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2.8 Optimal working conditions

756/831 KF Coulometer, Instructions for Use

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.

If the 768 KF oven is used it is recommended that the oven is al-

lowed to run overnight with the oven valve set to "purge".

For precise determination of amounts of water below 100 µg it may

also be an advantage to condition the instrument overnight before

use.

If the instrument is switched off for a longer period of time with a

filled titration vessel then a certain time is required for it to become

dry again after it is switched on.

During continuous operation the instrument should not be switched

off overnight.

2.8.1 Drift

A constant drift of the order of about

≤

4 µg/min is good. However,

lower values are certainly possible. If higher, stable values occur

then the results are normally still good as the drift can be compen-

sated (drift correction see page 29).

The drift is shown together with the "drift trend":

⇔

constant drift and drift below the start drift, see page 32.

↑

drift

increasing

↓

drift

falling

A drift which remains high may be caused by water-containing de-

pots in inaccessible locations inside the cell. In such cases a reduc-

tion in the value would be achieved by shaking the titration vessel.

Take care that no drops above the level of the liquid are formed in

the titration vessel.

For generator electrodes with diaphragms shaking must not be so

vigorous as to cause the catholyte and anolyte to become mixed

with each other.

If even after shaking the drift remains too high over longer periods of

time then the electrolyte solution must be exchanged.

When working with the oven a drift

≤

10 µg/min is good. The drift de-

pends on the gas flow (the smaller the gas flow the lower the drift).

Summary of Contents for 756 KF

Page 1: ...756 831 KF Coulometer Manual 8 831 1003 ...

Page 2: ......

Page 3: ...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 2003 chs ...

Page 4: ......

Page 5: ... 7 Optimal working conditions 11 2 7 1 Drift 12 2 7 2 Reagent exchange 13 2 7 3 Indicator electrode 13 3 Manual operation 14 3 1 Keypad 14 3 2 Principle of data input 15 3 3 Text input 16 3 4 Configuration key CONFIG 17 3 4 1 Reagent exchange procedure with Dosino 25 3 5 Mode selection key MODE 26 3 6 Parameters key PARAM 27 3 6 1 Titration sequence 31 3 6 2 Control parameters and Ipol 32 3 6 3 Dr...

Page 6: ...rror and special messages 105 5 3 Problem with an external printer 159 5 4 Initialize KF Coulometer 110 5 5 Testing the measuring input 111 6 Preparations 112 6 1 Coulometer setup 112 6 1 1 Connecting a Stirrer or Ti Stand 112 6 1 2 Insert paper into built in thermal printer 113 6 1 3 Titration vessel setup with Ti Stand 114 6 2 Connecting Coulometer to Dosino 115 6 2 1 Setup with aspiration equip...

Page 7: ... 7 4 2 Working with the 774 Oven Sample Processor 138 7 5 Warranty and certificates 140 7 5 1 Warranty 140 7 5 2 Certificate of Conformity and System Validation 756 KF Coulometer 141 7 5 3 EU Declaration of Conformity 756 KF Coulometer 142 7 5 4 Certificate of Conformity and System Validation 831 KF Coulometer 143 7 5 5 EU Declaration of Conformity 756 KF Coulometer 144 7 6 Scope of delivery and o...

Page 8: ...Contents 756 831 KF Coulometer Instructions for Use IV ...

Page 9: ...porated in a single document The report examples mapped in this document were generated by a 756 KF Coulometer They are identical for a 831 KF Coulometer except from the instrument number Functions which only apply on the 756 KF Coulometer are marked accordingly You can find a short summary of the Instructions for Use in the en closed 756 831 KF Coulometer Quick References You can request descript...

Page 10: ...F Key Switches stirrer ON OFF Key PAPER Only at 756 KF Coulometer Paper feed on printer where manually triggered reports are printed out Key STOP Stops procedures e g titration conditioning Key START Starts procedures e g titration conditioning Keys STOP and START are identical with the corre sponding keys of the separate keypad Indicator lampes COND Lamp flashes when conditioning is performed and...

Page 11: ...n of generator electro de 11 Connection for stirrer 728 Magnetic Stirrer or 703 Ti Stand Supply voltage 10 VDC I 200 mA 7 Remote lines input output for the connection of remote box Oven Sample Changer robots etc 12 Connection for power cable With power supplies where the volt age is subject to severe HF distur bances the Coulometer should be operated via an additional power fil ter e g Metrohm 615...

Page 12: ...he reagents Despite the progress made the classical volumetric Karl Fischer method suffers from the disadvantage that the reagents are not completely stable resulting in the need to redetermine the titer at intervals In the coulometric Karl Fischer titration the iodine needed is generated directly in the electrolyte by electrochemical means electronic buret The rigorously quantitative relationship...

Page 13: ...ground joint sleeves to the cor rect 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 El socket of the Coulom eter Mark the screw head of the electrode cable so that it is impossible to confuse the indicator and generator electrodes 5 Insert generator electrode in the cen...

Page 14: ...falling rising stable When the titration vessel is dry an acoustic signal is heard and the COND LED shows a steady light Press START and inject the first sample Enter the sample size and confirm it with ENTER During the titration you will see the curve µg H2O against time To the left of the curve the following measurements are displayed H2O in µg Rate in µg min Time in s After the titration the re...

Page 15: ...ents which are specially intended for use with generator electrodes without diaphragm see the reagent manufac turer s documentation 2 4 2 Cleaning The electrolyte solution can normally be exchanged without any spe cial cleaning of the parts being necessary If cleaning is necessary then care should be taken that the Pt grid of the generator electrode is not damaged Pollutants containing oil Clean w...

Page 16: ...sed for water determination in ketones and aldehydes please refer to the reagent manufacturer s instruc tions 2 5 2 Cleaning The electrolyte solution can normally be exchanged without any spe cial cleaning of the parts being necessary If cleaning is necessary then care should be taken that the Pt grid of the generator electrode is not damaged Resinous deposits on the diaphragm Hang the generator e...

Page 17: ...l the piston of the syringe up to the end and shake the syringe for a few seconds so that the inner part of the sy ringe is rinsed with standard and gets rid of water contamination 6 Splash the used standard into a waste bottle 7 Repeat the same procedure with another ml of the standard solution 8 Suck the whole rest of the standard into your syringe Thereafter verify that there is no more solutio...

Page 18: ...he titration time kept short However take care that the sample contains at least 50 µg H2O The following table provides guidelines for the sample weight Content of sample Sample weight H2O to be determined 100000 ppm 10 10000 ppm 1 1000 ppm 0 1 100 ppm 0 01 10 ppm 0 001 50 mg 10 mg 100 mg 100 mg 1 g 1 g 5 g 5000 µg 100 µg 1000 µg 100 µg 1000 µg 100 µg 50 µg 2 7 2 Liquid samples Liquid samples are ...

Page 19: ...ied With samples containing only a trace of water the syringe must be thoroughly dried beforehand If possible the syringe should be rinsed with the sample solution by taking up the sample solution several times and then discarding it 2 7 3 Solid samples Whenever possible solid samples should be extracted or dissolved in a suitable solvent and the resulting solution injected a blank value correctio...

Page 20: ...ument should not be switched off overnight 2 8 1 Drift A constant drift of the order of about 4 µg min is good However lower values are certainly possible If higher stable values occur then the results are normally still good as the drift can be compen sated drift correction see page 29 The drift is shown together with the drift trend constant drift and drift below the start drift see page 32 drif...

Page 21: ... 703 can be used to aspirate the electro lyte solutions see pages 114ff For the generator electrode with diaphragm the catholyte should be exchanged approx once a week Extended use may cause darken ing of the catholyte and yellow participation in the cathode com partment An unpleasant smell indicates the need for catholyte ex change also 2 8 3 Indicator electrode A new indicator electrode may requ...

Page 22: ...ected Dosino see page 25 C FMLA Calculation values see page 35 DEF Formulas data output see page 34ff USER METH Management of method memory see page 44 PRINT Printing of reports see page 42 REPORTS Result output at the end of titration see page 40 MODE Mode selection see page 26 Selection of special values dialog marked with switching result curve display Cursor key for navigation CLEAR Clears val...

Page 23: ...o this group pressing ENTER Move the cursor to preselections and press ENTER The first two lines indicate again where you are Then you find the inquiries If a dialog text of an inquiry is marked with you can select a value with keys and for ward backward A value is stored with ENTER and the cursor moves to the next inquiry With key QUIT you move one level up in our ex ample you go back to preselec...

Page 24: ...can correct typing errors with CLEAR CLEAR deletes the characters one by one If you wish to modify an existing name e g if you have names like Text 1 Text 2 Text 3 do not delete the existing name before you start the text input mode Proceed as follows 1 Press USER METH place the cursor to store method and press ENTER 2 Open the text writing mode directly Press key ABC 3 CLEAR now deletes the chara...

Page 25: ...ing dialog lan guage date time Settings for RS COM1 and 2 only in expert mode RS parameters for the interfaces Report only in expert mode Configuration of the report Common Variable only in expert mode Values of the common variables The display texts of the Coulometer are shown to the left The values are the default values monitoring reagent OFF Monitoring functions Monitoring the reagent ON OFF M...

Page 26: ... the generator electrode without diaphragm and a filling volume of 100 ml the capacity is 1000 mg water For the generator electrode with diaphragm the capacity of the katholyte is 300 mg with 5 ml filling volume OFF means that monitoring is not active Counting the capacity 0 9999 mg Adds the weight of water since the last time the counters were reset to zero Monitoring of drift 0 99 ug min OFF If ...

Page 27: ...n be carried out in the GLP mode see page 133 Time counter 0 9999 d Counts the number of days since the last time the counter was reset Monitoring the service interval ON OFF Monitoring is carried out after the Coulometer has been switched on If the monitoring responds the message Service is due appears The message vanishes with CLEAR If on has been set Date of next service YYYY MM DD System test ...

Page 28: ...ically For stirrer control the red switch on the stirrer unit must be ON Connection of a remote box on OFF To the remote socket for PC keyboard and barcode reader see page 124 If on has been set Type of PC keyboard US German French Spanish Swiss The PC keyboard is used as an input aid see page 125 Target for barcode reader input method id1 id2 id3 smpl size The barcode reader is used as an input a...

Page 29: ...ime with QUIT Type of result display at the end of the determination bold standard bold the calculated results are displayed in bold characters standard displays the whole information e g results water messages etc Individual identification of devices up to 8 ASCII characters Is automatically printed in reports Number of beeps 1 3 OFF when instrument is ready conditioning OK end of titration and C...

Page 30: ... instrument Id and program version Prints the line s date time ON OFF If you use Vesuv 3 then date time is switched on automatically Prints the sample number ON OFF The date line is printed without the sample number Prints the line Method ON OFF e g KFC Prints the line Smpl size ON OFF Prints the line Drift ON OFF Prints the line Titr time ON OFF Prints the line H2O ON OFF Continuously prints the ...

Page 31: ...ARAM and SMPL DATA EXCH 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 lock configuration OFF parameters OFF smpl data OFF exchange OFF recall method OFF store method OFF delete method OFF Lock ON means that the corresponding function is no longer accessible The corresponding key is locked The...

Page 32: ...re initialized according to the printer Grid drawing ON OFF Frame drawing ON OFF 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 2 1 00 1 is greatest width If you set 1 you may loose the label at the right margin Length 0 01 1 00 of time axis Curve ...

Page 33: ...olume slightly larger than that which is actually to be aspirated should be en tered if you want to empty the titration vessel completely Rinsing the titration vessel The rinsing volume is added the stirrer switched on for 10 s and then the rinsing vol ume 3 ml is aspirated off again This process is re peated for each rinsing cycle Normally rinsing is not necessary The reagent volume is added and ...

Page 34: ...ntent H2O C01 C00 C02 1 ppm C01 1 C02 1 KFC B blank C39 1 ug content H2O C39 C01 C00 C02 1 ppm C01 1 C02 1 C39 blank BLANK blank H2O 1 ug C39 MN1 GLP content H2O C01 C00 3 mg g recovery RS1 C22 2 C01 1000 C22 Id2 contents information of reagent manufacturer Limit value check for RS2 on 1 Lower limit 0 97 Upper limit 1 03 Inquiry of id1 and id2 text id1 charge id2 mg g H2O 1 The default limits for ...

Page 35: ...or EP Titration parameters Influence the course of the titration Statistics Mean values and standard deviations of the calculated results see page 37 Preselections Selection of various auxiliaries Automatic inquiries after the start etc control parameters EP at U 50 mV dynamics 70 mV titr max rate max ug min titr min rate 15 ug min titr Control parameters Endpoint 0 2000 mV The standard value shou...

Page 36: ...ime 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 QUIT Start Drift 1 999 ug min Drift value below which the start of the titration is pos sible conditioning OK see page 32 Polarization current 2 5 10 20 30 uA at the indicator electrode The set standa...

Page 37: ...w If an inquiry is OFF Titrate during the requests OFF ON With on the titration starts during the requests after 6 s The calculation of the result and the output of data only take place when the inquiries have been exited Method specific unit of sample size g mg ug ml ul pc 5 ASCII At the start of the method the sample size unit is over written by the method specific unit which has been preset Lim...

Page 38: ...urrent will be controlled at smaller values Connected oven COM1 COM2 no COM of the Coulometer to which the oven is con nected If an oven is connected via RS232 an inquiry will be made for the oven results and these will be inserted into the result report of the Coulometer The report out put on the oven must be switched OFF Set no if no oven has been connected or if you have not connected the oven ...

Page 39: ... START The sample identifications and the sample size are re quested Without any of these requests the display shows for 6s add sample This waiting time of 6 s can be aborted with QUIT The pause is waited off The titration is carried out If the extraction time has not expired when the endpoint has been reached the titration will only be terminated when the extraction time has elapsed Calculations ...

Page 40: ... optimal control parameters for various polarization currents Ipol 10 uA 20 uA 30 uA EP 50 mV 100 mV 150 mV dynamics 70 mV 100 mV 120 mV min rate max rate and stop drift standard values After a certain period of use in the same reagent the indicator electrode will become activated i e the titration curve becomes steeper If the titration curve is too steep then slowly varying drift values may occur...

Page 41: ... set by the parameter generator I under titration parameters The steps 400 200 and 100 mA are possible With the setting auto the current strength will be automatically reduced in the region of the endpoint The current strength will also be reduced if the conductivity of the reagent becomes too low Generator electrodes with diaphragm Work should normally be carried out with automatic switching of t...

Page 42: ... Enter formula by means of 3rd functions of keyboard Here you will find operands mathematical operations and parentheses Operands require a number as an identification You can use the following operands H2O Amount of water at the EP in ug RSX Results which have already been calculated with previous formulas X 1 9 CXX Calculation constants XX 00 45 Rules Calculation operations are performed in the ...

Page 43: ...f on has been set Lower limit 0 0 999 999 Upper limit 0 0 999 999 Sets line L13 of the remote socket OFF active pulse if the result lies outside the limits Enter next formula e g for RS2 Meaning of the calculation variables CXX C00 Sample size see page 46 C01 C19 Method specific operands see page 36 They are stored with the method in the method memory C21 C23 Sample specific operands see page 46ff...

Page 44: ...rt can be printed with the key sequence PRINT press keys repeatedly until calc appears in the display ENTER Operands C01 and C02 The following table gives the values for the operands C01 and C02 for the standard for mulas in the modes KFC and KFC B depending on the unit in which you want the result to be expressed and the unit in which you want to enter the sample size Result in Sample size in C01...

Page 45: ...g up to 9 results RSX endpoint H2O or variables CXX For MN1 the default value RS1 is entered for KFC B MN1 RS2 Delete allocation with CLEAR ENTER Each mode has an inquiry group statistics in key PARAM statistics status OFF mean n 2 res tab original delete n 1 Statistics calculation Status of statistics calculation OFF ON If the statistics calculation is switched off the following inquiries regardi...

Page 46: ...ATISTICS ENTER Rules Recalculated results are incorporated in the statistics calculation If a result of a particular titration can not be calculated no results for this determination are incorporated in the statistics calculation However the sample counter is still operative i e the statistics calculation starts again when the number of required individual determinations has been performed If the ...

Page 47: ...es The entries are specific to the method and are stored in the method memory Common variables in expert mode only Assigns values as common variables The display texts of the Coulometer are shown to the left The values are the default values common variables C30 C31 C39 Allocation for common variables Common variable C30 C39 RSX H2O CXX MNX Results RSX endpoint H2O variables CXX and means MNX can ...

Page 48: ...mb mplist param calc scalc full scalc srt ff Select a block with keys and If you require more than one report block set a as a separator between the blocks Identical for COM1 and COM2 Meaning of the report blocks result Result report with raw results calculations and statistics water crv Curve mass water in ug vs time rate crv Curve rate in ug min vs time meas crv Curve measured voltage vs time co...

Page 49: ...hod name Automatic drift correction Mass of water Calculated result water crv The following curves can also be printed out rate vs time measured voltage vs time combined curve water and rate vs time Scaling of time and mass of water axis fr 756 KF Coulometer 01109 5 756 0010 user Boss date 1998 10 27 3 time 08 54 KFC smpl size 0 372 g drift auto 3 2 ug min titr time 47 s H2O 206 5 ug content 555 1...

Page 50: ...19 C fmla C FMLA Content of key DEF def DEF Statistics report with the individual results statistics STATISTICS Current sample data smpl data SMPL DATA Sample data from silo memory silo SILO Full silo calculations report scalc full Short silo calculations report scalc srt Configuration report configuration CONFIG Contents of the method memory with memory require ments of the individual methods and...

Page 51: ...ppear in the standard mode are highlighted in gray name User name up to 10 ASCII characters User names can be entered directly or selected with the keys and The operator name is printed out in the report The operator name remains in the instrument until it is deleted or until the RAM is initialized If no operator name is to be printed out the operator blank can be selected delete name Delete user ...

Page 52: ...is included in the memory If a method identification is entered which is not found in the method memory the selected value blinks store method method Store method Store method from the working memory to the method memory up to 8 ASCII characters If a method with an identical name is already stored you are asked if you wish to overwrite the old method With ENTER it is overwritten with QUIT you retu...

Page 53: ...TH ENTER 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 ...

Page 54: ...The limits appear then in this window Smpl unit Unit of the sample size The display texts of the Coulometer are shown to the left The values are the default values Inquiries which also appear in the standard operation mode are high lighted in gray smpl data id1 or C21 id2 or C22 id3 or C23 smpl size 1 0 g smpl unit g Sample data Sample identification 1 3 or sample specific operand C21 C23 up to 12...

Page 55: ...n the instrument is started the sample data are fetched from the next silo line Organization of the silo memory Silo memory contains 35 lines Next free line is 36 6 of the 35 lines have been proc essed Free lines from 36 to 255 and from 1 to 6 1 silo line needs between 18 and 120 bytes memory capacity Filling the silo memory with a connected balance If the silo memory is filled from the balance yo...

Page 56: ...name has been entered the sample is processed with the method in the working memory Selection of the method with Sample identification 1 3 or sample specific calculation variables C21 C23 up to 12 characters Method specific texts for id s are not valid in the silo memory Sample size 6 digit number X XXXXX Method specific limits for the sample size are checked on start of the method Unit of sample ...

Page 57: ...such a case the processed silo line is not deleted but copied to the next free line see below If you work in this mode you should not enter any new silo lines during the determinations Store results in the silo memory ON OFF Determination results will be stored as C24 or C25 in the silo memory according to the allocations in the methods see page 50 save lines can only be set to OFF if the silo is ...

Page 58: ...ation results are assigned in key DEF The display texts of the Coulometer are shown to the left The values are the default values silo calculations C24 C25 Silo calculations Assignment to C24 RSX H2O CXX Calculated results RSX endpoint H2O or variables CXX can be stored as C24 Same procedure for C25 Important Ensure that there is still sufficient space for storing the results C24 and C25 In the re...

Page 59: ...tandard deviations of the results available in the silo memory can subsequently be calculated for the entire series The following details can be entered in the method under DEF silo calculations C24 C25 match id OFF Silo calculations in expert mode only Assignment to C24 RSX H2O CXX Calculated results RSX endpoint H2O and variables CXX can be stored as C24 Identical for C25 Which sample identifica...

Page 60: ...culations and assignments are carried out in the following order 1 Calculation of the results RSX 2 Calculation of means MNX 3 Assignment of silo results C24 and C25 4 Silo calculations 5 Assignment of means C26 and C27 from silo calculations 6 Assignment of common variables C3X si 756 KF Coulometer 012 101 5 756 0010 date 1998 10 27 time 08 54 14 silo cycle lines OFF save lines ON sl method id1 C...

Page 61: ... for the se lection of the dialog language the following must be sent Config Aux Language english whereby it is sufficient to only transmit the boldface characters thus C A L english The quantities of the commands above are Config configuration data Aux auxiliaries various data Language setting the dialog language The data are hierarchically structured tree form The quantities that occur in this t...

Page 62: ... may contain up to 24 ASCII characters Numerical values can contain up to 6 digits a negative sign and a decimal point Numbers with more than 6 characters are not accepted more than 4 decimal places are rounded off For numbers 1 it is necessary to enter leading zeros Entering the dialog language C A L english correct entry of numbers 0 1 incorrect entry of numbers 1 5 or 3 or 1 The current object ...

Page 63: ... path from the root of the tree up to the current node Q H Highest Queries the number of son nodes of the current node Index Q N i Name Queries the name of the son node with index i i 1 n D Detail Info Queries the detailed status information U qUit Aborts the data flow of the instrument for example after Q The triggers G and S are linked to particular objects see the summary table page 60ff All ot...

Page 64: ...mode requesting Id2 after start Id3 Instrument in the KFC mode requesting Id3 after start Smpl Instrument in the KFC mode requesting sample size after start Unit Instrument in the KFC mode requesting unit of sample size after start Start Instrument in the KFC mode waiting the pause ExtrTime Instrument in the KFC mode working off the extraction time Titr Instrument in the KFC mode titrating G Mode ...

Page 65: ...ath for object Start path at root E29 Wrong value or no value allowed Exit Send correct value or call up new object E30 Wrong trigger this trigger is not allowed or carrying out of action not possible Exit Send correct trigger exception D or call up new object E31 Command is not possible in active status Repeat command in inactive status Exit Send new command E32 Command is not possible during tit...

Page 66: ...t start or on recalculation E132 Silo empty and it has been started with open silo or empty silo has been opened Exit Send a silo entry E133 Silo full Exit Send new command E134 No method A method which is required from the silo memory does not exist Exit The error message disappears on next start E137 XXX Bytes are missing so that the method the silo line could not be stored Exit Send new command...

Page 67: ... Service Date E203 No Oven parameters Oven not correctly connected Exit The error message disappears on next start If you don t wish oven parameters in your report select Mode Parameter Presel Oven no in your method s E209 Temperature in the KF Coulometer instrument too high 60 C Exit The error message disappears if the Coulometer temperature is below 60 C E212 Transmission error from Remote Box U...

Page 68: ... tree can be divided into the following branches Root Mode Method parameters UserMeth Administration of the internal user memory for methods Config Instrument configuration SmplData Sample specific data HotKey Keys with direct access Info Current Data Assembly Component data Setup Setting the operating mode Diagnose Diagnostics program ...

Page 69: ...rized electrodes ON OFF ditto Temp Titration temperature 170 0 25 0 500 0 4 2 2 10 TDelta Time interv for meas acquisition 1 2 999 999 4 2 2 11 TMax Maximal titration time 1 999 999 OFF 4 2 2 12 Statistics Statistics Status Status of statistics calculation ON OFF 4 2 2 13 MeanN No of individual determinations 2 20 ditto ResTab Result table Select original delete n delete all ditto DelN Deletion of...

Page 70: ...im Lower limit 0 999 999 ditto UpLim Upper limit 0 999 999 ditto Output Output on L13 active pulse OFF ditto up to 9 results SiloCalc Silo calculations Assign Assignment C24 Store as variable C24 RSX H2O CXX 4 2 2 23 C25 Store as variable C25 RSX H2O CXX MatchId Matching of Id s id1 id1 2 all OFF ComVar Assignment of common variables C30 for C30 RSX H2O CXX MNX 4 2 2 24 up to C39 Report Reports at...

Page 71: ... 2 2 29 Name Method name 8 ASCII characters ditto Store Save method G ditto Name Method name 8 ASCII characters ditto Delete Delete method G ditto Name Method name 8 ASCII characters ditto DelAll Delete all methods G ditto List List of methods 1 Method 1 Name Method name read only 4 2 2 30 Mode Mode read only ditto Bytes Method size in bytes read only ditto Checksum Checksum of method read only di...

Page 72: ...s 1 9 ditto Validation Validation monitoring 4 2 2 33 Status Status of validation monitoring ON OFF ditto Interval Time interval for validation 1 365 9999 ditto Counter Time counter 0 9999 ditto ClearCount Clears the counter above G ditto Service Monitoring of Metrohm service G 4 2 2 34 Status Status of service monitoring ON OFF ditto Date Date of next service XXXX XX XX ditto DiagRep Printing of ...

Page 73: ... StopBit Number of stop bits 1 2 ditto Parity Parity even odd none ditto Handsh Handshake HWs SWchar SWline none ditto RSSet2 as for RS1 Report Report configuration 4 2 2 52 Id Print report id ON OFF ditto Instr Print line with instrument id ON OFF ditto DateTime Print line with date time ON OFF ditto Run Print run number ON OFF ditto Method Print line with method id ON OFF ditto Sample Print line...

Page 74: ... MaxLines Maximum lines read only 4 2 2 56 FirstLine First line read only ditto LastLine Last line read only ditto EditLine Editing silo lines 1 1st silo line Method Method name up to 8 ASCII char 4 2 2 57 Id1 Sample identification 1 up to 12 ASCII char ditto Id2 Sample identification 2 up to 12 ASCII char ditto Id3 Sample identification 3 up to 12 ASCII char ditto ValSmpl Sample size X XXXXX ditt...

Page 75: ... range Reference Root HotKey Keys with direct access User User name 4 2 2 62 Name Input of user name up to 10 ASCII char ditto Delete Delete user G ditto Name Input of user name up to 10 ASCII char ditto DelAll Delete all users G ditto List List of users 1 User 1 Name Name of user read only ditto up to 99 ...

Page 76: ...y Var Variables C4X C40 Start measured value read only read write ditto C41 Mass of water read only read write C42 Titration time read only read write C43 Drift at titration start read only read write C44 Titration temperature read only read write C45 Total charge mA s read only read write StatisticsVal Statistics values ActN Number of results in chart read only 4 2 2 67 1 1st mean Mean Mean read ...

Page 77: ... Pot Voltage at generator electrode read only ditto IPulse I of current pulse read only ditto MeasPt Entry in measuring point list Index Index of entry read only 4 2 2 72 X X coordinate read only ditto Y Y coordinate read only ditto Z1 Z1 coordinate read only ditto Z2 Z2 coordinate read only ditto EP EP entry Index Index of entry read only ditto X X coordinate read only ditto Y Y coordinate read o...

Page 78: ...L0 active inactive pulse OFF ditto up to L13 ResetLines Reset I O lines G ditto Stirrer Stirrer control Status Status ON OFF 4 2 2 80 Bur Buret Empty Empties the buret G S H C 4 2 2 81 Prep Prepares the buret G S H C ditto Rates Rates Forward Forward rate Select Type of rate control digital 4 2 2 82 Digital Digital rate 0 150 max ditto Reverse as for forward rate Select Type of rate control digita...

Page 79: ...XCH key ON OFF ditto Display Lock display function ON OFF ditto Mode Setting waiting intervals StartWait Waiting time after start ON OFF 4 2 2 90 FinWait Waiting time after run ON OFF ditto SendMeas Automatic sending of measured values SendStatus Connect disconnect sending ON OFF 4 2 2 91 Interval Time interval 0 4 4 16200 ditto MPList Select Selection Assembly Titrator 4 2 2 92 Assembly From asse...

Page 80: ...ready again ON OFF ditto B2 When COM2 sends a report ON OFF ditto R2 When COM2 is ready again ON OFF ditto PR only 756 Printer infos B When internal printer is printing ON OFF ditto R When internal printer is ready again ON OFF ditto I Changing an I O input ON OFF ditto O Changing an I O output ON OFF ditto Graphics Changing the curve output COM1 Graphic output on COM1 Grid Grid on curve ON OFF 4 ...

Page 81: ... range Reference Root Diagnose Diagnose Report Output of adjustment parameters G 4 2 2 101 Simulation Keycode Simulation of keys 0 29 4 2 2 102 ScreenDump Dump of 756 screen G 4 2 2 103 IntPrinter Settings for the internal printer HeatTime Heating time 1 4 0 10 4 2 2 104 MotorSpeed Motor Speed 2 3 0 9 ditto ...

Page 82: ...Parameter CtrlPara Special MaxRate 1 5 2240 max Mode Parameter CtrlPara Special MinRate 0 3 15 999 9 min Mode Parameter CtrlPara Special Stop Type drift rel drift Mode Parameter CtrlPara Special Stop Drift 1 5 999 Mode Parameter CtrlPara Special Stop Drift 0 5 999 Parameters for setting special 4 2 2 5 Dyn Dynamics in mV MaxRate Maximum allowed titration rate in ug min Max means maximum possible r...

Page 83: ...tration will be stopped 4 2 2 13 Mode Parameter Statistics Status ON OFF Mode Parameter Statistics MeanN 2 20 Mode Parameter Statistics ResTab Selected original delete n delete all Mode Parameter Statistics ResTab DelN 1 20 Entries for the statistics calculations Status On off switching Requirement for statistics calculations is a valid assignment see 4 2 2 26 MeanN Number of individual results fo...

Page 84: ...ON OFF Mode Parameter Presel LimSmplSize LoLim 0 0 999 999 Mode Parameter Presel LimSmplSize UpLim 0 0 999 999 Limit control for the sample size 4 2 2 18 Mode Parameter Presel Id1Text id1 C21 10 ASCII characters Mode Parameter Presel Id2Text id2 C22 10 ASCII characters Mode Parameter Presel Id3Text id3 C23 10 ASCII characters Text for sample identifications 4 2 2 19 Mode Parameter Presel Cell no d...

Page 85: ...output line L13 can be set 4 2 2 23 Mode Def SiloCalc Assign C24 RSX H2O CXX Mode Def SiloCalc Assign C25 RSX H2O 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 4 2 2 24 Mode Def ComVar C30 RSX MNX H2O CXX Mode Def ComVar C31 etc up to C39 As...

Page 86: ...ters UserMeth Store G UserMeth Store Name up to 8 ASCII characters UserMeth Delete G UserMeth Delete Name up to 8 ASCII characters UserMeth DelAll G Management of the internal method memory Load store and delete methods An action is performed if G is sent to the corresponding node just after en tering the name Do not use blank characters before and after method name DelAll Deletes all methods in t...

Page 87: ...e NoRinse 1 9 Changing of reagent With a connected Dosino the reagent is changed with Config Monitoring Change G The nod Config Monitoring change Status has to be OFF Parameters for automatic reagent change WaitTime Waiting time in s after switching off the stirrer AspVol Volume in ml of used reagent to be aspirated SolventVol Volume in ml of new reagent to be added Rinse Volume in ml of rinsing r...

Page 88: ...itched off again 4 2 2 40 Config PeriphUnit RemoteBox Status ON OFF Config PeriphUnit RemoteBox Keyboard US deutsch francais español schweiz Config PeriphUnit RemoteBox Barcode input method id1 id2 id3 smpl size Connections via Remote Box Status Select if a Remote Box is connected Keyboard Type of keyboard which is connected to the Remote Box Barcode Select target in Coulometer where you wish to h...

Page 89: ...same time If a name has been entered it will be printed out in the result report full short 4 2 2 48 Config Aux Beep 1 3 OFF Number of beep sounds 4 2 2 49 Config Aux DisplayMeas ON OFF Display of potentials during conditioning and titration 4 2 2 50 Config Aux Prog read only Output of the program version The Coulometer sends 5 756 0010 on requests with Q 4 2 2 51 Config RSSet1 G Config RSSet1 Bau...

Page 90: ...igits sign and decimal point SmplData OFFSilo UnitSmpl up to 5 ASCII characters SmplData OFFSilo Limits read only Current sample data The identifications Id1 Id3 can be used in formulas as sample specific calcu lation constants C21 C23 If no unit is desired for the unit of the sample size the blank string must be entered Limits Limits of sample size of current method 4 2 2 56 SmplData ONSilo Count...

Page 91: ...leted with SmplData ONSilo DelLine G If a formerly deleted line is edited again it becomes valid function unde lete 4 2 2 59 SmplData ONSilo DelAll G Deletes the entire silo memory Must be triggered with G 4 2 2 60 SmplData ONSilo CycleLines ON OFF Silo data cycling With ON executed lines are copied to the next free silo lines see page 49 Exercise caution if you edit the silo memory during the det...

Page 92: ...calculations config Configuration report user method Contents of the method memory all All reports ff Form feed on printer Reports which are sent from the Coulometer are marked with space ASCII 32 and at the beginning Then an individual identifier for each report follows 4 2 2 64 Info Checksums G Info Checksums ActualMethod read only The checksums can be used to identify the content of a file uneq...

Page 93: ...decimal place more than in result 0 0231 RelStd Relative standard deviation in 2 decimal places 0 14 4 2 2 68 Info SiloCalc C24 Name read only Info SiloCalc C24 Value read only Info SiloCalc C24 Unit read only for C25 as for C24 Info SiloCalc C26 ActN read only Info SiloCalc C26 Mean read only Info SiloCalc C26 Std read only Info SiloCalc C26 RelStd read only for C27 as for C26 The current values ...

Page 94: ... Smpl size out pin 19 13 Result out pin 20 4 2 2 70 Info ActualInfo Assembly CyclNo read only Info ActualInfo Assembly I read only Info ActualInfo Assembly Meas read only Info ActualInfo Assembly Pot read only Info ActualInfo Assembly IPulse read only Info ActualInfo Assembly Bur V read only Info ActualInfo Assembly Bur Clear G Q sends the current values CyclNo Cycle number of the voltage measurem...

Page 95: ...t for overrange 4 2 2 72 Info ActualInfo MeasPt Index read only Info ActualInfo MeasPt X read only Info ActualInfo MeasPt Y read only Info ActualInfo MeasPt Z1 read only Info ActualInfo MeasPt Z2 read only Info ActualInfo EP Index read only Info ActualInfo EP X read only Info ActualInfo EP Y read only Q sends the last entry into the measuring point list MeasPt or the last entry into the list of EP...

Page 96: ...er where the PC is connected 4 2 2 76 Info Assembly CycleTime read only Info Assembly ExV read only Info Assembly DeviceTemp read only Inquiries regarding basic variables of the assembly Cycle time Time of measuring cycles in s 0 4 ExV Volume of the Dosing Unit of the connected Dosino in mL DeviceTemp Internal temperature of Coulometer in C 4 2 2 77 Assembly GenEl Pulse G Assembly GenEl Pulse Leng...

Page 97: ...o in active by the activate pulse L5 is the error line It is continuously controlled by the Coulom eter program and can therefore not be set freely Line assignments in Coulometer program L0 Ready inactive state L1 Conditioning OK L2 Titration in progress L3 EOD End Of Determination L4 L5 Error L6 Activate pulse can be set in TIP L7 Pulses for recorder L8 Connected remote box L9 10 L11 Change reage...

Page 98: ... the Coulometer COM for the output of automatic info Setup Keycode Setup Trace Setup SendMeas Setup AutoInfo 4 2 2 86 Setup Keycode ON OFF ON means the key code of a key pressed on the Coulometer is outputted The key code comprises 2 ASCII characters table of the keys with their code see page 96 A keystroke of key 11 is sent as follows 11 The beginning of the message is marked by a space ASCII 32 ...

Page 99: ... they are ON the sequence stops until OFF is sent Switching the instrument on sets both nodes to OFF StartWait Holding point right after starting a method holding point after AutoInfo T GC FinWait Holding point at the end a method holding point after AutoInfo T F 4 2 2 91 Setup SendMeas SendStatus ON OFF Setup SendMeas Interval 0 4 4 16200 MPList SendStatus ON means the automatic transmission of m...

Page 100: ...e unit assembly must be preset see 4 2 2 92 4 2 2 94 Setup SendMeas Titrator CyclNo ON OFF Setup SendMeas Titrator Water ON OFF Setup SendMeas Titrator Meas ON OFF Setup SendMeas Titrator dWaterdt ON OFF Setup SendMeas Titrator I ON OFF Setup SendMeas Titrator Pot ON OFF Setup SendMeas Titrator IPulse ON OFF Selection of the values from the titrator which are sent in the set time interval see 4 2 ...

Page 101: ...all set AutoInfo P PowerOn Simulation of power on 4 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 has received a go command T S Stop Status Stop has been reached T B Begin of method T F Final End of determination the final steps will be carried out T E Error Message together with error number...

Page 102: ...appearance and the format of the curve for the output on COM1 Accordingly for COM2 and Int internal printer only at 756 Grid On off switching of grid over curve Frame On off switching of frame surrounding the curve If grid and frame are switched off the curve is printed faster as the printing head does not have to move to the end of the paper Scale Type of scaling of the measured value axis full m...

Page 103: ...Setup Initalise G 4 2 2 99 Setup RamInit G Initializes instrument see page 110 All parameters are set to their default value and error messages are cleared The user and silo memories will be de leted Command only possible in the inactive state of the Coulometer 4 2 2 100 Setup InstrNo G Setup InstrNo Value serial number 8 ASCII characters Instrument identification for report output Set the value w...

Page 104: ...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 MotorSpeed in ms per step 6 steps 1 dot Small numbers give high print ing speed If you wish to speed up the internal printer set low heat...

Page 105: ... Only a shielded data cable for example METROHM D 104 0201 may be used to couple the Coulometer with foreign devices The cable shield must be properly grounded on both instruments pay attention to current loops always ground in a star head formation Only plugs with sufficient shielding may be used for example METROHM K 210 0381 with K 210 9045 4 3 1 Handshake Software Handshake SWchar Handshake in...

Page 106: ...n 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 Coulometer as Receiver Coulometer external device Coulometer external device Time Data output Data input RxD TxD XOFF XON LF max characters Data output disabled Data output enabled Data output Data input max 128 characters 384 charac...

Page 107: ...ed If data output is disabled for more than 6 s by XOFF E43 appears in the display Hardware Handshake HWs Coulometer as Receiver Coulometer as Sender The data flow can be interrupted by deactivating the CTS line Coulometer external device Coulometer external device Coulometer external device XOFF XON Data output disabled Data output enabled Time Data output Data input RxD TxD 2nd line LF 1st line ...

Page 108: ...eady DTR ON condition Instrument is ready to receive data Protective earthing Direct connection from cable plug to the protective ground of the instrument Polarity allocation of the signals Data lines TxD RxD voltage negative 3 V signal state ON voltage positive 3 V signal state ZERO control or message lines CTS RTS DTR voltage negative 3 V OFF state voltage positive 3 V ON state In the transition...

Page 109: ...tions of Use 101 Contact arrangement at plug female for RS 232C socket male View of soldered side of plug Ordering numbers K 210 0381 and K 210 9045 No liability whatsoever will be accepted for damage or injury caused by im proper interconnection of instruments 5 1 6 9 ...

Page 110: ...4 3 Properties of the RS 232 Interface 756 831 KF Coulometer Instructions of Use 102 ...

Page 111: ... exhausted septum pierced seals not OK ground joint sleeves not smooth Generator electrode diaphragm polluted or moist Sample matrix consumes iodine Change reagent more often When working with Oven Oven Sample Processor molecular sieve of Oven Oven Sample Processor exhausted gas flow too high allow to run overnight screw seals tight Drift unstable Poor stirring Stir so that mixing is efficient but...

Page 112: ...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 Set stop drift higher Set control range smaller set max rate higher ...

Page 113: ...lectrode cable is broken use new cable The electrode test can be switched off under the key PARAM titration parameters Exit Rectify fault or STOP check exchange unit The Dosing Unit is not mounted properly Exit Mount Dosing Unit properly so that the coupling engages or STOP check generator electr There is too high a resistance at the generator electrode Not enough reagent in the titration vessel G...

Page 114: ...t be found at the given COM Remedy connect the oven to the given RS interface of the Coulometer or set the following in your method under PARAM preselections Oven no no titration data No curve can be printed as no data are available not valid A value is not available overrange The measuring range of 2 V has been exceeded Overrange replaces the corresponding measured value Exit Rectify error or STO...

Page 115: ...as a fault Remote Box has a fault Remedy Set under CONFIG peripheral units Remote Box OFF switch off Coulometer take away Remote Box and switch on Coulometer Contact Metrohm service time out PC keyboard A connected PC keyboard has been used to call up an ad dress e g F12 and the connection has then been inter rupted Possible causes Remote Box has a fault PC keyboard has a fault Exit Correct fault ...

Page 116: ...e same on both instruments error 37 Framing error Exit QUIT and set corresponding quantity the same on both instruments error 38 Overrun error At least 1 character could not be read Exit QUIT error 39 Overflow of the receive buffer of the Coulometer 128 characters Exit QUIT Send errors error 42 CTS OFF Handshake unsatisfactory for more than 1 s Exit QUIT Is the receiver switched on and ready to re...

Page 117: ...or 42 Transmission error Is the printer set to on line Is the connection cable properly wired The received characters are garbled Are the RS settings the same on both devices Has the correct printer been selected Data transfer has been interrupted on the hardware side during the printout of a curve Re establish connections and switch printer off on Wrong line spacing The printer does not emulate c...

Page 118: ... aid of a PC and the 6 6008 200 or 6 6008 500 Vesuv 3 Software and print out your configuration data PRINT CONFIG ENTER Initialize RAM 1 Switch off Coulometer 2 Switch on Coulometer and press key 9 at the same time The display shows diagnose press key 0 9 3 Press key 8 The display shows RAM init 4 Press key ENTER Initialization will be carried out The display then shows RAM init passed 5 Exit the ...

Page 119: ...and insert in socket 5 of the 767 The cover re mains closed on the 767 3 Switch on Coulometer and press key 9 at the same time The display shows diagnose press key 0 9 4 Press key 6 The display shows pol ADC test press 1 3 5 Press key 3 The display shows polarizer test 6 Press ENTER on the Coulometer The display shows dummy resistor 10 0 k Press ENTER and enter the resistance from the cover of the...

Page 120: ... to the mains The mains cable must therefore always be unplugged when certain adjustments are made or parts replaced The cable should only be plugged in and unplugged when the instruments are switched off 6 1 Coulometer setup 6 1 1 Connecting a Stirrer or Ti Stand Screw 6 2101 050 stand console onto the base of the Coulometer always use the screws provided and insert the support rod into the conso...

Page 121: ...strip projects 4 Insert the metal spindle through the new roll of paper 5 Place the metal spindle in the notches at the side of the paper compartment in the Coulometer and close the cover Notes Always operate the key PAPER to obtain a paper feed Never pull the paper with your hands as this could damage the printer Thermal paper has a limited shelf life Protect it from light Do not store it in plas...

Page 122: ...lar sieve and insert into generator electrode 7 Place septum in the screw cap and screw this onto the titration vessel Only tighten it enough to ensure that it is tight The septum should not be deformed 8 Insert 6 1439 010 feed aspiration tube order separately in the last joint opening and connect the aspiration and feed tubing of the Ti Stand Close the top of the tube with a glass stopper 1 When ...

Page 123: ...adapter cable For aspiration it is an advantage to use the 6 5617 000 aspiration equipment including 50 ml dosing unit order Dosino separately For aspirating oily samples where only the sample is to be aspirated and not the whole reagent a 20 ml dosing unit or for very viscous samples a 10 ml cylinder should be used see page 146ff for accessories 6 2 1 Setup with aspiration equipment 1 Screw 6 182...

Page 124: ...4 Insert indicator electrode in the left hand joint opening screw on 6 2104 020 elec trode cable and plug it into the Ind El socket of the Coulometer 5 Insert generator electrode in the central joint opening screw on 6 2104 120 electrode cable and plug it into the Gen El socket of the Coulometer 6 Fill the drying tube with molecular sieve and insert into generator electrode 7 Place septum in the s...

Page 125: ...esults in the Coulometer report Make sure there is no report output from the oven When the RS interfaces are not connected then the following setting must be made at the Coulometer PARAM preselections Oven no If you enter one of the COMs of the Coulometer for this parameter then your Coulometer result report will contain the oven data heating time sample temp lowest temp highest temp and gas flow ...

Page 126: ...170 stopper for the inlet tip If in addition to the gas inlet from the oven you want to use a Dosino for aspiration then the aspiration tip is inserted on the joint opening and the gas inlet is fitted with A 254 0104 seal which is placed in the screw cap instead of the septum the screw cap is then screwed down see below If you use the 6 1830 000 heatable outlet tubing then you should use A 254 010...

Page 127: ...le Processor The Oven Sample Processor heats the sample and transfers the moisture from the sam ple 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 ca ble 6 2125 110 774 6 2141 020 cable 774 6 2125 110 cable ...

Page 128: ...into the joint opening and the gas inlet is fitted with A 254 0102 seal which is placed in the screw cap instead of the septum the screw cap is then screwed down see illustration on page 118 If you require an additional opening for injections then 6 1465 320 titration vessel is avail able it has two side mounted screw threaded openings Stopper with 6 1446 170 O ring Generator electrode with drying...

Page 129: ...dapters Printer Cable Settings on Coulom eter Settings on Printer Seiko DPU 414 DPU 411 6 2134 110 6 2125 010 6 2125 020 baud rate 9600 data bit 8 stop bit 1 parity none handshake HWs send to Seiko none Citizen iDP562 RS 6 2134 050 baud rate 9600 data bit 8 stop bit 1 parity none handshake HWs send to Citizen Epson LX 300 6 2134 050 as above see printer manual HP Desk Jet with serial interface 6 2...

Page 130: ...20 6 2125 010 Precisa balances with RS232C interface 6 2125 080 6 2125 010 The balance type must be preselected at the Coulometer with the CONFIG key 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 identifications and method...

Page 131: ...le 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 CONFIG peripheral units send to IBM PC programs Vesuv 3 program for data management and method backup for up to 64 devices 6 6008 200 for 2 devices 6 6008 500 ...

Page 132: ...ilo memory is switched on the barcode string always goes to the method The cursor position has no effect If the silo memory is switched off the input has no meaning id1 The barcode string always goes to Id1 The cursor position has no effect id2 id3 As for id1 smpl size The barcode string always goes to the sample size The cursor position has no effect If the silo memory is switched on the silo lin...

Page 133: ... numerical keys Country specific special characters will probably not be converted correctly Operating via a PC keyboard The Coulometer can be operated from the PC keyboard The Coulometer functions are called up as follows Coulometer function Key combination on PC keyboard Remarks C FMLA Alt F CLEAR F5 CONFIG F10 Cursor Cursor Navigation Cursor Cursor Selection of inputs DEF Alt D DEF formula inpu...

Page 134: ... 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 You can copy this dia gram cut out the hatched part and place it above the func tion keys of your PC keyboard SmplData Param Config Start S...

Page 135: ... Resolution 0 1 ug H2O Reproducibility Sample Reagent manufacturer s standard With 10 ug 1000 ug H2O 3 ug With 1000 ug H2O 0 3 or better Drift compensation automatic manual or none Materials Housing Metal powder coated Keypad cover Polycarbonate PC Display Graphical LCD 192 x 64 dots Field 100 x 37 mm LED back lit Printer only at 756 Built in thermal printer Paper width 57 mm 144 pixel or 24 chara...

Page 136: ...ns Designed and tested in accordance to IEC publication 1010 safety class I This manual contains information and warnings which have to be followed by the user to ensure safe operation and to retain the apparatus in safe condition Mains connection Voltage 100 240 V 10 Frequency 50 60 Hz Power consumption max 38 W Fuse 2 x T1H 250 V only to be replaced by Metrohm Service using the same type Additio...

Page 137: ...put 0 pin 9 Input 1 pin 22 Input 2 pin 10 Input 3 pin 23 Input 4 pin 11 Input 5 pin 24 Input 6 pin 12 Input 7 Start Stop Enter Outputs pin 5 Output 0 pin 18 Output 1 pin 4 Output 2 Ready inactive Conditioning ok active if Cond ok Titration active during titration Functions see page 130 tp 100 ms tp 5 V 5 V 5 V 5 V 5 V 5 V 5 V 5 V 5 V 5 V 5 V Not used Not used ...

Page 138: ...Error active on errors Activate pulse see also page 132 Pulses for recorder tp 150 µs Remote box activated not used Reagent exchange Sample size out of limits Result out of limits adjustable see page 35 For all outputs VCE0 40 V IC 20 mA tPulse 100 ms Functions see page 131 Voltage pin 15 pin 14 pin 25 I 200 mA 0 V active 5 V inactive Ordering numbers for plug K 210 9004 shell and K 210 002 No lia...

Page 139: ...1 Enter 2 Cond ok 1 Titr 2 EOD 3 21 9 22 5 18 4 17 Error 1 5 16 Activate 2 6 1 Inputs Outputs Pulse 7 2 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 Pin Reag ex 11 13 ...

Page 140: ...nstructions for Use 132 7 2 2 Activate pulse An activate pulse may be set in key PARAM 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 EOD Data output ...

Page 141: ...meter is switched on electronic tests are carried out During this period system tests appears in the display The tests are documented in the system test report which can be printed out when the Coulometer is switched on see page 19 di 756 KF Coulometer 01109 5 756 0010 user Boss date 1998 10 27 time 08 54 RAM test OK real time clock OK A D converter OK LCD display OK COMPorts OK EPROM test OK Cont...

Page 142: ... the validation It contains the appropriate calculation formulas 1 content H2O C01 C00 3 mg g 2 recovery RS1 C22 2 where C01 1000 C22 id2 content according to the reagent manufacturer in mg g The second formula calculates the recovery rate and is therefore a measure of the accu racy The limit control for the second result is switched on and the limits are 0 97 1 03 These values apply for a 1 00 mg...

Page 143: ...010 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 If you use the Vesuv 3 PC program you should select at least the following reports on COM1 or COM2 result calc mplist ...

Page 144: ... the Coulometer report Determination method parameters pa 756 KF Coulometer 5 756 0010 date 1998 11 19 time 17 55 0 KFC B Oven Det 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 ...

Page 145: ...g 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 tab original preselections drift corr auto req ident OFF req smpl size OFF smpl unit g limit smpl size OFF text id1 id1 or C21 text id2 id2 or C22 text id3 id3 or C2...

Page 146: ... data in the Coulometer report Determination method parameters pa 756 KF Coulometer 5 756 0010 date 1997 11 19 time 17 56 0 KFC B 774 Det 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 in...

Page 147: ... 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 tab original preselections drift corr auto req ident OFF req smpl size OFF smpl unit g limit smpl size OFF text id1 id1 or C21 text id2 id2 or C22 text id3 id3 or C23...

Page 148: ... the absence of guaranteed features the purchaser has no rights or claims except those mentioned above If damage of the packaging is evident on receipt of a consignment or if the goods show signs of transport damage after unpacking the carrier must be informed immediately and a written damage report demanded Lack of an official damage report releases METROHM from any liability to pay compensation ...

Page 149: ...compatibility Emission IEC 61326 EN 55022 CISPR 22 Electromagnetic compatibility Immunity IEC 61326 IEC 61000 4 2 IEC 61000 4 3 IEC 61000 4 4 IEC 61000 4 5 IEC 61000 4 6 IEC 61000 4 11 Safety specifications IEC 61010 1 UL3101 1 It has also been certified by the Swiss Electrotechnical Association SEV which is member of the International Certification Body CB IEC The technical specifications are doc...

Page 150: ...nts of EU Directives 89 336 EEC and 73 23 EEC Source of specifications EN 61326 Electrical equipment for measurement control and laboratory use EMC requirements EN 61010 1 Safety requirements for electrical equipment for measurement control and laboratory use Description of apparatus Coulometer for water determinations according to Karl Fischer with LCD dis play and internal thermal printer Herisa...

Page 151: ...compatibility Emission IEC 61326 EN 55022 CISPR 22 Electromagnetic compatibility Immunity IEC 61326 IEC 61000 4 2 IEC 61000 4 3 IEC 61000 4 4 IEC 61000 4 5 IEC 61000 4 6 IEC 61000 4 11 Safety specifications IEC 61010 1 UL3101 1 It has also been certified by the Swiss Electrotechnical Association SEV which is member of the International Certification Body CB IEC The technical specifications are doc...

Page 152: ... mark requirements of EU Directives 89 336 EEC and 73 23 EEC Source of specifications EN 61326 Electrical equipment for measurement control and laboratory use EMC requirements EN 61010 1 Safety requirements for electrical equipment for measurement control and laboratory use Description of apparatus Coulometer for water determinations according to Karl Fischer with LCD dis play Herisau May 07 2002 ...

Page 153: ...030 1 Titration vessel holder 6 2047 020 1 Electrode cable for indicator electrode 6 2104 020 1 Electrode cable for generator electrode 6 2104 120 1 Keypad for 756 KF Coulometer 6 2130 040 3 Rolls of thermal paper 6 2237 020 1 Spindle for thermal paper roll 6 2241 030 1 Screw cap thread GL18 6 2701 040 3 PTFE joint sleeves SGJ14 6 2713 000 1 PTFE joint sleeve SGJ 29 6 2713 010 1 PTFE joint sleeve ...

Page 154: ...1 Electrode cable for indicator electrode 6 2104 020 1 Electrode cable for generator electrode 6 2104 120 1 Keypad for 756 KF Coulometer 6 2130 040 3 Rolls of thermal paper 6 2237 020 1 Spindle for thermal paper roll 6 2241 030 1 Screw cap thread GL18 6 2701 040 3 PTFE joint sleeves SGJ14 6 2713 000 1 PTFE joint sleeve SGJ 29 6 2713 010 1 PTFE joint sleeve SGJ 19 6 2713 020 1 Stopper with nipple 6...

Page 155: ...th 25 cm 6 2016 030 1 Titration vessel holder 6 2047 020 1 Electrode cable for indicator electrode 6 2104 020 1 Electrode cable for generator electrode 6 2104 120 1 Keypad for 831 KF Coulometer 6 2130 090 1 Screw cap thread GL18 6 2701 040 3 PTFE joint sleeves SGJ14 6 2713 000 1 PTFE joint sleeve SGJ 29 6 2713 010 1 PTFE joint sleeve SGJ 19 6 2713 020 1 Stopper with nipple 6 2730 030 1 Funnel 6 27...

Page 156: ... 1 Titration vessel holder 6 2047 020 1 Electrode cable for indicator electrode 6 2104 020 1 Electrode cable for generator electrode 6 2104 120 1 Keypad for 756 831 KF Coulometer 6 2130 090 1 Screw cap thread GL18 6 2701 040 3 PTFE joint sleeves SGJ14 6 2713 000 1 PTFE joint sleeve SGJ 29 6 2713 010 1 PTFE joint sleeve SGJ 19 6 2713 020 1 Stopper with nipple 6 2730 030 1 Funnel 6 2738 000 1 Bottle...

Page 157: ...805 080 Stopper for aspiration tip 6 1446 060 Nipple for aspiration tip 6 2730 030 O ring for nipple E 301 0022 Aspiration tip 6 1543 070 Waste bottle 1L 6 1608 030 Bottle attachment for waste bottle 6 1602 105 Adsorber tube for waste bottle 6 1609 000 SGJ clip for adsorber tube 6 2023 020 Thread stopper M8 6 1446 080 Double bottle holder 6 2055 100 Titration equipment Titration vessel amber glass...

Page 158: ... for connection of printer balance at the same COM 6 2125 010 6 2125 030 Connection of PC keyboard and or barcode reader Remote Box 6 2148 000 Printers Citizen printer iDP562 RS 230 V 2 140 0024 Citizen printer iDP562 RS 115 V 2 140 0025 Cable Coulometer Citizen printer iDP562 RS 9 25 pins 6 2134 050 Cable Coulometer Seiko DPU 414 6 2134 110 Cable Coulometer EPSON 6 pin plug 6 2125 040 6 2125 010 ...

Page 159: ... 13 automatic sequence 25 changing reagent 105 check drive unit 105 check electrode 105 check exchange unit 105 check generator electr 105 check remote box 105 C FMLA 35 CLEAR 14 common variables 22 39 Computer connection 123 Conditioning 31 CONFIG 17 Configuration 17 Connecting cables 150 Connection Balance 122 Barcode reader 124 Dosino 115 Electrodes 3 External printer 121 Oven Sample Processor ...

Page 160: ...rication number 3 formula 34 G Generator electrode with diaphragm 8 without diaphragm 7 generator I 30 GLP 133 Graphics changing output 24 display 42 example 41 printing 40 42 H H2O 22 Handshake 97 handshake 21 I Identification 46 request 29 id1 or C21 46 Indicator electrode 13 Initial measured value 35 Initialize Coulometer 110 initializing Dosino 106 Initializing 110 Input of text 16 of values 1...

Page 161: ... 35 number of determ 18 O Object tree 60 Operation mode 20 operator level 21 Operator name 43 Ordering numbers 145 Outputs 129 oven 30 Oven connection 117 methods 136 Oven Sample Processor connection 119 methods 138 overrange 106 overtitrated 106 Overview 2 P PAPER 2 113 Paper 113 PARAM 17ff Parameters 27 parity 21 pause 28 PC connection 123 PC keyboard connection 125 peripheral units 19 Pin assig...

Page 162: ...29 Sample size 46 48 limits 29 size of 10 sample size out 106 sample unfit 106 save lines 49 Scope of delivery 145 send to COMX 19 Sequence reagent exchange 25 titration 31 Serial number 3 service is due 106 service 19 Setup 112ff Setup of titration vessel 5 aspiration with Dosino 116 aspiration with Ti Stand 114 working with Oven 118 signature 22 SILO 47 silo calculations 51 silo empty 106 silo f...

Page 163: ...ion vessel setup 5 aspiration with Dosino 116 aspiration with Ti Stand 114 working with Oven 118 transmission error 107 Tree 60ff Troubles 57 103 external printer 109 titrations 103 U Unit method specific 29 result 35 sample size 29 46 up lim 29 35 USER 43 USER METH 44 User methods 135 User name 43 V validate instrument 107 Validation 133 validation 19 Value input 15 16 W Weight 46 48 limits 29 si...

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