CH-9101 Herisau/Switzerland E-Mail info@metrohm.com Internet www.metrohm.com 794 Basic Titrino Program version 5.794.0010 Instructions for Use 8.794.1003 02.
Table of contens Table of contents 1 Introduction...........................................................................................................1 1.1 Instrument description........................................................................................... 1 1.2 Controls and parts ................................................................................................. 2 2 Manual operation.........................................................................................
Table of contents 4 Error messages, Troubleshooting ...................................................................133 4.1 Error and special messages ............................................................................. 133 4.2 Diagnosis .......................................................................................................... 137 4.2.1 General ...................................................................................................... 137 4.2.2 Procedure .............
1.1 Instrument description 1 Introduction 1.1 Instrument description The 794 Basic Titrino is an all-purpose titrator. Titration modes of the 794 Basic Titrino are constant or – depending on the titration curve – variable dosing of the titration reagent and Endpoint-Titration. All operating modes of the Titrino can be combined to perform extensive analytical sequences. Ready-to-start methods for the most common applications are stored in the internal method memory.
1.2 Controls and parts 1.
1.2 Controls and parts 1 Exchange Unit 2 Display 3 Setting of display contrast 4 Controls the dosing rate during manual dosing with and subsequent filling 5 Control keys and indicator lamps on the Titrino Key Key Key Indicator lamps: "Statistics" "Silo" 794 Basic Titrino Dosing key. Dispensing is performed as long as is being pressed. Used e.g. to prepare the Exchange Unit. The dispensing rate can be set with potentiometer (4). - Stops procedures, e.g.
1.
1.2 Controls and parts 6 RS232 interface for the connection of printer, balance or a computer 7 Remote lines (input/output) for the connection of the Remote Box, Sample Changers, robots etc. 8 Connection of electrodes and temperature sensor • 2 high-impedance measuring inputs for pH and U measurements (Ind I/ Ind II). They can either be used separately or for differential potentiometry, see page 155.
2.1. Keypad 2 Manual operation 2.1 Keypad CONFIG PARAM SMPL DATA STATISTICS Configuration. Parameters. Sample data. ON/OFF switching of statistics calculations of consecutive determination, see page 55. 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 69. CAL.DATA Calibration data, see page 68. C-FMLA Calculation values, see page 54. DEF Formulas, data output, sequence for TIP, see page 52ff.
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 : In the first line you see where you are: You pressed key and you are now in the menu "configuration". configuration >peripheral units • In our example you are in the menu "configuration" on the title ">peripheral units". By pressing you can move to the other titles of this menu.
2.3. Text input 2.3 Text input Example storing a method: • Press key , the group ">recall method" appears. user methods >recall method • Choose ">store method" by pressing and press . The name of the method which is currently in the working memory is displayed. >store method method name: • Delete this name with . <<> >store method method name: • Open the "text writing mode" with key <<>.
2.4 Tutorial 2.4 Tutorial This short operating course teaches you to work quick and efficient with the 794 Basic 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. We change the dialog language.
2.4. Tutorial Because this inquiry follows no colon ":" the value can't be selected by
2.4 Tutorial 2.4.2 Development of a method, titration of an acid Selection of the mode mode mode DET DET pH DET: • Press repeatedly until "DET" appears in the display. For a description of the DET mode see page 25. • Confirm "DET" with ******** pH 4 ×
2.4. Tutorial If more than one equivalence point has been found, the others can be viewed with . Calculation of the result: formula entry With this equivalence point a result can be calculated. • Press the key. def >formula • Press to move on to the formula entry. The display now shows "RS?". <1> • Press "1", i.e. the first formula. RS? RS1= You now can enter a formula. Note here the top inscription on the keys of the keypad and the numbers.
2.4 Tutorial Entry of the calculation constants C-fmla >C01 0.0 • Press . The constants which have been used in the formula are requested: input with digit keys, confirm with . C01: Concentration of your titrant= 0.1 mol/L. Enter 0.1. C02: Molar mass of HCl = 36.47 g/mol Entry of the sample size 4 x smpl data smpl size • Press repeatedly until "sample size" appears in the display. • Enter 2.
2.4. Tutorial If you have a printer connected, you probably wish to have the curve and a result report printed out automatically at the end of a titration. To install a printer, see page 150. Print reports 4 x • Press repeatedly until the display shows: • Press to move to the definition of reports. 6 x
2.4 Tutorial So that you do not have to stop your titration manually each time, let us add a stop criterion for the titration. Stop criterion 2 x • Press twice to display the title ">stop conditions". parameters >stop conditions >stop conditions stop V: • abs. Open this group of inquiries with . Absolute stop volume. This can be used as a safety measure to prevent overflow of the titration vessel. >stop conditions stop V: 99.
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 methods >store method >store method method name: • Press repeatedly until the title ">store method" appears in the display. • Open the inquiry with . ******** • Enter an identifier, e.g. 1 or Acid. For text input see page 8. DET pH Acid The method now runs under the name "Acid". It is ready to titrate.
2.4 Tutorial 2.4.4 pH calibration pH calibrations are not a requirement for pH titrations, when the equivalence point is determined from a curve. 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 • Press repeatedly until "CAL" appears in the display and confirm the mode with . mode mode CAL CAL ******** pH(as) 7.00 slope 1.
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. First select the mode SET pH (keys and
2.4 Tutorial If the titration runs too slow or too fast, you can change the control parameters during the titration. If you wish to titrate faster, change the following parameters: • dynamics: lower value, the control range becomes smaller (Attention: possibility of titrating over the set EP) • max.rate: bigger value • min.rate: bigger value You will find further details of the control parameters on page 42. After the titration, end point volume and pH value at the end point are displayed.
2.4. Tutorial After the second titration you receive a printout with statistics calculations: 'fr 794 Titrino 01102 794.0010 date 2002-01-03 time 17:34 3 pHc(init) 6.29 SET pH ******** EP1 0.0628 ml 4.26 m value 5.02 mmol/l mean(2) +/s s/% m value 5.04 0.028 mmol/l 0.56 ============== If you have no printer connected, you can view the mean value and standard deviation: • Press
2.4 Tutorial You can now decide which of the results is an "outlier". You can delete it from the statistics calculation. Deleting a result from the statistics calculation • Press until the display shows: 5 × parameters >statistics • Select with the inquiry of the result table "res.tab:" 3 × >statistics res.tab: original • To delete a single result with index n from the result table, press
2.5. Configuration, key 2.5 Configuration, key Key serves to enter device specific data. The set values apply to all modes. CONFIG peripheral units: Selection of printer, balance and the curve at the analog output. auxiliaries: e.g. setting of dialog language, date, time, etc. RS232 settings: RS parameters for the COM interface. common variables: Values of common variables. configuration >peripheral units The display texts of the Titrino are shown to the left.
2.5 Configuration, key General settings >auxiliaries dialog: english date 2001-01-03 time 08:13 Selection of dialog language (english, deutsch, francais, español, italiano, portugese, svenska) Current date (YYYY-MM-DD) Format: Year-month-day, entry with leading zeros. Current time (HH-MM) Format: Hours-minutes, entry with leading zeros. Current run number for result output (0...9999) The sample number is set to 0 when the instrument is switched on and incremented on every determination.
2.6. Selection of the mode, key Values of the common variables >common variables C30 0.0 etc. Common variables C30...C39 (0.. ± 999 999) The values of all common variables are displayed. For creating of common variables see page 57. 2.6 Selection of the mode, key MODE > – ; Press key until the desired mode is displayed and confirm with . Select the measured quantity pH, U, Ipol, Upol, (T) with
2.6 Selection of the mode, key Overview of the titration modes DET Dynamic Equivalence point Titration Reagent feeding: Variable volume increments, depending on the slope of the curve. U/mV SET, KFT Endpoint Titration MET Monotonic Equivalence point Titration Reagent feeding: Constant volume increments, independent of the slope of the curve. Titration to preset end-point.
2.7. Parameters, key 2.7 Parameters, key The key is used for the entry of values that determine the modes. Values marked with "cond." are accessible during the conditioning in the SET mode. "**titr." means that these values can be changed during the titration. They influence the ongoing determination. Other values can only be changed in the inactive state. The display texts of the Titrino are shown to the left. The values are the default values. PARAM 2.7.
2.7 Parameters, key titr.rate Dosing rate for volume increments (0.01...150 mL/min, max.) sets "max.". The maximum rate depends on the Exchange Unit: Exchange Unit max. 5 mL 15 mL/min 10 mL 30 mL/min 20 mL 60 mL/min 50 mL 150 mL/min max. ml/min **titr. signal drift 50 mV/min Drift criterion for measured value acquisition. (input range depends on the measured quantity: pH, U, Ipol: 0.5...999 mV/min, OFF Upol: 0.05...99.9 µA/min, OFF) sets "OFF".
2.7. Parameters, key pause 0 s **titr. meas.input: 1 I(pol) 1 µA U(pol) 400 mV electrode test: temperature OFF 25.0 °C abs. **titr. stop V 99.99 ml **titr. factor 999999 **titr. stop pH **titr. 28 Measuring input for pH and U (1, 2, diff.) Request for measuring input for pH and U. Measuring input 1 or 2 or differential amplifier; connection of electrodes, see page 155. With polarized electrodes, instead of the measuring input the polarization current (-127...
2.7 Parameters, key stop EP 9 **titr. Filling rate (0.01...150 mL/min, max.) sets "max.". The maximum rate depends on the Exchange Unit: Exchange Unit max. 5 mL 15 mL/min 10 mL 30 mL/min 20 mL 60 mL/min 50 mL 150 mL/min filling rate max. ml/min **titr. Statistics calculation >statistics status: mean res.
2.7. Parameters, key low lim.1 pH up lim.1 pH -20.00 20.00 fix EP1 at pH OFF Interpolation of volumes at fixed times (input range depends on the measured quantity: pH: 0...±20.00, OFF U, Ipol: 0...±2000 mV, OFF Upol: 0...±200.0 µA, OFF) sets "OFF". If a fix end point has been set, the volume value for the input measured value is interpolated from the curve, see also page 35. The volume values are available as C5X. Fix EP's are inquired until "OFF" is set. Up to 9 fix EP's.
2.7 Parameters, key Titration sequence of DET and MET (Activate pulse) (Start delay) (Request ident.) (Request smpl size) After the start, the activate pulse is outputted. The start delay time is waited off. The sample identifications and the sample size are requested. (Start conditions) The start volume is dispensed (no meas.value acquisition) and the pause is waited off. Titration: Dispense increments Acquire meas.
2.7. Parameters, key Reagent feeding and EP evaluation of DET The reagent feeding of DET is similar to the controlling, a human being would apply in manually controlled titrations: Great volume increments are dosed far away from the EP, small increments in the region of the equivalence point. The size of the volume increments dosed by the Titrino is determined by the following parameters: meas.pt.density The measuring point density is entered as a relative value from 0...9.
2.7 Parameters, key Reagent feeding and EP evaluation of MET In monotonic titrations, the volume increment is constant over the whole titration curve. V step Volume increment. A prerequisite for good accuracy is the correct size of the volume increments. A good value is given by V step = 1/20 VEP (VEP = volume of the EP).
2.7. Parameters, key EP recognition criteria for DET and MET The parameter "EP recognition" offers you a range of possibilities to ensure selection of the EP you are interested in: If the desired jump is very large, you can select the "greatest" jump (with DET the steepest jump will be evaluated). Thus you always obtain just one EP per titration (EP1). If you wish to determine the sum of different components (e.g. acid or base numbers), the "last" jump can be the correct one.
2.7 Parameters, key Fix EP's Fix EP's allow determination of the associated volume value for every inputted measured value on the titration curve. This function is useful for performing standard methods such as TAN/TBN determinations. For the evaluation of fix EP's, the pH calibration is advisable. The volume values of the fix EP's are available for the calculation as C5X: Fix EP1 ⇒ C51 : Fix EP9 ⇒ C59 Maximum 9 fix EP's are possible.
2.7. Parameters, key 2.7.2 Parameters for SET SET1, SET2: Control parameters for EP1 and EP2. titration parameters are valid for the global titration sequence. stop conditions: Parameters for the termination of the titration. statistics: Calculation of mean values and standard deviation, see also page 55. preselections: ON/OFF of various auxiliary functions such as automatic requests after the start and activate pulse. parameters >SET1 Control parameters for EP1 or EP2, resp.
2.7 Parameters, key min.rate Minimum dosing rate (0.01...999.9 µL/min) This parameter determines the addition rate right at the start and the end of the titration, see also page 42. This parameter influences the titration speed and therefore its accuracy very strongly: A smaller min.rate results in a slower titration. 25.0 µl/min **titr. stop crit: Type of stop criteria (drift, time) drift **titr. stop drift 20 µl/min **titr. t(delay) 10 s **titr. stop time OFF s **titr.
2.7. Parameters, key Exchange Unit 5 mL 10 mL 20 mL 50 mL pause 0 s **titr. meas.input: I(pol) 1 µA U(pol) 400 mV electrode test: temperature cond. 38 1 OFF 25.0 °C max. 15 mL/min 30 mL/min 60 mL/min 150 mL/min Pause (0...999999 s) Waiting time after start volume, e.g. reaction time after dosing of a start volume. The waiting time can be aborted with . Measuring input (1, 2, diff.) Inquiry only with measured quantities pH and U.
2.7 Parameters, key Stop conditions for titration If this is not "normal", i.e. after reaching the EP. >stop conditions stop V: Type of stop volume (abs., rel., OFF) "abs.": absolute stop volume in mL. "rel.": relative stop volume to sample size. "OFF": stop volume switched off. Stop volume is not monitored. abs. **titr. stop V 99.99 ml **titr. factor 999999 **titr. Statistics calculation >statistics mean res.tab: delete 794 Basic Titrino If "rel.
2.7. Parameters, key Preselections for the sequence >preselections conditioning: display drift: OFF ON cond. req.ident: Request of identifications after start of titration (id1, id1&2, all, OFF) After start, sample identifications can be requested automatically: Only id1, id1 & id2, all three id's or no inquiries. OFF Request of sample size after start of titration (value, unit, all, OFF) "all" the value and the unit will be requested.
2.7 Parameters, key Titration sequence of SET (Activate pulse) (Start delay) (Preconditioning) ( (Activate pulse) (Start delay) After the start, the activate pulse is outputted. The start delay time is waited off. If conditioning is on, the sample solution is titrated until the (first) EP is reached. The display shows then drift OK or SET pH 2.3 µl/min conditioning The vessel is now conditioned. The titration can be started with . (Request ident.
2.7. Parameters, key 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. Initial dosing: Here the dosing rate increases constantly. The rate starts with "min.rate" and goes up to "max.rate". EP 2. Continuous dosing: Dosing is performed at the maximum rate "max.
2.7 Parameters, key 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. The size of this last increment depends on the volume of the Exchange Unit used. With a 20 mL Exchange Unit, the smallest possible increment is 2 µL.
2.7. Parameters, key 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 ... Problem Dosing at the end too long and with too small increments. "Never ends!" Possible causes and corrective measures • Increase "min.rate". Perform an experiment with a much higher min.rate.
2.7 Parameters, key 2.7.3 Parameters for MEAS measuring parameters determine the measurement. statistics: Calculation of mean values and standard deviation, see also page 55. preselections: ON/OFF of various auxiliary functions such as automatic requests after the start and activate pulse.
2.7. Parameters, key performed. temperature Temperature (-170.0...500.0 °C) Temperature is measured at the start if a T sensor is connected. This parameter is used for temperature compensation in pH measurements. 25.0 °C Statistics calculation >statistics status: mean res.tab: delete n= 2 original n= 1 Mean value calculation from n single results (2...20) Result table (original, delete n, delete all) "original": The original table is used.
2.7 Parameters, key 2.7.4 Parameters for CAL parameters >calibration parameters Calibration parameters >calibration parameters meas.input: cal.temp. calibration parameters determine the calibration procedure. statistics: Calculation of mean values and standard deviation, see also page 55. 1 25.0 °C Measuring input (1, 2, diff.) Measuring input 1 or 2 or differential amplifier; Connection of electrodes, see page 155. Calibration temperature (-20.0 ... 120.
2.7. Parameters, key Calibration temperature and pH values of the buffers (which are temperature dependent) must therefore be entered in advance. The inputs in key are valid. activate pulse: Pulse output on the line "activate" (L6, pin 1) of the remote socket (all, first, OFF) See page 163. OFF Statistics calculation >statistics status: mean res.
2.7 Parameters, key Calibration sequence (Activate pulse) (Start delay) Measuring cal.temp. or entry Buffer 1 pH Measuring buffer 1 Buffer 2 pH Measuring buffer 2 etc. Data output 794 Basic Titrino After the start, the activate pulse is output. The start delay time is waited off. Then, the calibration temperature is measured. It no T sensor is connected, you enter the temperature manually. Store the value with or continue with (T is not stored).
2.7. Parameters, key 2.7.5 Parameters for TIP In TIP, several commands and methods can be linked to make a titration procedure. The TIP sequence can be defined with , see page 62. sequence Parameters for the TIP sequence see page 63. statistics: Calculation of mean values and standard deviation, see also page 55. preselections: ON/OFF of various auxiliary functions such as automatic requests after the start and activate pulse.
2.7 Parameters, key I(pol) 1 µA U(pol) 400 mV electrode test: temperature 794 Basic Titrino OFF 25.0 °C With polarized electrodes, inquiry of polarization current (-127...127 µA) or polarization potential (-1270...1270 mV, steps of 10 mV) Electrode test (OFF, ON) Test for polarized electrodes. Performed on changeover from the inactive standby state to a measurement. "OFF" means that the test is not performed. Temperature (-170.0...500.0 °C) Temperature for pH compensation.
2.8. Result calculations 2.8 Result calculations Formula entry, key DEF 2 ( def >formula Key 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. The display texts of the Titrino are shown to the left. The values are the default values. >formula Input of formulas RS? Enter formula number (1...
2.8 Result calculations RS1 text RS1 Text for result output (up to 8 characters) Text input see page 8. RS1 decimal places 2 Number of decimal places for result (0...5) RS1 unit: % Selection of result unit (%, ppm, g/L, mg/mL, mol/L, mmol/L, g, mg, mL, mg/pc, s, mL/min, no unit or up to 6 characters). Enter next formula, e.g. for RS2. Meaning of the calculation variables CXX: C00 Sample size, see page 69. C01...C19 Method specific operands, see page 54.
2.8. Result calculations Input method specific operands C01...C19, key C-FMLA 1 C With the operands C01...C19 can be put in. For the calculation, the operands are used, which were introduced in the formula. The inputs method specific and are store in method memory.
2.9 Statistics calculation 2.9 Statistics calculation Mean values, absolute and relative standard deviations are calculated. DEF 2 The 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. def >mean The display texts of the Titrino are shown to the left. The values are the default values.
2.9. Statistics calculation How do you obtain statistics calculations? 1) Enter the allocations for the statistics calculation, see page 55. 2) Switch on the statistics calculations: Either with or set the status under , "> statistics" to "ON". The "Statistics" LED is on. Storing a method in the method memory, the status of the statistics calculation is retained. 3) Change the number of the individual values n under "mean n", if necessary. 4) Perform at least 2 titrations.
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. • Determination of a blank values with a method . Using this blank value in various other methods. • Determination of a result with method. Reconciliation of this result in various other methods. You may view the values of the common variables with .
2.11. Data output 2.11 Data output Reports for the output at the end of a determination DEF 2 ( def >report With , 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. report: Definition of report blocks to be printed automatically at the end of the determination. The display texts of the Titrino are shown to the left. The values are the default values.
2.11 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: . Original reports have double dashes ==== at the end, whereas recalculations are marked by single dashes ----. Report outputs can be stopped with . Example of reports: Full result report 'fr 794 Titrino date 01102 2002-01-03 pH(init) time 2.88 DET pH smpl size 0.372 g EP1 2.083 ml RS1 794.
2.11. 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)
2.11 Data output Result display without printer Results can also be viewed in the display. With
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 and . TIP is an "empty shell" in which the sequence of the determination must be defined. Definition of the sequence DEF 2 With key the TIP can be defined. ( sequence: Sequence of TIP. def >sequence The display texts of the Titrino are shown to the left. The values are the default values. Sequence >sequence 1.
2.12 TIP, Titration procedure Information for the commands (steps): Command Meaning Input range method Method from the user memory. This method runs as a submethod. Name pause Waiting time. The waiting time can be aborted with . sets "inf" (= infinitely long pause time). 0...999999 s, inf. L4, L6 output Set L4 output (pin 3) resp. L6 output (pin 1) of the active, remote socket. inactive, active = 0 V, inactive = 5 V, pulse > 100 ms, off = pulse, off output is not used.
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 delay) (Request ident.) (Request smpl size) Submethod Calculations Data output C7X Pause Set output Info 64 The start delay time is waited off. The sample identifications and the sample size are requested. Submethods are processed according to their parameters.
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. This allows them to be used in TIP for further calculations. Reevaluations of data of a submethod are not possible in TIP.
2.13. Method memory, keys 2.13 Method memory, keys USER METH 3 user methods >recall method ) Management of the internal method memory with key . Method identifications can be entered directly or selected with the
2.13 Method memory, keys The contents of the method memory can be printed with the key sequence 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.
2.14. Calibration data, key 2.14 Calibration data, key With , the current pH calibration data of all measuring inputs can be seen. Calibration data are entered here automatically on completion of a calibration. CAL.DATA 5 * input 1: Calibration data for measuring input 1. Identical for input 2 and diff. cal. data >input 1 The display texts of the Titrino are shown to the left. The values are the default values.
2.15 Current sample data, key 2.15 Current sample data, key The key can be used to enter the current sample data. The contents of this key change when the silo memory is switched on, see page 71. Instead of entering the current sample data with , you can request these data automatically after start of determinations. Configuration: , ">preselections". Current sample data can be entered live. For working with the silo memory see page 70. id#1...3 or C21.
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 smpl 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 74. SILO 9 Press the key for working with the silo memory. The status LED "silo" is on when the silo memory is switched on.
2.16 Silo memory for sample data Key with the silo memory switched on Sample data can be entered into the silo memory with key . SMPL DATA edit silo lines: Entering sample data into the silo memory. delete silo lines: Deletes single silo lines. delete all silo lines: Deletes the whole silo memory. smpl data >edit silo lines The display texts of the Titrino are shown to the left. The values are the default values. Input for silo memory >edit silo lines silo line 1 Silo line (1..
2.16. Silo memory for sample data Delete all silo lines >delete all silo lines delete all: Confirmation (yes, no) When all silo lines are deleted, the silo is completely empty: The line numbering starts again with 1. no cycle lines: OFF With "ON", worked off silo lines will be copied to the highest line of the silo memory (ON, OFF) Data cycling "on" is useful if you constantly have to process the same sample data.
2.17 Storing determination results and silo calculations 2.17 Storing determination results and silo calculations 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. In the method under Assignment of the determination results to C24 and/or C25: 2.
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 ): 'si 794 Titrino date 01102 2002-01-03 time 794.0010 08:54 14 >silo cycle lines: OFF save lines: sl method ON id 1/C21 id 2/C22 id 3/C23 C00 C24 C25 + 1 11-2 A/12 94-09-12 0.233g 0.142ml/min 98.53% + 2 11-2 A/13 94-09-12 0.286g 0.138ml/min 95.75% / 3 11-2 A/14 94-09-12 0.197g 0.
2.17 Storing determination results and silo calculations Starting from the following silo report: 'si 794 Titrino date 01102 2002-01-03 time 794.0010 08:54 14 >silo cycle lines: OFF save lines: ON sl method id 1/C21 id 2/C22 id 3/C23 + 1 11-2 A/12 94-09-12 0.233g C00 0.142ml/min C24 C25 + 2 0-15 A/13 94-09-12 0.286g 0.9976 + 3 0-15 A/13 94-09-12 0.197g 0.9947 + 4 11-2 A/12 94-09-12 0.288g 0.138ml/min / 5 11-2 A/15 94-09-12 0.263g 0.145ml/min 100.61% 98.53% NV NV 95.
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. Silo calculations 6. Assignment of means C26 and C27 from silo calculations 7.
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. CR and LF are used as terminators for the data transfer. The Titrino sends 2xCR and LF as termination of a data block, to differentiate between a data line which has CR and LF as terminators.
3.1. General rules 3.1.1 Call up of objects An excerpt from the object tree is represented below: 3rd node Language 2nd node 1st node Prog Aux RSSet 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. When calling up an object, it is sufficient to give only as many letters as necessary to uniquely assign the object.
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: $G Go $S $H $C $Q Stop Hold Continue Query $Q.P $Q.H Path Highest Index Name Detail-Info qUit $Q.N"i" $D $U Starts processes, for ex.
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. $S.Mode.SET;E26.
3.1 General rules .Req.Buf2: .Meas.Buf2: etc. $G .Assembly.Bur .Fill: Instrument in the CAL mode, requesting pH of buffer 2. Instrument in the CAL mode, measures buffer 2. Buret in filling process in DIS mode .ModeDis: Buret In TIP, its global status as well as the step number (X) is available. .Inac: Instrument at the beginning or at the end of a TIP. .Req .Id1: Instrument in the TIP mode, requesting Id1 after start. .Id2: Instrument in the TIP mode, requesting Id2 after start. .
3.1. General rules 3.1.4 Error messages Error messages are added to the status messages and separated from them by the sign ";". E20 E21 E22 E23 E26 E27 E28 E29 E30 E31 E32 E33 E34 E36 E37 E38 E39 82 Check exchange unit. Exit: Mount Exchange Unit (properly) or &m $S. Check electrode, short circuit. Exit: Rectify fault or &m $S. Check electrode, break. Exit: Rectify fault or &m $S. Division by zero. Exit: The error message disappears on next startup or on recalculation. Manual stop.
3.1 General rules E40 E41 E42 E43 E44 E45 E120 E121 E122 E123 E124 E125 E126 E128 E129 E130 E131 E132 794 Basic Titrino RS send errors: DSR=OFF No proper handshake for more than 1 s. Exit: Is the receiver switched on and ready to receive? DCD=ON No proper handshake for more than 1 s. Exit: Is the receiver switched on and ready to receive? CTS=OFF No proper handshake for more than 1 s.
3.1. General rules E133 E134 E135 E136 E137 E155 E157 E158 E160 E161 E166 E172 84 Silo full. Exit: Send new command. No method. A method, which is required from the silo memory or in TIP, does not exist. Exit: The error message disappears on next startup. Check temp.sensor in MEAS T. Exit: Correct error or &m $S. 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.
3.2 Remote control commands 3.2 Remote control commands 3.2.
3.2. Remote control commands &Mode Object Description & Root ├ Mode : ├ .QuickMeas ├ .Select Mode Rapid meas. in basic mode Mode selection │ ├ .DETQuantity ├ .METQuantity ├ .SETQuantity ├ .MEASQuantity ├ .Name ├ .Parameter* │ ├ .Def │ ├ .Formulas │ │ ├ .1 │ │ │ ├ .Formula │ │ │ ├ .TextRS │ │ │ ├ .Decimal │ │ │ ├ .Unit │ │ │ : │ ├ .SiloCalc │ │ ├ .Assign │ │ │ ├ .C24 │ │ │ ├ .C25 │ │ ├ .MatchId │ ├ .ComVar │ │ ├ .C30 │ │ ├ up to C39 │ ├ .Report │ │ ├ .Assign │ ├ .Mean │ │ ├ .1 │ │ │ ├ .
3.2 Remote control commands *Parameter ├ .TitrPara │ ├ .MptDensity │ ├ .MinIncr │ ├ .DosRate │ ├ .SignalDrift │ ├ .UnitSigDrift │ ├ .EquTime │ ├ .StartV │ │ ├ .Type │ │ ├ .V │ │ ├ .Factor │ │ ├ .Rate │ ├ .Pause │ ├ .MeasInput │ ├ .Ipol │ ├ .Upol │ ├ .PolElectrTest │ ├ .Temp │ ├ │ │ │ │ │ │ │ │ │ ├ │ │ │ │ │ │ ├ │ │ │ │ │ │ │ │ │ │ │ │ ├ │ │ │ .StopCond ├ .VStop │ ├ .Type │ ├ .V │ ├ .Factor ├ .MeasStop ├ .UnitMStop ├ .EPStop ├ .FillRate .Statistics ├ .Status ├ .MeanN ├ .ResTab │ ├ .Select │ ├ .
3.2. Remote control commands *Parameter ├ .TitrPara │ ├ .VStep │ ├ .DosRate │ ├ .SignalDrift │ ├ .UnitSigDrift │ ├ .EquTime │ ├ .StartV │ │ ├ .Type │ │ ├ .V │ │ ├ .Factor │ │ ├ .Rate │ ├ .Pause │ ├ .MeasInput │ ├ .Ipol │ ├ .Upol │ ├ .PolElectrTest │ ├ .Temp │ ├ │ │ │ │ │ │ │ │ │ ├ │ │ │ │ │ │ ├ │ │ │ │ │ │ │ │ │ │ │ │ ├ │ │ │ 88 .StopCond ├ .VStop │ ├ .Type │ ├ .V │ ├ .Factor ├ .MeasStop ├ .UnitMStop ├ .EPStop ├ .FillRate .Statistics ├ .Status ├ .MeanN ├ .ResTab │ ├ .Select │ ├ .
3.2 Remote control commands *Parameter ├ .SET1 │ ├ .EP Endpoint 1 │ ├ .UnitEp │ ├ .Dyn │ ├ .UnitDyn │ ├ .MaxRate │ ├ .MinRate │ ├ .Stop │ │ ├ .Type │ │ ├ .Drift │ │ ├ .Time │ │ ├ .StopT ├ .SET2 ├ .TitrPara │ ├ .Direction │ ├ .Start V │ │ ├ .Type │ │ ├ .V │ │ ├ .Factor │ │ ├ .Rate │ ├ .Pause │ ├ .MeasInput │ ├ .Ipol │ ├ .Upol │ ├ .PolElectrTest │ │ ├ .Temp ├ .StopCond │ ├ .VStop │ │ ├ .Type │ │ ├ .V │ │ ├ .Factor │ │ ├ .FillRate ├ .Statistics │ ├ .Status │ ├ .MeanN │ ├ .ResTab │ │ ├ .Select │ │ │ ├ .DelN ├ .
3.2. Remote control commands *Parameter ├ .Measuring │ ├ .SignalDrift │ ├ .UnitSigDrift │ ├ .EquTime │ ├ .MeasInput │ ├ .Ipol │ ├ .Upol │ ├ .PolElectrTest │ ├ .Temp │ ├ │ │ │ │ │ │ ├ │ │ │ │ .Statistics ├ .Status ├ .MeanN ├ .ResTab │ ├ .Select │ ├ .DelN │ .Presel ├ ├ ├ .IReq .SReq .ActPulse *Parameter .Calibration ├ .MeasInput ├ .CalTemp ├ .Buffer │ ├ .1 │ │ ├ .Value │ ├ .2 │ │ ├ .Value │ ├ : ├ .SignalDrift ├ .EquTime ├ .ElectrodeId ├ .SmplChanger ├ .
3.2 Remote control commands *Parameter ├ .Sequence │ ├ .1 │ │ ├ .Select │ │ │ │ │ │ │ ├ │ │ │ │ │ │ ├ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ ├ ├ ├ ├ ├ .Method .Pause .L4Output .L6Output .Info .Statistics ├ .Status ├ .MeanN ├ .ResTab │ ├ .Select │ ├ .DelN │ .Presel ├ ├ ├ ├ ├ ├ ├ ├ .IReq .SReq .MeasMode .MeasInput .Ipol .Upol .PolElectrTest .
3.2. Remote control commands &UserMeth Object Description Input range Reference & Root : ├ UserMeth : ├ .FreeMemory ├ .Recall │ ├ .Name ├ .Store │ ├ .Name ├ .Delete │ ├ .Name ├ .DelAll ├ .List │ ├ .1 │ │ ├ .Name │ │ ├ .Mode │ │ ├ .Quantity │ │ ├ .Bytes │ │ ├ .Checksum ├ .
3.2 Remote control commands &Config Object Description Input range Reference & Root : ├ Config ├ .PeriphUnit │ ├ .CharSet1 │ │ │ ├ .Balance │ │ │ ├ .Plot │ │ │ ├ .Aux │ ├ .Language │ │ │ │ │ ├ .Set │ │ ├ .Date │ │ ├ .Time │ ├ .RunNo │ ├ .AutoStart │ ├ .StartDelay │ ├ .DevName │ ├ .Prog │ ├ .RSSet │ ├ .Baud │ │ │ ├ .DataBit │ ├ .StopBit │ ├ .Parity │ ├ .Handsh │ │ │ ├ .ComVar │ ├ .
3.2. Remote control commands &SmplData Object Description Input range Reference & Root : ├ SmplData : ├ .Status ├ .OFFSilo │ ├ .Id1 │ ├ .Id2 │ ├ .Id3 │ ├ .ValSmpl │ ├ .UnitSmpl ├ .ONSilo │ ├ .Counter │ │ ├ .MaxLines │ │ ├ .FirstLine │ │ ├ .LastLine │ ├ .EditLine │ │ ├ .1 │ │ │ ├ .Method │ │ │ ├ .Id1 │ │ │ ├ .Id2 │ │ │ ├ .Id3 │ │ │ ├ .ValSmpl │ │ │ ├ .UnitSmpl │ │ │ ├ .C24 │ │ │ ├ .C25 │ │ │ ├ .Mark │ │ ├ up to 99 lines │ ├ .DelLine │ │ ├ .LineNum │ ├ .DelAll │ ├ .CycleLines │ ├ .
3.2 Remote control commands &Info Object Description Input range Reference & Root : ├ Info Current data : ├ .Report Transmission of formatted reports $G 3.2.2.67. │ ├ .Select Report type configuration, parameters, │ smpl data, statistics, silo, calib │ C-fmla, def, user method, full, │ short, mplist, curve, derive, comb, │ scalc full, scalc srt, calc, │ all, ff ditto │ ├ .CalibrationData pH calibration data $G 3.2.2.68. │ ├ .Inp1 For measuring input 1 │ │ ├ .pHas Asymmetry pH 0...7.00...±20.
3.2. Remote control commands │ │ ├ .C45 Start volume │ │ ├ .C46 Asymmetry pH │ │ ├ .C47 Slope of electrode │ ├ .FixEP Fix EP │ │ ├ .51 C51 │ │ │ ├ .Value Value │ │ │ up to 59 │ ├ .pK pK/HNP │ │ ├ .61 C61 │ │ │ ├ .Value Value │ │ │ up to 69 │ ├ .TempVar Temporary variables C7X │ │ ├ .C70 up to C79 │ ├ .StatisticsVal Statistics values │ ├ .ActN Number of results in chart │ ├ .1 1st mean │ │ ├ .Mean Mean │ │ ├ .Std Absolute standard deviation │ │ ├ .
3.2 Remote control commands │ │ ├ .Y │ ├ .EP │ │ ├ .Index │ │ ├ .X │ │ ├ .Y │ ├ .Display │ │ ├ .L1 │ │ ├ .L2 │ ├ .Assembly │ ├ CycleTime │ ├ ExV 794 Basic Titrino Y coordinate EP entry Index of entry X coordinate Y coordinate Display Text line 1 Text line 2 read only ditto read only read only read only ditto ditto ditto up to 24 ASCII char up to 24 ASCII char 3.2.2.81. ditto Assembly Cycle time Volume of Exchange unit read only read only 3.2.2.82.
3.2. Remote control commands &Assembly Object Description Input range Reference & Root : ├ Assembly ├ . Bur │ ├ .Rates │ │ ├ .Forward │ │ │ ├ .Select │ │ │ ├ .Digital │ │ ├ .Reverse │ │ │ ├ .Select │ │ │ ├ .Digital │ ├ .Fill │ ├ .ModeDis │ │ ├ .Select │ │ ├ .V │ │ ├ .Time │ │ ├ .VStop │ │ ├ .AutoFill │ ├ .Meas │ ├ .Status │ ├ .MeasInput │ ├ .Ipol │ ├ .Upol │ ├ .Outputs │ ├ .AutoEOD │ ├ .SetLines │ │ ├ .L0 │ │ ├ up to L 3 │ ├ .
3.2 Remote control commands &Setup Object Description Input range Reference & Root : ├ Setup ├ .Keycode ├ .Tree │ ├ .Short │ ├ .ChangedOnly │ ├ .Trace │ ├ .Lock │ ├ .Keyboard │ ├ .Config │ ├ .Parameter │ ├ .SmplData │ ├ .UserMeth │ │ ├ .Recall │ │ ├ .Store │ │ ├ .Delete │ └ .Display │ ├ .Mode │ ├ .StartWait │ ├ .FinWait │ ├ .SendMeas │ ├ .SendStatus │ ├ .Interval │ │ ├ .Select │ ├ .Assembly │ │ ├ .CyclNo │ │ ├ .V │ │ ├ .Meas │ ├ .Titrator │ │ ├ .CyclNo │ │ ├ .V │ │ ├ .Meas │ │ ├ .dVdt │ │ ├ .
3.2. Remote control commands │ │ ├ .E │ │ ├ .H │ │ ├ .C │ │ ├ .O │ │ ├ .N │ │ ├ .Re │ │ ├ .Si │ │ ├ .M │ │ ├ .EP │ │ ├ .RC │ ├ .I │ ├ .O │ ├ .Graphics │ ├ .Grid │ ├ .Frame │ ├ .Scale │ ├ .Recorder │ │ ├ .Right │ │ ├ .Feed │ ├ .PowerOn ├ .Initialise │ ├ .Select │ ├ .RamInit ├ .InstrNo ├ .
3.2 Remote control commands &Diagnose Object Description Input range Reference Diagnose Output of adjustment parameters $G 3.2.2.103. & Root : ├ Diagnose ├ .
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 after the start (see 3.2.2.25) as well as after inquiries of calibration temperature and pH values of buffers (see 3.2.2.36 and 3.2.2.37). 3.2.2.2. Mode.
3.2 Remote control commands 3.2.2.6. Mode.Def.SiloCalc.Assign.C24 RSX, EPX, CXX Mode.Def.SiloCalc.Assign.C25 RSX, EPX, CXX Mode.Def.SiloCalc.MatchId id1, id1&2, all, OFF .Assign.C2X: Assignment to store results in the silo as C2X. .MatchId: Indication which sample identification(s) have to match so that the results can be combined. 3.2.2.7. Mode.Def.ComVar.C30 RSX, MNX, EPX, CXX Mode.Def.ComVar.C31 etc., up to .C39 Assignment of common variables.
3.2. Remote control commands Mode.Parameter.TitrPara.VStep 0...0.10...9.999 .MptDensity: Parameter for DET: Measuring point density. .MinIncr: Parameter for DET: Minimum increment in µL. If the minimum increment is set to 0, measured values are stored vs. time. .VStep: Parameter for MET: Volume increment in mL. With "0", there is no dispensing and measured values vs. time are entered in the measuring point list. 3.2.2.13. Mode.Parameter.TitrPara.DosRate 0.01...150, max.
3.2 Remote control commands Selection of the measuring input; valid with measured quantities pH and U. "diff." means differential amplifier, see page 155. 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. Besides .PolElectrTest is valid.
3.2. Remote control commands Mode.Parameter.Statistics.ResTab.Selected original, delete n, delete all 1...20 Mode.Parameter.Statistics.ResTab.DelN Entries for the statistics calculations. .Status: On/off switching. Requirement for statistics calculations is a valid assignment, see 3.2.2.9. .MeanN: Number of individual results for statistics calculations. .ResTab.Select: Selection of the table for the statistics calculations. original: Original table. The original table is (again) set up, i.e.
3.2 Remote control commands .pK: pK or HNP evaluation. Possible only in pH and U titrations. 3.2.2.25. Mode.Parameter.Presel.IReq id1, id1&2, all, OFF Mode.Parameter.Presel.SReq value, unit, all, OFF Parameters for DET, MET, SET, MEAS: Automatic inquiry after the start of the determination. From such an inquiry, the determination continues if the requested entry/entries is/are made, e.g. &SmplData.OFFSilo.Id1 (see 3.2.2.84) or with &M $G, see 3.2.2.1. $H is not possible in requests. 3.2.2.26. Mode.
3.2. Remote control commands 3.2.2.30. Mode.Parameter.TitrPara.Direction +, -, auto Parameters for SET: Titration direction. "auto" means the titration direction is determined automatically by the instrument. If 2 EP's have been set in a SET titration, the titration direction is given by the two EP's. The entry of the titration direction is then invalid. 3.2.2.31. Mode.Parameter.Presel.Cond Mode.Parameter.Presel.DriftDisp Parameters for SET: .Cond: Conditioning ON/OFF .
3.2 Remote control commands 3.2.2.36. Mode.Parameter.Calibration.CalTemp -20.0...25.0...120.0 Parameters for CAL: Calibration temperature in °C. If a Pt 100 or Pt1000 is connected, the temperature is measured. 3.2.2.37. Mode.Parameter.Calibration.Buffer.1.Value 0...7.00...±20.00 Mode.Parameter.Calibration.Buffer.2.Value 0...4.00...±20.00, OFF etc. up to 9 buffers Parameters for CAL: pH of buffers. The first buffer which is set to "OFF" determines the number of buffers in the calibration. 3.2.2.38. Mode.
3.2. Remote control commands Parameters for TIP: Parameters of the elements of TIP. .Method: Method name of a method available in the user memory. Up to 8 ASCII characters. .Pause: Pause time in s. INF means infinite. Continue the sequence with &m $G. .L4 Output: Warning: A pulse triggered by the limit value monitoring at L4 (pin 3) in a submethod sets an output set to active in TIP to inactive. .
3.2 Remote control commands UserMeth.List.1.Bytes read only UserMeth.List.1.Checksum read only for each method List of the methods in the user method memory with the following characteristics: .Name: Name of the method .Mode: Mode .Quantity: Measured quantity .Bytes: Number of bytes of the user memory used by the method .Checksum: Checksum of the method, see 3.2.2.68. 3.2.2.48. Config.PeriphUnit.
3.2. Remote control commands 3.2.2.55. Config.Aux.DevName up to 8 ASCII characters Name of the instrument for connections with several units. It is advisable to use only the letters A...Z (ASCII No. 65...90), a...z (ASCII No. 97...122) and the numbers 0...9 (ASCII No. 48...57) when the function Setup.AutoInfo (3.2.2.97) is used at the same time. If a name has been entered, it will be printed out in the result report (full, short). 3.2.2.56. Config.Aux.Prog Output of the program version.
3.2 Remote control commands 3.2.2.61. SmplData.ONSilo.Counter.MaxLines SmplData.ONSilo.Counter.FirstLine SmplData.ONSilo.Counter.LastLine Information on silo memory. .MaxLines: Maximum possible number of silo lines. .FirstLine: Lowest valid silo line. .LastLine: Last occupied silo line. read only read only read only 3.2.2.62. 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 up to 8 ASCII characters SmplData.
3.2. Remote control commands 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 3.2.2.64. 3.2.2.67. Info.Report Info.Report.Select $G configuration, parameters, smpl data, statistics, silo, calib, C-fmla, def, user method, full, short, mplist, curve, deriv, comb, scalc full, scalc srt, calc, all, ff $G sends the selected report to the COM which is set in &Config.
3.2 Remote control commands Calibration data can be entered. They are accepted with &Info.CalibrationData $G. If calibration data are entered, the calibration date is deleted. 3.2.2.69. Info.Checksums $G Info.Checksums.MPList read only Info.Checksums.ActualMethod read only The checksums can be used to identify the content of a file unequivocally, e.g. files with identical content have identical results of the checksums. An empty file has checksum "0". The calculation of the checksums is triggered with $G.
3.2. Remote control commands C40: Initial measured value in pH "5.12", mV (with U and Ipol) "41", µA (with Upol) "43.7" or °C (with T) "25.0". In MEAS final measured value. C41: End volume with SET in ml, "12.5360". C42: Time from start of titration to end in s, "62". C43: Volume drift on start of a SET titration from the conditioning in ul/min, "3.5". C44: (Last measured) temperature in °C. Used for the temperature compensation in pH measurements. C45: Start volume with DET, MET, SET in ml, "2.800".
3.2 Remote control commands C24.Value: Value C24.Unit: Unit of the assigned value C26.ActN: Number of single results C26.Mean: Mean (decimal places as for the result itself) C26.Std: Standard deviation (decimal places as for the result + 1) C26.RelStd: Relative standard deviation (in %, 2 decimal places) "2.222" "%" "3" "3.421" "0.0231" "0.14" 3.2.2.75. Info.ActualInfo.Inputs.Status read only Info.ActualInfo.Inputs.Change read only Info.ActualInfo.Inputs.Clear $G Info.ActualInfo.Outputs.
3.2. Remote control commands 3.2.2.79. Info.ActualInfo.Titrator.CyclNo Info.ActualInfo.Titrator.V Info.ActualInfo.Titrator.Meas Info.ActualInfo.Titrator.dVdt Info.ActualInfo.Titrator.dMeasdt Info.ActualInfo.Titrator.dMeasdV Info.ActualInfo.Titrator.
3.2 Remote control commands 3.2.2.82. Info.Assembly.CycleTime read only Info.Assembly.ExV read only Inquiries regarding basic variables of the assembly: Cycle time in s, volume of the active Exchange Unit in mL. 3.2.2.83. 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.
3.2. Remote control commands Assembly.Outputs.SetLines $G Assembly.Outputs.SetLines.L0 active, inactive, pulse, OFF up to .L 3 Assembly.Outputs.ResetLines $G 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 performed in the same beaker. Before AutoEOD is switched on, line 3 must be set to "OFF". .
3.2 Remote control commands 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 key .Parameter: Disable the key .SmplData: Disable the key .UserMeth.Recall: Disable "recall" in key .UserMeth.Store: Disable "store" in key .UserMeth.
3.2. Remote control commands 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. .V: Volume .Meas: Measured value associated to the cycle number. The unit "assembly" must be preset (see 3.2.2.94). 3.2.2.96. Setup.SendMeas.Titrator.CyclNo ON, OFF Setup.SendMeas.Titrator.V ON, OFF Setup.SendMeas.Titrator.Meas ON, OFF Setup.SendMeas.Titrator.dVdt ON, OFF Setup.SendMeas.Titrator.dMeasdt ON, OFF Setup.SendMeas.Titrator.
3.2 Remote control commands .P PowerOn: Simulation of power on (3.2.2.99). Not from mains. Messages from node .T, Titrator: .T.R Ready: Status 'Ready' has been reached. .T.G Go: Instrument has been started. .T.GC GoCommand: Instrument (or submethod in TIP) has received a go command. .T.S Stop: Status 'Stop' has been reached. .T.B Begin of sequence (or submethod). .T.F Final: End of determination (or submethod), the final steps will be carried out. .T.E Error.
3.2. Remote control commands .Right: .Feed: Relative specification of the width of the output medium (e.g. paper width) for the length of the measured value axis. 1 means the measured value axis is plotted over the entire width of the paper (largest possible width). In extreme cases, the writing of the right tick may lie outside. Length of the volume axis referred to the burette cylinder volume, V(B) per cm (0.1 means, e.g. 1 mL/cm with a 10 mL Exchange Unit).
3.3 Properties of the RS 232 Interface 3.3 Properties of the RS 232 Interface Data Transfer Protocol The Titrino is configured as DTE (Data Terminal Equipment). The RS 232 interface has the following technical specifications: • Data interface according to the RS 232C standard, adjustable transfer parameters, see page 10. • Max. line length: 512 characters • Control characters: CR (ASCII DEC 13) LF (ASCII DEC 10) XON (ASCII DEC 17) XOFF (ASCII DEC 19) • Cable length: max. approx.
3.3 Properties of the RS 232 Interface Titrino as Receiver : Titrino external device 60 characters max. 22 characters LF RxD Data output XOFF Time of 4 characters XON XOFF Data input TxD String is processed 400 µs Time Titrino as Sender : Titrino external device XOFF XON Data output RxD LF Data input TxD max. 4 characters Data output disabled Data output enabled Time Software-Handshake, SWline Handshake input ports on the Titrino (CTS, DSR, DCD) are not checked.
3.3 Properties of the RS 232 Interface Titrino as Receiver : Titrino external device LF Input Titrino disabled LF RxD Data output XON XOFF Data input TxD 400 µs String is processed Time Titrino as Sender: Titrino external device XOFF Inquiry LF XON Data output RxD 1st line Response LF LF Data input TxD Data output disabled Data output enabled Time Titrino transmission can be stopped by external instruments with XOFF.
3.3 Properties of the RS 232 Interface Titrino as Sender: Titrino external device RTS RTS CTS CTS LF TxD TxD 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.
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 will only be sent when CTS and DSR are in the ”ON” condition and DCD is in the "OFF" condition. Received Data (RxD) Data are received only when DCD is "ON". Request to Send (RTS) ON condition: Titrino is ready to send data. Clear to Send (CTS) ON condition: Remote station is ready to receive data.
3.3 Properties of the RS 232 Interface Contact arrangement at plug (female) for RS 232C socket (male) 25 14 13 1 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 improper interconnection of instruments.
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 a connected printer. - Are the instruments switched on and cables plugged in correctly? Is the printer set to ”on-line”? Are baud rate, data bit and parity the same on both instruments? - Is the handshake set properly? If everything seems to be ok, try to print a report with the key sequence .
4.1 Error and special messages 4 Error messages, Troubleshooting Data transfer inoperative See measures on page 131. 4.1 Error and special messages XXX bytes missing check electrode check exchange unit check T-sensor data set reevaluation division by zero EP overflow manual stop meas.pt list overflow missing EP missing fix EP no.EP not corresponding no EP set no meas.quantity 794 Basic Titrino XXX bytes missing.
4.1. Error and special messages no method no new com.var. no new mean no new silo result no new temp.var. no sequence no titration data not valid outside overrange same buffer save lines OFF second TIP call silo empty silo full stop EP reached stop meas.val.reached stop time reached 134 The method required by the sample data from the silo memory or in a TIP sequence is not available in the method memory. Exit: .
4.1 Error and special messages stop V reached system error 3 TIP terminated wrong sample The determination has been stopped as the stop volume has been reached. The instrument adjustment data have been overwritten. Exit: . Default adjustment data are set. The error message appears each time the instrument is switched on until it has been readjusted (Metrohm service). TIP has been terminated. With SET, with preset titration direction the first measured value is outside the end point.
4.1. Error and special messages E44 E45 136 The RS interface parameters are no longer the same for both instruments. The receive buffer of the Titrino contains an incomplete string (missing LF). Transmission of the Titrino is thus blocked. Exit: Send LF or .
4.2. Diagnosis 4.2 Diagnosis 4.2.1 General The 794 Basic Titrino is a very precise and reliable instrument. Thanks to its rugged construction it is virtually impossible for external mechanical or electrical influences to have an adverse effect on its functions. Although the occasional fault in the instrument can not be excluded completely, it is certainly much more likely that malfunctions are caused by wrong operation or handling or through improper connections and operation with non-Metrohm instruments.
4.2. Diagnosis 4.2.3 Equipment required: − voltage calibrator, e.g. 1.773.0010 Metrohm pH Simulator − 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) − stop watch or watch with second hand − digital or analogue voltmeter (if need be, connect a calibrated recorder) − 2 connecting cables with 4 mm banana plugs − test plug 3.496.
4.2. Diagnosis keys test • Press . keys test matrix code • If any key is now pressed (on the 6.2132.080 keypad or on the fron panel of the 794), the appropriate matrix code appears in the display. Fig. 2 Fig. 1 Front panel 794 Keypad 794 • Block 1 is quit by pressing the key twice. diagnose press key 0...9 4 Cylinder code, date, time • Put exchange unit or dummy on the Titrino and put the burette tip into a collecting receptacle. • Press <0>.
4.2. Diagnosis date/time cylinder code • Press . date XX-XX-XX XX:XX:XX code:D0 XX ml activated dosing unit mL-code • Check date and time. • Check whether the mL-code does correspond with the exchange unit placed or not. For the sake of completeness, different exchange units can be inserted to check their mL code. If desired, the exchange unit can be removed again. If no exchange unit is inserted display does not show the mL-code but „check exchange unit !“. • Press .
4.2. Diagnosis pot.meter dV/dt 10? • Turn knob ‘dV/dt’ to the right stop and press . Test sequence: a) In a first step, the frequency of the RC oscillator (analogue rate) is tested over a period of 1 second. b) In a second step, the frequency of the quartz oscillator (digital rate) is tested over a period of 1 second. c) If no error is found, after about 3 s it appears motor-timer test o.k. • Press . diagnose press key 0...9 7 Analogue input test • Press <7>. analog input test 1...
4.2. Diagnosis Input 2 XX mV • Carry out the same measurements as with Input 1. • Press . analog input test 1...5 • Short-circuit input ‘Ind I’ (e.g. with cable 3.496.5070). • Press <3>. Input 1-2 XX mV The differencial voltage between inputs ‘Ind I‘ and ‘Ind II’ is displayed. Example: 0 - (+)1500 mV = -1500 mV • Remove cables from the inputs ‘Ind I’ and ‘Ind II’. • Press . analog input test 1...5 7.
4.2. Diagnosis dummy resistor 14.3kΩ ? • 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. • Press . Test sequence: 1. An asterisk flashes during the test. 2. In case of an error an error message appears. (If for example the switch-box is not connected, error 100 appears). 3. If no error is found, after about 15 s display shows polarizer test o.k. • Press . analog input test 1...5 • Press .
4.2. Diagnosis I/O-test-connector? • Insert the 3.496.8510 test plug in port B 'Remote'. (Do not switch off instrument!) • Press . Test sequence: 1. In case of an error an error message is displayed. If for example no test plug is connected, error message error 50 01HEX appears). 2. If no error is found, after about 1 s display shows extern input/output o.k. • Remove test plug. • Press . diagnose press key 0...9 9 RS 232 test A 3.496.
4.2. Diagnosis RS232 test-connector? • Insert the 3.496.8480 test plug in 'RS 232' port. • Press . Test sequence: 1. In case of an error an error message is displayed. If for example no test plug is connected, error message error 68 appears). 2. If no error is found, after about 5 s display shows RS232 test o.k. • Remove test plug. • Press . diagnose press key 0...9 10 Spindle drive and stopcock changeover • Press .
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). From the start point, the spindle travels 80 mm. Instead of the spindle height, the expelled volume can be measured (corresponds to max. vol. of Exchange Unit used).
4.3. Initialise and test RAM 4.3 Initialise and test RAM On the odd occasion large disturbing signals (e.g. mains spikes, lightning, etc.) can have an adverse effect on the processor functions and hence lead to a system crash. After such a crash the RAM area must be initialised. Although the basic instrument data remain stored, the RAM initialisation should be performed only when necessary since the stored user data (configuration, parameters, calculation variables, etc.) are cleared as a result.
4.4. Releasing a locked spindle with inserted Exchange Unit 4.4 Releasing a locked spindle with inserted Exchange Unit • The burette 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 removed. In this case, it is necessary to proceed as follows: 2 screws (M4 countersunk) 2 screws (M3 fillister head) knob edge of bench Fig.
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. Each break in the earthing inside or outside the instrument can make it a hazard. When the instrument is opened or if parts of it are removed, certain components may be live if the instrument is connected to the mains.
5.1. Setting up and connecting the instruments 5.1.2 Connection of a printer Printer Seiko DPU-414 Custom DP40-S4N A variety of printers can be connected to the RS232 interface of the Titrino. If you connect a printer other than one of those mentioned below, ensure that the Epson mode is emulated or that it uses the international character set following the IBM Standard Table 437 and IBM-compatible graphics control characters.
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 Ohaus Voyager, Explorer, Analytical Plus Titrino: Balance: balance delimiter SARTORIUS CR+LF from Ohaus: AS017-09 (Ohaus parts number)+ 6.2125.
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 manufacturer, in addition to the weight identifications and methods can be inputted from the balance. For this, the address of the identifications and method, resp. must be preselected on the input unit.
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. 794 A B C D Recorder The signal at the analogue output can be preselected on the Titrino (key , ">peripheral units", "curve:"): Preselection at Titrino U Meaning Voltage dU/dt Measured value drift V dV/dt U(rel) Volume Volume drift Control deviation T 794 Basic Titrino Temperature Resolution, Signal at analogue output pH = 0.00: − 700mV pH = 7.
5.1. Setting up and connecting the instruments 5.1.6 Connection of a computer 794 A C B D Cable 6.2125.060 (+6.2125.010) PC 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 ............................
5.2 Connection of electrodes, preparing titration vessel 5.2 Connection of electrodes, preparing titration vessel Rear panel: Ref Ref Connection for separate reference electrode. Input is free when a combined electrode is used. Pol Connection of polarized electrodes. If measured quantities Ipol or Upol are selected, this measuring input is automatically active. Ind I Connection of pH, redox, ISE electrodes. Combined or separate electrodes. Select measuring input 1 or 2 in the Titrino.
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. • As an "auxiliary electrode", the 6.1808.030 burette tip with earthing may be used in some cases.
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 • efficient stirring. But it should not be too fast, otherwise the stirrer vortex will suck in air bubbles and CO2 or O2 can disturb the titration.
6.1. Technical specifications 6 Appendix 6.1 Technical specifications Modes DET: Dynamic Equivalence Point Titration MET: Monotonic Equivalence Point 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. 1 reference input for a separate reference electrode. May also be used as a differential amplifier. 1 measuring input for polarized electrodes.
6.1 Technical specifications 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 17 Metrohm methods. Silo memory for sample data and results 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 Signal at analogoutput Ambient temperature Nom.
6.1. Technical specifications Mains connection Voltage Frequency Power consumption Fuse 100, 117, 220/230, 240 V (switchable) 50 ... 60 Hz 15 W Thermal fuse Dimensions with Exchange Unit Width 150 mm Height 450 mm Depth 275 mm Weight, incl. keypad 160 app. 3.
6.2 Pin assignment of the "Remote" socket 6.
6.2. Pin assignment of the "Remote" socket Outputs pin 17 (Output 3) End of determination EOD pin 3 (Output 4) L4 in TIP pin 16 (Output 5) Error, active with errors pin 1 (Output 6) Activate pulse, see page 163. L6 in TIP pin 2 (Output 7) Pulses for recorder (tp=150 µs) 10 000 per buret cylinder For all outputs: VCE0 = 40 V IC = 20 mA tPulse > 100 ms Functions see page 163. Voltage +5 V pin 15 I ≤ 75 mA 0V pin 14 0 V: active 5 V: inactive pin 25 Ordering numbers for plug: K.210.
6.2 Pin assignment of the "Remote" socket 6.2.
6.2. Pin assignment of the "Remote" socket 6.2.
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 . Stop volumes or other stop conditions should be entered depending on sample. If a printer is connected, the methods should be completed with report instructions (key ).
6.3. User methods 6.3.2 "Titer_pH" 'pa 794 Titrino 01102 794.0010 date 2002-01-03 time 09:34 0 DET pH Titer_pH parameters >titration parameters meas.pt.density 4 min.incr. 10.0 µl titr.rate max. ml/min signal drift 50 mV/min equilibr.time 26 s start V: OFF pause 0 s meas.input: 1 temperature 25.0 °C >stop conditions stop V: abs. stop V 20 ml stop pH OFF stop EP 9 filling rate max. ml/min >statistics status: ON mean n= 5 res.
6.3 User methods 6.3.3 "Blank" 'pa 794 Titrino 01102 794.0010 date 2002-01-03 time 09:38 0 DET U Blank parameters >titration parameters meas.pt.density 4 min.incr. 10.0 µl titr.rate max. ml/min signal drift 50 mV/min equilibr.time 26 s start V: OFF pause 0 s meas.input: 1 temperature 25.0 °C >stop conditions stop V: abs. stop V 30 ml stop U OFF mV stop EP 9 filling rate max. ml/min >statistics status: ON mean n= 3 res.
6.3. User methods 6.3.4 "Chloride" 'pa 794 Titrino 01102 794.0010 date 2002-01-03 time 09:40 0 DET U Chloride parameters >titration parameters meas.pt.density 4 min.incr. 10.0 µl titr.rate max. ml/min signal drift 50 mV/min equilibr.time 26 s start V: OFF pause 0 s meas.input: 1 temperature 25.0 °C >stop conditions stop V: abs. stop V 99.99 ml stop U OFF mV stop EP 1 filling rate max. ml/min >statistics status: OFF >evaluation EPC 5 EP recognition: all fix EP1 at U OFF mV pK/HNP: OFF >preselections req.
6.3 User methods 6.3.5 "TAN-TBN" Determination of the acid number according to ASTM D 5664-95 resp. of the base number according to ASTM D 2896-88. Electrodes: 6.0102.102 pH glass electrode at measuring input 1 ("Ind I") 6.0729.100 Ag/AgCl reference electrode (outer elektrolyte solution LiCl in sat. ethanol) at measuring input 2 (Ind II") 6.0301.100 Pt-Electrode at measuring input "Ref" Differential input Optional a Solvotrode can be used, in this case select meas.input: 1 in the method. TAN 6.0229.
6.3. User methods 6.3.6 "Diazo" Diazotation of sulfonamides and primary amines. 'pa 794 Titrino 01102 794.0010 date 2002-01-03 time 09:43 0 MET U Diazo parameters >titration parameters V step 0.10 ml titr.rate max. ml/min signal drift OFF mV/min equilibr.time 20 s start V: abs. start V 0.5 ml dos.rate max. ml/min pause 80 s meas.input: 1 temperature 25.0 °C >stop conditions stop V: abs. stop V 6.00 ml stop U OFF mV stop EP 9 filling rate max.
6.3 User methods 6.3.7 "Br-Index" Determination of the bromine index in petroleum hydrocarbons according to ASTM D 2710-72. 'pa 794 Titrino 01102 794.0010 date 2002-01-03 time 09:44 0 MET Ipol Br-Index parameters >titration parameters V step 0.05 ml titr.rate max. ml/min signal drift OFF mV/min equilibr.time 20 s start V: OFF pause 0 s I(pol) 1 µA electrode test: OFF temperature 25.0 °C >stop conditions stop V: abs. stop V 10 ml stop U 5 mV stop EP 9 filling rate max.
6.3. User methods 6.3.8 "Sapon.No" Determination of the saponification number of edible oils and fats. 'pa 794 Titrino 01102 794.0010 date 2002-01-03 time 09:50 0 DET U Sapon.No parameters >titration parameters meas.pt.density 4 min.incr. 10.0 µl titr.rate max. ml/min signal drift 50 mV/min equilibr.time 26 s start V: OFF pause 0 s meas.input: 1 temperature 25.0 °C >stop conditions stop V: abs. stop V 99.99 ml stop U OFF mV stop EP 1 filling rate max.
6.3 User methods 6.3.9 "Ca-Mg" Determination of the hardness of drinking water 'pa 794 Titrino 01102 794.0010 date 2002-01-03 time 09:52 0 DET U Ca-Mg parameters >titration parameters meas.pt.density 1 min.incr. 10.0 µl titr.rate max. ml/min signal drift 20 mV/min equilibr.time 38 s start V: OFF pause 0 s meas.input: 1 temperature 25.0 °C >stop conditions stop V: abs. stop V 5 ml stop U OFF mV stop EP 9 filling rate max.
6.3. User methods 6.3.10 "EDTA-NTA" EDTA und NTA in detergents. 'pa 794 Titrino 01102 794.0010 date 2002-01-03 time 09:53 0 DET U EDTA-NTA parameters >titration parameters meas.pt.density 4 min.incr. 10.0 µl titr.rate max. ml/min signal drift 50 mV/min equilibr.time 26 s start V: OFF pause 0 s meas.input: 1 temperature 25.0 °C >stop conditions stop V: abs. stop V 4 ml stop U OFF mV stop EP 9 filling rate max.
6.3 User methods 6.3.11 "Metals" The following metals can be detected according to this method: Barium Cadmium Cobalt Lead Nickel Water, total hardness Zinc Ba Cd Co Pb Ni (Ca+Mg) Zn 'pa 794 Titrino 01102 794.0010 date 2002-01-03 time 09:54 0 DET U Metals parameters >titration parameters meas.pt.density 2 min.incr. 10.0 µl titr.rate max. ml/min signal drift 20 mV/min equilibr.time 38 s start V: OFF pause 0 s meas.input: 1 temperature 25.0 °C >stop conditions stop V: abs.
6.3. User methods 6.3.12 "Perox.No" 'pa 794 Titrino 01102 794.0010 date 2002-01-03 time 09:56 0 DET U Perox.No parameters >titration parameters meas.pt.density 4 min.incr. 10.0 µl titr.rate max. ml/min signal drift 50 mV/min equilibr.time 26 s start V: OFF pause 0 s meas.input: 1 temperature 25.0 °C >stop conditions stop V: abs. stop V 99.99 ml stop U OFF mV stop EP 1 filling rate max. ml/min >statistics status: OFF >evaluation EPC 5 EP recognition: all fix EP1 at U OFF mV pK/HNP: OFF >preselections req.
6.3 User methods 6.3.13 "FormolNo"" Determination of the formaldehyde number in fruit juices. TIP method with the submethods "Form.Pre" and "Form.Det" Electrode: 6.0232.100 combined pH glass electrode, at measuring input 1. Additonal instrument: 765 Dosimat, connect to 794 Basic Titrino via Remote line. Titrant: c(NaOH) = 0.1 mol/L. Aux. reagent: w(formaldehyde) = 0.35 adjusted to pH 8.5 with NaOH. Sample: Pipette exactly 25 mL sample into the titration vessel.
6.3. User methods 'pa 794 Titrino 01102 794.0010 date 2002-01-03 time 09:58 0 SET pH Form.Det parameters >SET1 EP at pH 8.50 dynamics 1.5 max.rate 10.0 ml/min min.rate 25.0 µl/min stop crit: drift stop drift 20 µl/min >SET2 EP at pH OFF >titration parameters titr.direction: + start V: OFF pause 0 s meas.input: 1 temperature 25.0 °C >stop conditions stop V: abs. stop V 99.99 ml filling rate max. ml/min >statistics status: OFF >preselections conditioning: OFF req.ident: OFF req.
6.3 User methods 'pa 794 Titrino 01102 794.0010 date 2002-01-03 time 10:00 0 TIP FormolNo parameters >sequence 1.method: Form.Pre 2.L6 output: pulse 3.pause 60 s 4.method: Form.Det >statistics status: ON mean n= 3 res.tab: original >preselections req.ident: OFF req.smpl size: OFF meas.mode: OFF temperature 25.0 °C -----------'fm 794 Titrino 01102 794.0010 date 2002-01-03 time 10:00 0 TIP FormolNo >calculations FormolNo=C70*C01;1; C01= 4 C70= 5.
6.3. User methods 6.3.14 "P2O5Fert"" Determination of P2O5 in fertilizer. TIP method with submethods "P2O5-1" and "P2O5-2" Electrode: 6.0232.100 combined pH glass electrode, at measuring input 1. additional instrument: 765 Dosimat, connect to 794 Basic Titrino via Remote line. Titrant: c(NaOH) = 1.0 mol/L. Reagents: c(HCl) = 1.0 mol/L Sodium oxalate sat. Sample: Pipette exactly 10 mL liquid fertilizer into the titration vessel. Add 5 mL c(HCl) = 1.0 mol/L and dilute with 40 mL dist. water.
6.3 User methods 'de 794 Titrino 01102 794.0010 date 2002-01-03 time 10:03 DET pH P2O5-1 def >formula excess=C41-EP1 RS1 text excess RS1 decimal places 3 RS1 unit: ml >silo calculations match id: OFF >common variables >report >mean MN1=RS1 >temporary variables C70=RS1 -----------'pa 794 Titrino 01102 794.0010 date 2002-01-03 time 10:04 0 DET pH P2O5-2 parameters >titration parameters meas.pt.density 4 min.incr. 10.0 µl titr.rate max. ml/min signal drift 50 mV/min equilibr.
6.3. User methods 'pa 794 Titrino 01102 794.0010 date 2002-01-03 time 10:06 0 TIP P2O5Fert parameters >sequence 1.method: P2O5-1 2.L6 output: pulse 3.pause 30 s 4.method: P2O5-2 >statistics status: ON mean n= 3 res.tab: original >preselections req.ident: OFF req.smpl size: OFF meas.mode: OFF temperature 25.0 °C -----------'fm 794 Titrino 01102 794.0010 date 2002-01-03 time 10:06 0 TIP P2O5Fert >calculations P2O5=(C70+C71)*C01*C02/C00;2;% C00= 1.0 C01= 1 C02= 7.1 C70= 1.031 C71= 10.
6.4 Validation / GLP 6.4 Validation / GLP GLP (Good Laboratory Practice) requires the periodic validation of the analytical instruments. The reproducibility and accuracy of the instruments are checked according to standard operating procedures. Guidelines for the testing regulations (SOP, Standard Operating Procedure) are given in the following Metrohm Application Bulletin: No. 252: Validation of Metrohm Titrators (potentiometric) according to GLP/ISO 9001.
6.5. Warranty and conformity 6.5 Warranty and conformity 6.5.1 Warranty The warranty regarding our products is limited to rectification free of charge in our workshops of defects that can be proved to be due to material, design or manufacturing faults which appear within 12 months from the day of delivery. Transport costs are chargeable to the purchaser. For day and night operation, the warranty is valid for 6 months.
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: 794 Basic Titrino meets the requirements of EC Directives 89/336/EEC and 73/23/EEC.
6.5. Warranty and conformity 6.5.3 Certificate of Conformity and System Validation Certificate of Conformity and System Validation This is to certify the conformity to the standard specifications for electrical appliances and accessories, as well as to the standard specifications for security and to system validation issued by the manufacturing company. Name of commodity: 794 Basic Titrino System software: Stored in ROMs Name of manufacturer: Metrohm Ltd.
6.6 Scope of delivery and ordering designations 6.6 Scope of delivery and ordering designations 794 Basic Titrino ......................................................................................2.794.0010 inclusive the following accessories: 1 Titrino ................................................................................................................. 1.794.0010 1 Keypad for 794 Basic Titrino ............................................................................. 6.2132.
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 .........................................
6.6 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 ......
Index Index Keys are marked with < >, display texts are in bold characters and pages concerning the green part are printed in Italic. A Accessories........................................... 187ff activate pulse: ..................... 30, 40, 46, 47 Analogue output connection of a recorder..................... 153 resolution............................................. 153 test....................................................... 140 auto start ................................................
Index E Earthing .......................................................5 edit silo lines ........................................71 EDTA-NTA ...............................................174 electr.id.............................................47, 68 electrode test: ......................26, 37, 45, 50 Electrodes connection...........................................155 End volume................................................53 EP criterion..................................................
Index ................................................ 50 .......................... 133 meas.pt.density ................................. 26, 32 measuring parameters .............................. 45 Measuring point list print ....................................................... 60 Menu ........................................................... 7 MET ......................................................... 26ff Metals...................................................... 175 method ...................
Index S same buffer .............................................134 Sample data .......................................................69 identification ....................................30, 69 size ........................................................70 sample changer cal: ................................47 Sapon.No ................................................172 save lines OFF .......................................134 save lines: ...............................................72 Save method .
Index User methods.................................. 66, 165ff W V Warranty.................................................. 184 wrong sample .......................................... 135 V step .................................................. 26, 33 Validation................................................. 183 Values entry................................................. 7 194 X XXX bytes missing .................................
