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Sourcelanguage: Explicationofwarning Safety System Transportand Transportandstorage Scopeof Descriptionofsystem IKA®C6000calorimeterglobal ceof Connectiontothe Connectiontothe Connectiontotheoxygen Connectiontothemainspower Connectionof On/off yandoperating nationofthescreendis Switchingonthe System Switchingoffthe Thestandardcalorimetric Calorificvalue Noteonthe Complete Adjustment(onlyIKA®C6000global Instructionson Preparationfor Charging position (mainoverview) Servicing position 22Other Helpandservicing Disying/hidingthesample Cleaningthe ServicingandCleaningthe IKA®C6000global IKA®C6000 Explicationofwarning GeneralFailuretoobservethisinformationcancausedamagetohealthandinjuries.Thissymbolindicatesinformationwhichisimportantforensuringthattheappliancefunctionswithoutanytechnicalproblems.metricmeasurementsareperformedefficientlyandforusingthecalorime-tersystem.Failuretoobservethisinformationcanresultininaccurate33 Safety Readtheoperatinginstructionsinfullbeforestartingupandfollowthesafetyinstructions.Keeptheoperatinginstructionsinacewheretheycanbeaccessedbyeveryone.EnsurethatonlytrainedstaffworkwiththeFollowthesafetyinstructions,guidelines,occupationalhealthandsafetyandaccidentpreventionregulations.TheIKA®C6000globalstandards/isoperibolcalorimetersystemmaybeusedonlyinconjunctionwiththepositionvesselsC6010orC6012fordeterminationofthecalorificvaluesofsolidandliquidsubstancestonationalandinternationalstandards(suchasDIN51900,BS1016T5,ISO1928,ASTM5468,ASTM5865andASTM4809).Theumextraenergyaddedtothepositionvesselmustnotexceed40,000J(selectthetestmassaccordingly).Thepermittedtemperaturemustnotexceed50Onlyfillthe positionvesselwithoxygentoaumpressureof40bar(4MPa).Checkthepressuresettingonthepressurereducerforyouroxygensupply.PerformaleakagetestbeforeeachSomematerialstendtoexplodewhencombusted(e.g.duetoformationofperoxides),whichcouldcausethe positionvesseltocrack.TheIKA®C6000globalstandards/isoperibolcalorimetermaynotbeusedfortestingexplosivesamples.Iftheburningbehaviourofamaterialisunknown,itmustbetestedbeforecombustioninthepositionvessel(riskofexplosion).Ifyouareburningunknownsamples,leavetheroomkeepyourdistancefromtheBenzoicacidmayonlybecombustedinitspressedform!Flbledustandpowdermustbefirstpressed.Oven-drydustandpowdersuchassplints,hay,strawetc.explodewhencombusted!Alwayswetthesematerialsfirst!Highlyflbleliquidswithalowvapourpressure(e.g.tetramethyldihydrogendisiloxane)mustnotdirectlytouchthecottonthread!
gases,ashesorcondensation,forexample,ispossibleintheinnerwallofthepositionObservetheaccidentpreventionrequirementsapplicabletotheactivityandtheworkstation.WearyouralprotectiveWhenhandlingcombustionsamples,combustionresidueandauxiliarymaterials,pleaseobservehighlyflPleaseobservetherelevantregulationswhenhandlingoxygen.Warning:oxygenasacompressedgasisoxidising;intensivelyaidscombustion;canreactviolentlywithflblematerials.DonotuseoilorTubesandscrewedjointsforoxygenmustbekeptofgrease.Combustiongasesarehazardoustohealth,thereforethehosemustbeconnectedtoasuitablegascleaningsystemorextractionsystem.Attheendoftheworkperiod,closethemainvalvefortheoxygensupply.Performservicingworkonlywhentheequipmentisdepressurised.Whenusingstainlesssteelcruciblesthoroughlychecktheirconditionaftereachexperiment.Ifthematerialgetsthinner,thecruciblemaycatchfireanddamagethepositionvessel.Cruciblesmustnotbeusedformorethan25combustionsforsafetyreasons. positionvesselismanufacturedinaccordancewiththedirectiveforpressureequipment97/23/EC.ThisisindicatedbytheCEsymbolwiththeIDnumberofthenotifiedbody. positionvesselisacategoryIIIpressuredevice.The positionvesselhasundergoneanECprototypetest.TheCEdeclarationofconformityconfirmsthatthis vesselcorrespondstothepressuredevicedescribedintheECprototypetest.Thetestwithtestpressureof33MPaandaleakagetestwithoxygenat3MPa.ReferReferalsototheoperatinginstructionsfortheC6010/ „maintenanceof positionpositionvesselsareexperimentautoclavesandmustbetestedbyatechnicalexpertaftereachuse.Individualuseisunderstoodheretoincludeaseriesofexperimentsperformedunderroughlythesameconditionsintermsofpressureandtemperature.ExperimentautoclavesmustbeoperatedinspecialchambersThepositionvesselsmustundergorepeatedtests(internaltestsandpressuretests)performedbythetechnicalexpert.Thefrequencyofthesebasisofexperience,typeofoperationandthematerialusedinthepositionvessel.Thedeclarationofconformityesinvalidifmechanicalmodificationsarecarriedouttotheexperimentautoclavesoriftightnesscannolongerbeguaranteedasaresultofmajorcorrosion(e.g.pittingbyhalogens).InparticularthethreadsonthepressurevesselandtheunionnutaresubjecttoconsiderablestressTheconditionandfunctionofthesealsmustbecheckedandensuredbywayofaleakagetest(seetheoperatinginstructionsfortheC6010/6012positionvessel,section„Leaktightnesstesting“).Ifthemaintenance,andespeciallythepressuretesting,isnotperformedorisperformedincorrectly,thereisariskthepositionvesselmayburstoranuncontrolledinternalfiremayoccurattheelectrodeswhichcouldburnawaytheseals(oxyacetylenetorcheffect),thusposingarisktolifeandlimb.testsandserviceworkonthe
positionvesseltoourfactoryforinspection,andifnecessary,repairafter1000testsorafteroneyearordependingonApressuretestmustbeperformedafterapositionvesselhasreachedorexceededthethepressuretesthasbeenperformedareleasecodecanbeenteredtoenablethepositionthesections“MaintenanceofthepositionVessel”and“InputtingaServiceCode”).ThewarningmessagewillthenNote:Youcanthencontinuetousethedevice/positionvessel.ContacttheIKA®ServiceDepartmenttoperformthepressuretest.Complywiththesafetyinstructionsinthisrespect.Theuserwillbegivenspecificinstructionsontherelevantscreen.ForForthepurposesoftheseoperatinginstructionstechnicalexpertiswhoguaranteestoconductthetestsproperlyonthebasisofhistraining,knowledgeandexperiencegainedthroughpracticalwork,whoissufficientlywhoisnotsubjecttoanyinstructionsintermsofthetestactivity,whohassuitabletestequipmentifwhocanprovideappropriateproofoftherequirementslistedin1.Nationaldirectivesandlawsmustbeobservedforoperatingpressurevessels!Anyoneoperatingapressurevesselmustkeepitinapropercondition,operateitproperly,superviseworkimmediayandimplementthesafetymeasuresrequiredinthecircumstances.defectswhichcouldposearisktostafforthird Correct TheIKA®C6000globalstandards/isoperibolcalorimetersystemisusedforcalorificvalueThisisdonebycingaknowntyofasubstanceina positionvesselwhichissurroundedbyawaterjacket.Thesampleisthencombustedinanoxygenatmosphere.Thecalorifictheresultingincreaseintemperature,thesample
massandtheknownthermalcapacityoftheoverallsystem.TheIKA®C6000globalstandards/isoperibolcalorimetersystemissubjecttothePressureinstructionsaccordingly.Foradaptationtoindividuallaboratorytasks,useoriginalIKA®consumablesandaccessories. User InthischapteryoucanfindouthowtoworkthroughtheseOperatingInstructionsmosteffectivelytobeabletoworkreliablywiththecalorimetersystem.Theinstructionsinthesection„Safetyinstructions“mustbecompliedwith.theminorder.Thesection„Transportandstorage“isrelevantforsystemreliabilityandforensuringhighmeasuringaccuracy.Thesection„Descriptionofsystemcomponents“describesthesystemcomponents,
andthesection„Thestandardcalorimetricprocedure“describestheessentialsofcalorimetry.Thecalorimetersystemisreadytoperformmeasurementsonceyouhavecompletedtheproceduresinthesection„Commissioning“:-„Preparingameasurement“and„StartingOperationsmustalwaysbecarriedoutinthespecifiedsequence.SystemThecalorimetersystemIKA®C6000globalminationofgrosscalorificvaluesofsolidandThesystemischaracterizedbythefollowingRelievesyouofroutinetasksthroughautomatedmeasurementprocedureIntegraloxygenAutomaticdetection positionOperationwithoutthecoolingunit:ConnectionC25;temperaturerange12°Cupto27°C;waterconsumptionpermeasurementabout4l;waterpressuremax.1barupto1,5bar.
Operationwithactivecoolingunit17-27°C(e.g.IKA®KV600;optional)MeasurementandcalculationofgrosscalorificvalueaccordingtoDIN51900,ISO1928,ASTMD240,ASTMD4809,ASTMD5865,ASTMD1989,ASTMD5468,ASTME711CalculationofnetcalorificvalueaccordingtoDIN51900,ASTMD240,ASTMD4809,ASTMD5865,ASTMD1989,ASTMD5468,ASTM Measurementrange:max.40.000J(Thiscorrespondstoanincreaseintemperatureinthepositionvesselofapprox.5K).PC-operationofoneorseveralcalorimeters(SoftwareCalWin®)AsamplerackcanbeUSBprinterportis66Correct Operatingmodebasedontheadiabatic,°Cor30°C(thebeginningtemperatureof
waterintheinnervessel)dependingonthecoolingwatertemperature.CoolingC6000global12°Cto20Adiabatic22Isoperibolic22-Isoperibolic2220°Cto23Adiabatic25Isoperibolic25-Isoperibolic2523°Cto27Adiabatic30Isoperibolic30-Isoperibolic30 Warrantyand InaccordancewithIKA®warrantyconditions,thewarrantyperiodis12months.Forclaimsundermayalsosendthemachinedirecttoourfactory,fortheclaim.Youwillbeliableforfreightcosts.
Thewarrantydoesnotcoverwornoutparts,nordoesitapplytofaultsresultingfromimproperuse,insufficientcareormaintenancenotcarriedoutinaccordancewiththeinstructionsinthisoperatingIKA®onlyconsiderthemselvestoberesponsibleforthesafety,reliabilityandperformanceoftheappliancewhentheappliancehasbeenoperatedinaccordancewiththeoperatinginstructions,onlysauthorisedbythemanufacturerinterferewiththeappliance,onlyoriginalpartsandoriginalaccessoriesareusedforrepairs.
ThecalorimetersystemmaybeopenedonlybyanauthorisedServiceAgentorCustomerServiceIfserviceisrequired,wemendthatyoucontactourcustomerservicedepartmentFurthermore,wereferyoutotheapplicablesafetyconditionsandaccidentrequirements.IKA®isnotresponsiblefordamagesorcostsresultingfromaccident,improperuseofthedeviceorimpermissiblemodifications,repairsor Transportand TransportandstorageThesystemmustbeprotectedagainstmechanicalimpact,vibrations,dustdepositsandcorrosiveambientairduringtransportationandstorage.Itisdoesnotexceed80%.storingandtransportation.Incaseofrepairthedevicehastobecleanedandfromanymaterialswhichmayconstituteahealthhazard.
loadtheformfromtheIKA®websiteIfyourequireservicing,returntheapplianceinitsoriginalpackaging.Storagepackagingisnotsufficient.Pleasealsousesuitabletransportpackaging.7User7Pleaseunpackthesystemcomponentscarefullyandcheckforanydamage.Whenyouunpacktheequipment,checkforanydamageswhichmayhaveoccurredduringtransportation.
Inthecaseofanydamageafactreportmustbesentimmediay(post,railorforwarder). Scopeof CalorimeterIKA®C6000globalCalorimeterIKA®C6000globalAttaentDischargehose(1.5ConnectiontubeVentingMainsconnectionWarrantyWaterinflowOperating88Transportand Descriptionofsystem IKA®C6000calorimeterglobal StylusforoperatingtheTouchWaterMainspower Discharge CInflowReturn
CVentingO2connection
CCceofAconstantambienttemperatureisanimportantrequirementforensuringthehighmeasuringaccuracyofthesystem.ThefollowingconditionsmustthereforebefulfilledattheceofNodirectsolarNodraughts(e.g.besidewindows,doors,airSufficientdistancetoradiatorsandotherheatTheminimumdistancebetweenthewallandsuchasshelves,wireducts,ringlines,etc.installedaboveit.around20°C...25°C.Thesystemmustbesetupona
Foroperationofthesystemthefollowingmustbeavailableattheceofinstallation:Apowersupplycorrespondingtothenametesonthesystemwithpressuregauge.Ashut-offvalvefortheoxygensupplymustbeinstalled.Observetheinstructionsonhandlingoxygengiveninthechapter„Safetyconsiderthemselvesresponsibleforthesafety,reliabilityandperformanceoftheapplianceonlywhenthedevicehasbeenoperatedinaccordancewiththeoperatinginstructions,installationhavebeenmet.ConnectiontotheRearviewwithouthosessecurelyclosed(see„Servicingandcleaningthefilter“)!Inserttheinflowpipeinto„IN“portuntilitclickshome.Connecttheotherendofthepipetothe„OUT“portofthecondenser(waterpressuremax1.5bar).Insertthereturnpipeinto„OUT“portuntilitclickshome.Connecttheotherendofthepipetothe„IN“portofthecondenser.Theconnection„EMPTY“isintendedonlyforemptyingthedevice,e.g.fortransportpurposes.Innormaloperationthedischargehoseneednotbeinserted!ConnectiontotheOperatrionisonlyallowedwiththepressurevalveIKA®C25!TheIKA®C25pressurevalveisabsoluyessentialonthewaterfaucetforoperationofthecalorimeter,anditmustbepresettoanoutputpressureofapproximay1.5bar.Thevalveisinstalledintothelineofthewaterconnection,seeoperatinginstructionIKA®C25.InserttheO2connectiontubeintothe„IN“portuntilitclickshomeandconnectthedifnecessary.IKA®C29.RemovalentailsthesameoperationsperformedinthereverseNote:TheO2connectiontubecanberemovedonlyafterithasbeendepressurised.max.4Screwtheventinghosetothescrewcoupling(8AF)onthecalorimeterandpositiontheendundertheextractorhoodorconnectittoasafetyregulationsinmax.4IKA®IKA®CTheventinghosedischargesthecombustiongasesfrom positionvesselaftercombustiontrial.Whenlayingtheventing
Combustiongasesarehazardoustohealth,ventinghosemustbeensurethatitisnotcrushedorCheckthattheavailablemainspowersupplymatchesthemainspowersupplyparticularslistedontheratingte.
connectedtoasuitablegascleaningsystemorextractionsystem.Note:Whiletheperipheraldevicesarebeingconnected,theyandthecalorimetermustbeturned-offonthemainspowerswitch!RS232 SerialconnectionforcontrollingthecalorimeterusingStandardsettingBaudData8Stopbits:1RS232BALANCE: Standardsetting: Baudrate: Data Stop Networkconnectionfordatatransferviathenetwork,e.g.toanetworkprinter USBinterface(onlyfortestpurposes) Interfaceforconnectionofa InterfaceforconnectionoftheC5020sampleOn/offThedeviceisswitchedonandoffviatheon/offswitchlocatedontheright-handside.Switchthedeviceoffattheon/offLiftmovesSwitchtheapplianceoffonlybyusingthecommands.LiftmovesapplianceisswitchedotherthanbyfollowingtheNote:Switchthedeviceoffattheon/offswitchonlywhendirectedtodosoby AftertheIKA®C6000globalstandards/isoperibolcalorimeterhasbeenswitchedon,thetouchscreendisyisactiveandcanbeoperatedusingthestylusorfinger. nationofthescreen Schematicrepresentationofthedisy DE Arrowsymbol,Arrowsymbol,verticalscrollVerticalscrollInfoArrowsymbol,horizontalscrollHorizontalscrollControlOtherview-basedpresentationsofdisycomponentsaredescribedintherelevant
Thecontentsofthescreendisyareoftendistributedoverseveraltabs.Youcanswitchbetweentabsatanytimebyclickingonthem.Thusforinstancethescreendisyduringthethreeviews„Measurements“,„Device“andStatusGreenMeasurementcompletedbutnotyetevaluated,orselectionPocketMeasurementcompletedendevaluated,evaluationinputscannolongerbeBlankMeasurementpreparedbutnotyetFieldpropertynotselected,orcancelledbeforeRedCancellationafterMeasurement
ckingonthepaleareasofthescrollbarscrollsthelistdisyorreportfield.Clickinginthedarkareaanddraggingitallowsyoutomovecontinuouslythroughthedisy,asdoesclickingonthearrowsymbolsandmaintainingtheselection.Note:Greyed-outfieldscannotbeTheview„Graph“showsthetemperaturebyalongthebottomedgeofthescreen.
Toinitiateanactionitissufficienttoclickononeofthediscreteareasshowingtherelevantimagesortext.Forinstanceduringthe„Preparationformeasurement“dialoguethemostimportantac-tionsareexinedbelow.WeightedPermitsmanualinputofaweightvalueusingthevirtualkeyboard.SelectionfieldformarkingacalibrationpositionManualselectionboxwhen positionvesseldetectionisinactive.AlphanumericeditableAlphanumericeditableAlphanumericeditableIKA®SelectionboxwhichallowsaselectionlisttobeWeighted
Inputofanumericalvalue,suchasweigh-tedsample:Theentireareawiththeexceptionofthe„Ba-lance“buttonisavailabletobeclickedhere.Anumericalvirtualkeyboardisopenedandcanbeusedtoinputthevalue:Afterthevirtualkeyboardhasbeenclosednatively,clickingonthe„Balance“buttonauto-SelectionShiftkeyforupperandlowercaselettersandspecialcharacters
Inputofanalphanumericvalue,such„Designation“Acompletevirtualkeyboardisopened.Note: uminputis23Afterthevirtualkeyboardhasbeenclosed„OK“,thevalueintheinputfieldisSelectfromaselectionbox,e.g.fortheig-nitionaid:Aftertheselectionboxhasbeenclicked,alistoftheoptionsisdisyed.TheoptionthatisclickedisSingleselectionfield,suchascalibrationClickingontheentireareaallowsthepreparedmeasurementtobemarkedasacalibration.WorkingWorkingwiththeIKA®C6000globalstandards/isoperibolSwitchingontheSystem
TheIKA®C6000globalstandards/isoperibolisswitchedonwiththeOn/offswitch.Thecoverinitialisedandthesoftwareisloaded.ThesystemtestisperformedautomaticallyeverytimetheIKA®C6000globalstandards/isoperibolisswitchedon.again;clickingonthe„Showdetails“buttonpro-videsdetailedinformation.Testingtheexternalwatercircuitwiththecir-culationpumpandheater(approx.30to45Testingtheinternalwatercircuitwiththecon-again(approx.30to45seconds).TestingwhetherthetemperatureofthecoolingwatersiscorrectfortheselectedfunctionoftheIKA®C6000globalstandards/isoperibol.(ap-prox.60to180seconds).Ifanyoneofthesestepsisnotperformedsuc-sage.Afterallthecomponentshavebeenche-afteramanualcancellation.Todothis,presstheWiththesystemtestinstandby,nomeasure-mentscanbemade.Howeveritispossibletose-lectsomeoptions.IfthecoolingwaterconditionsarenotcorrectfortheselectedfunctionoftheIKA®C6000globalstandards/isoperibol,youcanselectadifferentfunctionfromthosecurrentlyavailable.Makesurehoweverthatthesystemconditionsarestable.ThefollowingarethedefaultmodesthatareAdiabat (IKA®C6000globalIsoperibol (IKA®C6000Ifthesystemischangedtoadifferentfunctionitmustberecalibrated.
FirstAtfirstcommissioningyoumustregistera positionvessel:Todothis,press„on“button.Selectthe„Function...“Selectthe„New Followtheinstructionsonpage36.
„End“:Thissavesthemeasurementstakendu-ringtheday;thecoverofthecalorimeterisIclosedandthesoftwareshutdown.Afterthis,switchoffthecalorimeterandalltheaccessories.Neverswitchthedeviceoffwithoutpre-viouslyhavingrun„End“,otherwisedatamaybeThestandardcalorimetricTestCombustioniscarriedoutinacalorimeterunderspecificconditions.TheIKA®C6000globalstandards/isoperibolisfilledwithaweighedfuelsample,thefuelsampleisignitedandtheThespecificcalorificvalueofthesampleiscalculatedasfollows:WeightoffuelcalorimetersystemForcompletecombustionthe vesselisfilledwithpureoxygen(quality3.5).Adjustthepressureoftheoxygenatmosphereinthe positionvessel
ThegrosscalorificvalueHoisformedasthequotientoftheamountofheatliberatedupontotalcombustionofasolidorliquidfuelandtheweightofthefuelsample.ThecompoundscomprisingthefuelthatcontainwatermustbeTheformulaforthecalorificvalueisHo=(CV*DT–Qext)/mHoCalorificmMassoftheDTMeasuredandcorrectedincreaseinQextAllexternalenergyoriginatingfromtheignitionwire,theignitionaids,thecombustionaidsandtheformationofat3MPa(possiblemax.4MPa).The determinationofthegrosscalorificvalueasubstancerequiresthatthe
Cvalue(thermalcapacity)oftheproceedunderpreciselydefinedconditions.Theapplicablestandardsarebasedonthefollowingassumptions: Dependingonthestarttemperaturethatisset,thetemperatureofthefuelbeforethecombustionis20°Cupto30°C. Thewatercontainedinthefuelbeforethecombustionandthewaterthatisformedwhencompoundscomprisingthefuelcontaininghydrogenundergocombustionispresentinaliquidstate.Nooxidationoftheatmosphericnitrogenhastakence.Thegaseousproductsaftercombustionconsistofoxygen,nitrogen,carbondioxide,sulfurdioxideandtheoxidationproductsoftheSolidsubstancesmaybeformed(forexampleOften,however,thecombustionproductsthatformthebasisofthestandardsarenottheonlyproductsthatareformed.Insuchcases,anysisofthefuelsampleandtheproductsofcombustionarenecessarytoprovidedataforacorrectioncal-culation.Thestandardgrosscalorificvalueisthendeterminedfromthemeasured
valuelesstheenergyofcondensationofthewaterthatwascontainedinthefuelandwasformedbythecombustion.Theheatvalueisthemoreimportanttyfortechnicalpurposes,sinceinallimportanttechnicalapplications,theheatvalueistheonlytythatcanbeevaluatedintermsofenergy.Forinformationonthefundamentalprinciplesofcalculationforgrosscalorificvalueandheatvalue,pleaserefertotheapplicablestandards(forexample:DIN51900;ASTMD240;ASTMD1989,ISOAsdeterminedbythesystem,duringacombustionexperiment,notonlyisheatgeneratedfromthecombustionofthesample,formofextraneousinproportiontotheheatenergyofthefuelsample.Thecombustionheatofthecottonthreatthatig-nitesthesampleandtheelectricalignitionenergywouldresultindistortedvaluesofthemeasure-ment.Thiseffectistakenintoconsiderationinthecalculationwithacorrectionvalue.Substanceswithlowflbilityorsubstancesthatburnpoorlyundergocombustionincombina-tionwithcombustionaids.Thecombustionaidisfirstweighedandthenaddedtothecruciblewiththesample.Fromtheweightofthecombustionaidanditsknownspecificgrosscalorificvalue,itisthenpossibletodeterminethetyofheatrimentmustbecorrectedbythisamountofheat.TheC14disposablecrucibleisacombustiblecruciblethatcanbeusedinsteadofatraditionalcrucible.Thedisposablecrucibleundergoestotalcombustionwithnoresidue.Ifadisposablecruci-bleisused,thereisthennoneedforacottonth-read.Thecrucibleisindirectcontactandisignitedbythefixedignitionwireofthepositioncrucible.Inmostcases,noadditionalcombustionitselfactsasthecombustionaid.
AcidAlmostallsubstancestobeyzedcontainsul-furandnitrogen.Undertheconditionsthatpre-vailduringcalorimetricmeasurements,sulfurandnitrogenundergocombustionandformSO2,SO3andNOX.Sulfuricandnitricacidariseincombi-nationwiththewaterresultingfromandhumidity.Heatofsolutionisalsogenerated.Toobtainthestandardgrosscalorificvalue,theeffectoftheheatofsolutiononthegrosscalorificvalueiscorrected.acidstatively,distilledwateroranothersuitableabsorptionsolutioniscedinthe positionvesselbeforethetrialaccordingtotherelevantstandards.Withthisabsorptionfluidandthecombustionwater,thecombustiongasesformacids.Afterthecombustion,the positionvesselisthoroughlywashedwithdistilledwatersoastocollectthecondensatethathassettledonthetainedinthismannercannowbeexaminedwithpositionintotherespectiveacidcontent.Formoreinformationonthissubject,pleasecon-tactIKA®‚oryournearestauthorizeddealer.NoteontheThecalorimetersystemIKA®C6000globalstan-mentfortheroutinedeterminationofcalorificvaluesofsolidandliquidsubstances.Exactmea-surementscanhoweverbeachievedonlyiftheindividualstepsofthetrialareperformedwithcare.Theprocedureasdescribedinthe„Foryoursafety“sectionandinthefollowingsectionsmustthereforebeadheredtoexactly.Ifyouareburningunknownsamples,leavetheroomorkeepwellawayfromtheca-Afewpointsshouldbenotedinrespectofthesubstancestobecombusted:lyinpowderform.Rapidlyburningsubstances(forexamplebenzoicacid)mustnotundergocombus-tioninlooseform.Benzoicacidmustonlybeburnedintheformbecompressedintopelletsbeforecombustion.Oven-drydustandpowdersuchaswoodchips,hay,strawetc.burninanexplosivemanner!Theyquidswithalowvaporpressuremustnotbecomeindirectcontactwiththecottonthread(e.g.tet-ramethyldihydrogendisiloxan).Rapidlyburningsubstancestendtosquirt.Suchsubstancesmustbepressedintotabletsbe-forecombustion.Suitableforthisise.g.theIKA®-pelletingpressC21,see„Accessories“.Mostliquidsubstancescanbeweigheddirect-lyintothecrucible.Liquidsubstancesexhibitingturbidityorcontainingwaterthatwillsettleoutmustbedriedorhomogenizedbeforetheyareweighedin.Thewatercontentofthesesamplesmustbedetermined.Highlyvolatilesubstancesarecedincombus-tioncapsules(gelatincapsulesoracetobutyratecapsules,see„Accessories“)andundergocom-bustiontogetherwiththecapsules.
Forsubstanceswithlowflbilityorlowcalorificsubstancesusecombustionaids(see„Accessories“).Beforethecapsulesorthecom-bustionbagisfilledwiththesubstancetobedetermined,itmustbeweighedinordertode-terminetheadditionalextraneousenergyintro-aidshouldbeaslittleaspossible.Undertheconditionsthatprevailduringcalori-metricmeasurements,sulfurandnitrogenun-dergocombustionandformSO2,SO3andNOX.Sulfuricandnitricacidariseincombinationwiththewaterresultingformcombustion.Heattakenintoconsiderationincalculatingthegrosscalorificvalue.Inordertotativelyrecordanddetermineallacidsthathavebeenformed,about5mlofdistilledwateroranothersuitablesubstancecanbeaddedtothepositionvesselbeforetheexperiment.Thecalibrationofthesystemmusthavebeenperformedinaccordancewiththeinstructions!Aftercombustion,thewaterthatwasadded,iscollectedandthepositionvesselisrinsedthroughlywithdistilledwater.Therinsingwaterandthesolutionformedfromthewaterthatwascombinedsolutionisexamined.Ifthesulfurcon-tentofthecombustionaidandthenitricacidcor-rectionareknown,thewaterdoesnotneedtoToincreasetheservicelifeofpartstowearandtear(Orings,sealsetc.)we workwithwateraddedtotheexperimentasamatterofgeneralprinciple.Substanceswithhighhalo-gencontentmustnotbecombustedintheC positionvessel;insteadusetheC positionvessel.CompleteTocorrectlydeterminethegrosscalorificvalue,periment,thecrucibleandallsolidresiduesmustbeexaminedforanysignsthatcombustionwasnotcomplete.isnotpossibletoensurecompletecombustion.Substanceswithlow bility
withahighcontentofmineralcompletecombustiononlywiththeaidofcom-bustioncapsulesorcombustion
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