756/831 KF Coulometer Manual 8.831.
CH-9101 Herisau/Switzerland E-Mail info@metrohm.com Internet www.metrohm.com 756 KF Coulometer 831 KF Coulometer Program version 5.756.0012 and 5.831.0011 Instructions for Use 8.831.1003 04.
Contents Contents 1 Introduction .......................................................... 1 1.1 Parts and controls............................................................................... 2 2 The wet chemistry workplace ............................. 4 2.1 2.2 2.3 2.4 2.5 2.6 2.7 2.7 Principle of coulometric KF determinations...................................... 4 Titration vessel setup.......................................................................... 5 Your first determination ......
Contents 3.13 Current sample data, key ...................................... 46 3.14 Silo memory for sample data ........................................................... 47 3.15 Storing determination results and silo calculations ....................... 50 3.15.1 Storing determination results..................................................... 50 3.15.2 Silo calculations ......................................................................... 51 4 Operation via RS232 Interface............
Contents 7 Appendix ........................................................... 127 7.1 Technical specifications ..................................................................... 127 7.2 Pin assignment of the "Remote" socket............................................. 129 7.2.1 Lines of socket "Remote" ............................................................131 7.2.2 Activate pulse .............................................................................132 7.3 Coulometer validation, GLP mode.
Contents IV 756/831 KF Coulometer, Instructions for Use
Introduction 1 Introduction These instructions provide you with a comprehensive overview of the installation, working principles and operation of the 756 KF Coulometer and the 831 KF Coulometer. As these two instruments are, aside from the built-in thermal printer of the 756 KF Coulometer, identical, the Instructions for Use for both have been incorporated in a single document. The report examples, mapped in this document, were generated by a 756 KF Coulometer.
1.1 Parts and controls 1.1 Parts and controls 1 2 3 4 Frontview KF Coulometer 1 Built-in thermal printer (only at 756) Ordering number for thermal paper: 6.2237.020 3 Control keys and indicator lamps on the KF Coulometer only at 756 KF Coulometer 2 Display 4 Setting of display contrast 3 Control keys and indicator lamps on the KF Coulometer Key < > Switches Coulometer ON/OFF Key < ∞ > Key Key Key Indicator lampes: "COND.
Introduction RS 232 Made by Metrohm Herisau Switzerland 5 1 1.756. Nr. 13 Gen. EL. 6 14 2 Remote 7 8 Dos 100 - 240 V f = 50-60 Hz P = 38 W 9 10 12 Keyboard Ind. EL. 11 Rearview KF Coulometer 5 RS232 interfaces 2 separate interfaces for the connection of balance, computer, printer etc.
2.1 Principle of coulometric KF determinations 2 The wet chemistry workplace 2.1 Principle of coulometric KF determinations The coulometric Karl Fischer titration is a version of the classical water determination method developed by Karl Fischer. The traditional method utilises a methanolic solution of iodine, sulphur dioxide and a base as buffer.
2.2 Titration vessel setup 2.2 Titration vessel setup Drying tube Generator electrode Indicator electrode Stirring bar Septum stopper 1) 2) 1. Attach titration vessel with holder to the support rod. 2. Place stirring bar in titration vessel. 3. Cut 6.2713.XXX ground joint sleeves to the correct lengths and use them for all the joints of the inserts1). 4. Insert indicator electrode in the left-hand joint opening, screw on 6.2104.020 electrode cable and plug it into the "Ind.
2.3 Your first determination 2.3 Your first determination The titration vessel has been prepared (see page 5) and the Coulometer is switched on. In the display appears KFC ******** KFC drift wait ⇓ 53 ug/min ⇔ 4.3 ug/min KFC drift ready smpl size 1.0 g Press the key. Pre-conditioning begins, i.e. the titration vessel is dried. The "COND" LED blinks. The arrow in the drift display shows the drift tendency (falling, rising, stable).
2.4 Generator electrode without diaphragm 2.4 Generator electrode without diaphragm The 6.0345.100 generator electrode without diaphragm poses no handling problems and is easy to clean. It only requires one reagent and is quickly ready for use (no moisture depots in the diaphragm!). The generator electrode without diaphragm is the best choice for most applications. It is particularly suitable for use with very polluting samples. 2.4.
2.5 Generator electrode with diaphragm 2.5 Generator electrode with diaphragm The 6.0344.100 generator electrode with diaphragm should be used when your samples contain ketones and aldehydes because special reagents for aldehydes and ketones are only available for generator electrodes with diaphragms. If your reagent has a low conductivity, e.g. if you have had to add chloroform because of the solubility of the sample then you should use the generator electrode with diaphragm as first choice.
2.6 Tips for working with water standards 2.6 Tips for working with water standards For validation of the instrument, as a fully integrated measuring system, commercial, certified water standard solutions with water contents of 1.00 ± 0.003 mg/g and/or 0.10 ± 0.005 mg/g should be applied (The 1.0 mg/g Standard is easier to handle and therefore to prefer). Recommended initial weight range: Liquid standard 1.0 mg/g 0.2-2.0 g Liquid standard 0.1 mg/g 0.5-1.5 g 2.6.
2.7 Sample addition 12. Close the syringe and put it back on the balance. 13. Read the indicated value off the balance and feed it at your Coulometer as sample size. 14. As soon as the determination has finished and the titration cell is conditioned again, you can start with the next determination. 2.7 Sample addition This section contains some information about sample addition. A detailed description of this topic is not possible here.
2.7 Sample addition Highly viscous samples can be warmed to lower their viscosity; the syringe must also be warmed. The same goal can also be reached by dilution with a suitable solvent. In this case the water content of the solvent must be determined and deducted as a blank value correction. Pastes, greases can be placed in the measuring cell by using a syringe without a needle. The joint opening can be used for this purpose.
2.8 Optimal working conditions 2.8 Optimal working conditions If a thoroughly dry titration vessel with a generator electrode without diaphragm is used then the basic drift is reached within approx. 30 minutes. It is recommended that the titration vessel is carefully shaken several times during this time. For generator electrodes with diaphragm a preparation period of approx. 2 hours must be expected.
2.8 Optimal working conditions 2.8.2 Reagent exchange In the following cases the electrolyte solutions should be exchanged: • When the titration vessel is too full. • When the capacity of the reagent is exhausted. • If the drift is too high and shaking the cell does not result in any improvement. • If a two-phase mixture is formed in the titration vessel. In this case only the sample phase can be aspirated off, see also page 25. • If during the determination the error message "check generator electr.
3.1 Keypad 3 Manual operation 3.1 Keypad CONFIG PARAM STATISTICS 7 SMPL DATA H2 O RS 4 C-FMLA C 1 PRINT 0 MN ← CLEAR STOP USER 8 + – EXCH 5 * DEF ( 2 REPORTS . ↑ ↓ QUIT ABC 6 / USER METH ) 3 MODE – Configuration. PARAM Parameters. SMPL DATA Sample data. SILO 9 CONFIG ; → ENTER START 6.2130.040 STATISTICS ON/OFF switching of statistics calculations of consecutive determination, see page 37. USER User name, see page 43.
3.2 Principle of data input 3.2 Principle of data input parameters >titration parameters >statistics >preselections • If you press a key you will find a group of inquiries in the display. Example key (in the standard operation level): In the first line you see where you are: you pressed key and you are now in the inquiries parameters. • The cursor is inverted. In our example the cursor is on the inquiry >titration parameters. You can move the cursor up and down with keys <↑> and <↓>.
3.3 Text input 3.3 Text input Example: storing a method: user methods >store method method name: ******** • Delete this name with . REPORTS . ABC user methods >store method: method name: ABCDEFGHIJKLMNOPQRSTUVWXYZ abcdefghijklmnopqrstuvwxyz µ°!"#$&'()*+,-./ 0123456789 user methods >store method method name: • Press key . Place the cursor to >store method and press . The name of the method which is currently in the working memory is displayed.
3.4 Configuration, key 3.4 Configuration, key The key is used for the entry of instrument-specific data. The set values apply for all modes. All entries are only possible in the inactive basic status of the Coulometer. Two different operating modes are available: standard mode and expert mode. Inquiries which appear in the standard mode are highlighted in gray.
3.4 Configuration, key If on has been set: number of determ. 1 determ.counter 0 reagent lifetime 7 d time counter 0 d reagent capacity 1000 mg capacity counter drift reagent change: waiting time 18 0 mg OFF ug/min OFF 0 s Monitoring according to the number of determinations carried out (1...999, OFF) The number of determinations which can be carried out depends on the type of sample (very polluting, lowering the conductivity) and on the amount of sample which is to be injected.
3.4 Configuration, key aspirate volume 100 ml Aspirate volume (0...9999 ml) Volume to be aspirated. reagent volume 100 ml Reagent volume (0...9999 ml) Volume to be added. rinsing volume 0 ml rinsing cycles 1 validation: OFF time interval 365 d time counter 0 d service: next service OFF YYYY-MM-DD system test report: OFF Rinsing volume (0...9999 ml) Normally rinsing is not necessary. When ≠ 0 ml has been set Number of rinsing cycles (1...
3.4 Configuration, key man.reports to: int.
3.4 Configuration, key run number 0 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. operator level: standard Operating mode (standard, expert) Determines the number of inquiries which are accessible. Operation in the standard mode contains only a few inquiries and is recommended for routine applications.
3.4 Configuration, key Configuration of the report Printing report lines or data can be switched on and off. This means that the report can be arranged according to your requirements. >report report id: ON Prints the line "Report-Id" (ON, OFF) e.g. 'fr. If you use Vesuv 3 the report identification is switched on automatically. instrument id: ON Prints the line(s) "instrument-Id" (ON, OFF) 756 (or 831) KF Coulometer, instrument-Id and program version.
3.4 Configuration, key Settings with key and power ON Proceed as follows: 1. Switch the Coulometer off. 2. Press and keep it pressed during switching the Coulometer on. The display shows the following: Setup >lock >curve Lock: Locking keys , and , and the functions recall method, store method and delete method of the method memory in the Coulometer. Curve: Changes the appearance of the curve printout.
3.4 Configuration, key Curve The settings are similar for COM1 and COM2. If you change the printer type, the following settings are initialized according to the printer. >curve >Int. 24 grid: ON Grid drawing (ON, OFF) frame: ON Frame drawing (ON, OFF) scaling: auto Type of scaling (Full, Auto) Full: the scaling goes from the greatest to the smallest value. auto: the scaling from tick to tick, e.g. the smallest/greatest values lie in between the first/last tick. width 0.90 Width (0.2.
3.4 Configuration, key 3.4.1 Reagent exchange procedure with Dosino or Automatic exchange Reagent exchange is automatic (if a reagent monitoring responds) or is triggered with . During the exchange changing reagent appears in the display. Conditioning off Stirrer off Current production and stirrer are switched off. (Waiting time) The waiting time is allowed to elapse. In this time it is possible to wait for the separation of e.g. a 2-phase mixture.
3.5 Mode selection, key 3.5 Mode selection, key MODE – The key is pressed repeatedly until the required mode is displayed. This is accepted with . ; mode mode: KFC The following modes can be selected: • KFC: coulometric KF titration. • KFC-B: KF titration with blank value correction • BLANK: determination of blank value • GLP: mode for system validation The newly loaded modes are provided with standard parameters and immediately ready for use.
3.6 Parameters, key 3.6 Parameters, key The key is used to enter mode-specific parameters. Values marked with cond. are accessible during conditioning, while **titr. means that these values can also be altered during the titration. In this case they will influence the run being carried out. All other values can only be altered in the inactive basic status. Two different operating modes are available: standard mode and expert mode.
3.6 Parameters, key stop crit: rel.drift **titr. stop drift 5 ug/min **titr. rel.drift 5 ug/min **titr. 0 s Pause (0...999 999 s) Waiting period in which no iodine is produced. The pause can be terminated with . 0 s Extraction time (0...999 999 s) The titration takes place during this time. However, it is not stopped until the extraction time has elapsed (even when the EP has been reached). The extraction time can be terminated with . **titr. extr.time **titr.
3.6 Parameters, key Preselections for the titration sequence >preselections drift corr: auto cond. drift value 0.0 ug/min Type of drift correction (auto, man., OFF) auto: drift value at start is valid and deducted. Value for manual drift correction (0...99.9 ug/min) cond. req.ident: OFF cond. req.smpl size: value Request of sample size after start of titration (value, unit, all, OFF) all: the value and the unit will be requested.
3.6 Parameters, key generator I: Oven: 400 mA Current at generator electrode (100, 200, 400 mA, auto) see also page 33. auto means that the current is automatically adapted to the conductivity of the reagent and that in the region of the endpoint the current will be controlled at smaller values. no Connected oven (COM1, COM2, no) COM of the Coulometer to which the oven is connected.
3.6 Parameters, key 3.6.1 Titration sequence (Activate pulse) (Stirrer ON) (Start delay) (Preconditioning) ( (Activate pulse) (Start delay) After the start, the activate pulse is outputted and the stirrer switched on. The start delay time is allowed to elapse. The solution is titrated until the EP is reached. The display then shows KFC wait and the "COND" indicator blinks. If the EP has been reached, the display shows KFC drift <=> ready 2.4 ug/min The indicator "COND" is ON.
3.6 Parameters, key 3.6.2 Control parameters and Ipol The standard control parameters are optimal for most applications and should not be altered. If you nevertheless need to alter the control parameters for special reagents and/or samples take care that the polarization current of the indicator electrode, the endpoint and the control range are linked to each other.
3.6 Parameters, key Drift in ug/min 100 80 60 40 Start drift Drift value at start Stop drift 20 Time 0 Cond. Start Titr. End Titr. Start drift When the actual drift during conditioning is smaller than the start drift a titration can be started. The "COND" LED remains on all the time. Stop drift The titration is terminated when the EP has been reached and the stop drift is undercut. For the relative stop drift the drift value at the start of the titration + the relative drift applies.
3.7 Result calculations 3.7 Result calculations Formula entry, key DEF 2 ( def >formula >silo calculations >common variables >report >mean >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 (in expert mode only): Formulas for result calculations. The display texts of the Coulometer are shown to the left. The values are the default values.
3.7 Result calculations RS1 text RS1 decimal places RS1 2 Text for result output (up to 8 characters) Text input see page 16. Number of decimal places for result (0...5) RS1 unit: ppm Selection of result unit (ppm, mg/g, mg/ml, mg, ug, mg/pc, %, no unit or up to 6 characters). RS1 limit control: OFF Limit control for the result (on, off) The limits are checked each time a result is calculated. RS1 low lim. 0.0 RS1 up lim. 0.0 RS1 L13 output: OFF If on has been set: Lower limit (0.0...
3.7 Result calculations Input of method-specific operands C01...C19, key C-FMLA 1 With the operands C01...C19 can be entered. For the calculation the operands which were introduced in the formula are used. The inputs are method-specific and are stored in the method memory.
3.8 Statistics calculations 3.8 Statistics calculations 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. ( def >formula >silo calculations >common variables >report >mean Mean (in expert mode only): Assigns values for statistics calculations. The display texts of the Coulometer are shown to the left.
3.8 Statistics calculations How do you obtain statistics calculations? 1) Enter the allocations for the statistics calculation (in expert mode only), see page 37. 2) Switch on the statistics calculations: either with or set the status under , >statistics to ON. The "STATISTICS" LED is on. The status of the statistics calculation is retained when a method is stored in the method memory. 3) Change the number of the individual values n under mean n, if necessary.
3.9 Common variables 3.9 Common variables Common variables are used for: • Determination of a blank value with method 1. Using this blank value in various other methods. Mode BLANK creates the common variable C39 (default setting). • Determination of a result with method 1. Reconciliation of this result in various other methods. You may view the values of the common variables with . DEF 2 ( With , results can be allocated as common variables.
3.10 Data output 3.10 Data output 3.10.1 Reports for the output at the end of a determination DEF 2 ( def >formula >silo calculations >common variables >report >mean 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 Coulometer are shown to the left.
3.10 Data output Original reports have double dashes ==== at the end, whereas recalculations are marked by single dashes ----. Report outputs can be stopped with . Report examples: 'fr 756 KF Coulometer 01109 5.756.0010 user Boss date 1998-10-27 time 08:54 KFC 3 ******** smpl size drift auto 0.372 g 3.2 ug/min titr.time H2O 47 s 206.5 ug content Result report: Report identification Instrument identification " User name, see page 43. 555.
3.10 Data output 3.10.2 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 for selecting the reports: 1) <←/→> 2) Cursor is pressed repeatedly until the desired report appears in the display. key X is the key under which the appropriate data are entered. Report Result report Curve water vs. time Curve rate vs. time Curve measured voltage vs.
3.11 User name, key 3.11 User name, key USER 8 user name: >delete The key manages the user names. User names can be entered directly or selected with the keys <←> and <→>. + Boss Name: Selection or input of user name. Delete: Delete user name. The display texts of the Coulometer are shown below at the left. Inquiries which also appear in the standard mode are highlighted in gray.
3.12 Method memory, key 3.12 Method memory, key USER METH 3 user methods >recall method >store method >delete method ) Management of the method memory with key . Select method name with keys <←> and <→> or enter names directly. Recall method: Loads a method from the method memory into the working memory. Store method: Stores the method which is in the working memory in the method memory. Delete method: Deletes a method from the method memory.
3.12 Method memory, key The contents of the method memory can be printed with the key sequence 'um 756 KF Coulometer 5.756.0010 date 1998-11-02 time 14:27 user methods bytes BLANK Oven-Blk 164 KFC-B Oven-Det 184 BLANK 774-Blk 168 KFC-B 774-Det 188 remaining bytes 39266 Document your methods (e.g. parameter report, def report and C-fmla report)! With a PC and the 6.6008.XXX Vesuv 3 program you should carry out a complete method backup from time to time.
3.13 Current sample data, key 3.13 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 47. Instead of entering the current sample data with , you can request these data automatically after start of determinations, see page 29. Current sample data can be entered live during the titration. Id1...3 or C21...
3.14 Silo memory for sample data 3.14 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 50. SILO 9 Press the key for working with the silo memory. The status LED "silo" is on when the silo memory is switched on.
3.14 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 >delete silo lines >delete all silo lines cycle lines: OFF save lines: OFF The display texts of the Coulometer are shown to the left.
3.14 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.
3.15 Storing determination results and silo calculations 3.15 Storing determination results and silo calculations 3.15.
3.15 Storing determination results and silo calculations After several samples have been processed, the silo memory report can have the following appearance (printout with ): 'si 756 KF Coulometer date 1998-10-27 012/101 time 5.756.0010 08:54 14 >silo cycle lines: OFF save lines: sl + 1 + 2 / 3 4 5 ON method id1/C21 11-2 A/12 11-2 A/13 11-2 A/14 11-2 A/15 11-2 A/16 ------------ id2/C22 98-11-12 98-11-12 98-11-12 98-11-12 98-11-12 id3/C23 C00 0.233 0.286 0.197 0.288 0.
3.15 Storing determination results and silo calculations Starting from the following silo report: 'si 756 KF Coulometer 012/101 date time 1998-10-27 5.756.0010 08:54 14 >silo cycle lines: OFF save lines: sl + 1 + 2 + 3 + 4 / 5 ON method id1/C21 11-2 A/12 0-15 A/13 0-15 A/13 11-2 A/12 11-2 A/15 ------------ id2/C22 98-11-12 98-11-12 98-11-12 98-11-12 98-11-12 id3/C23 C00 0.233 0.286 0.197 0.288 0.263 g g g g g C24 14.2 13.8 14.5 13.8 14.
4.1 General rules 4 Operation via RS232 Interface 4.1 General rules The KF Coulometer has an extensive remote control facility that allows full control of the KF Coulometer via the RS 232 interface, i.e. the KF Coulometer 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 KF Coulometer sends 2xCR and LF as termination of a data block, to differentiate between a data line which has CR and LF as terminators.
4.1 General rules 4.1.1 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.
4.1 General rules 4.1.2 Triggers Triggers initiate an action on the KF Coulometer, for example, starting a process or sending data. Triggers are marked by the introductory symbol $. The following triggers are possible: $G Go $S $Q Stop Query $Q.P $Q.H Path Highest Index Name Detail-Info qUit $Q.N"i" $D $U Starts processes, for ex.
4.1 General rules 4.1.3 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 KF Coulometer. 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.KFC.Inac;E26.
4.1 General rules 4.1.4 Error messages Error messages are added to the status messages and separated from them by the sign ";". E20 E21 E22 E23 E24 E25 E26 E28 E29 E30 E31 E32 E33 E36 E37 E38 E39 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 start or on recalculation. Check drive unit.
4.1 General rules E42 E43 E45 E120 E121 E123 E127 E128 E129 E132 E133 E134 E137 E155 E176 E190 E192 E194 58 RS send errors: CTS=OFF No proper handshake for more than 1 s. Exit: Is the receiver switched on and ready to receive? The transmission of the KF Coulometer has been interrupted with XOFF for at least 6 s. Exit: Send XON or The receive buffer of the KF Coulometer contains an incomplete command (LF missing). Sending from the KF Coulometer is therefore blocked.
4.1 General rules E196 E197 E198 E199 E203 E209 E212 E213 E214 Result is out of limits. Exit: The error message disappears on next start or on recalculation. Sample size is out of limits. Exit: The error message disappears on next start or on introduction of new sample size. Validation interval is expired. Exit: The error message disappears on next start or clear counter with &Config.Monitoring.Validation.Clear $G. Service date is reached.
4.2 Remote control commands 4.2 Remote control commands 4.2.
4.2 Remote control commands &Mode Object Description Input range & Root ├ Mode : ├ .Select ├ .Name Mode Mode selection Name of current method $G, $S KFC,KFC-B,BLANK,GLP read only/read+write 4.2.2.1. 4.2.2.2. 4.2.2.3. 0...50...±2000 content, special 4.2.2.4. ├ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ │ .Parameter Parameters of current mode .CtrlPara Control parameters ├ .EP Endpoint ├ .Control without meaning ├ .Content without meaning ├ .
4.2 Remote control commands │ │ ├ │ │ ├ │ │ ├ .GenI .Oven .ActPulse ├ .Def │ ├ .Formulas │ │ ├ .1 │ │ │ ├ .Formula │ │ │ ├ .TextRS │ │ │ ├ .Decimal │ │ │ ├ .Unit │ │ │ ├ .Limits │ │ │ ├ .LoLim │ │ │ ├ .UpLim │ │ │ ├ .Output │ │ │ : │ ├ .SiloCalc │ │ ├ .Assign │ │ │ ├ .C24 │ │ │ ├ .C25 │ │ ├ .MatchId │ ├ .ComVar │ │ ├ .C30 │ │ ├ up to C39 │ ├ .Report │ │ ├ .Internal │ │ ├ .Assign1 │ │ ├ .Assign2 │ ├ .Mean │ │ ├ .1 │ │ │ ├ .Assign │ │ │ : ├ .CFmla │ ├ .1 │ │ ├ .
4.2 Remote control commands &UserMeth Object Description Input range Reference & Root : ├ UserMeth : ├ .FreeMemory ├ .Recall │ ├ .Name ├ .Store │ ├ .Name ├ .Delete │ ├ .Name ├ .DelAll ├ .List │ ├ .1 │ │ ├ .Name │ │ ├ .Mode │ │ ├ .Bytes │ │ ├ .Checksum ├ .
4.2 Remote control commands &Config Object Description Input range Reference & Root : ├ Config : ├ .Monitoring │ ├ .Reagent │ │ ├ .Status │ │ ├ .Determ │ │ ├ .DCounter │ │ ├ .MaxTime │ │ ├ .TCounter │ │ ├ .ReagCap │ │ ├ .RCounter │ │ ├ .ClearCount │ │ ├ .Drift │ ├ .Change │ │ ├ .Status │ │ ├ .WaitTime │ │ ├ .AspVol │ │ ├ .SolventVol │ │ ├ .Rinse │ │ ├ .NoRinse │ ├ .Validation │ │ ├ .Status │ │ ├ .Interval │ │ ├ .Counter │ │ ├ .ClearCount │ ├ .Service │ │ ├ .Status │ │ ├ .Date │ ├ .DiagRep ├ .
4.2 Remote control commands │ │ ├ .Time │ ├ .RunNo │ ├ .OpLevel │ ├ .StartDelay │ ├ .ResDisplay │ ├ .DevName │ ├ .Beep │ ├ .DisplayMeas │ ├ .Prog │ ├ .RSSet1 │ ├ .Baud │ │ │ ├ .DataBit │ ├ .StopBit │ ├ .Parity │ ├ .Handsh │ │ ├ .RSSet2 │ ├ .Report │ ├ .Id │ ├ .Instr │ ├ .DateTime │ ├ .Run │ ├ .Method │ ├ .Sample │ ├ .Drift │ ├ .TitrTime │ ├ .EPH2O │ ├ .Statistics │ ├ .Visum │ ├ .ComVar │ ├ .
4.2 Remote control commands &SmplData Object Description Input range Reference & Root : ├ SmplData Sample data : ├ .Status Status of silo memory ├ .OFFSilo Current sample data │ ├ .Id1 Sample identification 1 │ ├ .Id2 Sample identification 2 │ ├ .Id3 Sample identification 3 │ ├ .ValSmpl Sample size │ ├ .UnitSmpl Unit of sample size │ ├ .Limits Limits of sample size ├ .ONSiloCurrent sample data │ ├ .Counter Counter of silo memory │ │ ├ .MaxLines Maximum lines │ │ ├ .FirstLine First line │ │ ├ .
4.2 Remote control commands &HotKey Object Description Input range Reference & Root : ├ HotKey : ├ .User │ ├ .Name │ ├ .Delete │ │ ├ .Name │ ├ .DelAll │ ├ .List │ │ ├ .1 │ │ │ ├ .Name │ │ ├ up to 99 Keys with direct access User name Input of user name Delete user Input of user name Delete all users List of users User 1 Name of user 756/831 KF Coulometer, Instructions of Use up to 10 ASCII char $G up to 10 ASCII char $G read only 4.2.2.62.
4.2 Remote control commands &Info Object Description Input range Reference & Root : ├ Info Current data : ├ .Report Transmission of formatted reports │ ├ .Select Report type │ │ │ │ │ │ ├ .Checksums Checksums │ ├ .ActualMethod Checksum of current method │ ├ .DetermData Determination data │ ├ .Write Read/write for several nods │ ├ .TitrResults Titration results │ ├ .RS Calculated results │ │ ├ .1 1st result │ │ │ ├ .Value Value │ │ ├ up to 9 results │ ├ .EP Endpoint │ │ ├ .V Value │ │ ├ .
4.2 Remote control commands │ ├ .ActualInfo │ ├ .Inputs │ │ ├ .Status │ │ ├ .Change │ │ ├ .Clear │ ├ .Outputs │ ├ .Assembly │ │ ├ .CyclNo │ │ ├ .I │ │ ├ .Meas │ │ ├ .Pot │ │ ├ .IPulse │ │ ├ .Bur │ │ │ ├ .V │ │ │ ├ .Clear │ ├ .Titrator │ │ ├ .CyclNo │ │ ├ .Water │ │ ├ .Meas │ │ ├ .dWaterdt │ │ ├ .I │ │ ├ .Pot │ │ ├ .IPulse │ ├ .MeasPt │ │ ├ .Index │ │ ├ .X │ │ ├ .Y │ │ ├ .Z1 │ │ ├ .Z2 │ ├ .EP │ │ ├ .Index │ │ ├ .X │ │ ├ .Y │ ├ .Oven │ │ ├ .HeatTime │ │ ├ .SampleTemp │ │ ├ .LowTemp │ │ ├ .HighTemp │ │ ├ .
4.2 Remote control commands &Assembly Object Description Input range Reference Assembly control Generator electrode Pulses Length of pulses Current of generator electrode $G 0...2000 0, 100, 200, 400 4.2.2.77. ditto ditto Measuring of indicator electrode Status Polarization current of electrode ON, OFF 2, 10, 20, 40 4.2.2.78. ditto I/O outputs Automatic output of EOD Set I/O lines Signal on L0 ON, OFF 4.2.2.79.
4.2 Remote control commands &Setup Object Description Input range Reference & Root : ├ Setup ├ .Comport ├ .Keycode ├ .Tree │ ├ .Short │ ├ .ChangedOnly │ ├ .Trace │ ├ .Lock │ ├ .Keyboard │ ├ .Config │ ├ .Parameter │ ├ .SmplData │ ├ .UserMeth │ │ ├ .Recall │ │ ├ .Store │ │ ├ .Delete │ ├ .Exchange │ └ .Display │ ├ .Mode │ ├ .StartWait │ ├ .FinWait │ ├ .SendMeas │ ├ .SendStatus │ ├ .Interval │ │ ├ .Select │ ├ .Assembly │ │ ├ .CyclNo │ │ ├ .I │ │ ├ .Meas │ │ ├ .Pot │ │ ├ .IPulse │ │ ├ .Bur │ │ │ ├ .V │ ├ .
4.2 Remote control commands ├ .AutoInfo │ ├ .Status │ ├ .P │ ├ .T │ │ ├ .R │ │ ├ .G │ │ ├ .GC │ │ ├ .S │ │ ├ .B │ │ ├ .F │ │ ├ .E │ │ ├ .O │ │ ├ .N │ │ ├ .Re │ │ ├ .Si │ │ ├ .M │ │ ├ .EP │ │ ├ .RC │ ├ .C │ │ ├ .B1 │ │ ├ .R1 │ │ ├ .B2 │ │ ├ .R2 │ ├ .PR (only 756) │ │ ├ .B │ │ ├ .R │ ├ .I │ ├ .O │ ├ .Graphics │ ├ .COM1 │ │ ├ .Grid │ │ ├ .Frame │ │ ├ .Scale │ │ ├ .Recorder │ │ │ ├ .Right │ │ │ ├ .Feed │ ├ .COM2 │ ├ .Int │ ├ .PowerOn ├ .Initialise │ ├ .Select │ ├ .RamInit ├ .InstrNo ├ .
4.2 Remote control commands &Diagnose Object Description Input range Reference Diagnose Output of adjustment parameters $G 4.2.2.101. 0...29 $G 4.2.2.102. 4.2.2.103. 1...4.0...10 2...3.0...9 4.2.2.104. ditto & Root : ├ Diagnose ├ .Report ├ .Simulation │ ├ .Keycode ├ .ScreenDump ├ .IntPrinter │ ├ .HeatTime │ ├ .
4.2 Remote control commands 4.2.2 Description of the remote control commands 4.2.2.1. Mode $G, $S Start and stop ($G, $S) of the current method (4.2.2.3) $G also serves to continue after inquiries of identifications and sample size after the start (see 4.2.2.15) 4.2.2.2. Mode.Select KFC, KFC-B, BLANK, GLP Selection of the standard mode. If a method is selected from the method memory, the node &Mode.Select is overwritten with the mode of the corresponding user method. 4.2.2.3. Mode.
4.2 Remote control commands .ExtrT: Extraction time in s. During this time controlling occurs but the titration will not be stopped. 4.2.2.8. Mode.Parameter.TitrPara.StartDrift 1...20..999 StartDrift in ug/min. Drift for "conditioning ok" and start of titration possible. 4.2.2.9. Mode.Parameter.TitrPara.Ipol 2, 5, 10, 20, 30 Mode.Parameter.TitrPara.PolElectrTest ON, OFF .Ipol: Selection of polarization current.
4.2 Remote control commands .Cond: Conditioning ON/OFF .DCor.Type: Type of drift take-over for the drift correction. auto: Take-over of the drift value at start. .DCor.Value: Drift value for the manual drift correction. 4.2.2.15. Mode.Parameter.Presel.IReq id1, id1&2, all, OFF Mode.Parameter.Presel.SReq value, unit, all, OFF Mode.Parameter.Presel.ReqTitr ON, OFF Automatic inquiries after the start of the determination.
4.2 Remote control commands Mode.Def.Formulas.1.Decimal 0...2...5 Mode.Def.Formulas.1.Unit 6 ASCII characters Mode.Def.Formulas.1.Limits ON, OFF Mode.Def.Formulas.1.LoLim 0...±999 999 Mode.Def.Formulas.1.UpLim 0...±999 999 Mode.Def.Formulas.1.Output active, pulse, OFF Mode.Def.Formulas.2.Formula etc. up to .9 Entry of formulas. Rules for formula entry, see page 34.
4.2 Remote control commands Assignment of the statistics calculations. Valid assignments are a requirement for statistics calculations. In addition, the statistics calculation must be switched on, see 4.2.2.13. Rules for statistics calculations see page 37. 4.2.2.27. Mode.CFmla Mode.CFmla.1.Value 0...±999 999 Mode.CFmla.2.Value etc., up to .19 Calculation constants specific to a method. Stored in the method memory of the Coulometer. Operands specific to the sample (4.2.2.57 and 4.2.2.
4.2 Remote control commands Config.Monitoring.Reagent.ReagCap 1...1000...9999, OFF Config.Monitoring.Reagent.RCounter 0...9999 Config.Monitoring.Reagent.ClearCount $G Config.Monitoring.Reagent.Drift 0...99, OFF Monitoring of reagent live time. .Determ: Number of determinations. .DCounter: Counter of determinations already carried out. .MaxTime: Maximum live time of reagent in days. .TCounter: Time already elapsed since last reagent change. .ReagCap: Reagent capacity in mg water. .
4.2 Remote control commands Config.PeriphUnit.CharSet2 Selection of the character set and the graphics control characters for COM1 resp. COM2 of the Coulometer. IBM means the IBM character set following character set table 437 and IBM graphics control characters. Select 'IBM' for work with the computer. 4.2.2.37. Config.PeriphUnit.RepToComport 1,2,1&2. And at 756: int.,1&int., 2&int.,all. Selection of target for manually triggered reports. int. Internal printer. 1: COM1 2: COM2 4.2.2.38. Config.PeriphUnit.
4.2 Remote control commands Current sample number. Set to 0 on power on and initialization. After 9999, counting starts again at 0. 4.2.2.44. Config.Aux.OpLevel Operator level for manual operation. standard, expert 4.2.2.45. Config.Aux.StartDelay 0...999 999 Start delay time in s. During this time, the data of the preceding determination are retained. 4.2.2.46. Config.Aux.ResDisplay bold, standard Character set for the result display at the end of the determination. 4.2.2.47. Config.Aux.
4.2 Remote control commands 4.2.2.52. Config.Report.Id ON, OFF Config.Report.Instr ON, OFF : Report configuration. If a report line is switched off, the corresponding line will not be outputted in the reports. With "Run" on "OFF", only the run number will not be outputted, date (and time) are available. 4.2.2.53. Config.ComVar.C30 with up to .C39, etc. 0... ±999 999 Values of the common variables from C30 up to C39.
4.2 Remote control commands SmplData.ONSilo.EditLine.1.Mark read only etc., up to .255 Contents of a silo line. .Method: Method used to process the sample, from the method memory or from the card. .Id: The identifications Id1...Id3 can also be used as sample-specific calculation constants C21...C23 in formulas. .UnitSmpl: If "no unit" is desired for the sample size, the blank string must be entered. .C24, .C25: Results which have been assigned to C24 and C25. .
4.2 Remote control commands mplist, param, calc, C-fmla, def, statistics, smpl data, silo, scalc full, scalc srt, config, user method, all, ff $G sends the selected report to the COM which is set in &Config.PeriphUnit.RepToComport: result: Result report of the last completed determination. water crv: Mass of water in ug vs. time rate crv: Rate in ug/min vs. time meas crv: Potential vs. Time comb: Mass of water in ug & rate in ug/min vs. time mplist: Measuring point list of the running determination.
4.2 Remote control commands .EP: Endpoint: Mass coordinate in ug, e.g. "10.3" Potential coordinate in mV e.g. "43.7". .Var: Various variables. You may overwrite the variables C40...C45, see 4.2.2.66. C40: Initial measured value in mV, e.g. "226". C41: Mass of water in ug, e.g. "126.5" C42: Time from start of titration to end in s, e.g. "26". C43: Drift at titration start in ug/min, e.g. "5.1". C44: Titration temperature in °C, e.g. "25.0" C45: Total charge in mA·s, e.g. "1355.5" 4.2.2.67. Info.
4.2 Remote control commands Info.ActualInfo.Outputs.Clear $G Status sends the current status of the I/O lines, Change sends the information regarding whether a change in status of a line has taken place since the last clearing, Clear clears the change information. For the output, there is a conversion from binary to decimal, e.g. | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 1 | 0 | 1 | 0 | Line No.
4.2 Remote control commands Info.ActualInfo.Titrator.Meas read only Info.ActualInfo.Titrator.dWaterdt read only Info.ActualInfo.Titrator.I read only Info.ActualInfo.Titrator.Pot read only Info.ActualInfo.Titrator.IPulse read only $Q sends the current values. .CyclNo: Cycle number of the voltage measurement cycle, e.g. "127". From the cycle number and the cycle time (see 4.2.2.77), a time frame can be set up. The cycle number is set to 0 on switching on the instrument and on every start.
4.2 Remote control commands .GasFlow: Average gas flow during sample heating time. .UnitFlow: Unit of gas flow. 4.2.2.74. Info.ActualInfo.Display.L1 up to 32 ASCII characters Info.ActualInfo.Display.L8 up to 32 ASCII characters Info.ActualInfo.Display.DelAll $G Lines of the display. The display can be written to from the computer. Proceed as follows: 1. Lock the display, see 4.2.2.90. 2. Delete the whole display (.DelAll). 3. For writing onto the display, the standard character set will be used. 4.
4.2 Remote control commands 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 Coulometer several determinations can be performed in the same beaker. Before AutoEOD is switched on, line 3 must be set to "OFF". .SetLines: With $G, all lines are set. .SetLines.LX: Set the line LX.
4.2 Remote control commands 4.2.2.83. Assembly.Bur.Fill $G starts the 'FILL' mode of the connected Dosino. $G, $H, $C 4.2.2.84. Assembly.Bur.ModeDis $G, $S, $H, $C Assembly.Bur.ModeDis.Selected volume, time Assembly.Bur.ModeDis.V 0.0001...0.1...9999 Assembly.Bur.ModeDis.Time 0.25...1...86400 Assembly.Bur.ModeDis.VStop 0.0001...9999, OFF Assembly.Bur.ModeDis.AutoFill ON, OFF Dispensing mode for the connected Dosino. The dispensing mode can only be started and stopped via the RS Control.
4.2 Remote control commands 4.2.2.89. 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.Exchange ON, OFF Setup.Lock.Display ON, OFF ON means disable the corresponding function: .Keyboard: Disable all keys of the Coulometer .Config: Disable the key .Parameter: Disable the key .SmplData: Disable the key .
4.2 Remote control commands 4.2.2.93. Setup.SendMeas.Assembly.CyclNo ON, OFF Setup.SendMeas.Assembly.I ON, OFF Setup.SendMeas.Assembly.Meas ON, OFF Setup.SendMeas.Assembly.Pot ON, OFF Setup.SendMeas.Assembly.IPulse ON, OFF Setup.SendMeas.Assembly.Bur.V ON, OFF Selection of the values from Assembly for the output in the set time interval (see 4.2.2.92): .CyclNo: Cycle number of the potential measurement. Together with the cycle time (4.2.2.77), a time frame can be set up.
4.2 Remote control commands 4.2.2.95. Setup.AutoInfo.Status ON, OFF Setup.AutoInfo.P ON, OFF Setup.AutoInfo.T.R ON, OFF Setup.AutoInfo.T.G ON, OFF Setup.AutoInfo.T.GC ON, OFF Setup.AutoInfo.T.S ON, OFF Setup.AutoInfo.T.B ON, OFF Setup.AutoInfo.T.F ON, OFF Setup.AutoInfo.T.E ON, OFF Setup.AutoInfo.T.O ON, OFF Setup.AutoInfo.T.N ON, OFF Setup.AutoInfo.T.Re ON, OFF Setup.AutoInfo.T.Si ON, OFF Setup.AutoInfo.T.M ON, OFF Setup.AutoInfo.T.EP ON, OFF Setup.AutoInfo.T.RC ON, OFF Setup.AutoInfo.C.B1 ON, OFF Setup.
4.2 Remote control commands .PR.B A report is outputted on the internal printer. During this time, COM1 and COM2 are blocked. .PR.R The COM's are ready again. (Comes also when you an error.) Messages for changes in the I/O lines. If the changes are made simultaneously, there is 1 message. Pulses receive 2 messages: one message each for line active and inactive. .I Input: Change of an input line. .O Output: Change of an output line (except 7, pin 2, for recorder pulses).
4.2 Remote control commands 4.2.2.98. Setup.Initialise Setup.Initialise.Select $G ActMeth, Config, Silo, Assembly, Setup, All Setting of default values for the following areas: ActMeth: Current method. Parameters, calculations, and assignments for the data output, operands C01...C19. Config: All values under &Config. Silo: The silo memory is deleted. Same function as delete entire silo. Assembly: All values under &Assembly. Setup: All values under &Setup.
4.2 Remote control commands 4.2.2.103. Diagnose.ScreenDump $G The content of the 756 Screen will be dumped to the COM which is given for manual reports (key , >peripheral units). A screen dump onto the internal printer is not possible. 4.2.2.104. Diagnose.IntPrinter.HeatTime 1...4.0...10 Diagnose.IntPrinter.MotorSpeed 2...3.0...9 Settings for the internal printer. .HeatTime: Heating time for the dots in ms. Input in steps of 0.5 ms. Longer heating times give darker printouts. .
4.3 Properties of the RS 232 Interface 4.3 Properties of the RS 232 Interface Data Transfer Protocol The Coulometer 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 21. • 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.
4.3 Properties of the RS 232 Interface Coulometer as Sender : Coulometer external device XOFF XON Data output RxD LF Data input TxD max. characters Data output disabled Data output enabled Time max. characters: 2 characters at 300...9600 baud 16 characters at ≥ 19200 baud Software-Handshake, SWline Handshake input ports on the Coulometer (CTS) are not checked. Handshake output ports (DTR, RTS) are set by the Coulometer. The Coulometer has an input buffer which can accept up to 512 characters.
4.3 Properties of the RS 232 Interface Coulometer as Sender: Coulometer external device XOFF XON Data output RxD 1st line LF 2nd line LF Data input TxD Data output disabled Data output enabled Time Coulometer transmission can be stopped by external instruments with XOFF. After XOFF is received the Coulometer completes sending the line already started. If data output is disabled for more than 6 s by XOFF, E43 appears in the display.
4.3 Properties of the RS 232 Interface 4.3.2 Pin Assignment RS232C Interface Pin 3 Transmitted Data (TxD). If no data are transmitted, the line is held in the “ON” condition. Data will only be sent when CTS is in the ”ON” condition. Transmitted Data Pin 2 Received Data (RxD) Received Data Request to Send (RTS) ON condition: Coulometer is ready to send data. Pin 7 Clear to Send (CTS) ON condition: Remote station is ready to receive data.
4.3 Properties of the RS 232 Interface Contact arrangement at plug (female) for RS 232C socket (male) 6 9 1 5 View of soldered side of plug Ordering numbers: K.210.0381 and K.210.9045 No liability whatsoever will be accepted for damage or injury caused by improper interconnection of instruments.
4.
5.1 Troubleshooting 5 Error messages, troubleshooting 5.1 Troubleshooting The determination of the free water is easily done as far as the specifications of the reagent manufacturer regarding the "water capacity" of the reagents are concerned. Problems may occur with specific sample matrices. The relevant literature contains many precise analysis instructions. In the following table we attempt to show you solutions concerned more with the instrument.
5.1 Troubleshooting Problem Possible causes and remedies Result too low • Drift correction too large, i.e. the drift was too high at the start or unstable drift. • Stop drift too high. • Min.rate too low • Sample releases iodine. Results widely scattered • Inhomogeneous sample? Poor reproducibility of sample addition? • Drift unstable. Titration times too long • Wait until drift during conditioning becomes stable. • Amount of water too large, see sample size guidelines on page 10.
5.2 Error and special messages 5.2 Error and special messages blinking value The value entered lies outside the permitted range of entries. Error messages appear in the display as soon as the error has been recognized. XXX bytes missing For the storage of a method or a silo line XXX bytes are missing. Remedy: . Delete methods no longer needed or use fewer silo lines. changing reagent The reagent monitoring has responded. Exit: or . The reagent monitoring counters are reset to zero.
5.2 Error and special messages division by zero The result could not be calculated as a divisor in the formula was equal to zero. Exit: Enter appropriate value. initializing Dosino When the Coulometer is switched on the connected Dosino is initialized. instr.temp.too high The temperature in the Coulometer is too high (≥ 60 °C). Exit: Wait until temperature is <60 °C. The determination has been manually stopped. Maximum 500 measured points can be stored. Exit: Select larger time interval.
5.2 Error and special messages silo empty silo full stop time reached system error 3 system error 14 pear each time the Coulometer is switched on. Exit: New start. The silo memory is switched on but is empty and a titration has been started. Corrective action: Fill at least the first 1 silo line before starting the first titration. Exit: . The silo memory is full (255 lines). Exit: . The titration has been stopped as the max.titration time has been reached.
5.2 Error and special messages - Reagent exhausted ⇒ exchange. - Conductivity of the reagent is too low: work with a generator electrode with diaphragm and automatic current switching (, >preselections generator I), see also page 33. - Generator electrode or its cable faulty Exit: Rectify the fault. Error messages in connection with the data transfer Receive errors: error 36 Parity Exit: and set corresponding quantity the same on both instruments error 37 Framing error.
5.3 Problem with an external printer 5.3 Problem with an external printer 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 .
5.4 Initialize KF Coulometer 5.4 Initialize KF Coulometer In rare cases the RAM of the Coulometer may need to be initialized. This causes the deletion of all methods, silo data and results. Whenever possible you should first make a method backup with the aid of a PC and the 6.6008.200 or 6.6008.500 Vesuv 3 Software and print out your configuration data (). Initialize RAM 1. Switch off Coulometer 2. Switch on Coulometer and press key <9> at the same time.
5.5 Testing the measuring input 5.5 Testing the measuring input With the aid of the "767.0010 Calibrated Reference for mV, pH, Ω, uS, °C" you can check the measuring input "Ipol" and the indicator electrode cable. If a Remote Box is connected: Deactivate the Remote Box (key , >peripheral units, Remote Box: off). Switch the Coulometer off and screw off the Remote Box. Switch the Coulometer on again (so that the new configuration will be recognized). Procedure: 1. Switch off Coulometer. 2.
6.1 Coulometer setup 6 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.
6.1 Coulometer setup 6.1.2 Insert paper into built-in thermal printer (only at 756) Insert the paper with the Coulometer switched on. 1. Remove old paper strips with the key . If the key does not trigger a paper feed, make the following setting: , >peripheral units man.reports to COM:int. 2. Open cover, take out the spindle and remove the cardboard part of the old paper roll. 3. Cut a straight edge on the new paper roll.
6.1 Coulometer setup 6.1.3 Titration vessel setup with Ti Stand Drying tube Generator electrode Indicator electrode Feed/aspiration tube Inlet Outlet Septum stopper 1. Attach titration vessel with holder to the support rod. 2. Place stirring bar in titration vessel. 3. Cut 6.2713.XXX ground joint sleeves to the correct length and use for all the joints of the inserts1). 4. Insert indicator electrode in the left-hand joint opening, screw on 6.2104.020 electrode cable and plug it into the "Ind.
6.2 Connecting Coulometer to Dosino 6.2 Connecting Coulometer to Dosino Automatic reagent exchange is possible with the Dosino. The inquiry reagent change under , >monitoring must be set to auto or "man.". The key is then used to carry out a reagent exchange. With reagent change auto the reagent change is carried out automatically as soon as the reagent monitoring has responded. 700 The 2.700.0020 Dosino can be connected directly. If you want to connect a 2.700.
6.2 Connecting Coulometer to Dosino 3. Screw 6.1602.105 bottle attachment onto the waste bottle, fill adsorber tube with molecular sieve and place it in the bottle attachment. Close the larger threaded opening of the bottle attachment with 6.1446.080 stopper. 4. Place the waste bottle in the bottle holder. Connect the bottle attachment and Port 3 of the dosing unit with 6.1805.080 tubing. 5. Equip the titration vessel with the aspiration equipment, see below. The aspiration equipment consists of 6.1543.
6.3 Connecting the 768 KF Oven 6.3 Connecting the 768 KF Oven It is expedient to place the oven on 6.2041.180 instrument bridge. Take care that the gas outlet of the oven enters the titration vessel as directly as is possible to prevent the formation of condensed water in the outlet tubing. Instrument setup: Oven on 6.2041.180 instrument bridge Connecting the instruments: 768 6.2141.010 cable 6.2125.110 cable Connection of both RS interfaces (cable 6.2125.
6.3 Connecting the 768 KF Oven 6.3.1 Equipping the titration vessel with an oven The titration vessel is equipped in a similar way to that for aspiration with a Dosino, see page 116. The gas outlet of the oven is connected to the tip. Take care that connection between the oven outlet and the titration vessel is short, as otherwise condensed water may form in the tubing! If you use the 6.1830.000 heatable outlet tubing then you require 6.1446.170 stopper for the inlet tip.
6.4 Connecting the 774 Oven Sample Processor 6.4 Connecting the 774 Oven Sample Processor The Oven Sample Processor heats the sample and transfers the moisture from the sample to the titration vessel of the Coulometer. Coulometer and Oven Sample Processor are connected via the remote sockets (cable 6.2141.020) as well as via the RS interfaces (cable 6.2125.110): 774 774 6.2141.020 cable 6.2125.
6.4 Connecting the 774 Oven Sample Processor 6.4.1 Equipping the titration vessel with the Oven Sample Processor Lead the tip of 6.1830.010 heatable outlet tube into the titration vessel with the aid of 6.1446.170 stopper. Transfer hose with outlet heating 6.1830.010 Connection for outlet heating Outlet heater Generator electrode with drying Indicator electrode Stopper with 6.1446.170 O-ring Septum stopper 6.1464.
6.5 Connecting an external printer 6.5 Connecting an external printer A variety of printers can be connected to the RS232 interface of the Coulometer. 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. If a balance is connected at the same COM of the Coulometer as a printer, you need the 6.2125.010 + 6.2125.030 Adapters.
6.6 Connecting a balance 6.6 Connecting a balance The following balances can be connected to the RS232 output of the Coulometer: Balance Cable Sartorius MP8, MC1 6.2134.060 Mettler AB, AG (LC-RS25) in the scope of delivery of the balance Mettler AM, PM 6.2146.020 + 6.2125.
6.7 Connecting a PC 6.7 Connecting a PC Cable: Coulometer-PC, 9/9-pole................................................................................. 6.2134.040 Coulometer-PC, 9/25-pole............................................................................... 6.2125.110 Settings at the Coulometer: RS settings: .................................................................................... according to program , >peripheral units, send to: ................................................
6.8 Connecting a Remote Box 6.8 Connecting a Remote Box A barcode reader and/or a PC keyboard can be connected to 6.2148.000 Remote Box. The barcode reader and PC keyboard are used as input aids. Only plug in and unplug the Remote Box when the Coulometer is switched off! The Remote Box is screwed onto the "Remote" socket of the Coulometer. The remote lines of the Coulometer are then accessible at the "Remote" socket of the Remote Box. 6.8.
6.8 Connecting a Remote Box 6.8.2 Connecting a PC keyboard PC keyboards with a 5-pole DIN plug can be connected to 6.2148.000 Remote Box. For keyboards with a PS/2 plug an adapter PS/2→DIN is available in PC shops. Settings at the Coulometer: Under key , >peripheral units, "Remote Box: on" Keyboard: Select the country-specific keyboard layout of your PC keyboard.
6.8 Connecting a Remote Box The numerical block (with NumLock) and the number keys on the PC keyboard simulate the functions of the numerical keys on the Coulometer. For example, entering <7> in the basic state of the Coulometer switches the statistics on. Keys which are used for setting an accent (e.g. ^, ´) are converted immediately. If you try to enter ê the Coulometer will display ^e instead. The occupancy of the PC function keys (F1 till F12) is shown to the right as an overlay.
7.1 Technical specifications 7 Appendix 7.1 Technical specifications Modes KFC: Coulometric KF titration KFC-B: Coulometric KF titration with blank deduction BLANK: Blank determination GLP: Validation of the Coulometer Endpoint indication Voltametric, AC indication Ipol: 2, 5, 10, 20 or 30 uA adjustable Iodine production Pulse with variable current strength and length Current at the generator electrode: 100, 200, 400 mA Titration speed max. 2.
7.1 Technical specifications Remote Input/Outputlines Connection for Oven, Oven Sample Processor, robot. With optional Remote Box: Connection for barcode reader and PC keyboard Dosino connection For automatic reagent exchange Ambient temperature Nom. operation range Storage Transport 5 ... 40 °C – 20 ... 60 °C – 40 ... 60 °C Safety specifications Mains connection Voltage Frequency Power consumption Fuse Designed and tested in accordance to IEC publication 1010, safety class I.
7.2 Pin assignment of the "Remote" socket 7.2 Pin assignment of the "Remote" socket external Inputs Function +5 V pin 21 (Input 0) Start pin 9 (Input 1) Stop +5 V +5 V tp pin 22 (Input 2) Enter tp > 100 ms Functions see page 130. +5 V pin 10 (Input 3) +5 V Not used pin 23 (Input 4) +5 V pin 11 (Input 5) +5 V pin 24 (Input 6) Not used +5 V pin 12 (Input 7) Outputs pin 5 (Output 0) Ready inactive pin 18 (Output 1) Conditioning ok, active if Cond.
7.2 Pin assignment of the "Remote" socket Outputs pin 17 (Output 3) End of determination EOD pin 3 (Output 4) not used pin 16 (Output 5) Error, active on errors pin 1 (Output 6) Activate pulse, see also page 132.
756/831 KF Coulometer, Instructions of Use 21 9 Stop 1 22 Enter 2 Inputs 1: The error line is reset if the error is rectified. 2: Activate pulse according to setting, see page 132. 3: Line is active if a remote box is connected, see page 20. 4: Line is active if sample size is out of limits, see page 29. 5: Line is active if result is out of limits, see page 35. end of det. (EOD) Data output start titration request id,.. START cond.ok cond.
7.2 Pin assignment of the "Remote" socket 7.2.2 Activate pulse An activate pulse may be set in key , >preselections, "activate pulse:". These settings will be carried out as follows: first cond. all inactive START Conditioning START Request id... Start titration end of det.
7.3 Coulometer validation, GLP mode 7.3 Coulometer validation, GLP mode Checking and maintenance of the Coulometer is carried out in 3 steps: 1. Testing the electronic components when the Coulometer is switched on. 2. Wet-chemistry validation of the whole coulometric analysis setup 3. Maintenance and adjustment of the Coulometer by Metrohm service. 7.3.1 Electronic tests When the Coulometer is switched on electronic tests are carried out. During this period system tests appears in the display.
7.3 Coulometer validation, GLP mode 7.3.2 Wet tests GLP (Good Laboratory Practice) requires the periodic validation of the analytical instruments. The reproducibility and accuracy of the instruments are checked. An annual repetition of the procedure appears to be sensible. Depending on the requirements a more frequent check may be indicated, e.g. every 3 or 6 months. Guidelines for the testing regulations (SOP, Standard Operating Procedure) are given in Metrohm Application Bulletin No.
7.4 User methods 7.4 User methods The methods can be modified and overwritten. The following methods are available: 'um 756 KF Coulometer 5.756.0010 date 1998-11-02 time 14:27 user methods bytes BLANK Oven-Blk 164 KFC-B Oven-Det 184 BLANK 774-Blk 168 KFC-B 774-Det 188 remaining bytes 39266 If you want to have the results in units other than ppm, you must alter the operands and possibly also the formula, see page 36.
7.4 User methods 7.4.1 Working with the KF Oven When working with the KF oven an extraction period is required in order to prevent the titration being switched off prematurely. The RS interface of the 768 KF oven is connected to COM1 of the Coulometer (cable 6.2125.110). If you do not make this connection or you work with the 832 Thermoprep, the parameter oven under preselections must be set to off (no oven data in the Coulometer report). Determination method, parameters: 'pa 756 KF Coulometer 5.756.
7.4 User methods Blank value method, parameters: 'pa 756 KF Coulometer 5.756.0010 date 1997-11-19 time 17:51 0 BLANK Oven-Blk parameters >control parameters EP at U 50 mV dynamics 70 mV max.rate max. ug/min min.rate 15 ug/min stop crit: rel.drift rel.drift 5 ug/min >titration parameters pause 0 s extr.time 300 s start drift 20 ug/min I(pol): 10 uA electrode test: ON temperature 25.0 °C time interval 2 s max.titr.time OFF s >statistics status: ON mean n= 3 res.
7.4 User methods 7.4.2 Working with the 774 Oven Sample Processor When working with the 774 Oven Sample Processor an extraction period is required in order to prevent the titration being switched off prematurely. The RS interface of the Oven Sample Processor is connected to COM1 of the Coulometer (cable 6.2125.110). If you do not make this connection then the parameter oven under preselections must be set to off (no oven data in the Coulometer report).
7.4 User methods Blank value method, parameters: 'pa 756 KF Coulometer 5.756.0010 date 1997-11-19 time 17:56 0 BLANK 774-Blk parameters >control parameters EP at U 50 mV dynamics 70 mV max.rate max. ug/min min.rate 15 ug/min stop crit: rel.drift rel.drift 5 ug/min >titration parameters pause 0 s extr.time 180 s start drift 10 ug/min I(pol): 10 uA electrode test: ON temperature 25.0 °C time interval 2 s max.titr.time OFF s >statistics status: ON mean n= 3 res.
7.5 Warranty and certificates 7.5 Warranty and certificates 7.5.1 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.
7.5 Warranty and certificates 7.5.2 Certificate of Conformity and System Validation: 756 KF Coulometer 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: 756 KF Coulometer System software: Stored in ROMs Name of manufacturer: Metrohm Ltd.
7.5 Warranty and certificates 7.5.3 EU Declaration of Conformity: 756 KF Coulometer EU Declaration of Conformity The company Metrohm AG, Herisau, Switzerland, certifies herewith, that the following instrument: 756 KF Coulometer meets the CE mark requirements of EU Directives 89/336/EEC and 73/23/EEC.
7.5 Warranty and certificates 7.5.4 Certificate of Conformity and System Validation: 831 KF Coulometer 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: 831 KF Coulometer System software: Stored in ROMs Name of manufacturer: Metrohm Ltd.
7.5 Warranty and certificates 7.5.5 EU Declaration of Conformity: 831 KF Coulometer EU Declaration of Conformity The company Metrohm AG, Herisau, Switzerland, certifies herewith, that the following instrument: 831 KF Coulometer meets the CE mark requirements of EU Directives 89/336/EEC and 73/23/EEC.
7.6 Scope of delivery and ordering designations 7.6 Scope of delivery and ordering designations 756 KF Coulometer, generator electrode without diaphragm...................2.756.0110 including the following accessories 1 Indicator electrode, double Pt ........................................................................... 6.0341.100 1 Generator electrode without diaphragm ........................................................... 6.0345.100 1 Drying tube ................................................
7.6 Scope of delivery and ordering designations 756 KF Coulometer, generator electrode with diaphragm ........................2.756.0010 including the following accessories 1 Magnetic stirrer ................................................................................................. 1.728.0010 1 Indicator electrode, double Pt ........................................................................... 6.0341.100 1 Generator electrode with diaphragm ......................................................
7.6 Scope of delivery and ordering designations 831 KF Coulometer, generator electrode without diaphragm...................2.831.0110 including the following accessories 1 Indicator electrode, double Pt ........................................................................... 6.0341.100 1 Generator electrode without diaphragm ........................................................... 6.0345.100 1 Drying tube .................................................................................................
7.6 Scope of delivery and ordering designations 831 KF Coulometer, generator electrode with diaphragm ........................2.831.0010 including the following accessories 1 Magnetic stirrer ................................................................................................. 1.728.0010 1 Indicator electrode, double Pt ........................................................................... 6.0341.100 1 Generator electrode with diaphragm ......................................................
7.6 Scope of delivery and ordering designations Options Accessories to separate order and on payment of extra charge: Stirrers, Ti Stands 728 Magnetic Stirrer ............................................................................................. 2.728.0010 Stirring bars, length 12 mm........................................................................................................... 6.1903.010 16 mm.................................................................................................
7.6 Scope of delivery and ordering designations Oven Sample Processor 774 Oven Sample Processor ............................................................................... 2.774.0010 Stopper for gas inlet............................................................................................6.1446.170 Control cable Oven Sample Processor – Coulometer ........................................6.2141.020 Data cable Oven Sample Processor – Coulometer ............................................6.2125.
Index Index Keys are marked with < >, display texts are in bold characters, and pages concerning the green part are printed in italic. Page number + ff means this and following pages. A .....................................................16 Accessories .............................................145 activate pulse: ........................................30 Addition of sample ....................................10 aspirate volume ........................................
Index Deleting - common variables............................. 39 - formulas............................................. 34 - methods............................................. 44 - silo lines ............................................. 48 - statistics results ................................. 37 - text ..................................................... 16 determ.counter ......................................... 18 dev.label .................................................. 21 dialog: .............
Index L Language of dialog ...................................20 LED ..............................................................2 Limits - result ..................................................35 - sample size........................................29 limit smpl size: ......................................29 lock ............................................................23 low lim. ..............................................29, 35 M Ordering numbers...................................
Index remote box: ............................................... 20 Remote control - via "Remote"..................................... 129 - via RS232........................................... 53 Remote control commands - detailed description........................... 74 - overview............................................. 60 Remote lines ........................................... 129 Report - printing......................................... 40, 42 - reproduction ....................................
Index Termination criterion..................................28 text idX ....................................................29 Text input ...................................................16 Thermal printer ........................................ 113 time counter .......................................18, 19 time interval .....................................19, 28 time ............................................................20 time-out PC keyboard.............................
