Metrohm 787 KF Titrino Instructions For Use Manual
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Metrohm 787 KF Titrino Instructions For Use Manual

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CH-9101 Herisau/Switzerland
E-Mail
info@metrohm.com
Internet
www.metrohm.com
787 KF Titrino
Program version 5.787.0010
Instructions for Use
8.787.1003
03.2002 / pkl

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  • Page 1 CH-9101 Herisau/Switzerland E-Mail info@metrohm.com Internet www.metrohm.com 787 KF Titrino Program version 5.787.0010 Instructions for Use 8.787.1003 03.2002 / pkl...

  • Page 3: Table Of Contents

    Connection of a computer ................60 Connection of electrodes, preparing titration vessel........... 61 Appendix ......................63 Technical specifications ..................63 Pin assignment of the "Remote" socket............... 65 5.2.1 Lines of the "Remote" socket during the titration ......... 67 RS232 interface ....................68 787 KF Titrino...
  • Page 4 Table of contents Validation / GLP....................69 Warranty and conformity ..................70 5.5.1 Warranty....................... 70 5.5.2 EU Declaration of conformity............... 71 5.5.3 Certificate of Conformity and System Validation ......... 72 Scope of delivery and ordering designations ............. 73 Index...........................77 787 KF Titrino...

  • Page 5: Introduction

    1.1 Instrument description Introduction 1.1 Instrument description The 787 KF Titrino is a fast and precise titrator for the water determination according to Karl Fischer. With the Metrodata VESUV Software determination data can be saved on a PC. 787 KF Titrino...

  • Page 6: Controls And Parts

    1.2 Controls and parts 1.2 Controls and parts Front view of instrument: 787 KF Titrino...
  • Page 7 - Filling after manual dosing with <DOS>. Key <START> Starts procedures, e.g. titrations, conditioning. Identical with key <START> of the separate keypad. Indicator lamp: "Cond." Lamp flashes during conditioning. Lamp is on when the titration cell is conditioned. 787 KF Titrino...
  • Page 8 1.2 Controls and parts Rear view of instrument: 787 KF Titrino...
  • Page 9 Analog output for the connection of a recorder Connection for power cable With power supplies where the voltage is subject to severe HF disturbances, the Ti- trino should be operated via an additional power filter, e.g. Metrohm 615 model. Mains switch Earthing socket...

  • Page 10: Manual Operation

    ":") MODE Mode selection, see page 18. PRINT Printing of reports, see page 37. CLEAR Clears values, set special values. ENTER Stores values. STOP Stops methods. QUIT Quits inquiries, waiting times, printing. START Starts methods. 787 KF Titrino...

  • Page 11: Principle Of Data Input

    • With key <QUIT> you leave an inquiry or a group of inquiries, it always moves you one level up. • In this example you leave the menu "configuration" ******** by pressing <QUIT> and return to the standby state with the display of the titration mode. 787 KF Titrino...

  • Page 12: Tutorial

    • Accept the new "value" with <ENTER>. The next inquiry "fecha" (date) of the group "ajustes varios" (auxiliaries) is shown. ******** You can open this inquiry by pressing <ENTER> fecha 2002-03-27 too and go through all the inquiries of this group this 787 KF Titrino...
  • Page 13 • Press <QUIT> once again to exit the "configuration" menu and return to the standby state. ******** All the dialog texts will now be displayed in Spanish. If you prefer English as the displayed dialog lan- guage, proceed as before and select "English". 787 KF Titrino...

  • Page 14: Titer Determination

    "OFF". req.ident: <ENTER> Request of the sample size after the titration start: TITER ******** "ON". req.smpl size: <ENTER> If no printer is attached, the report printout after the TITER ******** titration must be switched off. report: 787 KF Titrino...
  • Page 15 Since the mean value is recalculated mean: after every determination, the maximum value can re- main set at 20. The mean calculation is terminated when the operating mode is changed. 2 × <QUIT> • Exit the inquiry. 787 KF Titrino...
  • Page 16 On completion of the titration, the mean value of the two determinations is calculated. The report on the printer has the following appearance: date 2002-03-27 time 13:55:10 smpl size 0.03 g titer 5.3686 mg/ml mean (2) 5.3477 mg/ml +/-s 0.02973 mg/ml s(rel) 0.56 % ============ 787 KF Titrino...
  • Page 17 5.676 ml res.tab: original <SELECT> • Press <SELECT> to display "delete n". This means that you wish to delete a single result with the index KFR volume 5.676 ml n in the result table. res.tab: delete n <ENTER> 787 KF Titrino...
  • Page 18 If you have connected a printer, a new report is printed out. Following this titer determination, you now decide to perform Karl Fischer determinations. The titer just determined will be automatically used here. 787 KF Titrino...

  • Page 19: Karl Fischer Titration

    3.459 ml you that you can now enter a number. Enter here, result unit: mg/ml;3 e.g. 1 decimal place and exit the inquiry by pressing <1> <QUIT> twice. <ENTER> <QUIT> The result is outputted in the new unit. 787 KF Titrino...

  • Page 20: Drift

    You can follow the progress of the drift. In fresh solvent Drift 4.3 µl/min the drift value should drop to less than 10 µL/min after a few minutes. <DRIFT> • Pressing <DRIFT> once again switches the drift display off. 787 KF Titrino...
  • Page 21 If you have connected a printer, the full report provides you with all data for recalculation of the result: date 2002-03-27 time 13:55:10 smpl size 0.03 g KFR volume 3.459 ml drift man. 2.2 µl/min (-d)time 1.03 water 922.2 mg/ml ============ 787 KF Titrino...

  • Page 22: Selection Of The Mode, Key

    The set values under the <CONFIG> and <PARAM> keys apply to all modes, whereas the calculations differ for each mode. Once values have been set they remain effective even if the instrument is switched off. 787 KF Titrino...

  • Page 23: Configuration, Key

    Selection of the polarization mode (I(pol), U(pol)) polarizer: I(pol) Polarization current(-127...127 µA) I(pol) 50 µA Endpoint voltage(-1500 mV...1500 mV) 250 mV cond. Polarization voltage(-1270...1270 mV, in steps of 10 mV) U(pol) 400 mV Endpoint current (-150...150 µA) 25 µA cond. 787 KF Titrino...
  • Page 24 (V vs. t, dV/dt vs. t, U vs. t, -U vs. t) V vs. t: Volume vs. time curve dV/dt vs. t: Drift vs. time curve U vs. t: Control deviation (current value – EP) vs. time curve 787 KF Titrino...
  • Page 25 KFR vol.: (ON, OFF) "ON" means the dispensed KFR volume will be displayed in the result output on the first line. Individual identification of devices (up to 8 ASCII device label characters) Display of program version program 787.0010 787 KF Titrino...

  • Page 26: Parameters, Key

    Safety stop, e.g. if no endpoint is found. **titr. <CLEAR> sets "OFF". Start volume (0.00…99.99 mL.) start V: 0.00 ml Performed and inquired only in KFT mode. cond. Start volume is dispensed before titration start. In the 787 KF Titrino...
  • Page 27 A smaller min.rate results in a slower titration. The minimum increment depends on the Exchange Unit: Exchange Unit min. 5 mL 0.5 µL 10 mL 1.0 µL 20 mL 2.0 µL 50 mL 5.0 µL 787 KF Titrino...
  • Page 28 Request of sample size after start of titration (ON, OFF) req.smpl size: Not performed or inquired in the "BLANK" mode. Selection of the result report on titration completion report: (short, full, OFF) cond. See also page 38. 787 KF Titrino...
  • Page 29 Titration with test of only be terminated after the extraction time is over. stop criterion Calculations Calculations are carried out. Data output Data are outputted. (Reconditioning) Conditioning is carried out. 787 KF Titrino...
  • Page 30 Remarks: • Titer determination should have the same parameters as the sample titrations. • In most cases the preset default parameters provide precise and reproducible results. • Ipol gives relatively steep curves. They are flatter with Upol. 787 KF Titrino...
  • Page 31 • If you select negative values for a polarization, you should choose negative values for all other parameters too in order to have compatible parameter sets. • In measurements with the setting "Upol", all parameters work in a similar manner as in measurements with the setting " Ipol". 787 KF Titrino...
  • Page 32 If the sample size request is switched off, and preconditioning is set, you are explicitly prompted to add your sample. For six seconds, the message "add sample" is displayed after which the titration is started by the Titrino itself. 787 KF Titrino...
  • Page 33 If you still have to open the titration cell for any reason, determine a blank value and take it into account for the calculation of the titration result (see page 34). 787 KF Titrino...
  • Page 34 • Reduce "max.rate". rapidly". The titration times become • With 2-component reagents the buffer capacity of the longer and longer. solvent can be exhausted. Change solution. • If the drift increases at the same time, see above. 787 KF Titrino...

  • Page 35: Result Calculations

    The titer is written in automatically from the titer cond. determination modes. Request only in the "KFT" mode. Factor ( 1000000) ± factor in the numerator of the formula. Entries for factors with cond. different units for results and sample size, see page 33f. 787 KF Titrino...
  • Page 36 "delete n": Deletion of single results with the index n. "delete all": The entire table is deleted. Delete data from sample number n (1...20) delete The deleted result is removed from the statistics cond. calculation. 787 KF Titrino...
  • Page 37 The factor is used to enter the water content of the standard. Standard used Sample size in... Factor Water 1000 Water µl density H O [g/mL] ≈ 1 Methanol content of methanol [g/mL] Methanol µl 0.001 * content of methanol [g/mL] Tart*2H 156.6 Tart*2H 0.1566 787 KF Titrino...
  • Page 38 The number of decimal places in the result output follows the separator ";". The number flashes to draw attention to the fact that this value can now be entered. Unit for the sample size (g, mg, mL, µL, pc, no unit ) smpl size unit: 787 KF Titrino...
  • Page 39 "delete all". • Recalculated single results are immediately incorporated in the statistics calculation. • If a result can not be calculated, the run counter is incremented. The counter for the number of reconciled single results remains unchanged, however. 787 KF Titrino...

  • Page 40: Drift Display, Key

    Do side reactions take place? • Does the sample contain ketones or aldehydes? etc. the magnitude of the stop drift as a stop criterion • (value above basic drift). 787 KF Titrino...

  • Page 41: Data Output

    Original reports which are put out automatically at the end of the titration and after every recalculation of the result. Original reports have double dashes ==== at the end, whereas recalculations are marked by single dashes ---- . Report outputs can be stopped with <QUIT>. 787 KF Titrino...
  • Page 42 Results can also be viewed in the display. After a determination the calculated result and the single results of the statistics calculations can be displayed with <SELECT>. <SELECT> switches to the next result, view also page 13. 787 KF Titrino...

  • Page 43: Error Messages, Troubleshooting

    The instrument adjustment data have been overwritten. system error 3 Exit: <CLEAR>. Default adjustment data are set. The error message appears each time the instrument is switched on until it has been readjusted (Metrohm service). 787 KF Titrino...
  • Page 44 Exit: <QUIT> Is the receiver switched on and ready to receive? The transmission of the Titrino has been interrupted with XOFF for at least 3 s. Exit: <QUIT>. The RS interface parameters are no longer the same for both instruments. 787 KF Titrino...

  • Page 45: What Can You Do If The Data Transfer Does Not Work

    Are the RS settings the same on both devices? garbled. Has the correct printer been selected? The printer does not emulate completely the preset Wrong line spacing. mode. Usually these problems arise with the IBM mode. Set the printer to a different mode (e.g. Epson). 787 KF Titrino...

  • Page 46: Diagnosis

    3.3. Diagnosis 3.3 Diagnosis 3.3.1 General The 787 KF Titrino is a very precise and reliable instrument. Thanks to its rugged con- struction it is virtually impossible for external mechanical or electrical influences to have an adverse effect on its functions.

  • Page 47: Equipment Required

    3.3. Diagnosis 3.3.3 Equipment required: voltage calibrator, e.g. 1.773.0010 Metrohm pH Simulator − or 1.767.0010 Calibrated Reference for mV, pH, Ω µS, °C highly insulated interconnection cable 6.2108.060 − cable 3.496.5070 − exchange units, if possible with different cylinder volumes (or 3.496.0070 dummy exchange unit) −...
  • Page 48 0 . . . 9 4 Cylinder code, date, time • Put exchange unit or dummy on the Titrino and put the burette tip into a collecting receptacle. 787 KF Titrino...
  • Page 49 Read off value an the connected voltmeter and compare with the mV value on the display. (Tolerance 2 mV) ± • Press <Quit>. • Disconnect voltmeter. 6 Motor timer test • Press <6>. m o t o r - t i m e r t e s t • Press <Enter>. 787 KF Titrino...
  • Page 50 . k . • Press <Clear>. d i a g n o s e p r e s s k e y 0 . . . 9 • Remove cable and resistor switch-box. 787 KF Titrino...
  • Page 51 8 External inputs and outputs This test is meaningful only if the 787 KF Titrino is used interconnected with other instruments via the 'Remote' con- nection. In addition, a 3.496.8510 test plug normally used in the repair service is required for this test. However, this plug can also be purchased by customers under the above number.
  • Page 52 R S 2 3 2 t e s t o . k . • Remove test plug. • Press <Clear>. d i a g n o s e p r e s s k e y 0 . . . 9 787 KF Titrino...
  • Page 53 • Set potentiometer 'dV/dt' to left stop. • Press <DOS> (on instrument) at same time and use a stopwatch to measure the time for 1/10 of the cylinder volume to be expelled. The time should be ca. 90 ... 110 787 KF Titrino...
  • Page 54 3.3. Diagnosis • Set potentiometer 'dV/dt' to right stop. • Press <FILL>. Setting up original arrangement Reconnect all peripherals disconnected at the start of the diagnostic routine and perform a short function test with these. 787 KF Titrino...
  • Page 55 However, possibly a small loss in accuracy must be antici- pated. A new optimum adjustment can be performed by Metrohm service. The error mes- sage 'system error 3' always appears after the instrument is switched on until this adjust- ment has been performed.

  • Page 56: Initialise And Test Ram

    The electronic circuits are now accessible! On no account touch these! • Remove spindle from mechanical stop by turning the large gear wheel. (In case that the motor is inoperative, position spindle by hand to zero position.) 787 KF Titrino...

  • Page 57: Releasing A Locked Spindle With Inserted Exchange Unit

    4.1 Setting up and connecting the instruments 4.1.1 Titrino with Titration Stand or Stirrer Cable Ti Stand or Stirrer 6.2130.060 Keypad The 728 Magnetic Stirrer can also be connected instead of the 703 Ti Stand. 787 KF Titrino...

  • Page 58: Connection Of A Printer

    DPU-414 data bit: stop bit: none parity: none handshake: send to: Seiko Custom 6.2125.130 baud rate: 9600 none, pre-set on Metrohm version DP40-S4N data bit: IDP-560 EMULATION FONT MAP =GERMANY stop bit: PRINT=REVERSE parity: none LITTLE CR CODE=VOID handshake: CR AFTER B :FULL=VOID...

  • Page 59: Connection Of A Balance

    The balance type must be preselected at the Titrino with the <CONFIG> key. Balance and printer can be connected at the same time with the aid of the 6.2125.030 adapter. The balance must then be plugged into the "data in" receptable of the adapter. 787 KF Titrino...
  • Page 60 If the balance works only with 7 bit and the printer with 8 bit and if they are at the same Titrino, the balance has to bet to "space parity" and Titrino/printer to 8 bit, "no parity". 787 KF Titrino...

  • Page 61: Connection Of A Kf Oven

    Oven Sample Processor are connected via the remote sockets (cable 6.2141.020). Cable (Remote) 6.2141.020 • The "Remote" socket allows not only connection of a sample changer but also additional control functions. Pin assignment of the "Remote" socket and control possibilities, see page 64f. 787 KF Titrino...

  • Page 62: Connection Of A Sample Changer

    730 or 760 Sample Changer at the same time. • The "Remote" socket allows not only connection of a sample changer but also additional control functions. Pin assignment of the "Remote" socket and control possibilities, see page 64f. 787 KF Titrino...

  • Page 63: Connection Of A Recorder

    Drift vs. time 100 µL/min: 1000 mV Drift curve, e.g. to observe the basic drift U vs. t Control deviation vs. 1 mV +1 mV timet -U vs. t Control deviation vs. 1 mV -1 mV time 787 KF Titrino...

  • Page 64: Connection Of A Computer

    Cable 6.2125.060 (+6.2125.010) Preselections on the Titrino: RS232 settings: ......... depend on the control program of the computer Send to:..........................IBM Vesuv 3.0, PC program for data acquisition and method backup for up to 64 devices ..................6.6008.200 787 KF Titrino...

  • Page 65: Connection Of Electrodes, Preparing Titration Vessel

    4.2 Connection of electrodes, preparing titration vessel Connection of electrodes, preparing titration ves- The 787 KF Titrino has one measuring input. Rear panel: Connection of polarized electrodes. If measured quantities Ipol or Upol are selected, this measuring input is automatically active.
  • Page 66 Arrangement of the parts on the titration vessel lid View from above: Electrode Sample addition Drying tube Stopper or aspirating tube Buret tip with titrant Stopper or dispensing tip This arrangement applies to the shown stir- ring direction. Stirrer 787 KF Titrino...

  • Page 67: Appendix

    10 000 steps per buret cylinder Titrating buret 1 internal buret Auxiliary buret additional: 776 or 765 Dosimat Materials Housing Polybutyleneterephthalate (PBTP) Keypad cover Polycarbonate (PC) Display LCD, 2 lines of 24 characters each Height of characters 5 mm LED back-lit 787 KF Titrino...
  • Page 68 100, 117, 220/230, 240 V (switchable) Frequency 50 ... 60 Hz Power consumption 15 W Fuse Thermal fuse Dimensions with Exchange Unit Width 150 mm Height 450 mm Depth 275 mm Weight, incl. keypad app. 3.6 kg 787 KF Titrino...

  • Page 69: Pin Assignment Of The "Remote" Socket

    +5 V not used pin 24 (Input 6) +5 V pin 12 (Input 7) Outputs pin 5 (Output 0) Ready inactive pin 18 (Output 1) Conditioning ok, active if Cond.ok pin 4 (Output 2) Titration, active during titration 787 KF Titrino...
  • Page 70 I ≤ 75 mA +5 V pin 14 0 V: active 5 V: inactive pin 25 Ordering numbers for plug: K.210.9004 (shell) and K.210.002 No liability whatsoever will be accepted for damage caused by im- proper interconnection of instruments. 787 KF Titrino...

  • Page 71: Lines Of The "Remote" Socket During The Titration

    5.2 Pin assignment of the "Remote" socket 5.2.1 Lines of the "Remote" socket during the titration 787 KF Titrino...

  • Page 72: Rs232 Interface

    The interface complies to the standard RS 232C. The RS232 interface allows full remote control of the Titrino with an external controller. Refer to your Metrohm agency if you need a detailed description of the RS232 interface and the remote control commands.

  • Page 73: Validation / Glp

    No. 255: Validation of Metrohm KF titrators and KF ovens according to GLP/ISO 9001. Contact your Metrohm agency for support with the validation of your Titrino. There you get a validation documentation, which helps you to perform the installation qualification (IQ) and the operational qualification (OQ).

  • Page 74: Warranty And Conformity

    Lack of an official damage report releases METROHM from any liability to pay compensation. If any instruments and parts have to be returned, the original pack- aging should be used if at all possible.

  • Page 75: Eu Declaration Of Conformity

    5.5 Warranty and conformity 5.5.2 EU Declaration of conformity EU Declaration of Conformity The METROHM AG company, Herisau, Switzerland hereby certifies, that the instrument: 787 KF Titrino meets the requirements of EC Directives 89/336/EEC and 73/23/EEC. Source of the specifications: EN 50081 Electromagnetic compatibility, basic specification;...

  • Page 76: Certificate Of Conformity And System Validation

    The features of the system software are docu- mented in the instruction manual. Metrohm Ltd. is holder of the SQS-certificate of the quality system ISO 9001 for quality assurance in design/development, production, installation and servic- ing.

  • Page 77: Scope Of Delivery And Ordering Designations

    NEMA/ASA (USA...) ................. 6.2122.070 1 Vesuv 3.0 light, PC program for data acquisition and method backup for 2 devices ....................6.6008.500 1 Instructions for Use for 787 KF Titrino ............... 8.787.1003 1 Quick Reference for 787 KF Titrino..............8.787.1013 787 KF Titrino...
  • Page 78 5... 70 mL ....................6.1418.150 10... 90 mL, order 6.2036.000 holding ring separately ........6.9914.023 20... 90 mL ....................6.1418.220 50... 150 mL ....................6.1418.250 Titration vessel lid (5 openings) ................6.1414.010 Magnetic stirring bars, length 12 mm......................6.1903.010 16 mm......................6.1903.020 25 mm......................6.1903.030 787 KF Titrino...
  • Page 79 AND balances (with RS232 interface OP-03) ............6.2125.020 Precisa balances ....................6.2125.080 Adapter for connection of printer/balance at the same COM ......6.2125.030 Connection of 768 KF Oven KF Oven........................ 2.768.0010 Cable 795 KFT Titrino — 768 KF Oven, control ........... 6.2141.010 787 KF Titrino...
  • Page 80 Cable Titrino — 730, 760 Sample Changer+665, 725, 765, 776 Dosimat ..6.2141.040 Cable Titrino — 730, 760 Sample Changer+ 2x 665, 725, 765, 776 Dosimat ... 6.2141.050 Cable Titrino — Control Unit 664 for Sample Changer 673/674......3.980.3560 787 KF Titrino...

  • Page 81: Index

    Fabrication number........5 printer ............54 ............31 factor recorder ..........59 ..........19 filling rate sample changer ........58 Formulas ........... 33 stirrer............53 Ti stand..........53 GLP ............69 Contrast of display ........3 Control lines .............65ff ..........20 handshake: .........39 cylinder empty 787 KF Titrino...
  • Page 82 Mean ..........21 run number delete result........... 32 Menu ............7 Sample ........22 min.volume incr. changer..........58 Mode Scope of delivery ........73 selection ..........18 Selection balance ..........20 Operating course ........8ff mode............. 18 787 KF Titrino...
  • Page 83 ........... 34 ...........20 stop bit: ..........22 stop crit: Stop criteria ..........28 Validation........... 69 ..........22 stop drift Values entry..........7 ............22 stop V .........39 stop V reached ............11 wait .........39 system error 3 Warranty ............ 70 ............22 t(delay) 787 KF Titrino...

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