1、INTERNATIONA1.STANDARDISO975editionFifth2O21-1.2Browncoa1.sand1.ignites一Determinationofyie1.dofbenzene-so1.ub1.eextractSemi-automaticmethodCharbonsbrunset1.ignitesDeterminationdurendementenextraitdebenzeneso1.ub1.eMethodeSembautomatiqueRSacncciW1.(E)ISO2021COPYRIGHTPROTECTEDDOCUMENTISO2021IUirhM*hed
2、bdi1.iUedotherwiseupdhi.o啪InyM1.ttti0oemhxitronioktu-Dkirietf1.vMqnIrHHBt1.Onmaytheinternetoranintranet,withoutpriorwrittenpermission.PermissioncanberequestedfromeitherISOattheaddressbe1.oworISOsmemberbodyinthecountr)oftherequester.f),WVfifiU81.andonnet8CH-1214Vernier,GenevaPhone：M1.22749O1.11觥曲ite：
3、图洲跳触OQrgPub1.ishedinSwitzer1.andContentsPageForeword_ivIntroductionv2 Scope13 Normativereferences14 Termsanddefinitions15 P6 Reagent17 Apparatus18 Preparationofsamp1.e2Pre1.iminaryadjustmentOfinstrument28.1 Adjustmentoftheextractiontemperature28.2 Se1.ectionofperiodsofextraction,rinsingandevaporatio
4、n一.29I。Ca1.cu1.ationandexpressionofresu1.ts3Precision410.1Repeatabi1.ity1.imit41110.2Reproducibi1.ity1.imit4TeeStreport4ForewordISO(theInternationa1.OrganizationforStandardization)isawor1.dwidefederationofnationa1.standardsttiugh(ISOmrtm匕0)bMdmi)rwcekdHPfff1.QbbGgbodyI1tf1.nmtiJMiai6sndrifc3owhtd1.y
5、sQcchit2committeehasbeenestab1.ishedhastherighttoberepresentedonthatcommittee.Internationa1.organizations,governmenta1.andnon-governmenta1.,in1.iaisonwithISO,a1.sotakepartinthework.ISOco1.1.aboratesc1.ose1.ywiththee1.ectrotechnica1.standardization.Internationa1.E1.ectrotechnica1.Commission(IEC)ona1.
6、1.mattersofTheproceduresusedtodeve1.opthisdocumentandthoseintendedforitsfurthermaintenanceareof1.SO1.EC(VifY1的Mtheeditoria1.ru1.esoftheISO/IECDirectives,Part2(secwww.iso.org/direc1.ives).时歌Onrightsd随秘姐n棍蜘琳蛾ns由能献吸灰创微盘口府doc1.三棉犯鼠跟监ssubjectofanypatentrightsidentifiedduringthedeve1.opmerUW4iouwMM41.bein
7、theIntroductionand/orontheISO1.istofpatentdec1.arationsreceived(seewww.iso.org/patents).Anytradeusedinthisconstitutenameendorsement,documentisinformationgivenfortheconvenienceofusersanddoesnotForanexp1.anationofthevo1.untarynatureofstandards,themeaningofISOspecifictermsandU明泉加OrRan里幅5悯SaSS忠!S窿inwJ憎f
8、tknBar池部Udead焦es地ww.isO.orgisoforeword.htm1.帏田。祈盼册5肽炉spreparedbyTechnica1.CommitteeISO/TC27,Coa1.andcoke1.SubcommitteeSC5,Thisfiftheditioncance1.sandrep1.acesthefourthedition(ISO975:2013),ofwhichitconstitutesaminorrevision.Thechangescomparedtothepreviouseditionareasfo1.1.ows： referenceddocumentshave
9、beenupdated; termsanddefinitionshavebeenadded; samp1.ehasbeenadded; ca1.cu1.ationandexpressionofresu1.tshavebeenamended； precisionhasbeenamended; testreporthasbeenamended.AnyfeedbackorquestionsonthisdocumentShWUd跖小毛&:皿。th。use1.inationa1.standardsbody.Acomp1.ete1.istingofthesebodiescanbefoundatwww.is
10、o.org/members.htm1.IntroductionThedeterminationofyie1.dofbenzene-so1.ub1.eextractiscarriedoutusingasemi-automaticinstrument;C间UtjQeIocMtininginwrnuiiU)itt&rin!raiificevaaMt2rtiM1.iAJ1.y.1.ongasthesamp1.eisputintheextractionBrowncoa1.sand1.ignitesDeterminationofyie1.dofbenzene-so1.ub1.eextractSemi-au
11、tomaticmethod1 ScopeThisdocumentspecifiesasemi-automaticmethodfordeterminationoftheyie1.dofbenzene-so1.ub1.e2(tractNd11bativere11fpeses.阙网帆神眼9fAhtsQwnt.蚓则nref.cFg/ObPIECE1.ectropedia:avai1.ab1.eathttps:/www.e1.ectropedia.org/4 Princip1.eAtestportionofthebrowncoa1.or1.igniteisextractedwithbenzeneinas
12、emi-automaticextraction,irt11niIteofs(HvnBewethb1.ereHXtvecib5,cUf1.ptawdndthBtbriut6oidueresidueafa*ri9tgurtdriass.reportedonthedrybasis.5 Reagent5.1Benzene,ofana1.ytica1.reagentgrade,p20=0,876gm1.,disti1.1.ationrange80to81,At1.east1vtenzenier,Ys8e11ammab1.eandtoxicbyinha1.ation,ingestionorskinabso
13、rption.Thetestmustbecarriedoutinahoodandthebenzenemustberecoveredascomp1.ete1.yaspossib1.e.6 Apparatus6.1 Semi-automaticextractioninstrument,containingmain1.ytwounits:thecontinuousconsistsOf100m1.deviceandthecontro1.1.er.Theandacondenser.Thedericeextrac1.ion-cvaporationconica1.f1.ask,anextractionCha
14、mbercontinuousextrac1.ion-evaporationcharnberISO2021-AHrightsreserved1Ifc(IaQthmmvta丽SndSfHhcdininrdnnd1.aiftts111.itapnetidn(Iauieratvrttarqutfkbt1.thttiighextivrtaodnchamber.12madeE3ftWtftyftthimb1.er25mmdiameterX80mm1.ength.Ce1.1.u1.oseorotherthimb1.esarepurchasedCutfi1.terpaperintopiecesof75mm75
15、mm(1.arge)and25mm25mm(sma1.1.).Moistenone1.arge徐吸曲珈随曲器ers格帅艇MedPi酰身驶孤般M那命眇。怵用臃Xte询(IM品isnex1.褪%edandro1.1.edontothebottom.Three1.argepiecesandtwosma1.1.piecesarethenro1.1.eda1.ternate1.yontothetesttube.Removetheformedmoistthimb1.ebyb1.owingatthemouthofthetest1.ubeanddryitinairorinanovenat100.6.3 Air
16、oven,capab1.eofmaintainingatemperaturebetween105and110oC1.orvacuumoven,e1.ectrica1.1.ymaintained.heatedrinwhichatemperatureof802andapressureofabout50kPacanbe6.4 Ana1.ytica1.ba1.ance,withareso1.utionof0,1mgorbetter.7 Preparationofsamp1.eThesamp1.esha1.1.bethegenera1.ana1.ysistestsamp1.e,preparedtoano
17、mina1.topsizeof212mbythepreparationproceduresspecifiedinISO139094orISO18283.Thesamp1.eshou1.dbebroughtinmoistureequi1.ibriumwiththe1.aboratoryatmospherebyexposureinathin1.ayeronatray.Exposuretimesha1.1.bekepttoaminimum.Thesamp1.esha1.1.bethorough1.ymixedimmediate1.ybeforeana1.ysis,preferab1.ybymecha
18、nica1.means.Dup1.icatedeterminationsofmoisturefromthesame1.estsamp1.esha1.1.beconductedconcurrent1.ywiththedetenninationoftheyie1.dofbenzene-so1.ub1.eextractbythemethodspecifiedinISO5068-2.8 Pre1.iminaryadjustmentOfinstrument8.1 AdjustmentoftheextractiontemperatureP1.aceanextractionthimb1.evrithabou
19、t2gofcoa1.samp1.eintheextractionchamber.Add60m1.MUeribfHbeaGndMHhectov血tiipf1.a或aSnnebiUtbt1.1.Ihgkextthction-evaporatioixttarateSwitchAfemHHrautomatica1.1.y1.oweredunti1.theHaskisimmersedinthewaterbathandthewaterhathstartsheating.sthefirstdropofcondensedbenzenedripsfromthecondenseradjustthetemperat
20、ureofthewaterfe由由heb明阳峰&务期魂ReCoreM甜酬廊Pn而用和屈帕。制加睛硼蝴Fecontro1.1.er.Thistemperatureshou1.dbereadjustedforchangedambienttemperature.8.2 Se1.ectionOfperiodsofextraction,rinsingandevaporationIngenera1.,thesuitab1.eperiodsofextraction,rinsingandevaporationare,respective1.y,180min,10minImd橘)cio1.i1.%屿EmMgnt
21、diiP枷RrtHS)htheexcTO例yttngbaimBb汕ptest阳efs,IrigidjuettnBnufoftheextractionperiodmaybenecessitatedinordertoensurethecorrectend-pointOtextraction1whichistohejudgedbytheco1.our1.essnessofthe1.astdropsofextractso1.ution.8.3 Procedureextractionthimb1.e(6.2)andcoverwithapadofabsorbentcotton,whichisfitteds
22、nug1.yonthewa1.1.ofAddmg),m1.to70m1.Ofbenzenetoaprevious1.ydriedf1.askofknownmass(determinedtothenearestPerfornionthetheexperimentaccordancedowntheprogrammesequence:Theinstrumentwi1.1.automatica1.1.yheatingpre1.iminaryadjustmentstartedsimu1.taneous1.y,aninc1.inedpositionpermittingref1.uxing.Thewater
23、betwcenthroughbathextractionChambertheandextractioncondenser,benzenecondensedandAfter180thebath.Thetemperaturetime,extractionchamberextractionistemperatureWhichf1.owstheaskbythecondensedbenzene.Thisistherinsingstage.vapourcondensesinthecondenserandf1.owstothereceiver.Thestageofevaporationstarts,term
24、inated.dryingsdoesConstancyin0,001isconsideredtohavebeenachievedwhenthedifferencebetweensuccessive9 Ca1.cu1.ationandexpressionofresu1.ts9.1m2mzTransferamassofabout2g(determinedtothenearest0,1mg)ofgenera1.ana1.ysistestsamp1.etothethethimb1.e.P1.acetheextractionthimb1.ewithsamp1.eintheextractionchambe
25、r(6.1).0460Assemb1.etheinstrument.Switche1.ectrica1.inpower.Pushwithfo1.1.owingbutton. Theextraction-evaporationdeviceis1.oweredunti1.thef1.askisimmersedinthewaterbathasinofthewaterbathisandthecondenser Whentheextractiontemperatureprevious1.ysetisreached,thepumpbeginstocircu1.atethehotf1.askpassesth
26、etheandthejacketofreachesthechamher.Thewhereitisvapourfromthedripsontothethimb1.e.Theextractionstageisthusinprogress.backtominforanOtherWiSesetofthethepumpstopsanddropsafinished.Hotwaterthebenzenevapourcanon1.yreachtheextractionchamberandcondensesthere.Thusarinsingactionisachieved,bymeansofwhichtheb
27、enzene-so1.ub1.eextractadheredtothewa1.1.iswasheddowninto After10min,rinsingisfinished.Thecondenserisautomatica1.1.ychangedtoaninvertedpositionpermittingdisti1.1.ation.Thepumpworksagainsoastoresumehot-watercircu1.ation.Thebenzene After50minOfevaporationisfinished,theextraction-evaporationsystemise1.
28、evatedtotheorigina1.position,permittingthef1.asktobedetachedfromtheextractionchamber.Theprogrammeisthus Detachthef1.askwithso1.ub1.eresidue.Dryitintheairoven(6.3)maintainedat105to110orinthevacuumoven(6.3)maintainedat802andabout50kPatoconstantmassaftera1.1.owingittocoo1.toambienttemperature.NOTEexcee
29、dmassg.percent,isgiven瑞:OrmUIa(1):WEqd=Theyie1.dofbenzene-so1.ub1.eextract,inthegenera1.ana1.ysistestsamp1.e,expressedasawheremiisthemass,ingrams,ofbenzene-so1.ub1.eextract;isthemass,ingrams,ofthetestsamp1.e；9.2 100isconversionfactorfromdimension1.essmassfractiontopercent,in%.Theyie1.dspressedonthed
30、rybasis,IvEd=WEQd100Wrudv,d,isgivenbyFormu1.a(2):(2)whereisthemassfractionofmoisture,inpercent,ofthegenera1.ana1.ysistestsamp1.e.9.3 -thenearestresuIt%.(themeanofdup1.icatedeterminations,see10.1)sha1.1.bereportedonthedrybasisto10Precision10.1 Repeatabi1.ity1.imitTheresu1.tsofdup1.icatedeterminations
31、carriedoutinthesame1.aboratorybythesameoperatorwithttaareis11ppvhuaHthrtdiftrsfti)rtinte!thdrtbfet11iue5i115iernpt3ta1.pbtibnitrr,fchkwnftorWbsahie10.2Reproducibi1.ity1.imitThemeansoftheresu1.tsOfdup1.icatedeterminations,carriedoutineachoftwodifferent1.aboratories,toa1.1.rutIffenbydffibrbpothort8Ko
32、iuesfi1.hnthqTabksamp1.epreparation,Tab1.e1Repeatabi1.ity1.imitandreproducibi1.ity1.imitTestparameterIVE.dMaximumacceptab1.edifferencesbetweenresu1.tsRepeatabi1.ity1.imitrReproducibi1.ity1.imitR5toIOincIusive0,5%abso1.ute0,7%abso1.utemorethan105%ofthemeanresu1.t7%ofthemeanresu1.t11TestreportThetestreportsha1.1.inc1.udethefo1.1.owinginformation：a) identificationofthesamp1.etested;b) themethodusedbyreferencetothisdocument,i.e.ISO975:2021;c) thedateofthedetermination;d) theresu1.tsandthemethodofexpressionused.ICS73.040
