Validation of the Metrohm 743 Rancimat using Standard Operating ...

Application Bulletin 278/1 eValidation of the Metrohm 743 Rancimatusing Standard Operating ProceduresOf interest for:General analysis, organic chemistry, pharmaceuticals, petrochemistry, food industry, biology, cosmetics, paintsB 1, 3, 4, 5, 7, 8, 12, 14SummaryGLP (Good Laboratory Practice) requires periodicchecking of the reproducibility and accuracy ofanalytical instruments by using Standard OperatingProcedures (SOPs).This Application Bulletin is intended to provide youwith a guideline for the validation of your Rancimat. Astandard operating procedure is proposed whichallows all the Rancimat functions which are relevantfor the measurement to be checked. The limits givenare to be taken as being examples of what can beachieved under normal laboratory conditions.Depending on the demands placed upon the accuracyof the measuring system, it may be necessary toredefine these limits in the standard operatingprocedure. If very careful work is carried out underappropriate conditions then it may be possible toachieve lower limits.The operating software for the 743 Rancimat containsprepared GLP tests for the temperature, conductivityand gas flow measurements. The operator candetermine whether and which tests are to be carriedout, in addition the interval between the tests and therequired accuracy can also be defined. If the GLPfunction is activated then a comment will be made oneach result report as to whether the GLP testrequirements have been fulfilled. In order to be able tocarry out the most important tests Metrohm offers the6.5616.000 GLP Test Set as an option.Further information about the topics of QA, GLP andvalidation can also be found in the brochure "Qualitymanagement with Metrohm" which is available fromyour local Metrohm agency.Field of applicationThese instructions are applicable to the followingMetrohm instrument:• 743 RancimatChecking periodIt is a good idea to repeat the check on the Rancimatat yearly intervals. Apart from this, an extra validationshould be carried out after one or more Rancimatcomponents have been exchanged.Internal instrument checking routinesMetrohm instruments have their own internal start-upchecking routines. During the switch-on test thedisplay elements and the contents of the programmemory are checked by carrying out check sum tests.The functioning of the data memory sector is testedby a write/read test. With the 743 Rancimat a check ismade as to whether a PC is connected and that thecontrol software has been started. If no error messageis produced then it can be assumed that theinstrument is working perfectly.If Rancimats are checked within the context of regularservice work being carried out then a specialvalidation of the instrument electronics is no longernecessary.Maintenance / ServiceAn essential requirement for ensuring the GLPconformoperation of each individual instrument usedin the laboratory is that instrument care and cleansingare carried out with great care and, in particular, thatthe instruments are handled properly. The'Instructions for Use' provided for the particularinstrument must be available to all laboratorytechnicians.Checking the electronic and mechanical functionalgroups of Metrohm instruments can and should becarried out by specialists from the manufacturingcompany within the framework of regular servicework. Many Metrohm agencies offer favorably-pricedservice contracts for your instruments. For this reasonif faults or errors should occur the 743 Rancimat isequipped with a built-in diagnostics program whichallows the service technician to check the functioningof particular assemblies in order to localize the error.We also recommend that all the instruments used inthe validation process are subjected to a regularannual service.MethodsThe 6.5616.000 GLP Test Set is necessary in order tovalidate the Rancimat. It contains a certified Pt-100temperature sensor, an insert for the heating blockand a test resistor (10 kΩ). The Rancimat has ameasuring input for making measurements with thetemperature sensor.

Application Bulletin 278/1 eValidation of Metrohm Rancimats with the help ofStandard Operating Procedures (SOPs)Page 3/14Procedure1. In the window 743 Rancimat Control select theinstrument 1...4 for which the GLP temperaturetest is to be carried out.2. In the window 743 Rancimat Control select thedetermination method whose temperature is to beused in the GLP test and alter the temperature ifnecessary.3. Click on 743 Rancimat Control / Tools / GLP-Test /Temperature and then click on in the GLPTest window.4. Enter the calibration data of the temperaturesensor used (entered data are retained) and clickon . A certified temperature sensor hasthree calibration points. Each point consists of atemperature-resistance pair.5. Under TEST-PARAMETER for Block A and Block Bselect the channels in which the temperature testis to be carried out. At least one channel must beselected per block. Enter the required Testduration per channel and click on .Metrohm recommends checking one channel perblock and entering a delay period of 10 min.6. The selected channels are checked insuccession. The entered test duration applies toeach channel.7. Insert the temperature sensor with PTFE andaluminum cylinder in the first selected channeland click on to start the measurement.8. If the temperature defined in the method has notyet been reached then heating is startedautomatically. In the Measure status window themessage Waiting until temperature is reached...appears.9. When the temperature defined in the method hasbeen reached the message Measuringtemperature. Please wait... appears.10. When the measurement has been carried out youare requested to insert the external temperaturesensor and GLP insert into the next selectedchannel and to start the measurement. Care mustbe taken that changing the temperature sensorfrom one channel to the next is carried out asquickly as possible in order to prevent coolingdown.11. Carry out the GLP temperature measurement forall channels in succession.12. When the last temperature measurement hasbeen carried out the test results for the measuredchannels are shown.13. Check the results and click on in order tostore the results of the GLP test.Assessing the results:The variation between the measured temperature andthe set temperature displayed should not exceed± 0.5 °C, otherwise the measurements should berepeated and the test duration per channel should beextended if necessary.3.1. Validation of the conductivity inputs withthe test resistorThis test is carried out with the 6.2109.030 TestResistor which belongs to the 6.5616.000 GLP TestSet available from Metrohm as an option. The testresistor must be connected to the electrodeconnections of the 743 Rancimat.Procedure1. In the window 743 Rancimat Control select theinstrument 1...4 for which the GLP conductivitytest is to be carried out.2. Click on 743 Rancimat Control / Tools / GLP-Test /Conductivity and then click on in the GLPTest window.3. Switch on the test resistor option and enter theresistance of 6.2109.030 Test Resistor: 10000 Ω.Then click on .4. Attach the 6.2109.030 Test Resistor to theelectrode connections of each selected channelin succession. Click on each time.5. When the last conductivity measurement hasbeen carried out the test results for the measuredchannels are shown.6. Check the results and click on in order tostore the results of the GLP test.Assessing the results:The variation between the measured conductivity andthe set conductivity displayed should not exceed± 5 µS/cm.3.2. Validation of the conductivitymeasurement with a standardconductivity solutionThis test is carried out with a standard solution ofknown conductivity. Before the GLP conductivity testwith a standard solution is carried out for the first timethe cell constant of the conductivity cell must bedetermined. The determination of the cell constant isdescribed in Section 4.4.1 of the 'Instructions for Use'of the 743 Rancimat..If a calibrated conductivity cell is used then care mustbe taken that it is always used in the same channel.As the absolute correctness of the measuredconductivity plays no part in the determination of theinduction time it is not necessary to routinely validatethe cell constant of the conductivity cell. This is onlyimportant if the stability time is to be determined inaddition to the induction time.Conductivity of the standard solutionc(KCl) = 1 mmol/L can be used as the standardsolution; this is prepared from the 6.2301.060

Application Bulletin 278/1 eValidation of Metrohm Rancimats with the help ofStandard Operating Procedures (SOPs)Page 4/14Conductivity Standard (KCl 0.1 mol/L) available as anoption. The conductivity standard is diluted 1:100 withdistilled water.This solution has a conductivity of:TemperatureConductivity18 °C 127 µS/cm19 °C 130 µS/cm20 °C 133 µS/cm21 °C 136 µS/cm22 °C 138 µS/cm23 °C 141 µS/cm24 °C 144 µS/cm25 °C 147 µS/cmInstead of the standard solution c(KCl) = 0.1 mol/L,ready-to-use dilute standard solutions withconductivities in the range 100 - 140 µS/cm can also beused. These solutions are available commercially andare supplied with a quality certificate.Preparation1. Place a measuring vessel with cover and filledwith 60 mL standard solution in each measuringposition.Procedure1. In the window 743 Rancimat Control select theinstrument 1...4 for which the GLP conductivitytest is to be carried out.2. Click on 743 Rancimat Control / Tools / GLP-Test /Conductivity and then click on in the GLPTest window.3. Switch on the Standard solution option and enterthe value for the conductivity of the standardsolution in the appropriate field. Click on .4. Click on in the GLP Test window. Theconductivity is now measured in all channels.5. When the last conductivity measurement hasbeen carried out the test results for the measuredchannels are shown.6. Check the results and click on in order tostore the results of the GLP test.Assessing the results:The variation between the measured conductivity andthe set conductivity displayed should not exceed± 10 µS/cm, otherwise the measurement must berepeated with a new standard conductivity solution. Ifthe variation is still too large then the conductivity cellmust be recalibrated and the GLP test repeated.4. Validation of the temperature correctionThe temperature correction Delta T describes thevariation of the actual temperature of the sample fromthe temperature of the heating block and is one of theparameters of the method. The variation between thetemperature of the heating block and that of thesample is mainly caused by the flow of air which coolsthe sample. This means that it must be determinedseparately for each temperature, each gas flow andeach heating block. It can be determinedautomatically with the external 6.1111.010Temperature Sensor (included in the 6.5616.000 GLPTest Set available from Metrohm as an option).If work is carried out properly then the variationremains within very narrow limits so that instead ofindividually determined values the values given in thetable below can be used as an approximation. Thesevalues apply to a gas flow of 20 L/h:Set temperature Delta T80 °C +1.1 °C90 °C +1.3 °C100 °C +1.4 °C110 °C +1.5 °C120 °C +1.6 °C130 °C +1.7 °C140 °C +1.8 °C150 °C +1.9 °C160 °C +2.0 °CIf the temperature correction is to be determinedexperimentally then Metrohm recommends that aseparate method is drawn up for each heating blockand each temperature and that the temperaturecorrection is determined separately for each of thesemethods. This should be carried out before thevalidation of the temperature correction.If measurements are to be made at differenttemperatures then it is sufficient to check thevalidation at a single temperature.Preparation1. Fill a reaction vessel with 5 g silicone oil.2. Insert the air tube and temperature sensor in thereaction vessel cover and fix in place withdistance pieces.3. Place reaction vessel cover with temperaturesensor on the reaction vessel.4. Push temperature sensor right down to thebottom (the sensor must contact the vesselbase).5. Place reaction vessel in Position 2 or 3 andconnect to the gas inlet tube.Procedure1. In the window 743 Rancimat Control select therequired method for the heating block for whichyou want to validate the temperature correctionDelta T.2. Open the window containing the methodparameters. Note the previous value for Delta T

Application Bulletin 278/1 eValidation of Metrohm Rancimats with the help ofStandard Operating Procedures (SOPs)Page 5/14in the validation protocol and set the value forDelta T to 0. Then click on .3. Start the gas flow and the heating manually.4. Click on 743 Rancimat Control / Tools / Determinedelta T / Block A or 743 Rancimat Control / Tools /Determine delta T / Block B to start thedetermination of the temperature correction.5. The first window to open contains dataconcerning the external temperature sensor; thecalibration data of the temperature sensor usedcan be entered here (the last data to be enteredare displayed here).6. Click on OK. The window Determination of Delta Tappears.7. If the temperature defined in the method has notyet been reached then the message Waiting untiltemperature is reached... appears in the window.8. When the temperature defined in the method hasbeen reached the message Measuringtemperature. Please wait... appears in the window.9. As soon as the two measured temperatures arestable the message Measured temperature is nowstable! appears. The temperature correction DeltaT which has been determined can now beaccepted in the method with . Themessage Delta T is now set in the correspondingmethod now appears. The value determined forDelta T can also be taken over manually in othermethods which use the same temperature.Assessment of the results:The variation between the measured temperaturecorrection and the previously used temperaturecorrection should not exceed ± 0.3 °C.5. Measuring the reproducibility in oilIn order to check the functioning of the completemeasuring setup we recommend that a measurementis carried out on edible oil. As the absolute inductiontime is unknown and is also not stable over longerperiods of time only the scatter of the measurementsis to be checked. Metrohm recommends that a doubledetermination is carried out.Even if measurements are to be made at differenttemperatures it is sufficient to check the reproducibilityat a single temperature.Preparation1. Fill each of two measuring vessels with 60 mLdistilled water.2. Place the measuring vessels together with themeasuring vessel covers in the openingsprovided for them in the 743 Rancimat andconnect the electrode plug of the cover to thecorresponding socket of the 743 Rancimat.3. Fill each of two reaction vessels with 3 gsunflower oil.4. Attach an air tube to the reaction vessel covers.5. Place the reaction vessel cover on the reactionvessel. Rotate the cover so that the air tube is asclose as possible to the vessel wall.6. Attach the white connecting tube to the reactionvessel cover connection.Procedure7. In the window 743 Rancimat Control select therequired method for which you want to determinethe reproducibility.8. Start the heating manually.9. Enter the sample identifications ID1 and ID2 inthe corresponding fields in the 743 RancimatControl window.10. Wait until the required temperature has beenreached in the heating block.11. Insert the two reaction vessels in the 743Rancimat and connect the gas inlet tube and thewhite connection tube to the measuring vessel.12. Click on the Start button in the operating field ofthe 743 Rancimat Control window.13. When the measurement is finished the resultscan be seen in the 743 Rancimat Results /Determination data window.14. To print out the results click on 743 RancimatResults / File / Print / Determination acc. to method/Print.Assessing the results:The absolute difference between the measuredinduction times of two samples should not exceedmore than 10% of the mean value of the two induction

Application Bulletin 278/1 eValidation of Metrohm Rancimats with the help ofStandard Operating Procedures (SOPs)Page 6/14times. The induction time of the oil sample should bebetween 4 hours and 10 hours.6. Printing GLP resultsIn order to print out the GLP certificate click on 743Rancimat Control / Tools / GLP-Test / Print GLP-Results.The GLP certificate contains information about theGLP tests for temperature and conductivity.The GLP certificate printout for the selectedinstrument contains the printing date, the serialnumber of the instrument and the results of the lastGLP test carried out on this instrument. Each of theGLP tests for temperature, conductivity and gas flowcontains the following information:Date Date of the last GLP test carried out.Tester Person who carried out the GLP test.Test result Information about whether the test waspassed or not.If the test results are to be printed out then GLPmonitoring must be switched on.In the Program settings window activate the Header,Results, Curve, Method parameters fields and Methoddescription and click on .Click on Print in the Printing of... window and on .Procedure if the values obtained do not fulfilthe requirementsAll such values must be documented in the validationprotocol and the further procedure must also bedocumented.If the variations are too large then the various pointsgiven under "Recommendations for remedying faults"must be thoroughly checked and the causes of thefaults must be removed. The validation must berepeated.Literature• 743 Rancimat 'Instructions for Use'In order to print out all the GLP results click on 743Rancimat Results / View / GLP and on File / Print / AllTemperature GLP's and on OK and OK. Click on File /Print / All Conductivity GLP's and on OK and OK.The detailed GLP results of all the GLP tests carriedout will be printed out.Printing out the temperature correction valueIn order to print out the value determined for thetemperature correction the corresponding methodmust be opened in the 743 Rancimat Control / File /Open Method window. Click on Print in order to printout a report of the corresponding method. This mustbe repeated for each validated method.Printing out the results of the reproducibilitymeasurementMark the determinations in the 743 Rancimat Results /Determination Data window and click on File / Print. Inthe Printing of... window activate the fieldDetermination acc. to method and click on Settings.

Application Bulletin 278/1 eValidation of Metrohm Rancimats with the help ofStandard Operating Procedures (SOPs)Page 7/14Recommendations for remedying faultsInformation about remedying faults can also be foundin the 'Instructions for Use' for the 743 Rancimat. Thefollowing lists are not exhaustive and are onlyexamples of possible sources of error.Possible sources of errorError Cause RemedyHigh variationsbetweenmeasurements indifferent channelsDirty reaction vessels Blow out disposablevessels with nitrogenbefore use, remove dustfrom the outside ofdisposable vesselsThoroughly cleanreusable vesselsCheck reusable vesselsfor damage andscratches and exchangeif necessaryMolecular sieveexhaustedDry or replacemolecular sieveDifferent amounts ofsamplesEnsure sample weightsare correctHigh variationsbetweenmeasurements inthe two heatingblocksSamples not inserted atthe same time or notstarted immediatelyafter insertionDirty reaction vesselopenings in the heatingblockInhomogeneoussamplesSample contaminationduring weighing outPlace samples in theheating block and startwithout delayClean heating blockopeningsHomogenize samplesAvoid contaminationIncorrect Delta T setting Determine temperaturecorrection for eachheating block separatelyMolecular sieve Dry or replaceexhaustedmolecular sieve6.1111.010 Replace or recalibrateError Cause RemedyTemperature sensor not temperature sensorfunctioning properlyDirty reaction vesselopenings in the heatingblockClean heating blockopeningsHigh variationsbetweenmeasurements indifferentinstrumentsAtypical curveswith particularsamplesVery noisy curvesIncorrect Delta T setting Determine temperaturecorrection againMolecular sieve Dry or replaceexhaustedmolecular sieveIncorrect weight of Use the weight given insilicone oil forthe instructions fordetermining the determining Delta Ttemperature correctionIncorrect sample weight Correct sample weight6.1111.010Replace or recalibrateTemperature sensor not temperature sensorfunctioning properlyDirty reaction vesselopenings in the heatingblockSamples release othersubstances beforeinduction time isreachedMeasuring vessel coveror tubing releasessubstancesConductivity cell notworking properlyConductivity cellcontaminatedFatty particles inmeasuring vesselClean heating blockopeningsEnter evaluation delayor evaluationsuppressionHeat measuring vesselcover and tubing for 1 to2 hours at 80°C indrying oven.Clean conductivity cellClean measuring vesseland conductivity cell,use foam barrier

Application Bulletin 278/1 eValidation of Metrohm Rancimats with the help ofStandard Operating Procedures (SOPs)Page 8/14AppendixValidation certificateValidation certificate for temperature validation of the Rancimat heating blocks using the 6.5616.000 GLP Set

Application Bulletin 278/1 eValidation of Metrohm Rancimats with the help ofStandard Operating Procedures (SOPs)Page 9/14Validation certificate for validation of the conductivity inputs using the 10kΩ test resistorValidation certificate for validation of the conductivity cell using a standard conductivity solutionMethod printout for documentation of the determined temperature correction using a measurement in inertoilMethod "120deg" print. date 17.11.2000 11:07CreatorunknownCreation date 17.11.2000 11:07ParametersTemperature 120 °CDelta T 1.60 °CGas flow20 L/hUse pumpYesStart delay0 minStart modeper channelStop criteria TimeNoTime0.0 hStop criteria ConductivityNoConductivity0 uS/cmStop criteria Endpoint(s)YesShut off heater at end of determinationNoShut off gas flow at end of determination NoEvaluationEvaluate induction timeYesEvaluate stability timeNoDelta kappa 0Interpretation delay0.0 hInterpretation suppression Start0.0 h

Application Bulletin 278/1 eValidation of Metrohm Rancimats with the help ofStandard Operating Procedures (SOPs)Page 10/14Interpretation suppression End 0.0 hCurvesTime-axis (x) scaling AutomaticEnd ValueConductivity-axis (y) scalingEnd Value6.0 hAutomatic200 uS/cmFormulasFormula 1 for induction timeNoFormula R1 = InductionTime * 1.000/1.000 + 0.0Formula 2 for stability timeNoFormula R2 = StabTime² * 0.000 + StabTime * 1.000/1.000 +0.000Formula 3 for stability timeNoFormula R3 = StabTime² * 0.000 + StabTime * 1.000/1.000 +0.000StandardsStandard formula activeYesFormula according to AOCS Cd 12b-92Factor 2.000Target temperature 110.0 °CDocumentationInclude HeaderInclude ResultsInclude induction timeInclude stability timeInclude formula 1 resultInclude formula 2 resultInclude formula 3 resultInclude standards resultInclude Curve(s)Include Method ParametersInclude DescriptionSend to PrinterSend to FileDirectoryYesYesYesNoYesNoNoYesYesYesNoYesNoDescriptionMeasuring the reproducibility in sunflower oilBlock ABlock BID 1 Channe Temperature Induction time ID 1 Channe Temperature Induction timesunflower oil 2 110°C 4.08 h sunflower oil 2 110°C 4.10 hsunflower oil 1 110°C 4.17 h sunflower oil 1 110°C 4.16 hInduction timeStability timesunflower oil / 2 sunflower oil / 1Induction timeStability timesunflower oil / 3 sunflower oil / 434.9 µS/cm30.3 µS/cm0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5h0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5h

Application Bulletin 278/1 eValidation of Metrohm Rancimats with the help ofStandard Operating Procedures (SOPs)Page 11/14Example of a validation record of the 743 RancimatValidation Record 743 RancimatCompany: Metrohm AG Division: Applications LabDate: 16 June 2000 Time: 15:30User:B. ZumbrägelSerial number: 021361. Calibration points of the temperature sensorDesignation: no. 15 Temperature [°C] Resistance [Ohm]Point 1 50 119.41Point 2 100 138.52Point 3 200 175.862. Temperature validationBlock ATemperature[°C]Requestedtemperature[°C]Tolerance Block B Temperature[°C]Requestedtemperature[°C]ToleranceChannel 1 121.28 121.6 ± 0.5 °C Channel 1 121.44 121.6 ± 0.5 °CChannel 2 121.36 121.6 ± 0.5 °C Channel 2 121.52 121.6 ± 0.5 °CChannel 3 121.28 121.6 ± 0.5 °C Channel 3 121.52 121.6 ± 0.5 °CChannel 4 121.23 121.6 ± 0.5 °C Channel 4 121.44 121.6 ± 0.5 °Cpassednot passed3.1. Validation of the conductivity inputstest donetest not doneBlock AConductivity[µS/cm]Requestedvalue [µS/cm]Tolerance Block B Conductivity[µS/cm]Requestedvalue [µS/cm]ToleranceChannel 1 98.8 100 ± 5 µS/cm Channel 1 98.9 100 ± 5 µS/cmChannel 2 98.9 100 ± 5 µS/cm Channel 2 98.9 100 ± 5 µS/cmChannel 3 98.8 100 ± 5 µS/cm Channel 3 98.8 100 ± 5 µS/cmChannel 4 98.8 100 ± 5 µS/cm Channel 4 98.8 100 ± 5 µS/cmpassednot passed

Application Bulletin 278/1 eValidation of Metrohm Rancimats with the help ofStandard Operating Procedures (SOPs)Page 12/143.2. Validation of the conductivity measurement with conductivity standardtest doneTemperature 23 °Ctest not doneBlock AConductivity[µS/cm]Requestedvalue [µS/cm]Tolerance Block B Conductivity[µS/cm]Requestedvalue [µS/cm]ToleranceChannel 1 141.3 141.0 ± 10 µS/cm Channel 1 141.5 141.0 ± 10 µS/cmChannel 2 141.2 141.0 ± 10 µS/cm Channel 2 141.3 141.0 ± 10 µS/cmChannel 3 140.9 141.0 ± 10 µS/cm Channel 3 141.5 141.0 ± 10 µS/cmChannel 4 141.0 141.0 ± 10 µS/cm Channel 4 141.1 141.0 ± 10 µS/cmpassednot passed4. Validation of the temperature correctiontest donetest not doneTemperature 120 °CBlock A Method Block B MethodDelta T [°C]Old delta T[°C]ToleranceDelta T [°C]Old delta T[°C]Tolerance1.60 1.60 ± 0.3 °C 1.60 1.60 ± 0.3 °Cpassednot passed5. Determination of the reproducibility in oiltest donetest not doneMethod R_110 Method R_110Temperature 110 °C Temperature 110 °CSample sunflower oil Sample sunflower oilBlock AInduction time[h]Difference ofinductiontimes [h]Tolerance(10% ofmean) [h]Block BInduction time[h]Difference ofinductiontimes [h]Tolerance(10% ofmean) [h]Determin. 1 4.08 0.09 0.41 Determin. 1 4.10 0.06 0.41Determin. 2 4.17 Determin. 2 4.16Mean 4.13 Mean 4.13passednot passedSignature:Visa:

Validation Record 743 RancimatCompany:Date:User:Serial number:Division:Time:1. Calibration points of the temperature sensorDesignation: Temperature [°C] Resistance [Ohm]Point 1Point 2Point 32. Temperature validationBlock ATemperature[°C]Requestedtemperature[°C]Tolerance Block B Temperature[°C]Requestedtemperature[°C]ToleranceChannel 1 ± 0.5 °C Channel 1 ± 0.5 °CChannel 2 ± 0.5 °C Channel 2 ± 0.5 °CChannel 3 ± 0.5 °C Channel 3 ± 0.5 °CChannel 4 ± 0.5 °C Channel 4 ± 0.5 °Cpassednot passed3.1. Validation of the conductivity inputstest donetest not doneBlock AConductivity[µS/cm]Requestedvalue [µS/cm]Tolerance Block B Conductivity[µS/cm]Requestedvalue [µS/cm]ToleranceChannel 1 100 ± 5 µS/cm Channel 1 100 ± 5 µS/cmChannel 2 100 ± 5 µS/cm Channel 2 100 ± 5 µS/cmChannel 3 100 ± 5 µS/cm Channel 3 100 ± 5 µS/cmChannel 4 100 ± 5 µS/cm Channel 4 100 ± 5 µS/cmpassednot passed

3.2. Validation of the conductivity measurement with conductivity standardtest donetest not doneTemperature °CBlock AConductivity[µS/cm]Requestedvalue [µS/cm]Tolerance Block B Conductivity[µS/cm]Requestedvalue [µS/cm]ToleranceChannel 1 ± 10 µS/cm Channel 1 ± 10 µS/cmChannel 2 ± 10 µS/cm Channel 2 ± 10 µS/cmChannel 3 ± 10 µS/cm Channel 3 ± 10 µS/cmChannel 4 ± 10 µS/cm Channel 4 ± 10 µS/cmpassednot passed4. Validation of the temperature correctiontest donetemperature correction used from tableTemperature °CBlock A Method Block B MethodDelta T [°C]Old delta T[°C]ToleranceDelta T [°C]Old delta T[°C]Tolerance± 0.3 °C ± 0.3 °Cpassednot passed5. Determination of the reproducibility in oiltest doneMethodMethodtest not doneTemperature °C Temperature °CSampleBlock AInduction time[h]Difference ofinductiontimes [h]Tolerance(10% ofmean) [h]SampleBlock BDetermin. 1 Determin. 1Determin. 2 Determin. 2MeanpassedMeanInduction time[h]not passedDifference ofinductiontimes [h]Tolerance(10% ofmean) [h]Signature:Visa: