1 021 0 001 1 8564 0 012 Mean 4 1055 0 3435 mg g 3 runs 10 May 1999 16 46 kkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkk Volume ml this corresponds to the volume delivered by the burette during the titration The uncertainty given is the uncertainty of the volume delivered Drift ug min this corresponds to the stable drift reading before the sample is introduced to the KF cell The uncertainty given is the uncer tainty of the drift This drift value will be used for calculation purposes 72 Chapter 5 Condensed 40 c
60. spersion of the re sults around m To calculate the standard deviation of the distribution S using the standard deviation of the mean S obtained from n measurements use the following equation Sa Sin X Nn Resultsand archives 6 3 Reproducibility Use the following equation to calculate the reproducibility Sais Reproducibility x 100 mean result This value can be entered in the reproducibility display in the Edit mode if the Uncertainty calculation option has been selected Refer to pages 39 and 44 For further details refer to the Uncertainty Plug in R31T009 6 4 Chapter 5 Successive titrations 1 From the result display at the end of the titration OIL 422 Press V 12 54 mg ml W Repeat analysis Select Yes and press Vv Yes No w 2 From the Accept result display Accept result Select Yes or No and press V Yes No w Repeat analysis For more analysis select yes and press V Yes No w Select no to stop the titration cycle Resultsand archives 6 5 GLP Table The GLP table is divided into 3 groups Sample groups titration method results for all the methods Last 200 results are stored in chronological order Blank groups blank results Last 10 blank results are stored in chronological order Last blank result is stored for each titration method KF reagent groups manually entered or calibrated KF reagent titres Last 10 c
61. stop stirring Stirrer to start A i Replacing the molecular sieve Use Press to valid the replacement of the molecular sieve and continue to lt Mol Sieve gt W the next step When is pressed the internal counters empty cell and molecular mol sieve v sieve replacement date will be reset Replace A This message will appear when the Empty cell function is activated and Saturated 4 the number of empty cells is greater than 50 or the molecular sieve replacement date has exceed 7 days Molecular Sieve Manualfunctions 3 3 Automatic moisture drift compensation stand by Stand by remains activated at the end of titrations The stand by function maintains the cell ready for the next analysis Follow the procedure given below to activate the stand by Stand by ra Press V to start the stand by to start When stand by is activated the para meter values of the current KF titration method are used The TIM550 displays the drift reading in the method display 30 ug min A Milk lt 50 gt v Press V to stop the stand by Stand by is stopped automatically when 1 Amanual pump function is started Note the stand by is reactivated if the titration is continued 2 Amanual burette function is started except for a reagent calibration procedure The TIM550 is switched off The method key is pressed to stop a titration while the TIM550 is busy compensating the drift 5
62. take This parameter is used to avoid never ending titrations Max volume 1 to 99 10 ml This setting should be used as a stop criterion corresponding to the maximum volume of titrant to be added during the titration The titration will stop when the volume reaches the entered value Quality control Yes or No Yes This is the quality control option It will help you determine whether or not you should accept or reject a result Select Yes to enter an acceptance range See the minimum and maximum titre values on the next page 40 Chapter 4 Parameter Range Default Description available value Minimum titre 0 001 to 0 001 mg ml This is a Quality control maximum titer parameter setting Quality control Yes Set the minimum acceptance value for the KF reagent titer An alarm message will appear if the titre lies below this value Refer to chapter 7 Maximum titre minimum titer to 9999 999 mg ml This is a Quality control 9999 999 parameter setting Quality control Yes Set the maximum acceptance value for the KF reagent titre An alarm message will appear if the titre lies above this value Refer to chapter 7 Programming and running analysis 4 1 Edit Standard menu Parameter Range Default Description available value Advised amount 0 001 to 1 000 ml The recommended amount of 9999 999 standard to be added to th
63. th the electrode treatments may be required These treatments will depend on the last measure mentperformed Mild cleaning e Place the electrode overnight in RENOVO N Normal Cleaning Solution Degreasing 103 mm Remove mineral oils by rinsing the electrode E S with trichlorethylene and dabbing dry with a 12mm soft tissue After cleaning Dabthe electrode dry with soft tissue before performing the titration Double platinum electrode 9 7 Chemical cleaning The electrode can be cleaned with a sulphochromic solution or with a boiling solution of hydrochloric acid WARNING hazardous corrosive chemical Storage Replace the protection cap and store the electrode in it s box at room temperature Accessories Description Part No oRENOVO N Normal Cleaning Solution 250 ml S16M001 Specifications Temperature range 10 to 100 C Sensing element 2 platinum wires Diameter of Pt wire 0 5mm Distance between the Pt wires 4mm Connection BNC plug Cable length 0 55 cm Min immersion depth 22mm 98 Chapter 8 9 General information Specifications Measuring ranges Resolution Uncertainty Electrode Input BNC Inputs Outputs Methods Datastorage GLP Functions Stirring Typical titration time Printouts Workingtemperature Ambienttemperature 0 1 to 100 0 5 ug of water refer to Guide to Uncertainty Calculations R31T009 1 AC polarised electrode input 56
64. the edit menu parameters can be scrolled Down arrow Down arrow Within the edit menu parameters can be scrolled Left arrow Left arrow Select an option which appears within the arrows on the display Right arrow Right arrow Select an option which appears within the arrows on the display lt Inser gt Insert text lt Del gt Delation of an input digit character under which the cursor is positioned lt Home gt Go to start of text lt End gt Go to end of text Numeric keypad Numeric input is possible Page up page A Z keys Alphanumeric input down Print screen Print Printout data QWERTY Keyboard Alphanumeric input possibleparameters Connection of Peripherals 8 5 86 Chapter 6 7 Troubleshooting Changing the battery The 3 6 V lithium battery part no 430 127 which has a lifetime of mini mum 2 years should be replaced when the following message appears BATTERY LOW V The battery s function is to ensure the titrator s permanent memory facility The battery must be changed while the instrument is switched on to avoid loss of data in the memory Change the battery in the following way 1 The cap onthe rear plate of the TIM550 behind which the battery is positioned is shown in the illustration 2 nsertthe edge of a coin into the slit on the cap surface and turn 3 The cap will now open providing access to the old battery which should be removed The
65. to perform a new calibration if the current calibration is older than an x number of days KF reagent ID Calibrate A to Z Use A Z to enter the ID Enter 0 to 9 blank space Reproducibility Calibrate 0 to 999 99 10 Appears if Uncert calc Yes in the setup menu If you are to perform only one titration enter the reproducibility of the result This corresponds to the the relative standard deviation in estimated from a previous series of measurements refer to chapter 5 Press the W key and Edit Standard and Edit lt Parameters gt Programming and running analysis 3 9 Calibration procedure parameters The following parameters are available when you press the Burette key for 3 seconds Press W to accept the values and continue to the next display Edit Parameters menu Parameter Range Default Description available value Drift Threshold 0 to 999 g min 50 g min This is the maximum drift allowed to start the titration Max burette speed 1 to 200 150 min The maximum speed at which the burette will deliver KF reagent Min titr time 00 01 to 00 30 min s This is the minimum time the max titr time titration will take The timer will start as soon as the sample is introduced into the KF cell if autostart otherwise as soon as v has been pressed Max titr time Min titr time 00 05 h min This is the maximum time the to 99 59 titration will
66. to the metal rod Release the two clips to secure the head in place Filling the desiccant tube Fill the tube with molecular seive S72T004 IMPORTANT if you are using the molecular seive for the first time you must activate it by placing it in an oven temp 250 to 300 C for at least 10 hours refer to page 104 Getting the best results Make sure that the two platinum wires of the double platinum electrode are covered by the solvent Stirring must be effective without causing air bubbles Replacing the used silicon septa After approximately 20 injections it is recommended m diii to replace the blue silicon septa in the following way Simply remove the old one and replace it with a new one X31T038 Thermostated KF cell X31T036 When working with temperatures above ambient temperature the release of alcohol vapours and SO contained in the KF solvents is accelerated It is therefore recommended to keep the solvent and waste bottles cool to reduce the rate of saturation of the molecular sieve found in the bottle stopper dessiccant tubes 10 Chapter2 TIM550 front panel Select an option and move from Run method one display to another Moves the display cursor left or right Stop and edit method Waste key Confirm Function Archives to empty cell printout keys access key data Solvent key Enter alphanumeric to fill cell parameters Getting started 1 1 Description of k

TitraLab 550 Volumetric Karl Fischer Titrator

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