Metrohm Titrino 758 KFD Instructions For Use Manual
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Metrohm Titrino 758 KFD Instructions For Use Manual

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CH-9101 Herisau/Switzerland
E-Mail
info@metrohm.com
Internet
www.metrohm.com
758 KFD Titrino
Program version 5.758.0022
Instructions for Use
8.758.1203
11.2001 / pkl

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  • Page 1 CH-9101 Herisau/Switzerland E-Mail info@metrohm.com Internet www.metrohm.com 758 KFD Titrino Program version 5.758.0022 Instructions for Use 8.758.1203 11.2001 / pkl...

  • Page 3: Table Of Contents

    Table of contents Table of contents 1 Introduction ........................ 1 1.1 Instrument description ....................1 1.2 Controls and parts ...................... 2 2 Manual operation ....................... 6 2.1 Keypad........................6 2.2 Principle of data input ....................7 2.3 Text input ........................8 2.4 Configuration, key <CONFIG>.................
  • Page 4 Table of contents 4 Error messages and Troubleshooting ..............137 4.1 Error and special messages.................. 137 4.2 Diagnosis....................... 142 4.2.1 General ......................142 4.2.2 Procedure ....................... 142 4.2.3 Equipment required: ..................143 4.2.4 Diagnosis steps ....................143 4.3 Initialize and test RAM ................... 154 4.4 Releasing a locked spindle ...................

  • Page 5: Introduction

    Introduction 1 Introduction 1.1 Instrument description The 758 KFD Titrino is a titrator for fast and precise water determination and endpoint titration with LCD graphical display. Titration curves can be observed in real-time. The 758 KFD Titrino controls up to three dosing units. The operator is almost free to define his titrations.

  • Page 6: Controls And Parts

    Introduction 1.2 Controls and parts Front view of instrument: 758 KFD Titrino...
  • Page 7 Introduction Exchange Unit Display Setting of display contrast Opening for the memory card Controls the dosing rate during manual dosing with <DOS> and subsequent filling Control keys and indicator lamps on the Titrino Key < > Power switch Key < >...
  • Page 8 Introduction Rear view of instrument: 758 KFD Titrino...
  • Page 9 With power supplies where the voltage is subject to severe HF distur- bances, the Titrino should be operated via an additional power filter, e.g. Metrohm 615 model. Connection for external dosing units D1 and D2 685 Dosimats or 700 Dosinos...

  • Page 10: Manual Operation

    2.1 Keypad 2 Manual operation 2.1 Keypad CONFIG Configuration. PARAM Parameters. SMPL DATA Sample data. STATISTICS ON/OFF switching of statistics calcula- tions of consecutive determination, see page 45. MEAS/HOLD ON/OFF switching of measurements between titrations and hold during titrations. SILO ON/OFF switching of silo memory for sample data, see page 63.

  • Page 11: Principle Of Data Input

    2.2 Principle of data input 2.2 Principle of data input • If you press a key, you will find a group of inquiries in the display. Example key <CONFIG>: configuration In the first line you see where you are: You pressed >monitoring key <CONFIG>...

  • Page 12: Text Input

    2.3 Text input 2.3 Text input Example storing a method: user methods • Press key <USER METH>. >store method Place the cursor to ">store method" and press method name: ******** <ENTER>. The name of the method which is currently in the working memory is displayed.

  • Page 13: Configuration, Key

    2.4 Configuration, key <CONFIG> 2.4 Configuration, key <CONFIG> Key <CONFIG> serves to enter device specific data. The set values apply to all modes. CONFIG monitoring: Monitoring of instrument validation, pH calibration, ser- vice interval and printout of diagnostic report. configuration >monitoring peripheral units: >peripheral units...
  • Page 14 2.4 Configuration, key <CONFIG> If "ON" has been set: Measuring input (1, 2, diff.) meas.input: Time interval for validation (1...9999 d) time interval Time counter (0...9999 d) time counter Counts the number of days since the last valid calibration at the selected measuring input. Monitoring the service interval (ON, OFF) service: Monitoring is carried out after the Titrino has been...
  • Page 15 2.4 Configuration, key <CONFIG> Automatic switching ON/OFF of the stirrer in the titration stirrer control: sequence (ON, OFF) If stirrer control is ON, the stirrer will be switched on at the beginning and switched OFF at the end of a de- termination.
  • Page 16 2.4 Configuration, key <CONFIG> Start delay (0...999999 s) start delay Delay time after start of methods. Abort start delay time with <QUIT>. Type of result display at the end of the determination result display: bold (bold, standard) bold: The calculated results are displayed in bold characters.
  • Page 17 2.4 Configuration, key <CONFIG> Selection of the dosing element (internal D0, external D1, external D2) dos.element: internal D0 internal D0: buret of the Titrino external D1/2: buret D1, D2, resp. Warning interval for prep (5...9999 min, OFF) warn.interv.DX OFF min Selection of the type of dosing element (Dosimat, Dosino) dos.drive:...
  • Page 18 2.4 Configuration, key <CONFIG> Settings with key <CONFIG> and power ON Proceed as follows: 1. Switch the Titrino OFF. 2. Press <CONFIG> and keep it pressed during switching the Titrino ON. The display shows the following: Setup lock: >lock Locking keys <CONFIG>, <PARAM> and <SMPL >curve DATA>, and the functions "recall method", "store method"...
  • Page 19 2.4 Configuration, key <CONFIG> curve >curve The settings are valid for COM1 and COM2. If you change the printer type, the following settings are initialized according to the printer. Grid drawing (ON, OFF) grid: Frame drawing (ON, OFF) frame: Type of scaling (Full, Auto) scaling: Full Full: The scaling goes from the greatest to the smallest...

  • Page 20: Selection Of The Mode, Key

    2.5 Selection of the mode, key <MODE> 2.5 Selection of the mode, key <MODE> Press key <MODE> until the desired mode is MODE displayed and confirm with <ENTER>. – Select the measured quantity pH, U, Ipol, Upol, (T) with <←> or <→> and confirm it also with <enter>. mode The following modes can be selected: mode:...

  • Page 21: Parameters, Key

    2.6 Parameters, key <PARAM> 2.6 Parameters, key <PARAM> The key <PARAM> is used for the entry of values that determine the modes. Values marked with "cond." are PARAM accessible during the conditioning in the SET and KFT mode. "**titr." means that these values can be changed during the titration.
  • Page 22 2.6 Parameters, key <PARAM> Maximum dosing rate (0.01...150 mL/min, max.) max.rate max. ml/min <CLEAR> sets "max.". **titr. This parameter determines primarily the addition rate outside the control range, see page 23. The maximum rate depends on the Exchange Unit: Exchange Unit max.
  • Page 23 2.6 Parameters, key <PARAM> Type of start volume (OFF, abs., rel.) start V: "OFF": start volume switched off cond. "abs.": absolute start volume in mL "rel.": relative start volume to sample size. If "abs." is set: start V 0.0 ml Absolute start volume (0...999.99 mL) cond.
  • Page 24 2.6 Parameters, key <PARAM> Stop conditions for titration >stop conditions If this is not "normal", i.e. after reaching the EP Type of stop volume (abs., rel., OFF) stop V: abs. "abs.": absolute stop volume in mL **titr. "rel.": relative stop volume to sample size "OFF": stop volume switched off.
  • Page 25 2.6 Parameters, key <PARAM> Request of identifications after start of titration (id1, req.ident: id1&2, all, OFF) cond. After start, sample identifications can be requested automatically: Only id1, id1 & id2, all three id's or no inquiries. Request of sample size after start of titration (value, req.smpl size: unit, all, OFF) cond.
  • Page 26 2.6 Parameters, key <PARAM> Titration sequence of KFT <START> After the start, the activate pulse is outputted and the stir- (Activate pulse) rer switched on. (Stirrer ON) (Start delay) The start delay time is waited off. If conditioning is on, the sample solution is titrated until (Preconditioning) the EP is reached.
  • Page 27 2.6 Parameters, key <PARAM> Control parameters for KFT The control parameters can be set according to your samples. The default parameters are already set to get satisfactory results. Optimize the control parameters for specific samples only. During the titration, reagent dosing is carried out in 3 phases: U/mV 1.
  • Page 28 2.6 Parameters, key <PARAM> Mechanisms of the KFT parameters in Ipol mode U/mV Excess H Titration (direct titration) EP at U Excess Iodine- Titration (Back titration) darker solution I(pol) I/µA • The position and curve characteristics of the line between the ranges of excess water or excess iodine depends on the type of sample and the ingredients of the working media.
  • Page 29 2.6 Parameters, key <PARAM> The determination of the free water is easily done, as far as the specifications of the reagent manufacturer regarding the "water capacity" of the reagents are considered. Problems may occur with specific sample matrices. The relevant literature contains many precise analysis instructions.
  • Page 30 2.6 Parameters, key <PARAM> In the following table we attempt to show you solutions related more to the instrument's side: What to do if ... Problem Possible causes and remedial action Dosing at end too long and • Increase "min.volume incr.". increments too small.

  • Page 31: Parameters For Set

    2.6 Parameters, key <PARAM> 2.6.2 Parameters for SET SET1, SET2: parameters >SET1 Control parameters for EP1 and EP2. >SET2 titration parameters >titration parameters are valid for the global titration sequence. >stop conditions >statistics stop conditions: >preselections Parameters for the termination of the titration. statistics: Calculation of mean values and standard deviation, see page 45.
  • Page 32 2.6 Parameters, key <PARAM> Minimum dosing rate (0.01...999.9 L/min) µ min.rate 25.0 µl/min This parameter determines the addition rate right at the **titr. start and the end of the titration, see also page 33. This parameter influences the titration speed and therefore its accuracy very strongly: A smaller min.rate results in a slower titration.
  • Page 33 2.6 Parameters, key <PARAM> Dosing rate for start volume dos.rate max. ml/min (0.01...150 mL/min, max.) **titr. <CLEAR> sets "max.". The maximum rate depends on the Exchange Unit: Exchange Unit max. rate 5 mL 15 mL/min 10 mL 30 mL/min 20 mL 60 mL/min 50 mL 150 mL/min...
  • Page 34 2.6 Parameters, key <PARAM> Stop conditions for titration >stop conditions If this is not "normal", i.e. after reaching the EP. Type of stop volume (abs., rel., OFF) stop V: abs. "abs.": absolute stop volume in mL. **titr. "rel.": relative stop volume to sample size. "OFF": stop volume switched off.
  • Page 35 2.6 Parameters, key <PARAM> Request of sample size after start of titration (value, unit, req.smpl size: all, OFF) cond. "all" the value and the unit will be requested. Limiting value check for sample size (ON, OFF) limit smpl size: With "ON" the error message "sample size out." ap- cond.
  • Page 36 2.6 Parameters, key <PARAM> Titration sequence of SET <START> After the start, the activate pulse is outputted and the stir- (Activate pulse) rer switched on. (Stirrer ON) (Start delay) The start delay time is waited off. If conditioning is on, the sample solution is titrated until (Preconditioning) the (first) EP is reached.
  • Page 37 2.6 Parameters, key <PARAM> Control parameters The control parameters can be set separately for each end point. Optimize your control parameters for routine analyses for samples with a rather low content. During the titration, reagent dosing occurs in 3 phases: U/mV 1.
  • Page 38 2.6 Parameters, key <PARAM> Relation between the stop criteria "time" and "drift" The stop criterion "time", t(delay), means that the end point must be exceeded for a certain period of time. In other words, after the last dosed increment, time t is allowed to elapse before the titration is stopped.
  • Page 39 2.6 Parameters, key <PARAM> If you have entered the endpoint and the control range (dynamics), the default values for the other control parameters should suffice for the first titration. If you encounter difficulties in optimizing your titration, the following table will be of use. How to proceed if ...

  • Page 40: Parameters For Meas

    2.6 Parameters, key <PARAM> 2.6.3 Parameters for MEAS measuring parameters parameters >measuring parameters determine the measurement. >statistics statistics: >preselections Calculation of mean values and standard deviation, see page 45. preselections: ON/OFF of various auxiliary functions such as auto- matic requests after the start and activate pulse. Measuring parameters >measuring parameters Drift criterion for measured value acquisition (input...
  • Page 41 2.6 Parameters, key <PARAM> Electrode test (OFF, ON) electrode test: Test for polarized electrodes. Performed on changeover from the inactive standby mode to a measurement. "OFF" means that the test is not performed. Temperature (–170.0...500.0 °C) temperature 25.0 °C Temperature is measured at the start if a T sensor is connected.

  • Page 42: Parameters For Cal

    2.6 Parameters, key <PARAM> 2.6.4 Parameters for CAL The calibration interval may be monitored, see page 9. calibration parameters parameters >calibration parameters determine the calibration procedure. >statistics statistics: Calculation of mean values and standard deviation, see page 45. Calibration parameters >calibration parameters Measuring input (1, 2, diff.) meas.input:...
  • Page 43 2.6 Parameters, key <PARAM> Calibration temperature and pH values of the buffers (which are temperature dependent) must therefore be entered in advance. The inputs in key <PARAM> are valid. Pulse output on the line "activate" (L6, pin 1) of the activate pulse: remote socket (all, first, OFF) See page 174.

  • Page 44: Parameters For Tip

    2.6 Parameters, key <PARAM> 2.6.5 Parameters for TIP In TIP, several commands and methods can be linked to make a titration procedure. The TIP sequence can be defined with <DEF>, see page 52. sequence parameters >sequence Parameters for the TIP sequence see page 52. >statistics statistics: >preselections...
  • Page 45 2.6 Parameters, key <PARAM> With polarized electrodes, instead of the measuring input the polarization current (–127...127 µ I(pol) 1 µA or the polarization potential (–1270...1270 mV, in steps of U(pol) 400 mV 10 mV) is inquired. Electrode test (OFF, ON) electrode test: Test for polarized electrodes.

  • Page 46: Result Calculations

    2.7 Result calculations 2.7 Result calculations Formula entry, key <DEF> Key <DEF> contains various inquiries for result calculations and data output. The data of this key are method specific and they are stored in the method memory together with the method. >formula formula: >silo calculations...
  • Page 47 2.7 Result calculations Text for result output (up to 8 characters) RS1 text Text input see page 8. Number of decimal places for result (0...5) RS1 decimal places Selection of result unit (%, ppm, g/L, mg/mL, mol/L, RS1 unit: mmol/L, g, mg, mL, mg/pc, s, mL/min, no unit or up to 6 characters).
  • Page 48 2.7 Result calculations Input of method specific operands C01...C19, key <C-FMLA> With <C-FMLA> the operands C01...C19 can be put C-FMLA in. For the calculation, the operands are used, which were introduced in the formula. The inputs method specific and are store in method memory.

  • Page 49: Statistics Calculation

    2.8 Statistics calculation 2.8 Statistics calculation Mean values, absolute and relative standard deviations are calculated. The <DEF> key is used to allocate results for statistics calculation. The entries are specific to the method and are stored in the method memory. mean: >formula Assigns values for statistics calculations.
  • Page 50 2.8 Statistics calculation How do you obtain statistics calculations? 1) Enter the allocations for the statistics calculation, see page 45. 2) Switch on the statistics calculations: Either with <STATISTICS> or set the status under <PARAM>, "> statistics" to "ON". The "STATISTICS" LED is on. Storing a method in the method memory, the status of the statistics calculation is retained.

  • Page 51: Common Variables

    2.9 Common variables 2.9 Common variables Common variables are used for: • Determination of a titer with a method. This titer is stored permanently as C3X. The operand C3X can be used in various other methods like any other operand. •...

  • Page 52: Data Output

    2.10 Data output 2.10 Data output 2.10.1 Reports for the output at the end of a determination With <DEF>, the report sequence at the end of the determination is defined. The entries are specific to the method and are stored in the method memory.
  • Page 53 2.10 Data output Original reports which are put out automatically at the end of the titration can be printed with recalculated values at any time. Key sequence: <PRINT><REPORTS><ENTER>. Original reports have double dashes ==== at the end, whereas recalculations are marked by single dashes ----.

  • Page 54: Display Of The Curve

    2.10 Data output Additional possibilities for report outputs In addition to the reports which are printed at the end of the titration, various other reports can be put out. There are 2 possibilities to select the reports: 1) <PRINT><←/→><ENTER> Cursor is pressed repeatedly until the desired report appears in the display.

  • Page 55: User Name, Key

    2.11 User name, key <USER> 2.11 User name, key <USER> USER The key <USER> manages the user names. User names can be entered directly or selected with ← the keys <←> and <→>. name: user Selection or input of user name. name: boss >delete...

  • Page 56: Tip, Titration Procedure

    2.12 TIP, Titration procedure 2.12 TIP, Titration procedure TIP (Titration Procedure) is used to link several commands in a sequence. TIP is selected with <MODE> and <ENTER>. TIP is an "empty shell" in which the sequence of the determination must be defined. Definition of the sequence With key <DEF>...
  • Page 57 2.12 TIP, Titration procedure Information for the commands (steps): Command Meaning Input range method Method from the user memory or from the card. This Name method runs as a submethod. pause Waiting time. The waiting time can be aborted with 0...999999 s, <QUIT>.
  • Page 58 2.12 TIP, Titration procedure Sequence of TIP As there is no preset sequence of TIP, in what follows the procedure is illustrated by a sequence that contains all available commands. <START> (Start delay) The start delay time is waited off. (Request ident.) The sample identifications and the sample size (Request smpl size)
  • Page 59 2.12 TIP, Titration procedure Preparation of submethods for use in TIP All titration data, i.e. curves and lists of measured points must be put out in the submethod as they are overwritten on return to TIP. Individual values from the submethod, e.g. endpoints or calculated results must be stored as temporary variables C7X.

  • Page 60: Method Memory, Keys And

    2.13 Method memory, keys <USER METH> and <CARD> 2.13 Method memory, keys <USER METH> and <CARD> 2.13.1 Key <USER METH> USER METH Management of the internal method memory with key <USER METH>. Select method name with keys <←> and <→>. recall method: user methods Loads a method from the internal method memory into...
  • Page 61 2.13 Method memory, keys <USER METH> and <CARD> The contents of the method memory can be printed with the key sequence <PRINT><USER METH><ENTER> Document your methods (e.g. parameter report, def. report and C-fmla report)! With a PC and the 6.6008.XXX Vesuv program, you should carry out a complete method backup periodically.

  • Page 62: Key

    2.13 Method memory, keys <USER METH> and <CARD> 2.13.2 Key <CARD> CARD Management of the method memory on the card with key <CARD >. Method names can be entered directly or select names with keys <←> and <→>. user meth. On the first line you find the name of the current >recall method directory (here user meth.).
  • Page 63 2.13 Method memory, keys <USER METH> and <CARD> Backup of the internal method memory on the >backup card (directory name with up to 10 characters) dir.name: Existing methods in this directory will be deleted, and all methods from the internal method memory are stored in the directory.
  • Page 64 2.13 Method memory, keys <USER METH> and <CARD> Internal method memory and methods on the card If methods are called from TIP or from the silo memory, the Titrino will search these methods primary in the internal method memory, and afterwards in the current directory of the card.

  • Page 65: Calibration Data, Key

    2.14 Calibration data, key <CAL.DATA> 2.14 Calibration data, key <CAL.DATA> With <CAL.DATA>, the current pH calibration data of CAL.DATA all measuring inputs can be seen. Calibration data are entered here automatically on completion of a calibration. cal.data input 1: >input 1 Calibration data for measuring input 1.

  • Page 66: Current Sample Data, Key

    2.15 Current sample data, key <SMPL DATA> 2.15 Current sample data, key <SMPL DATA> The key <SMPL DATA> can be used to enter the SMPL current sample data. The content of this key changes DATA when the silo memory is switched on, see page 64. Instead of entering the current sample data with <SMPL DATA>, you can request these data smpl data...

  • Page 67: Silo Memory For Sample Data

    2.16 Silo memory for sample data 2.16 Silo memory for sample data In the silo memory or pushup storage, sample data (method, identifications and sample size) can be stored. This is useful, e.g. when you work with Sample Changers and other automatic sample addition systems or if you wish an overview of your determination results, see page 66.
  • Page 68 2.16 Silo memory for sample data Key <SMPL DATA> with the silo memory switched on Sample data can be entered into the silo memory with SMPL key <SMPL DATA>. DATA edit silo lines: Entering sample data into the silo memory. smpl data delete silo lines: >edit silo lines...
  • Page 69 2.16 Silo memory for sample data Delete all silo lines >delete all silo lines Confirmation (yes, no) delete all: When all silo lines are deleted, the silo is completely empty: The line numbering starts again with 1. With "ON", worked off silo lines will be copied to the cycle lines: highest line of the silo memory (ON, OFF) Data cycling "on"...

  • Page 70: Storing Determination Results And Silo Calculations

    2.17 Storing determination results and silo calculations 2.17 Storing determination results and silo calcula- tions 2.17.1 Storing determination results If the sample-specific data of the silo memory should be kept after the determination and supplemented by results, the following entries are necessary: 1.

  • Page 71: Silo Calculations

    2.17 Storing determination results and silo calculations After several samples have been processed, the silo memory report can have the following appearance (printout with <PRINT><SILO><ENTER>): 758 KFD Titrino 10196 758.0022 date 2001-11-21 time 15:03 >silo cycle lines: save lines: sl method id 1/C21 id 2/C22 id 3/C23 processed silo 11-2...
  • Page 72 2.17 Storing determination results and silo calculations Starting from the following silo report: 758 KFD Titrino 10196 758.0022 date 2001-11-21 time 15:03 >silo cycle lines: save lines: method id 1/C21 id 2/C22 id 3/C23 ∗ 11-2 A/12 99-08-12 0.903g 2.6427ml 1.48% Assignment 0-15...
  • Page 73 2.17 Storing determination results and silo calculations • Calculations and assignments are carried out in the following order: 1. Calculation of the results RSX 2. Assignment of temporary variables C7X for TIP 3. Calculation of means MNX 4. Assignment of silo results C24 and C25 5.

  • Page 74: Manual Dosing And Preparation Of Titration Burets

    2.18 Manual dosing and preparation of titration burets 2.18 Manual dosing and preparation of titration burets 2.18.1 Manual dosing <PREP> serves as preselection for the buret: internal PREP D0, external D1, external D2. With <DOS>, the preselected buret will dose as long as <DOS>...

  • Page 75: Operation Via Rs232 Interface (Green Part)

    3.1 General rules 3 Operation via RS232 Interface 3.1 General rules The Titrino has an extensive remote control facility that allows full control of the Titrino via the RS 232 interface, i.e. the Titrino can receive data from an external controller or send data to an external controller. C R and L F are used as terminators for the data transfer.

  • Page 76: Call Up Of Objects

    3.1 General rules 3.1.1 Call up of objects An excerpt from the object tree is represented below: 3rd node Language Prog 2nd node RSSet 1st node Config Mode 0st node & Root Rules Example The root of the tree is designated by &. The branches (levels) of a tree are marked with a dot (.) when calling up an object.

  • Page 77: Triggers

    3.1 General rules 3.1.2 Triggers Triggers initiate an action on the Titrino, for example, starting a process or sending data. Triggers are marked by the introductory symbol $. The following triggers are possible: Starts processes, e.g. starting the mode run or setting the RS 232 interface parameters Stop Stops processes...

  • Page 78: Status Messages

    3.1 General rules 3.1.3 Status messages In order to have an efficient control by an external control device, it must also be possible to query status conditions; they provide information on the status of the Titrino. The trigger $D initiates output of the status. Status messages consist of the global status, the detailed status and eventual error messages, e.g.
  • Page 79 3.1 General rules Instrument in the TIP mode, requesting Id1 after start. .Req .Id1: Instrument in the TIP mode, requesting Id2 after start. .Id2: Instrument in the TIP mode, requesting Id3 after start. .Id3: Instrument in the TIP mode, requesting sample size after start. .Smpl: Instrument in the TIP mode, requesting unit of sample size after start.

  • Page 80: Error Messages

    3.1 General rules 3.1.4 Error messages Error messages are added to the status messages and separated from them by the sign ";". Card read/write error. Exit: Send new command. Wrong card, i.e. card has been removed/inserted during the inquiry. Exit: Send new command. The card has lost data.
  • Page 81 3.1 General rules RS receive errors: Parity. Exit: <QUIT> and ensure settings of appropriate parameters at both devices are the same. Framing error. Exit: <QUIT> and ensure settings of appropriate parameters at both devices are the same. Overrun error. At least 1 character could not be read. Exit: <QUIT>...
  • Page 82 3.1 General rules E135 Check temp.sensor in MEAS T or with activated temperature monitoring. Exit: Correct error or &m $S. E136 Same buffer in CAL. Measured value of the second buffer differs less than 6 mV from the measured value of the first buffer. Exit: Correct error or &m $S.
  • Page 83 3.1 General rules E197 Sample size is out of limits. Exit: The error message disappears on next start or on introduction of new sample size. E198 Validation interval is expired. Exit: The error message disappears on next start or clear counter with &Config.Monitoring.Validation.ClearCount $G.

  • Page 84: Remote Control Commands

    3.2 Remote control commands 3.2 Remote control commands 3.2.1 Overview The internal object tree can be divided into the following branches: & Root ├ Mode Method parameters ├ UserMeth Administration of the internal user-memory for methods ├ MemoryCard Administration of the memory card ├...
  • Page 85 3.2 Remote control commands &Mode Object Description Input range Reference & Root ├ Mode Mode $G, $S, $H, $C 3.2.2.1. : ├ QuickMeas Rapid meas. in basic mode $G, $S 3.2.2.2. ├ Select Mode selection KFT,SET,MEAS,CAL,TIP 3.2.2.3. ├ .SETQuantity Measured quantity for SET pH, U, Ipol, Upol ditto ├...
  • Page 86 3.2 Remote control commands *Parameter Tree part "Parameters for SET" ├ SET1 Control parameters for EP1 │ ├ Endpoint 1 depends on meas.quant. 3.2.2.12. │ ├ .UnitEp Unit of endpoint read only ditto │ ├ .Dyn Dynamics depends on meas.quant. 3.2.2.13. │...
  • Page 87 3.2 Remote control commands *Parameter Tree part "Parameters for KFT" ├ CtrlPara Control parameters │ ├ Endpoint depends on meas.quant. 3.2.2.31. │ ├ .UnitEp Unit of endpoint read only ditto │ ├ .Dyn Dynamics depends on meas.quant. 3.2.2.32. │ ├ .UnitDyn Unit of dynamics read only...
  • Page 88 3.2 Remote control commands *Parameter Tree part "Parameters for MEAS" ├ Measuring Measuring parameters │ ├ .SignalDrift Drift for meas.value acquisition depends on meas.quant. 3.2.2.34. │ ├ .UnitSigDrift Unit of measured value drift read only ditto │ ├ .EquTime Equilibrium time 0...9999, OFF ditto │...
  • Page 89 3.2 Remote control commands *Parameter Tree part "Parameters for TIP" ├ Sequence Sequence │ ├ Step 1 │ │ ├ .Select Step selection method,pause,L4 output,L6 output, │ │ info,prep,stirrer,OFF 3.2.2.45. │ │ ├ .Method Method from mem.or card special 3.2.2.46. │...
  • Page 90 3.2 Remote control commands &UserMeth Object Description Input range Reference & Root ├ UserMeth Method memory : ├ .FreeMemory Memory available read only 3.2.2.48. ├ .Recall Load method 3.2.2.49. │ ├ .Name Method name 8 ASCII characters ditto ├ .Store Save method ditto │...
  • Page 91 3.2 Remote control commands &MemoryCard Object Description Input range Reference & Root ├ MemoryCard Administration of the memory card : ├ .Recall Load method 3.2.2.51. │ ├ .Name Method name 8 ASCII characters ditto ├ .Store Save method ditto │ ├ .Name Method name 8 ASCII characters...
  • Page 92 Time interval for validation 1...7...9999 ditto │ │ ├ .Counter Time counter 0...9999 ditto │ ├ .Service Monitoring of Metrohm service 3.2.2.64. │ │ ├ .Status Status of service monitoring ON, OFF ditto │ │ ├ .Date Date of next service...
  • Page 93 3.2 Remote control commands "Configuration", continuation ├ .RSSet1 Settings RS232, 1 3.2.2.79. │ ├ .Baud Baud rate 300,600,1200,2400,4800, │ │ 9600,19200,38400,57600, │ │ 115200 ditto │ ├ .DataBit Number of data bits 7, 8 ditto │ ├ .StopBit Number of stop bits 1, 2 ditto │...
  • Page 94 3.2 Remote control commands &SmplData Object Description Input range Reference & Root ├ SmplData Sample data : ├ .Status Status of silo memory ON, OFF 3.2.2.92. ├ .OFFSilo Current sample data │ ├ .Id1 Sample identification 1 up to 8 ASCII char 3.2.2.93.
  • Page 95 3.2 Remote control commands &HotKey Object Description Input range Reference & Root ├ HotKey Keys with direct access : ├ .User User name 3.2.2.100. │ ├ .Name Input of user name up to 10 ASCII char ditto │ ├ .Delete Delete user ditto │...
  • Page 96 3.2 Remote control commands &Info Object Description Input range Reference & Root ├ Info Current data : ├ .Report Transmission of formatted reports $G 3.2.2.101. │ ├ .Select Report type configuration, parameters, │ smpl data, statistics, silo, calib │ C-fmla, def, user method, full, │...
  • Page 97 3.2 Remote control commands "Info", continuation │ ├ Endpoint │ │ ├ result │ │ │ ├ Value read only ditto │ │ │ ├ .Meas Measured value read only │ │ │ ├ .Mark without meaning │ │ ├ up to 9 EP's │...
  • Page 98 3.2 Remote control commands "Info", continuation ├ .ActualInfo Current data │ ├ .Inputs I/O Inputs │ │ ├ .Status Line status read only 3.2.2.109. │ │ ├ .Change Change of line status read only ditto │ │ ├ .Clear Clear change ditto │...
  • Page 99 3.2 Remote control commands &Assembly Object Description Input range Reference & Root ├ Assembly Assembly control ├ . Bur Buret │ ├ .Select Selection of buret internal D0, external D1 │ │ external D2 3.2.2.119. │ ├ .Empty Empties the buret $G,$S,$H,$C 3.2.2.120.
  • Page 100 3.2 Remote control commands &Setup Object Description Input range Reference & Root ├ Setup Settings for the operating mode ├ .Comport Output of automatic info 1,2,1&2 3.2.2.128. ├ .Keycode Send key code ON, OFF 3.2.2.129. ├ .Tree Sending format of path info │...
  • Page 101 3.2 Remote control commands "Setup", continuation ├ .AutoInfo Automatic message for changes 3.2.2.138. │ ├ .Status Switch AutoInfo on/off ON, OFF ditto │ ├ When mains is switched on ON, OFF ditto │ ├ Titrator infos │ │ ├ When "ready" ON, OFF ditto │...
  • Page 102 3.2 Remote control commands &Diagnose Object Description Input range Reference & Root ├ Diagnose Diagnose ├ .Report Output of adjustment parameters 3.2.2.144. 758 KFD Titrino...

  • Page 103: Description Of The Remote Control Commands

    3.2 Remote control commands 3.2.2 Description of the remote control commands 3.2.2.1. Mode $G, $S, $H, $C Start and stop ($G, $S) or hold of the current method (3.2.2.3) with $H and continue with $C. $G also serves to continue after inquiries of identifications and sample size af- ter the start (see 3.2.2.28) as well as after inquiries of calibration temperature and pH values of buffers (see 3.2.2.39 and 3.2.2.40).
  • Page 104 3.2 Remote control commands In place of "RSX", a result name may be entered (.TextRS). This name is out- putted in the report full, short, scalc full and scalc srt. It is used for the result and the corresponding mean value. The limit control for results can also be activated.
  • Page 105 3.2 Remote control commands 3.2.2.11. Mode.CFmla Mode.CFmla.1.Value 0...±999999 Mode.CFmla.2.Value etc., up to .19 Calculation constants specific to a method. Stored in the method memory of the Titrino. Operands specific to the sample (3.2.2.93 and 3.2.2.106) and val- ues of common variables (3.2.2.80) on the other hand are not stored with the methods.
  • Page 106 3.2 Remote control commands 3.2.2.16. Mode.Parameter.TitrPara.XPause 0...999999 Parameter for SET, KFT: Pause time in s. Runs before dosing the start vol- ume. 3.2.2.17. Mode.Parameter.TitrPara.StartV.Type abs., rel., OFF Mode.Parameter.TitrPara.StartV.V 0...999.99 Mode.Parameter.TitrPara.StartV.Factor 0...±999999 Mode.Parameter.TitrPara.StartV.Rate 0.01...150, max. Parameters for SET, KFT: Start volume. If an absolute start volume (abs.) has been selected, the volume in mL is valid.
  • Page 107 3.2 Remote control commands 3.2.2.22. Mode.Parameter.TitrPara.Temp –170.0...25.0...500.0 Parameters for SET, KFT: Titration temperature in °C. If a Pt100 or Pt1000 is connected, the temperature is measured continuously and the parameter .Temp is updated. The temperature is used for the temperature correction in pH measurements. 3.2.2.23.
  • Page 108 3.2 Remote control commands 3.2.2.27. Mode.Parameter.Presel.Cond ON, OFF Mode.Parameter.Presel.DriftDisp ON, OFF Mode.Parameter.Presel.DCor.Type auto, man., OFF Mode.Parameter.Presel.DCor.Value 0.0...99.9 Parameters for SET, KFT: .Cond: Conditioning ON/OFF .DriftDisp: Drift display during conditioning ON/OFF. .DCor.Type: Type of drift take-over for the drift correction. auto: Take-over of the drift value at start.
  • Page 109 3.2 Remote control commands 3.2.2.32. Mode.Parameter.CtrlPara.Dyn pH: 0.01...20.00, OFF U, Ipol: 1...2000, OFF Upol: 0.1...200.0, OFF Mode.Parameter.CtrlPara.UnitDyn read only Mode.Parameter.CtrlPara.MaxRate 0.01...10...150, max. Mode.Parameter.CtrlPara.MinIncr 0.1...9.9, min. Parameters for KFT: Control parameters. .Dyn: Dynamics (control range) in pH, mV (with U and Ipol) or µA (with Upol). The corresponding unit can be read with .UnitDyn.
  • Page 110 3.2 Remote control commands 3.2.2.36. Mode.Parameter.Measuring.Temp –170.0...25.0...500.0 Parameters for MEAS: Measurement temperature in °C. If a Pt100 or Pt1000 is connected, the temperature is measured. The temperature is used for the temperature correction in pH measurements. 3.2.2.37. Mode.Parameter.Measuring.TDelta 1...2...999999 Parameters for MEAS: Time interval in s for the acquisition of a measured value into the measuring point list.
  • Page 111 3.2 Remote control commands 3.2.2.44. Mode.Parameter.Calibration.ActPulse first, all, OFF Parameters for CAL: Output of a pulse on the I/O line "Activate", see page 174. 3.2.2.45. Mode.Parameter.Sequence.X.Select method, pause, L4 output, L6 output, info, prep, stirrer, OFF Parameters for TIP: Selection of an element for step X (X = 1...30). For the parameters of the elements see 3.2.2.46.
  • Page 112 3.2 Remote control commands 3.2.2.48. UserMeth.FreeMem read only Memory space, available for user methods or silo lines. $Q sends the number of free bytes, e.g. "4928". 3.2.2.49. UserMeth.Recall UserMeth.Recall.Name up to 8 ASCII characters UserMeth.Store UserMeth.Store.Name up to 8 ASCII characters UserMeth.Delete UserMeth.Delete.Name up to 8 ASCII characters...
  • Page 113 3.2 Remote control commands 3.2.2.52. MemoryCard.ChangeDir MemoryCard.ChangeDir.Name up to 10 ASCII characters MemoryCard.ChangeDir.Checksum MemoryCard.ChangeDir.Checksum.Value read only Changing the current directory. The action is carried out if "$G" is transmitted to the corresponding node. Do not use blank characters before and after name! The checksum characterizes the content of the directory.
  • Page 114 3.2 Remote control commands 3.2.2.60. MemoryCard.List.Card.1.Name read only MemoryCard.List.Card.1.Bytes read only for each directory List of all directories on the memory card with the following information: .Name: Name of the directory .Bytes: Number of bytes used by the directory 3.2.2.61. MemoryCard.List.ActDir.1.Name read only MemoryCard.List.ActDir.1.Mode read only...
  • Page 115 3.2 Remote control commands 3.2.2.65. Config.Monitoring.DiagRep ON, OFF Printing of system test report after each switching on of the Titrino. 3.2.2.66. Config.PeriphUnit.CharSet1 Epson, Seiko, Citizen, HP, IBM Config.PeriphUnit.CharSet2 Selection of the character set and the graphics control characters for COM1 resp.
  • Page 116 3.2 Remote control commands 3.2.2.72. Config.Aux.Set Config.Aux.Set.Date YYYY-MM-DD Config.Aux.Set.Time hh:mm Date and time. Input format of the date: Year-month-day, two-digit, enter leading zeros. Input format for the time: Hours:minutes, two-digit, enter leading zeros. Date and time have to be set with &Config.Aux.Set $G just after entry of the value.
  • Page 117 3.2 Remote control commands 3.2.2.79. Config.RSSet1 Config.RSSet1.Baud 300, 600, 1200, 2400, 4800, 9600, 19200, 38400, 57600, 115200 Config.RSSet1.DataBit 7, 8 Config.RSSet1.StopBit 1, 2 Config.RSSet1.Parity even, odd, none Config.RSSet1.Handsh HWs, SWchar, SWline, none $G sets all RS settings. The changes are performed only if the instrument is inactive.
  • Page 118 3.2 Remote control commands 3.2.2.87. Config.DosPrep.DX(.Dosimat).DosRate 0.01...150, max. Config.DosPrep.DX(.Dosimat).FillRate 0.01...150, max. Dosing and filling rate in mL/in for the preparation. Start sequence see 3.2.2.121. 3.2.2.88. Config.DosPrep.DX.Select Dosimat, Dosino Selection of buret type. Start sequence see 3.2.2.121. 3.2.2.89. Config.DosPrep.DX.Dosino.Outlet tip, flask Place where the liquid of the preparation is expelled.
  • Page 119 3.2 Remote control commands 3.2.2.94. SmplData.ONSilo.Counter.MaxLines read only SmplData.ONSilo.Counter.FirstLine read only SmplData.ONSilo.Counter.LastLine read only Information on silo memory. .MaxLines: Maximum possible number of silo lines. .FirstLine: Lowest valid silo line. .LastLine: Last occupied silo line. 3.2.2.95. SmplData.ONSilo.EditLine.1.Method up to 8 ASCII characters SmplData.ONSilo.EditLine.1.Id1 up to 8 ASCII characters SmplData.ONSilo.EditLine.1.Id2...
  • Page 120 3.2 Remote control commands 3.2.2.99. SmplData.ONSilo.SaveLines ON, OFF Silo lines are not deleted when they are worked off. Assigned results are stored as C24 and C25. "Save lines" can only be set to "ON" if the silo is completely empty. Delete the silo, see 3.2.2.97. 3.2.2.100.
  • Page 121 3.2 Remote control commands Reports which are sent from the Titrino are marked with space (ASCII 32) and ' at the beginning. Then an individual identifier for each report follows. Reports which are triggered by RS232 ($G) have the same introducer but without pre- ceding space, i.e.
  • Page 122 3.2 Remote control commands Recalculation of the measuring data is triggered with $G. .Write: With "ON", the following nodes can be overwritten: &Info.DetermData.MP.List, &Info.TitrResults.Var.C4X (X = 0...5), &Info.TitrResults.TempVar.C7X (X = 0...9), and &Mode.Name. .ExV: Volume of the exchange unit, with which the determination was executed .MPList.1.Attribute: Attribute .MPList.X: X coordinate, time...
  • Page 123 3.2 Remote control commands 3.2.2.107. Info.StatisticsVal.ActN read only Info.Statistics.1.Mean read only Info.Statistics.1.Std read only Info.Statistics.1.RelStd read only etc. up to .9 The current values of the statistics calculation. $Q sends, e.g. ActN: Current value of the individual results "3" Data for MN1: Mean: Mean value (decimal places as in result) "3.421"...
  • Page 124 3.2 Remote control commands 3.2.2.109. Info.ActualInfo.Inputs.Status read only Info.ActualInfo.Inputs.Change read only Info.ActualInfo.Inputs.Clear Info.ActualInfo.Outputs.Status read only Info.ActualInfo.Outputs.Change read only Info.ActualInfo.Outputs.Clear Status sends the current status of the I/O lines, Change sends the information regarding whether a change in status of a line has taken place since the last clearing, Clear clears the change information.
  • Page 125 3.2 Remote control commands 3.2.2.113. Info.ActualInfo.Titrator.CyclNo read only Info.ActualInfo.Titrator.V read only Info.ActualInfo.Titrator.Meas read only Info.ActualInfo.Titrator.dVdt read only Info.ActualInfo.Titrator.dMeasdt read only Info.ActualInfo.Titrator.dMeasdV read only Info.ActualInfo.Titrator.T read only $Q sends the current values in the following formats: MEAS CyclNo V(mL) 1.2345 1.2345 Meas: 3.6(mV) 3.345...
  • Page 126 3.2 Remote control commands 3.2.2.115. Info.ActualInfo.Oven.HeatTime read only Info.ActualInfo.Oven.SampleTemp read only Info.ActualInfo.Oven.LowTemp read only Info.ActualInfo.Oven.HighTemp read only Info.ActualInfo.Oven.GasFlow read only Info.ActualInfo.Oven.UnitFlow read only $Q sends the current values from a connected KF Oven. If no Oven is con- nected, the values are empty. .HeatTime: Heating time of sample in s.
  • Page 127 3.2 Remote control commands 3.2.2.121. Assembly.Bur.Prep $G, $S, $H, $C Starts the function "preparation". The parameters are under the function &Config.DosPrep, see 3.2.2.84 up to 3.2.2.91. 3.2.2.122. Assembly.Bur.Rates.Forward.Selected digital, analog Assembly.Bur.Rates.Forward.Digital 0...150, max. Assembly.Bur.Rates.Reverse.Selected digital, analog Assembly.Bur.Rates.Reverse.Digital 0...150, max. Expel and aspirating rate. Digital or analog control.
  • Page 128 3.2 Remote control commands 3.2.2.126. Assembly.Outputs.AutoEOD ON, OFF Assembly.Outputs.SetLines Assembly.Outputs.SetLines.L0 active, inactive, pulse, OFF up to .L13 Assembly.Outputs.ResetLines Setting the I/O output lines. .AutoEOD: The automatic output of the EOD (End of Determination) at the end of the determination can be switched off. Thus, for example, in conjunction with a Titrino several determinations can be per- formed in the same beaker.
  • Page 129 3.2 Remote control commands 3.2.2.129. Setup.Keycode ON, OFF ON means the key code of a key pressed on the Titrino is outputted. The key code comprises 2 ASCII characters. A keystroke of key 11 is sent as follows: The beginning of the message is marked by a space (ASCII 32). 3.2.2.130.
  • Page 130 3.2 Remote control commands 3.2.2.133. Setup.Mode.StartWait ON, OFF Setup.Mode.FinWait ON, OFF Holding points in the method sequence. If they are "ON", the sequence stops until "OFF" is sent. Switching the instrument on sets both nodes to OFF: .StartWait: Holding point right after starting a method or submethod in TIP (holding point after AutoInfo !".T.GC").
  • Page 131 3.2 Remote control commands .CyclNo: Cycle number. Together with the cycle time (see 3.2.2.118), a time frame can be set up. The other data belong to the corre- sponding cycle number. The cycle number is set to 0 at the start of a method and it is incremented until the end of the method.
  • Page 132 3.2 Remote control commands .T.N Conditioning Not OK: EP not reached (in SET, KFT with condition- ing). .T.Re Request: In the inquiry of an identification or the sample size after start of titration. .T.Si SiloEmpty: Silo empty, i.e. the last line has been removed from the silo memory.
  • Page 133 Initializes instrument, see page 153. All parameters are set to their default value and error messages are cleared. The user and silo memories will be de- leted. The user memory contains the default user methods from Metrohm. 3.2.2.143. Setup.InstrNo Setup.InstrNo.Value serial number, 8 ASCII characters Instrument identification for report output.

  • Page 134: Properties Of The Rs 232 Interface

    Parity Bit 1 or 2 Stop Bit Only a shielded data cable (for example, METROHM D.104.0201) may be used to couple the Titrino with foreign devices. The cable shield must be properly grounded on both instruments (pay attention to current loops; always ground in a star-head formation).
  • Page 135 3.3 Properties of the RS 232 Interface Titrino as Sender : Titrino external device XOFF Data output Data input Data output max. Data output disabled enabled characters Time max. characters: 2 characters at 300...9600 baud 16 characters at ≥ 19200 baud Software-Handshake, SWline Handshake input ports on the Titrino (CTS) are not checked.
  • Page 136 3.3 Properties of the RS 232 Interface Titrino as Sender: Titrino external device XOFF Data output line 1st line Data input Data output Data output disabled enabled Time Titrino transmission can be stopped by external instruments with XOFF. After XOFF is received the Titrino completes sending the line already started. If data output is disabled for more than 6 s by XOFF, E43 appears in the display.

  • Page 137: Pin Assignment

    3.3 Properties of the RS 232 Interface 3.3.2 Pin Assignment RS232C Interface Pin 3 Transmitted Data (TxD). If no data are transmitted, the line is held in the “ON” condition. Data Transmitted Data will only be sent when CTS is in the ”ON” condition. Pin 2 Received Data (RxD) Received Data...
  • Page 138 3.3 Properties of the RS 232 Interface Contact arrangement at plug (female) for RS 232C socket (male) View of soldered side of plug Ordering numbers: K.210.0381 and K.210.9045 No liability whatsoever will be accepted for damage or injury caused by im- proper interconnection of instruments.

  • Page 139: What Can You Do If The Data Transfer Does Not Work

    3.3 Properties of the RS 232 Interface 3.3.3 What can you do if the data transfer does not work? Problem Questions for remedial action No characters can be received on - Are the instruments switched on and cables plugged in a connected printer.

  • Page 141: Error Messages And Troubleshooting

    4.1 Error and special messages 4 Error messages and Troubleshooting Data transfer inoperative See measures on page 135. 4.1 Error and special messages XXX bytes missing. For the storage of a method or a silo line XXX bytes missing XXX bytes are missing or there is insufficient RAM for a TIP sequence.
  • Page 142 4.1 Error and special messages No temperature sensor is attached (with MEAS T or if the check T-sensor temperature monitoring is active). Exit: Connect Pt100 or Pt1000 or <STOP>. The data of the memory card are lost as the battery tension data lost was lower than 2.37 V.
  • Page 143 4.1 Error and special messages The method required by the sample data from the silo memory no method or in a TIP sequence is not available in the method memory. Exit: <CLEAR>. The common variable could not be assigned as the result or no new com.var.
  • Page 144 In TIP no further TIP can be called up as a submethod. second TIP call Exit: <CLEAR> and define new sequence. The service interval has elapsed. Contact Metrohm service so service is due that the Titrino can be serviced. This message will appear each time the Titrino is switched on.
  • Page 145 4.1 Error and special messages Validation interval has elapsed. validate instrument Exit: <CLEAR> or new start. The memory card is from an other apparatus or the card was wrong card inserted/removed during an operation with <CARD>. Exit: <CLEAR> With SET or KFT with preset titration direction, the first wrong sample measured value is outside the end point.

  • Page 146: Diagnosis

    It is advisable in each case to isolate the fault with the rapid and easy to perform diagnos- tic tests. The customer thus need not call METROHM service until there is a true fault in the instrument. In addition, with the aid of the numbering in the diagnostic program he can provide the service engineer with much more accurate information.

  • Page 147: Equipment Required

    4.2 Diagnosis 4.2.3 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 − resistor switch-box, class 0.1 % (or resistor 14.3 k, 0.1 %) −...
  • Page 148 4.2 Diagnosis Fig. 1 Complete character set Keypad test • Press <1>. k e y s t e s t • Press <ENTER>. k e y s t e s t matrix code • If any key is now pressed (on the 6.2130.080 keypad or on the front panel of the 758), the appropriate matrix code appears in the display.
  • Page 149 4.2 Diagnosis Cylinder code, date, time • Insert exchange unit or dummy to the internal dosing unit D0 and put the buret tip into a collecting receptacle. • If available, connect the external dosing units D1 or D2 with the exchange units. •...
  • Page 150 1 . . . 5 6.1 Examination of highly insulated measuring inputs • Connect ‘Ind I’ measuring input to a voltage calibrator (e.g. Metrohm 773 pH simu- lator) by means of a highly insulated cable (e.g. 6.2108.060). Set calibrator to 0 V.
  • Page 151 4.2 Diagnosis • Press <CLEAR>. a n a l o g i n p u t t e s t 1 . . . 5 6.2 To check Pt 100 / 1000 connection • Connect a Pt 100 or Pt 1000 sensor, or sockets 1 and 2 or 2 and 3, respectively of the 767.0010 Calibrated reference to the sockets ‘Pt 100/1000’...
  • Page 152 4.2 Diagnosis d i a g n o s e p r e s s k e y 0 . . . 9 • Remove 767 or cable and resistor switch-box. External inputs and outputs This test is meaningful only if the 758 KFD Titrino is used interconnected with other instruments via the 'Remote' con- nection.
  • Page 153 4.2 Diagnosis • Press <CLEAR>. d i a g n o s e p r e s s k e y 0 . . . 9 7.2 Test of the remote box The remote box needs to be connected before the Titrino is switched on. Insert 3.496.8550 test plug in the remote box.
  • Page 154 4.2 Diagnosis 8.1 RS232 test 1 • Press <1>. RS232 test-connector? 1 • Insert the 3.496.8560 test plug in port ‘A1’. • Press <ENTER>. Test sequence: 1. In case of an error an error message is displayed. If for example no test plug is con- nected, error message error 69 appears).
  • Page 155 4.2 Diagnosis Memory card test • Press <9>. memory card test • Insert memory card. The memory card has to be formatted from a 758 KFD Titrino otherwise the test does not recognize the card and on the display appears „memory card 000 KB end“.
  • Page 156 4.2 Diagnosis • Remove exchange unit. • Check spindle zero position, see Fig. 3. 0.2 - 0.6 mm Fig. 6 Fig. 7 The spindle must be 0.2 – 0.6 mm below the edge of the sliding plate. The bar of the stopcock coupling must be exactly parallel to the lateral edges of the KFD Titrino, see Fig.4.
  • Page 157 4.2 Diagnosis 11 External dosing units D 1 or D 2 This test makes sense only when the 758 KFD Titrino is operated in connection with ex- ternal dosing units (685 Dosimat or 700 Dosino). The spindle drive and the cock changeover drive of the internal dispensing unit can be checked with the aid of the function <PREP>...

  • Page 158: Initialize And Test Ram

    The initialization values are loaded automatically. The instrument thus remains capable of measurement. However, possibly a small loss in accuracy must be anticipated. A new optimum adjustment can be performed by Metrohm service. The error message always appears after the instrument is switched on until this 'system error 3' adjustment has been performed.

  • Page 159: Releasing A Locked Spindle

    4.4 Releasing a locked spindle 4.4 Releasing a locked spindle with inserted Exchange Unit • The buret drive may very occasionally jam at the top or bottom end of the cylinder. If jamming occurs at the top or when the drive is out of function, the Exchange Unit can no longer be removed.

  • Page 160: Preparations

    5.1 Setting up and connecting the instruments 5 Preparations The mains cables supplied with the instrument are three-core and equipped with a plug with an earthing pin. If a different plug has to be fitted, the yellow/green lead must be connected to the protective earth.

  • Page 161: Titrino With External Burets

    5.1 Setting up and connecting the instruments 5.1.2 Titrino with external burets 685 Dosimat: 6.2134.030 Cable 700 Dosino The 2.700.0020 Dosino can be directly connected. If you wish to connect a 2.700.0010 Dosino, you need the 6.2134.020 adapter cable. 758 KFD Titrino...

  • Page 162: Connection Of A Printer

    DPU-414 data bit: stop bit: none parity: none handshake: send to: Seiko Custom 6.2134.110 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 163: Connection Of A Balance

    5.1 Setting up and connecting the instruments 5.1.4 Connection of a balance The following balances can be connected to the RS232 output of the Titrino: Balance Cable Sartorius MP8, MC1 6.2134.060 Shimadzu BX, BW 6.2125.080+6.2125.010 Settings on Titrino: balance SARTORIUS Balance: delimiter CR+LF...

  • Page 164: Connection Of A Kf Oven

    5.1 Setting up and connecting the instruments inputted from the balance. For this, the address of the identifications and method, resp. must be preselected on the input unit. Balance Method Sartorius METH or 27 ID.1 or 26 ID.2 or 24 C-20 or 23 Mettler (AT) D (Mthd)

  • Page 165: Connection Of A Sample Changer

    5.1 Setting up and connecting the instruments When the RS interfaces are not connected then the following setting must be made at the Titrino: <PARAM>, >preselections, "Oven: no". If you enter one of the COMs of the Titrino for this parameter then your Titrino result report will contain the oven data "heating time", "sample temp.", "lowest temp.", "highest temp."...

  • Page 166: Connection Of The 774 Oven Sample Processor

    5.1 Setting up and connecting the instruments 5.1.7 Connection of the 774 Oven Sample Processor The Oven Sample Processor heats the sample and transfers the moisture from the sample to the titration vessel of the Titino. Titrino and Oven Sample Processor are connected via the remote sockets (cable 6.2141.020) as well as via the RS interfaces (cable 6.2125.110) 6.2141.020 Cable...

  • Page 167: Connection Of A Computer

    5.1 Setting up and connecting the instruments 5.1.8 Connection of a computer 6.2134.040 Cable (9/9 pins) 6.2125.010+6.2125.060 Cables (9/25 pins) 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..................
  • Page 168 5.1 Setting up and connecting the instruments Settings at the Titrino: Under key <CONFIG>, >peripheral units, "Remote Box: on" Barcode: The barcode string goes to the entry field in which the cursor is currently lo- input cated. If the silo memory is switched on the barcode string always goes to the method method.
  • Page 169 5.1 Setting up and connecting the instruments 5.1.9.3 Operating via a PC keyboard: The Titrino can be operated from the PC keyboard. The Titrino functions are called up as follows: Titrino function Key combination Remarks on PC keyboard <C-FMLA> Alt F <CAL.DATA>...
  • Page 170 5.1 Setting up and connecting the instruments The numerical block (with NumLock) and the number keys on the PC keyboard simulate the functions of the numerical keys on the Titrino. For example, entering <7> in the basic state of the Titrino switches the statistics on. Keys which are used for setting an accent (e.g.

  • Page 171: Connection Of Electrodes And Preparing Titration Vessel

    5.2 Connection of electrodes and preparing titration vessel 5.2 Connection of electrodes and preparing titration vessel Connection for separate reference electrode. Rear panel: Input is free when a combined electrode is used. Connection of polarized electrodes. If measured quantities Ipol or Upol are selected, this measuring input is automatically active.
  • Page 172 5.2 Connection of electrodes and preparing titration vessel Practical tips • Glass electrodes should be preconditioned in the solvent used for ca. 1 hour. • If the potential jump after the first dispensing step is too large, a small start volume may help. •...
  • Page 173 5.2 Connection of electrodes and preparing titration vessel Setting up the KF titration vessel For volumetric KF titrations install the titration vessel according to the following figure: Electrode cable 6.2104.020 Drying tube Double Pt-electrode 6.1403.040 6.0338.100 Stopper Screw nipple 6.2730.030 6.2730.010 Titration vessel lid...

  • Page 174: Appendix

    6.1 Technical specifications 6 Appendix 6.1 Technical specifications Modes KFT: Karl Fisher Titration SET: Set End point Titration MEAS: Measurement CAL: pH calibration TIP: Links commands to titration procedure Measuring inputs 2 high-impedance measuring inputs for pH, redox and ISE electrodes.
  • Page 175 Flash Read only Internal memory Method memory for up to 100 methods Data bank with 25 Metrohm methods Silo memory for sample data and results RS232 interface 2 separate interfaces, each can be configured for printer, balance or computer connection: completely...
  • Page 176 Voltage 100...240 V Frequency 50...60 Hz Power consumption 15 W Fuse 2 x 1 ATH (to be replaced by Metrohm Service only using the same type) Additional electronic overload protection Dimensions with Exchange Unit Width 150 mm Height 450 mm...

  • Page 177: Pin Assignment Of The "Remote" Socket

    6.2 Pin assignment of the "Remote" socket 6.2 Pin assignment of the "Remote" socket external Function Inputs +5 V +5 V pin 21 (Input 0) Start +5 V +5 V pin 9 (Input 1) Stop +5 V +5 V > 100 ms pin 22 (Input 2) Enter Functions see page 175.
  • Page 178 6.2 Pin assignment of the "Remote" socket Outputs pin 17 (Output 3) End of determination pin 3 (Output 4) L4 in TIP pin 16 (Output 5) Error, active with errors pin 1 (Output 6) Activate pulse, see page 175. L6 in TIP pin 2 (Output 7) Pulses for recorder (t =150 µs)

  • Page 179: Lines Of The "Remote" Socket During The Titration

    6.2 Pin assignment of the "Remote" socket 6.2.1 Lines of the "Remote" socket during the titration 758 KFD Titrino...

  • Page 180: Possible Configurations Of The Activate Pulse In Set, Kft And Cal

    6.2 Pin assignment of the "Remote" socket 6.2.2 Possible configurations of the activate pulse in SET, KFT and CAL 758 KFD Titrino...

  • Page 181: User Methods

    6.3 User methods 6.3 User methods 6.3.1 General The methods are stored in the user memory ready for use. They can be loaded, modified and overwritten. Connect the printer to COM1 of the Titrino. If you have no printer connected, you have to delete the reports under the key <DEF>, >report.

  • Page 182: Kf Titer Determination With H O Or Methanol Standard "H2Otiter

    Karl-Fischer-Titration according to display drift: Eugen Scholz, Riedel de Haën, Seelze, Ger- drift corr: many req.ident: req.smpl size: value METROHM Application Bulletin No. 77: limit smpl size: Karl Fischer Water Determinations oven: activate pulse: ------------ 758 KFD Titrino 758.0022...

  • Page 183: Kf Titer Determination With Sodium Tartrate "Tartiter

    Karl-Fischer-Titration according to display drift: drift corr: Eugen Scholz, Riedel de Haën, Seelze, Ger- req.ident: many req.smpl size: value METROHM Application Bulletin No. 77: limit smpl size: Karl Fischer Water Determinations oven: activate pulse: ------------ 758 KFD Titrino 758.0022...

  • Page 184: Blank Determination For Kft "Blank_Kf

    HYDRANAL® Practical Course, Water re- req.ident: agents for Karl-Fischer-Titration according to req.smpl size: Eugen Scholz, Riedel de Haën, Seelze, Ger- limit smpl size: many oven: METROHM Application Bulletin No. 77: activate pulse: Karl Fischer Water Determinations ------------ 758 KFD Titrino 758.0022 date 2001-11-21...

  • Page 185: Kf-Titration With Blank Value Subtraction "Kf-Blank

    Karl-Fischer-Titration according to req.ident: Eugen Scholz, Riedel de Haën, Seelze, Ger- req.smpl size: many limit smpl size: METROHM Application Bulletin No. 77: oven: Karl Fischer Water Determinations activate pulse: ------------ 758 KFD Titrino 758.0022 date...
  • Page 186 6.3 User methods 758 KFD Titrino 758.0022 date 2001-11-21 time 18:04 Ipol KF-Blank >formula Water=(EP1-C38)*C39*C01/C00/C02 RS1 text Water RS1 decimal places RS1 unit: RS1 limit control: Titer=C39 RS2 text Titer RS2 decimal places RS2 unit: mg/ml RS2 limit control: Blank=C38 RS3 text Blank RS3 decimal places...

  • Page 187: Kf-Titration Without Blank Value Subtraction "Kf

    Karl-Fischer-Titration according to mean res.tab: original Eugen Scholz, Riedel de Haën, Seelze, Ger- >preselections many conditioning: METROHM Application Bulletin No. 77: display drift: Karl Fischer Water Determinations drift corr: req.ident: req.smpl size: limit smpl size: oven: activate pulse:...
  • Page 188 6.3 User methods 758 KFD Titrino 758.0022 date 2001-11-21 time 18:06 Ipol >formula Water=EP1*C39*C01/C00/C02 RS1 text Water RS1 decimal places RS1 unit: RS1 limit control: Titer=C39 RS2 text Titer RS2 decimal places RS2 unit: mg/ml RS2 limit control: >silo calculations match id: >common variables >report...

  • Page 189: Kf Titrations With Various Kf Reagents

    6.3 User methods 6.3.7 KF titrations with various KF reagents If you work parallel with different KF reagents, you can use different methods for each KF reagent. The titer determination is performed with H O or methanol standard as described for the method "H2OTiter".

  • Page 190: 8Titer Determination Of Sodium Hydroxide "Tit.naoh

    Dissolve in 40 mL distilled water (free of car- meas.input: temperature 25.0 °C bonate). time interval >stop conditions References: stop V: abs. METROHM Application Bulletin No. 206: stop V 99.99 ml Titer determinations in potentiometry filling rate max. ml/min >statistics status: mean res.tab: original >preselections...

  • Page 191: Titer Determination Of Hydrochloric Acid "Tit.hcl

    D0 Dissolve in 40 mL distilled water. meas.input: temperature 25.0 °C References: time interval >stop conditions METROHM Application Bulletin No. 206: stop V: abs. Titer determinations in potentiometry stop V 99.99 ml filling rate max. ml/min >statistics status: mean res.tab:...

  • Page 192: P- And M-Value "P+M Val

    6.3 User methods 6.3.10 p- and m-Value "p+m val." Determination of the acid capacity of water 758 KFD Titrino 758.0022 and waste water. date 2001-11-21 time 14:48 p+m val. parameters The p-value represents the amount of acid to >SET1 be added to reach the pH value 8.2 (color EP at pH 8.20 change of phenolphthalein).
  • Page 193 6.3 User methods 758 KFD Titrino 758.0022 date 2001-11-21 time 14:48 p+m val. >formula p value=EP1*C36 RS1 text p value RS1 decimal places RS1 unit: mmol/l RS1 limit control: m value=EP2*C36 RS2 text m value RS2 decimal places RS2 unit: mmol/l RS2 limit control: >silo calculations...

  • Page 194: Determination Of The Bromine Number "Brnumber

    RS1 decimal places References: RS1 unit: RS1 limit control: ASTM D 1159-84 >silo calculations Metrohm Application Bulletin No. 177 match id: Remark: >common variables In this titration, sharp changes of the meas- >report ured potential may occur and therefore, the report COM1:full;...

  • Page 195: Determination Of The Formaldehyde Number "Formolno

    FormolNo=C70*C01 RS1 text FormolNo RS1 decimal places RS1 unit: RS1 limit control: References: >silo calculations Metrohm Application Bulletin No. 180: match id: Automatic determination of the formol number >common variables in fruit and vegetable juices. >report report COM1:full; >mean MN1=RS1 >temporary variables...
  • Page 196 6.3 User methods Submethods preparation and addition of formaldehyde "FormoPre" 758 KFD Titrino 758.0022 date 2001-11-21 time 18:08 In a first SET titration the sample solution is ti- FormoPre trated to pH 8.5 with NaOH. parameters >SET1 EP at pH 8.50 dynamics max.rate...
  • Page 197 6.3 User methods Submethod determination of the formaldehyde number "FormoDet" Second SET titration with NaOH to pH 8.5 758 KFD Titrino 758.0022 after the addition of formaldehyde. date 2001-11-21 time 18:11 FormoDet parameters >SET1 EP at pH 8.50 dynamics max.rate 10.0 ml/min min.rate 25.0 µl/min...

  • Page 198: Titrino Validation

    Metrohm Application Bulletin No. 252: Validation of Metrohm Titrators (potentiometric) according to GLP/ISO 9001. No. 255: Validation of Metrohm KF Titrators and KF Oven according to GLP/ISO 9001. The validation interval can be checked by the Titrino (set under <CONFIG>, monitoring).

  • Page 199: 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 200: Eu Declaration Of Conformity

    6.5 Warranty and conformity 6.5.2 EU Declaration of conformity EU Declaration of Conformity The company Metrohm AG, Herisau, Switzerland, certifies herewith, that the following instrument: 758 KFD Titrino meets the CE mark requirements of EU Directives 89/336/EWG and 73/23/EWG. Source of specifications: EN 50081 Electromagnetic compatibility —...

  • Page 201: 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 202: Scope Of Delivery And Ordering Designations

    6.6 Scope of delivery and ordering designations 6.6 Scope of delivery and ordering designations 758 KFD Titrino ..................2.758.0010 inclusive the following accessories: 1 Keypad for KFD Titrino 758 ................6.2130.080 1 Memory card for methods................. 6.2245.010 1 Key for Exchange Units..................6.2739.010 1 Double Pt-electrode with plug-in head, without cable ........
  • Page 203 6.6 Scope of delivery and ordering designations Options Accessories to separate order and on payment of extra charge: Burets Titrating burets 685 Dosimat ......................2.685.0010 Cable 758 KFD Titrino — 685 Dosimat ..............6.2134.030 700 Dosino ......................2.700.0020 Auxiliary burets 765 Dosimat ......................
  • Page 204 6.6 Scope of delivery and ordering designations Titration equipment Equipment for KF titrations .................6.5609.000 Titration vessel, volumes 1... 50 mL ....................6.1415.110 5... 70 mL ....................6.1415.150 10... 90 mL, order 6.2036.000 holding ring separately ........6.1415.210 20... 90 mL ....................6.1415.220 50... 150 mL ....................6.1415.250 70...
  • Page 205 6.6 Scope of delivery and ordering designations Balance For Mettler cables you need an adapter 9/25 pins ..........6.2125.010 Cable Sartorius – balances MP8, MC1 (9/25 pins) ..........6.2134.060 Cable Shimadzu – balances BX, BW ..........6.2125.080+6.2125.010 Ohaus Voyager, Explorer, Analytical Plus balances........cable from Ohaus Mettler AB, AG balances (interface LC-RS25)..........cable with balance Mettler AT balance ...............

  • Page 206: Index

    Index Index Keys are marked with < >, are in bold characters, and pages concerning the display texts green part are printed in italic. Computer connection ......163 COM X characteristics ........130ff <ABC> ............8 configuration........12 Accessories........... 198ff pin assignment........133 .....
  • Page 207 Index <DEF>..........6, 42ff ..........65 delete all: Fabrication number........5 ......65 delete all silo lines ........19, 20, 28, 30 factor ...........64 delete line n ..........13 fill rate ............45 delete n Filling rate Delete after determination......20, 30 common variables .......47 after manual dosing.......
  • Page 208 Index <DOS> ..........3 ........18 min.volume incr. <ENTER> ..........6 ..........138 missing EP <MEAS/HOLD>........6 <MODE> ..........16 <MODE> ..........16 Mode <PARAM> ........17ff CAL ............38 <PREP>..........70 KFT ............17 <PRINT>........49, 50 MEAS ........... 36 <QUIT>..........
  • Page 209 Index Printing.............48ff RS232 interface Printer characteristics........130ff connection .........158 configuration ........12 problems ..........135 pin assignment ........133 selection ..........10 ..........11 run number Problems KF titrations ..........26 printer ..........135 ..........139 same buffer SET titrations ........38 Sample addition ........25 ............12 program Sample changer........
  • Page 210 Index Statistics values Titration modes ......... 16 delete results........46 Titration parameters report............ 48 KFT ............17 silo............67 SET ............27 Stirrer connection ........156 Titration sequence ............ 52 KFT ............22 stirrer: ........11 SET ............32 stirrer control: <STOP>.............

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