Metrohm Titrino 719 S Instructions For Use Manual
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Metrohm Titrino 719 S Instructions For Use Manual

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CH-9101 Herisau/Switzerland
E-Mail
info@metrohm.com
Internet
www.metrohm.com
719 S Titrino
Program version 5.719.0021
Instructions for Use
8.719.1103
03.2002 / pkl

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  • Page 1 CH-9101 Herisau/Switzerland E-Mail info@metrohm.com Internet www.metrohm.com 719 S Titrino Program version 5.719.0021 Instructions for Use 8.719.1103 03.2002 / pkl...

  • Page 3: Table Of Contents

    Table of contens Table of contents Introduction ......................1 Instrument description................... 1 Controls and parts ....................2 Manual operation....................6 Keypad ........................6 Principle of data input.................... 7 Text input ....................... 8 Tutorial ........................9 2.4.1 Entering data, setting the dialog language............ 9 2.4.2 Development of a method, titration of an acid..........
  • Page 4 Table of contents 4.2.3 Equipment required: .................. 107 4.2.4 Diagnosis steps ..................107 Initialise and test RAM..................116 Releasing a locked spindle with inserted Exchange Unit ......... 117 Preparations .....................118 Setting up and connecting the instruments ............118 5.1.1 Titrino with Stirrer or Titration Stand............118 5.1.2 Connection of a printer ................

  • Page 5: Introduction

    1.1 Instrument description Introduction 1.1 Instrument description The 719 S Titrino is a titrator to perform fast and precise endpoint titrations. Ready-to-start methods for the most common applications are stored in the internal method memory. The operator is free to modify and overwrite this methods or to create and store his own titration sequences.

  • Page 6: Controls And Parts

    1.2 Controls and parts 1.2 Controls and parts Front view of instrument: 719 S Titrino...
  • Page 7 1.2 Controls and parts Exchange Unit Display Setting of display contrast Controls the dosing rate during manual dosing with <DOS> and subse- quent filling Control keys and indicator lamps on the Titrino Key <DOS> Dosing key. Dispensing is performed as long as <DOS> is being pressed.
  • Page 8 1.2 Controls and parts Rear view of instrument: 719 S 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

    2.1. Keypad 2 Manual operation 2.1 Keypad CONFIG Configuration. PARAM Parameters. SMPL DATA Sample data. STATISTICS ON/OFF switching of statistics calcu- lations of consecutive determination, see page 41. MEAS/HOLD ON/OFF switching of measurements between titrations and hold during ti- trations. SILO ON/OFF switching of silo memory for sample data, see page 51.

  • 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 the corresponding menu in the display. Example key <CONFIG>: In the first line you see where you are: You pressed configuration key <CONFIG>...

  • Page 12: Text Input

    2.3. Text input 2.3 Text input Example storing a method: <USER METH> • Press key <USER METH>, the group ">recall method" appears. user methods >recall method <USER METH> <ENTER> • Choose ">store method" by pressing <USER METH> and press <ENTER>. >store method The name of the method which is currently in the method name:...

  • Page 13: Tutorial

    2.4 Tutorial 2.4 Tutorial This short operating course teaches you to work quick and efficient with the 719 S Titrino, by means of the most important applications. Set up your Titrino and connect the peripheral devices needed, see chapter 5. 2.4.1 Entering data, setting the dialog language We can thus make a start and first take a look at the fundamentals of the entry of data.
  • Page 14 2.4. Tutorial Because this inquiry follows no colon ":" the value can't be selected by <SELECT>, the date "fecha" has to be entered with the numeric keys. <QUIT> • Exit the inquiries with <QUIT>. You are one level higher in the "configuration" menu showing the title configuration "ajustes varios"...

  • Page 15: Development Of A Method, Titration Of An Acid

    2.4 Tutorial 2.4.2 Development of a method, titration of an acid Selection of the mode <MODE> • Press <MODE> repeatedly until "SET" appears in the display. For a description of the SET mode see mode page 30ff. mode <ENTER> • Confirm "SET" with <ENTER> SET pH ******** SET:...
  • Page 16 2.4. Tutorial Minimum titration rate inside the control range. >SET1 min.rate 25.0µl/min 2 × <QUIT> • Quit the inquiry with <QUIT>. For the titration put a Exchange Unit with c(NaOH) = 0.1 mol/L on the Titrino and rinse the tubing and the buret Tipp with <DOS>. Fill the buret again with <STOP/FILL>. Plug a combined pH glass electrode into measuring input 1 (Ind I).
  • Page 17 2.4 Tutorial Calculate the content of your hydrochloric acid in g/L: RS1=EP1*C01*C02/C00 RS1=EP1*C01*C02/C00 End point*conc.(titrant)*molecular weight/sample size <ENTER> To correct a formula, delete it with <CLEAR>. Confirm the formula with <ENTER>. • >formula You may enter a text for the result output, see page RS1 text •...
  • Page 18 2.4. Tutorial Entry of the sample size 4 x <SMPL DATA> Press <SMPL DATA> repeatedly until "sample size" • appears in the display. smpl data smpl size 1.0 g <2> Enter 2. • <ENTER> smpl data smpl unit: <SELECT> Use <SELECT> to select the unit "mL" and confirm •...
  • Page 19 2.4 Tutorial Print reports 3 x <DEF> Press <DEF> repeatedly until the display shows: • >report <ENTER> Press <ENTER> to move to the definition of reports. • report: 3 x <SELECT> With <SELECT> you select the individual repot • <;> blocks.

  • Page 20: Storage And Loading Of Methods

    2.4. Tutorial 2.4.3 Storage and loading of methods Now store the method you have just developed in the method memory. Storage of a method 2 × <USER METH> • Press <USER METH> repeatedly until the title ">store method" appears in the display. user methods >store method <ENTER>...

  • Page 21: Ph Calibration

    2.4 Tutorial 2.4.4 pH calibration For end-point titrations, however, where titration is performed to a fixed, specified pH value, a calibration should be performed. Selection of the calibration mode, CAL <MODE> • Press <MODE> repeatedly until "CAL" appears in the display and confirm the mode with <ENTER>. mode mode <ENTER>...

  • Page 22: Statistics, Acid Capacity Of Drinking Water

    2.4. Tutorial 2.4.5 Statistics, acid capacity of drinking water Let us now determine the acid capacity of drinking water. For this, the SET (set endpoint titration) mode is used to titrate to pH = 4.3. Load the method "Acid", the one that you just have stored in the method memory, see page 16 .
  • Page 23 2.4 Tutorial If the previous titration has run to your satisfaction, you can start thinking about perform- ing statistics calculations. Have you already added a new sample to the titration vessel? If you are no longer certain, you can find out immediately with <MEAS/HOLD>. Rapid measurement between titrations Press <MEAS/HOLD>.
  • Page 24 2.4. Tutorial Mean value of 2 single determinations. >statistics • Enter "3" to include an additional determination. mean: <3> <ENTER> 2 × <QUIT> • Quit the inquiry. Perform another titration. You can now decide which of the results is an "outlier". You can delete it from the statistics calculation.

  • Page 25: Configuration, Key

    2.5 Configuration, key <CONFIG> 2.5 Configuration, key <CONFIG> Key <CONFIG> serves to enter device specific data. The set values apply to all modes. CONFIG peripheral units: configuration Selection of printer, balance and the curve at the ana- >peripheral units log output. auxiliaries: e.g.
  • Page 26 2.5. Configuration, key <CONFIG> General settings >auxiliaries Selection of dialog language (english, deutsch, dialog: english francais, español, italiano, portugese, svenska) Current date (YYYY-MM-DD) date 2001-03-13 Format: Year-month-day, entry with leading zeros. Current time (HH-MM) time 08:13 Format: Hours-minutes, entry with leading zeros. Current run number for result output (0...9999) run number The sample number is set to 0 when the instrument is...
  • Page 27 2.5 Configuration, key <CONFIG> Values of the common variables >common variables Common variables C30...C39 (0.. 999 999) ± The values of all common variables are displayed. For etc. creating of common variables see page 43. 719 S Titrino...

  • Page 28: Selection Of The Mode, Key

    2.6. Selection of the mode, key <MODE> 2.6 Selection of the mode, key <MODE> MODE Press key <MODE> until the desired mode is displayed and confirm with <ENTER>. – Select the measured quantity pH, U, Ipol, Upol, (T) with > <SELECT>...

  • Page 29: Parameters, Key

    2.7 Parameters, key <PARAM> 2.7 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 mode. "**titr." means that these values can be changed dur- ing the titration.
  • Page 30 2.7. Parameters, key <PARAM> Maximum dosing rate (0.01...150 mL/min, max.) max.rate 10.0 ml/min <CLEAR> sets "max.". **titr. This parameter determines primarily the addition rate outside the control range, see also page 31. The maximum rate depends on the Exchange Unit: Exchange Unit max.
  • Page 31 2.7 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 32 2.7. 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 33 2.7 Parameters, key <PARAM> Preselections for the sequence >preselections Automatic conditioning of titration vessel. (ON, OFF) conditioning: If conditioning is "on", between the titrations the titration solution is constantly maintained at the (1st) end point. When conditioning is performed, the volume drift can be displayed during the conditioning: Display of drift during conditioning (ON, OFF).
  • Page 34 2.7. Parameters, key <PARAM> Titration sequence of SET <START> After the start, the activate pulse is outputted. (Activate pulse) (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. The display shows then (<START>...
  • Page 35 2.7 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 36 2.7. 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 37 2.7 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 38: Parameters For Meas

    2.7. Parameters, key <PARAM> 2.7.2 Parameters for MEAS measuring parameters parameters determine the measurement. >measuring parameters statistics: Calculation of mean values and standard deviation, see also page 41. 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 39 2.7 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 40: Parameters For Cal

    2.7. Parameters, key <PARAM> 2.7.3 Parameters for CAL calibration parameters parameters determine the calibration procedure. >calibration parameters statistics : Calculation of mean values and standard deviation, see also page 41. Calibration parameters >calibration parameters Measuring input (1, 2, diff.) meas.input: Measuring input 1 or 2 or differential amplifier;...
  • Page 41 2.7 Parameters, key <PARAM> Calibration with sample changer (ON, OFF) sample changer cal: In calibrations with a sample changer, there are no hold points in the calibration sequence for inputs. Calibration temperature and pH values of the buffers (which are temperature dependent) must therefore be entered in advance.
  • Page 42 2.7. Parameters, key <PARAM> Calibration sequence <START> After the start, the activate pulse is output. (Activate pulse) (Start delay) The start delay time is waited off. Then, the calibration temperature is measured. Measuring cal.temp. It no T sensor is connected, you enter the temperature manually.

  • Page 43: Result Calculations

    2.8 Result calculations 2.8 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: Formulas for result calculations.
  • Page 44 2.8. 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 45: Statistics Calculation

    2.9 Statistics calculation 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: Assigns values for statistics calculations.
  • Page 46 2.9. Statistics calculation How do you obtain statistics calculations? 1) Enter the allocations for the statistics calculation, see page 41. 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 47: Common Variables

    2.10 Common variables 2.10 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 48: Data Output

    2.11. Data output 2.11 Data output 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 49 2.11 Data output Example of reports: Full result report 719 S Titrino 18200 719.0021 date 2002-03-13 time 17:34 pHc(init) 6.29 SET pH Acid 0.0628 ml 4.26 m value 5.02 mmol/l mean(2) m value 5.04 0.028 mmol/l 0.56 Device label (if there is a designation, see page device label Titr 1 sign:...
  • Page 50 2.11. Data output Result display without printer Results can also be viewed in the display. With <SELECT> key, the appropriate section (EP's, results, etc.) can be selected and <ENTER> can be used to view the individual EP's, results etc. <SELECT>: display <ENTER>: display Remarks calculated results...

  • Page 51: Method Memory, Keys

    2.12 Method memory, keys <USER METH> 2.12 Method memory, keys <USER METH> Management of the internal method memory with key USER METH <USER METH>. Method identifications can be entered directly or selected with the <SELECT> key. recall method: user methods Loads a method from the internal method memory into >recall method the working memory.
  • Page 52 2.12. Method memory, keys <USER METH> 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 from time to time.

  • Page 53: Calibration Data, Key

    2.13 Calibration data, key <CAL.DATA> 2.13 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. input 1: cal. data Calibration data for measuring input 1.

  • Page 54: Current Sample Data, Key

    2.14. Current sample data, key <SMPL DATA> 2.14 Current sample data, key <SMPL DATA> The key <SMPL DATA> can be used to enter the SMPL current sample data. The contents of this key change DATA when the silo memory is switched on, see page 52. Instead of entering the current sample data with <SMPL DATA>, you can request these data smpl data...

  • Page 55: Silo Memory For Sample Data

    2.15 Silo memory for sample data 2.15 Silo memory for sample data In the silo memory or pushup storage, sample data (method, identifications and smpl size) can be stored. This is useful, e.g. when you work with Sample Changers and other automatic sample addition systems.
  • Page 56 2.15. 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: smpl data Entering sample data into the silo memory. >edit silo lines delete silo lines: Deletes single silo lines.
  • Page 57 2.15 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 59: Operation Via Rs232 Interface

    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 60: 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 61: 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, for ex. starting the mode run or setting the RS 232 interface parameters Stop Stops processes...

  • Page 62: 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 63 3.1 General rules Status conditions of the global $C: The status conditions of the global $C are identical with the ones of the global status $G. They appear when the process has been restarted actively from the status "Hold" ($C, key <meas/hold> or automatically after elimination of an error).

  • Page 64: 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 ";". Check exchange unit. Exit: Mount Exchange Unit (properly) or &m $S. Check electrode, short circuit. Exit: Rectify fault or &m $S. Check electrode, break.
  • Page 65 3.1 General rules RS receive errors: Parity Exit: <QUIT> and ensure settings of appropriate parameters at both devices are the same. Stop Bit 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 66 3.1. General rules E120 Overrange of the primary measured value (pH, U, Ipol, Upol or T with MEAS T). The secondary measured value (temperature) may be instable as well. Exit: Correct error or &m $S. E123 Missing EP for calculation. Exit: The error message disappears on next startup or on recalculation.

  • Page 67: 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 ├ Config Instrument configuration ├...
  • Page 68 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 SET, MEAS,CAL 3.2.2.3. ├ .SETQuantity Measured quantity for SET pH, U, Ipol, Upol ditto...
  • Page 69 3.2 Remote control commands *Parameter Tree part "Parameters for SET" ├ SET1 Control parameters for EP1 │ ├ Endpoint 1 depends on meas.quant. 3.2.2.10. │ ├ .UnitEp Unit of endpoint read only ditto │ ├ .Dyn Dynamics depends on meas.quant. 3.2.2.11. │...
  • Page 70 3.2. Remote control commands *Parameter Tree part "Parameters for MEAS" ├ Measuring Measuring parameters │ ├ .SignalDrift Drift for meas.value acquisition depends on meas.quant. 3.2.2.27. │ ├ .UnitSigDrift Unit of measured value drift read only ditto │ ├ .EquTime Equilibrium time 0...9999, OFF ditto │...
  • Page 71 3.2 Remote control commands &UserMeth Object Description Input range Reference & Root ├ UserMeth Method memory : ├ .FreeMemory Memory available read only 3.2.2.37. ├ .Recall Load method 3.2.2.38. │ ├ .Name Method name 8 ASCII characters ditto ├ .Store Save method ditto │...
  • Page 72 3.2. Remote control commands &Config Object Description Input range Reference & Root ├ Config Instrument configuration ├ .PeriphUnit Selection of peripheral units │ ├ .CharSet External printer Epson,Seiko,Citizen │ │ IBM,HP 3.2.2.40. │ ├ .Balance Selection of balance Sartorius,Mettler,Mettler AT │...
  • Page 73 3.2 Remote control commands &SmplData Object Description Input range Reference & Root ├ SmplData Sample data : ├ .Status Status of silo memory ON, OFF 3.2.2.51. ├ .OFFSilo Current sample data │ ├ .Id1 Sample identification 1 up to 8 ASCII char 3.2.2.52.
  • Page 74 3.2. Remote control commands &Info Object Description Input range Reference & Root ├ Info Current data : ├ .Report Transmission of formatted reports $G 3.2.2.58. │ ├ .Select Report type configuration, parameters, │ smpl data, statistics, silo, calib │ C-fmla, def, user method, full, │...
  • Page 75 3.2 Remote control commands │ ├ up to 9 mean values │ ├ .ActualInfo Current data │ ├ .Inputs I/O Inputs │ │ ├ .Status Line status read only 3.2.2.64. │ │ ├ .Change Change of line status read only ditto │...
  • Page 76 3.2. Remote control commands &Assembly Object Description Input range Reference & Root ├ Assembly Assembly control ├ . Bur Buret │ ├ .Rates Rates │ │ ├ .Forward Forward rate │ │ │ ├ .Select Type of rate control digital, analog 3.2.2.72.
  • Page 77 3.2 Remote control commands &Setup Object Description Input range Reference & Root ├ Setup Settings for the operating mode ├ .Keycode Send key code ON, OFF 3.2.2.77. ├ .Tree Sending format of path info │ ├ .Short Short format of path ON, OFF 3.2.2.78.
  • Page 78 3.2. Remote control commands │ │ ├ Continue after "hold" ON, OFF ditto │ │ ├ Conditioning OK ON, OFF ditto │ │ ├ Conditioning not OK ON, OFF ditto │ │ ├ Request after start ON, OFF ditto │ │ ├ Silo empty ON, OFF ditto...
  • Page 79 3.2 Remote control commands &Diagnose Object Description Input range Reference & Root ├ Diagnose Diagnose ├ .Report Output of adjustment parameters 3.2.2.91. 719 S Titrino...

  • Page 80: 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 3.2.2.25) as well as after inquiries of calibration temperature and pH values of buffers (see 3.2.2.31 and 3.2.2.32).
  • Page 81 3.2 Remote control commands Assignment of common variables. The values of the common variables are to be found in &Config.ComVar. They can be viewed and entered there, see 3.2.2.50. 3.2.2.7. Mode.Def.Report.Assign SET, MEAS, CAL: full, short, calc, param, calib, ff Definition of the report sequence, which is outputted automatically at the end of the determination.
  • Page 82 3.2. Remote control commands 3.2.2.12. Mode.Parameter.SET1.Stop.Type drift, time Mode.Parameter.SET1.Stop.Drift 1...20...999 Mode.Parameter.SET1.Stop.Time 0...10...999, inf Mode.Parameter.SET1.Stop.StopT 0...99 999, OFF Parameters for SET: Type and size of the stop criterion of the titration. .Type: Type of stop criterion after stop drift or switch-off delay time. .Drift: Stop drift in µL/min.
  • Page 83 3.2 Remote control commands Selection of the measuring input; valid with measured quantities pH and U. "diff." means differential amplifier, see page 124. With Ipol, the inquiries for the polarization current in µA (Ipol) and .PolElectrTest are valid. With Upol, the inquiry for the polarization voltage in mV (Upol) is valid. Entry in steps of 10 mV.
  • Page 84 3.2. Remote control commands delete all: Clear entire statistics table. The results can not be reac- tivated. .ResTab.DelN: Specification of the line number to be deleted. 3.2.2.23. Mode.Parameter.Presel.Cond ON, OFF Mode.Parameter.Presel.DriftDisp ON, OFF Parameters for SET: .Cond: Conditioning ON/OFF .DriftDisp: Drift display during conditioning ON/OFF. 3.2.2.24.
  • Page 85 3.2 Remote control commands Mode.Parameter.Measuring.PolElectrTest ON, OFF Parameters for MEAS: Selection of the measuring input; valid with measured quantities pH and U. "diff." means differential amplifier, see page 124. With Ipol, the inquiries for the polarization current in µA (Ipol) and .PolElectrTest are valid.
  • Page 86 3.2. Remote control commands Parameters for CAL: Calibration at Titrino. With "ON", there are no hold points in the calibration sequence for entries, the first buffer is measured directly. 3.2.2.36. Mode.Parameter.Calibration.ActPulse first, all, OFF Parameters for CAL: Output of a pulse on the I/O line "Activate", see page 131.
  • Page 87 3.2 Remote control commands Selection of the balance type and the signal at the analog output. 3.2.2.42. Config.Aux.Language english, deutsch, francais, espanol, italiano, portugese, svenska Selection of the dialog language. 3.2.2.43. 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.
  • Page 88 3.2. Remote control commands $G sets all RS settings. The changes are performed only if the instrument is inactive. After the setting of the interface parameters, wait at least 2 s to allow the components to equilibrate. Settings of the values for the data transmission via the RS interface: baud rate, data bit, stop bit, parity and type of handshake, see also page 95ff.
  • Page 89 3.2 Remote control commands .UnitSmpl: If "no unit" is desired for the sample size, the blank string must be entered. 3.2.2.55. SmplData.ONSilo.DelLine SmplData.ONSilo.DelLine.LineNum 1...99, OFF Deletion of a silo line. The line # is deleted with &SmplData.ONSilo.DelLine $G. If a formerly deleted line is edited again, it becomes valid (function "unde- lete").
  • Page 90 3.2. Remote control commands Info.CalibrationData.Inp1.Date read only Info.CalibrationData.Inp1.ElectrodeId read only identical for .Inp2 and .Diff pH calibration data for measuring input 1. After the calibration, the data are entered automatically together with the date of the calibration and the elec- trode identification, see 3.2.2.34.
  • Page 91 3.2 Remote control commands C44: (Last measured) temperature in °C. Used for the temperature compensation in pH measurements. C45: Start volume with SET in ml, "2.800". C46: Asymmetry pH of CAL, "6.89". C47: Relative electrode slope of CAL, "0.9950". 3.2.2.63. Info.StatisticsVal.ActN read only Info.Statistics.1.Mean read only...
  • Page 92 3.2. Remote control commands 3.2.2.66. Info.ActualInfo.Assembly.Counter.V read only Info.ActualInfo.Assembly.Counter.Clear $Q sends the volume. With the function &Info.Assembly.Counter.Clear $G, the volume counter is set to zero. 3.2.2.67. Info.ActualInfo.Assembly.Meas read only Info.ActualInfo.Assembly.PistonPos read only $Q sends the current measured value from the assembly. Piston position: initial position (filled) 10 000 =...
  • Page 93 3.2 Remote control commands Info.ActualInfo.Display.L2 up to 24 ASCII characters Lines of the display. The display can be written to from the computer. Pro- ceed as follows: Lock the display, see 3.2.2.80. $Q sends the contents of the corresponding display line. 3.2.2.71.
  • Page 94 3.2. Remote control commands .Ipol: Polarization current in µA. .Upol: Polarization potential in mV, entry in steps of 10 mV. 3.2.2.76. Assembly.Outputs.AutoEOD ON, OFF Assembly.Outputs.SetLines Assembly.Outputs.SetLines.L0 active, inactive, pulse, OFF up to .L 3 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.
  • Page 95 3.2 Remote control commands 3.2.2.80. Setup.Lock.Keyboard ON, OFF Setup.Lock.Config ON, OFF Setup.Lock.Parameter ON, OFF Setup.Lock.SmplData ON, OFF Setup.Lock.UserMeth.Recall ON, OFF Setup.Lock.UserMeth.Store ON, OFF Setup.Lock.UserMeth.Delete ON, OFF Setup.Lock.Display ON, OFF ON means disable the corresponding function: .Keyboard: Disable all keys of the Titrino .Config: Disable the <configuration>...
  • Page 96 3.2. Remote control commands Selection of the values from Assembly for the output in the set time interval (see 3.2.2.82): .CyclNo: Cycle number of the potential measurement. Together with the cycle time (3.2.2.81), a time frame can be set up. The cycle number is set to 0 on switching on the instrument and it is always incremented as long as the instrument remains switched on.
  • Page 97 3.2 Remote control commands ON means that the Titrino reports automatically the moment the correspond- ing change occurs. .Status: Global switch for all set AutoInfo. PowerOn: Simulation of power on (3.2.2.87). Not from mains. Messages from node .T, Titrator: .T.R Ready: Status 'Ready' has been reached.
  • Page 98 Initializes instrument, see page 116. 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. 3.2.2.90. Setup.InstrNo Setup.InstrNo.Value serial number, 8 ASCII characters Instrument identification for report output.

  • Page 99: 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 100 3.3 Properties of the RS 232 Interface Titrino as Receiver : Titrino external device max. 22 60 characters characters Data output Time of 4 XOFF characters XOFF Data input String is 400 µs processed Time Titrino as Sender : Titrino external device XOFF Data output...
  • Page 101 3.3 Properties of the RS 232 Interface Titrino as Receiver : Titrino external device Input Titrino disabled Data output XOFF Data input String is 400 µs processed Time Titrino as Sender: Titrino external device XOFF Inquiry Data output Response L 1st line Data input Data output...
  • Page 102 3.3 Properties of the RS 232 Interface Titrino as Sender: Titrino external device Time The data flow can be interrupted by deactivating the CTS line. Hardware-Handshake, HWf All handshake inputs are checked at the Titrino, handshake outputs are set. Titrino as Receiver : Titrino external device Time...

  • Page 103: Pin Assignment

    3.3 Properties of the RS 232 Interface 3.3.2 Pin Assignment RS232C Interface 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 and DSR are in the ”ON” condition and DCD is in the "OFF"...
  • Page 104 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.210.9004 and K.210.0001 No liability whatsoever will be accepted for damage or injury caused by im- proper interconnection of instruments.

  • Page 105: 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 107: Error Messages, Troubleshooting

    4.1 Error and special messages 4 Error messages, Troubleshooting Data transfer inoperative See measures on page 101. 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. Remedy: <QUIT>.
  • Page 108 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). With SET, with preset titration direction the first measured wrong sample value is outside the end point.
  • Page 109 4.1 Error and special messages 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.

  • Page 110: 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 111: 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 − cable 3.496.5070 − exchange units, if possible with different cylinder volumes (or 3.496.0070 dummy exchange unit) −...
  • Page 112 4.2. Diagnosis 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 6.2132.110 keypad or on the fron panel of the 719), the appropriate matrix code appears in the display.
  • Page 113 4.2. Diagnosis d a t e / t i m e cylinder code • Press <Enter>. d a t e X X - X X - X X X X : X X : X X code:D0 XX ml activated dosing unit mL-code •...
  • Page 114 1 . . . 5 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 115 4.2. Diagnosis I n p u t 2 X X m V • Carry out the same measurements as with Input 1. • Press <Clear>. a n a l o g i n p u t t e s t 1 . . . 5 •...
  • Page 116 4.2. Diagnosis d u m m y r e s i s t o r 1 4 . 3 k Ω ? • Connect resistor switch-box (or suitable resistor 14.3 kΩ 0.1%) using 3.496.5070 cable to ‘Pol’ socket. Switch-box to 14.3 kΩ. •...
  • Page 117 4.2. Diagnosis I / O - t e s t - c o n n e c t o r ? • Insert the 3.496.8510 test plug in port B 'Remote'. (Do not switch off instrument!) • Press <ENTER>. Test sequence: 1.
  • Page 118 4.2. Diagnosis R S 2 3 2 t e s t - c o n n e c t o r ? • Insert the 3.496.8480 test plug in 'RS 232' port. • Press <Enter>. Test sequence: 1. In case of an error an error message is displayed. If for example no test plug is con- error 68 nected, error message appears).
  • Page 119 4.2. Diagnosis Spindle remains at maximum position. The transit time of the spindle is 20 s. • Measure spindle lifting (can be performed only if the 3.496.0070 Dummy Exchange Unit is inserted or the locking switch (in right hole) is carefully operated with a screwdriver after removal of the Exchange Unit).

  • Page 120: Initialise And Test Ram

    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 121: Releasing A Locked Spindle With Inserted Exchange Unit

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

  • Page 122: 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 123: 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 124: Connection Of A Balance

    5.1. Setting up and connecting the instruments 5.1.3 Connection of a balance The following balances can be connected to the RS232 output of the Titrino: Balance Cable Sartorius MP8, MC1 6.2125.070 Shimadzu BX, BW 6.2125.080 Settings on Titrino: balance SARTORIUS Balance: delimiter CR+LF...

  • Page 125: Connection Of A Sample Changer

    5.1 Setting up and connecting the instruments The weight is transferred as a number with up to 6 digits, sign and decimal point. Units and control characters sent by the balance are not transmitted. With the aid of a special input unit supplied by the balance manufac- turer, in addition to the weight identifications and methods can be inputted from the balance.

  • Page 126: Connection Of A Recorder

    5.1. Setting up and connecting the instruments 5.1.5 Connection of a recorder The recorder is connected to the analog output of the Titrino. Recorder The signal at the analogue output can be preselected on the Titrino (key <CONFIG>, ">peripheral units", "curve:"): Preselection at Meaning Resolution,...

  • Page 127: Connection Of A Computer

    5.1 Setting up and connecting the instruments 5.1.6 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..................

  • Page 128: Connection Of Electrodes, Preparing Titration Vessel

    5.2. Connection of electrodes, preparing titration vessel 5.2 Connection of electrodes, preparing titration ves- Rear panel: Connection for separate reference electrode. 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 129 5.2 Connection of electrodes, 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 130 5.2. Connection of electrodes, preparing titration vessel Setting up the titration vessel The titration vessel is set up as shown below. During a titration, it is important to ensure that the solution in contact with the electrode is thoroughly mixed. This is achieved by •...

  • Page 131: Appendix

    Display LCD, 2 lines of 24 characters each Height of characters 5 mm LED back-lit Internal memory Method memory for up to 100 methods. Data bank with 4 Metrohm methods. Silo memory for sample data and results 719 S Titrino...
  • Page 132 6.1. Technical specifications RS232 interface for printer, balance or computer connection: completely controllable from external control unit Remote input/output lines for Sample Changer, robot connection, etc. Analog output Output signal -2000 ... 2000 mV Signal at analog- depending on preselection: output U (measuring value) dU/dt (measured value drift)

  • Page 133: 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 131...
  • Page 134 6.2. Pin assignment of the "Remote" socket Outputs pin 17 (Output 3) End of determination pin 3 (Output 4) To be set via RS232 control pin 16 (Output 5) Error, active with errors pin 1 (Output 6) Activate pulse, see page 131. pin 2 (Output 7) Pulses for recorder (t =150 µ...

  • Page 135: 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 719 S Titrino...

  • Page 136: Possible Configurations Of The Activate Pulse In Set And Cal

    6.2. Pin assignment of the "Remote" socket 6.2.2 Possible configurations of the activate pulse in SET and 719 S Titrino...

  • Page 137: 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. If the result should have another unit, you need to adjust the calculation constants using the key <C-FMLA>.

  • Page 138: Tit.hcl

    Sample size according to the buret volume. dos.rate max. ml/min Dilute in 40 mL dist. water. pause 2 extr.time meas.input: Reference: temperature 25.0 °C METROHM Application Bulletin Nr. 206: >stop conditions stop V: abs. stop V 99.99 ml filling rate max. ml/min >statistics status: mean res.tab:...

  • Page 139: Tit.naoh

    Sample size according to the buret volume. pause 2 Dilute in 40 mL dist. Water (free of carbonate). extr.time meas.input: Reference: temperature 25.0 °C METROHM Application Bulletin Nr. 206: >stop conditions stop V: abs. stop V 99.99 ml filling rate max. ml/min >statistics...

  • Page 140: P+M_Val

    6.3. User methods 6.3.4 "p+m_Val" Determination of the acid capacity, resp. 719 S Titrino 18200 719.0021 and pK of water and waste water. date 2002-03-13 time 12:49 A 8.2 A 4.3 p+m_Val The p-value represents the amount of acid to parameters be added to reach the pH value 8.2 (color >SET1...

  • Page 141: Br_No

    >preselections conditioning: req.ident: req.smpl size: value Reference: activate pulse: ASTM D1159-84 ------------ ISO 3839:1996 Metrohm Application Bulletin Nr. 177 719 S Titrino 18200 719.0021 date 2002-03-13 time 13:05 Ipol Br_No. >calculations – Result in mg bromine/100 g sample Br_No.=(EP1-C01)*C02*C03*C04/C00;0;...

  • Page 142: Validation / Glp

    Metrohm Application Bulletin: No. 252: Validation of Metrohm Titrators (potentiometric) 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 143: 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 144: Eu Declaration Of Conformity

    6.5. Warranty and conformity 6.5.2 EU Declaration of conformity EU Declaration of Conformity The METROHM AG company, Herisau, Switzerland hereby certifies, that the instrument: 719 S 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 145: 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 146: Scope Of Delivery And Ordering Designations

    6.6. Scope of delivery and ordering designations 6.6 Scope of delivery and ordering designations 719 S Titrino ..................2.719.0020 inclusive the following accessories: 1 Titrino......................... 1.719.0020 1 Keypad for 719 S Titrino..................6.2132.110 1 Key for Exchange Units..................6.2739.010 1 Mains cable with cable socket, type CEE(22), V Cable plug to customer's specifications type SEV 12 (Switzerland...) ................
  • Page 147 6.6 Scope of delivery and ordering designations Titration equipment Titration vessel, volumes 1... 50 mL ....................6.1415.110 5... 70 mL ....................6.1415.150 10... 90 mL ....................6.1415.210 20... 90 mL ....................6.1415.220 50... 150 mL ....................6.1415.250 70... 200 mL ....................6.1415.310 Titration vessel with thermostatic jacket, volumes 1...
  • Page 148 6.6. Scope of delivery and ordering designations Balances Cable Sartorius – balances MP8, MC1 (9/25 pins) ..........6.2125.070 Cable Shimadzu – balances BX, BW ..............6.2125.080 Ohaus Voyager, Explorer, Analytical Plus ..........cable from Ohaus Mettler AB, AG balances (interface LC-RS25) ......... cable with balance Mettler AT balance ....................

  • Page 149: Index

    Index Index Keys are marked with < >, are in bold characters and pages concerning the green display texts part are printed in Italic. stirrer ........... 118 Ti stand ..........118 Accessories ...........142ff Contrast of display ........3 ......29, 35, 36 activate pulse: Control Analogue output...
  • Page 150 Index ......... 26, 34 <SMPL DATA>........ 6, 50 electrode test: End volume ..........40 <START>........... 3, 6 <STATISTICS> ........ 6, 42 titration..........25ff <STOP/FILL> ........3 ............ 25 <STOP> ..........6 EP at pH ........34, 36 <USER METH> ....... 6, 47 equilibr.time Error messages.......
  • Page 151 Index CAL............36 properties ..........95ff MEAS.............34 Rules for operation via RS232 ....55ff SET ............25 ..........22 run number ............22 parity: ............26 pause 1 ..........103 same buffer ............26 pause 2 Sample ........21 peripheral units changer ..........121 Perturbation ...........103ff data ............
  • Page 152 Index ............28 ......26 stop V titration parameters ........104 Tree ............63ff stop V reached ..........47 Troubleshooting........103ff store method ........104 Tutorial ............9ff system error 3 ............ 25 ..........26, 34 t(delay) U(pol) Technical specifications......127 Unit ............

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