Course-ASAP2020LaboratoryPracticalExerciseGu

1ASAP2020PHYSISORPTIONLABORATORYPRACTICALEXERCISEGUIDE2TableofContentsASAP2020PHYSISORPTION.......................................................................................1DAY1-INTRODUCTIONTOSAMPLEFILEUSAGEANDSAMPLEPREP.............3LABSession1-Introtosampleprepandsamplefiles..............................................3LABSession3-Initiatingcarbonanalysis.................................................................24LABSession5-PreparingY-Zeoliteforanalysis......................................................28LABSession6-InitiatingSilicaAluminaanalysis.....................................................31DAY2-MICROPOROUSSAMPLESANDSAMPLEPREP......................................31LABSession1-BuildingY-ZeoliteSamplefile.........................................................31LABSession3-Y-Zeoliteseconddegas...................................................................35LABSession4-CreatingentireAluminasamplefile.................................................36DAY3-INDEPENDENTALUMINAANALYSIS.........................................................39LABSession1-AnalyzinganAluminasample.........................................................393DAY1-INTRODUCTIONTOSAMPLEFILEUSAGEANDSAMPLEPREPLABSession1-IntrotosampleprepandsamplefilesPhysiSamplePrepSamplepreparationisthefoundationuponwhichanygood,reliable,reproducibleanalysisisbuilt.WiththeASAP2020veryfewthingscangowronginsamplepreparation.Inthissectionwewillexaminethesecriticalaspects.SampleQuantityTheASAP2020measurespressureandthencomputesvolumeadsorbedasaresultofchangesinpressure.Veryslighterrorsinmeasurementmaybecausedbyminute,inherenttransducererror.Thereisasacrificeofaccuracywhenthetotalamountofsampleinthetesttubeisverylow.Forthehighestaccuracypossible,greateramountsofsampleshouldbeused.Totalsurfaceareaamountsapproaching50m2arenotuncommonforhighlyaccurateanalyses.Remember,however,thatthegreatertheamountoftotalsurfaceareapresentforanalysisthemoretimemustbeallowedfortheanalysis.Youshoulddevelopyourownstandardsasyoudiscoverthebestmethodsforyourneeds.Ofcourse,anyweighingerrors,nomatterhowsmall,aremagnifiedwhenlowsamplemassesareused.Thisiswhyaminimumof0.1gisspecified.Whenanalyzingalightorfluffymaterial,theentireareaofthetesttubewithintheheatingmantlecanbefilledwithsampleinanattempttoattainsufficientsamplemass.Rememberthatthesamplemassinitiallyplacedinthesampletubewillbereducedasaresultoftheremovaloftrappedmoisture(degassing).Itisusuallyagoodideatouse5-20%excesssamplemassthanrequiredsoasufficientmasswillremainafterthesamplehasbeencleaned.Thesealfritisaconvenientmethodtoinsuresamplematerialisnotcontaminatedasitistransferredfromthedegasporttotheanalysisport.Itissimplertousethanarubberstopperandwerecommenditsuseaspartofstandardsamplepreparation.4LAB–InitialSamplePreparationPleaseusethefollowingitems,ananalyticalbalance,andthesampledatasheet(below)toperformthestepsbelow.CleanSampleTubeFillerRodSealFritWeighingSupport5ReferenceMaterial(Carbon)1.Tarethebalancewithweighingsupportinplace.2.Weightheassembledsampletube(includingfillerrodandsealfrit)usingtheweighingsupportforstability.3.Recordthismassonthesampledatasheet.4.Tarebalancewithweighingdish.5.Weighapproximately0.60gramsofCarbonreferencematerial.6.Loadthesampleintothesampletube.7.Insertthesealfritintothetopofthesampletube.8.Prepareasecondsampletube,thistimeusingabout0.25gramsoftheSilica-Aluminareferencematerial.6ASAPSeriesSampleDataRecordSampletube:_____________________Sample:__Carbon_____________BeforeDegas:1.Massofemptysampletubeassembly(sampletube,sealfritandfillerrod)________g2.Massofsampletubeassemblyplussample________g3.Massofsample(Step2)–(Step1)________gAfterDegas:4.Massofsampletubeassemblyplussample________g5.Massofsample(Step4)–(Step1)________gAfterAnalysis:6.Massofsampletubeassemblyplussample________g7.Massofsample(Step6)–(Step1)________gYoumayusetheAfterDegasvalue(Step5)ortheAfterAnalysisvalue(Step7),providedtheyareclosetothesamevalue.Comparethesamplemassobtainedafteranalysis(Step7)withthesamplemassafterdegas(Step5).Thesetwovaluesshouldbecloseinrange.Ifasignificantdifferenceisnoted,analysisproblemsmayexistorthesamplemayhavebeenimproperlydegassed.7ASAPSeriesSampleDataRecordSampletube:_____________________Sample:_SilicaAlumina_______BeforeDegas:1.Massofemptysampletubeassembly(sampletube,sealfritandfillerrod)________g2.Massofsampletubeassemblyplussample________g3.Massofsample(Step2)–(Step1)________gAfterDegas:4.Massofsampletubeassemblyplussample________g5.Massofsample(Step4)–(Step1)________gAfterAnalysis:6.Massofsampletubeassemblyplussample________g7.Massofsample(Step6)–(Step1)________g8TRAININGACTIVITY–UNITSSomeofthevaluesdisplayedbythe2020canbepresentedinavarietyofunits.TheselectionofunitsisfoundintheOptionsmenu.Beforeyoubeginyourotherlaboratoryactivities,youneedtochangeafewofthedefaultunitassignments.PleaseselectUnitsontheOptionsmenuandmaketheUnitSelectionsoutlinedbelow.CLEANINGTHESAMPLEBeforeasamplecanbeanalyzed,thesamplesurfacemustbecleaned.Anyvolatilematerialsadsorbedonthesur