BS ISO 15672-2000 Rubber and rubber additives - Determination of total nitrogen content using an automatic analyser《橡胶和橡胶添加剂 采用自动分析仪对含氮总量的测定》.pdf

1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS ISO 15672:2000 ICS 83.

2、040.20; 83.060 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Rubber and rubber additives Determination of total nitrogen content using an automatic analyserThis British Standard, having been prepared under the direction of the Sector Committee for Materials and Chemicals , w

3、as published under the authority of the Standards Committee and comes into effect on 15 October 2000 BSI 10-2000 ISBN 0 580 36516 6 BS ISO 15672:2000 Amendments issued since publication Amd. No. Date Comments National foreword This British Standard reproduces verbatim ISO 15672:2000 and implements i

4、t as the UK national standard. The UK participation in its preparation was entrusted to Technical Committee PRI/23, Chemical testing of rubber, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the inte

5、rpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards wh

6、ich implement international publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport

7、to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover

8、, the ISO title page, pages ii and iii, a blank page, pages 1 to 5 and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued.INTERNATIONAL STANDARD ISO 15672 Firstedition 2000-07-15 Referencenumber ISO15672:2000(E) Rubberandrubberadditives Dete

9、rminationoftotalnitrogencontent usinganautomaticanalyser Caoutchouc et additifs pour caoutchouc Dosage de lazote total laide dun analyseur automatiqueISO15672:2000(E) ii ISO15672:2000(E)iii Foreword ISO(theInternationalOrganizationforStandardization)isaworldwidefederationofnationalstandardsbodies(IS

10、O memberbodies).TheworkofpreparingInternationalStandardsisnormallycarriedoutthroughISOtechnicalcom- mittees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhasthe righttoberepresentedonthatcommittee.Internationalorganizations,governmentalandnon-governmental,inliai- son

11、withISO,alsotakepartinthework.ISOcollaboratescloselywiththeInternationalElectrotechnicalCommission (IEC)onallmattersofelectrotechnicalstandardization. InternationalStandardsaredraftedinaccordancewiththerulesgivenintheISO/IECDirectives,Part3. DraftInternationalStandardsadoptedbythetechnicalcommittees

12、arecirculatedtothememberbodiesforvoting. PublicationasanInternationalStandardrequiresapprovalbyatleast75%ofthememberbodiescastingavote. AttentionisdrawntothepossibilitythatsomeoftheelementsofthisInternationalStandardmaybethesubjectof patentrights.ISOshallnotbeheldresponsibleforidentifyinganyorallsuc

13、hpatentrights. InternationalStandardISO15672waspreparedbyTechnicalCommitteeISO/TC45, Rubber and rubber products, SubcommitteeSC2, Testing and analyses.INTERNATIONALSTANDARD ISO15672:2000(E)1 RubberandrubberadditivesDeterminationoftotalnitrogen contentusinganautomaticanalyser WARNINGPersonsusingthisI

14、nternationalStandardshouldbefamiliarwithnormallaboratorypractice. Thisstandarddoesnotpurporttoaddressallofthesafetyproblems,ifany,associatedwithitsuse.Itisthe responsibilityoftheusertoestablishappropriatesafetyandhealthpracticesandtoensurecompliancewith anynationalregulatoryconditions. 1Scope ThisIn

15、ternationalStandardspecifiesaninstrumental(automaticanalyser)methodforthedeterminationoftotal nitrogeninrubberandrubberadditives. 2Termsanddefinitions ForthepurposesofthisInternationalStandard,thefollowingtermsanddefinitionsapply. 2.1 sample unitselectedtorepresentthematerialtobeanalysed 2.2 testpor

16、tion actualmaterialusedintheanalysis 2.3 controlsample materialwitharecognizedlevelofnitrogen,analysedwitheachsetoftestportions 3Principle 3.1Specifiedisareliable,rapid,instrumental(automatic)methodfordeterminingtotalnitrogeninrubberandrub- beradditives.Thenitrogenisdeterminedbyasingleinstrumentalpr

17、ocedureconsistingofweighingatestportion, placingitintheinstrumentandinitiatingthe(subsequentlyautomatic)analyticalprocess.Theanalysismaybecon- trolledmanuallytoalimiteddegree,andacapabilitytoperformcomputationsautomaticallymaybeprovidedbythe instrumentusedtoperformtheanalysis. 3.2Theactualprocesscan

18、varysubstantiallyfrominstrumenttoinstrumentbecauseavarietyofmeanscanbe usedtomeettheprimaryrequirementsofthemethod.Themethodincludesthefollowing: a)conversionofnitrogen-containingmaterialstonitrogenoxidesinanoxygenstream; b)reductionofthenitrogenoxidestoelementalnitrogenbypassingthemovercopperatanel

19、evatedtemperature; c)determiningthenitrogenbyoneofthreedetectionschemes. 3.3Inthethermalconductivitydetectionconfiguration,thecombustiongasesareconductedthroughaseriesof thermalconductivitydetectorsandgasabsorbersalignedsothatthegasespassfirstthroughthesamplesideofa watervapourdetector,throughawater

20、vapourabsorberandthroughthereferencesideofthedetector.Thegases arethenconductedthroughthesamplesideofacarbondioxidedetector,throughacarbondioxideabsorberandISO15672:2000(E) 2 throughthereferencesideofthedetector.Finally,theresultantgases,whichcontainonlynitrogenandthecarrier gas,passthroughthesample

21、sideofanitrogendetectorandarevented.Forthisdetector,high-puritycarriergasis usedasthereferencegas.Inthisway,thedetectorsdeterminethethermalconductivitiessolelyofthespecifiedcom- ponents. 3.4Inthecombinedabsorbance/conductivitydetectionconfiguration,thecarbondioxideandwatervapourare determinedbyinfra

22、reddetection,usinganaliquotofthecombustiongasesfromwhichonlythehalidesandsulfurox- ideshavebeenremoved.Thesedetectorsdeterminetheinfraredabsorbanceofthepertinentgasesatprecisewave- lengthwindowssothattheabsorbancesresultfromonlythespecifiedcomponents.Insuchasystem,nitrogenis determinedbythermalcondu

23、ctivity,usingasecondaliquotofthegasesadditionallytreatedtoreducethenitrogen oxidestonitrogenandtoremovetheresidualoxygen,carbondioxideandwatervapour. 3.5Inthemodifiedchromatographicdetectionconfiguration,whichisessentiallyamodifiedgaschromato- graphicsystem,thenitrogen,carbondioxideandwatervapourint

24、hetreatedcombustiongasesareelutedfroma chromatographiccolumnanddetermined(atappropriateretentiontimes)bythermalconductivitydetection. 3.6Theconcentrationofnitrogeniscalculatedineachconfigurationasafunctionofthefollowing: a)themeasuredinstrumental(automaticanalyser)responsesperunitmassforelementalnit

25、rogen(establishedvia instrumentcalibration); b)themassofthetestportion. 4 Requirementsforapparatus 4.1Becauseavarietyofinstrumental(automaticanalyser)componentconfigurationscanbeusedsatisfactorilyfor thismethod,nospecificationsarepresentedwithregardtooverallsystemdesign.Functionally,however,thefollo

26、w- ingrequirementsarespecifiedforallinstruments. 4.2Theconditionsforcombustionofthesampleshallbesuchthat(forthefullrangeofapplicablesamples) nitrogen-containingcomponentsshallbeconvertedcompletelytonitrogenornitrogenoxides.Generalinstrumental conditionsthataffectcompletecombustioninclude: a)availabi

27、lityoftheoxidant; b)temperature; c)time. 4.3Representativealiquotsofthecombustiongasesshallthenbetreatedtoreducenitrogenoxidestoelemental nitrogen. 4.4Fortheconfigurationdescribedin3.3,halides,sulfuroxidesandresidualoxygenareremovedwhenwater,car- bondioxideandnitrogenaredeterminedsequentially. 4.5Fo

28、rtheconfigurationdescribedin3.4,inwhichnitrogenisdetermined,water,carbondioxideandresidualoxy- genareremoved. 4.6Fortheconfigurationdescribedin3.5,halidesandsulfuroxidesareremoved. 4.7Thedetectionsystemshalldeterminenitrogenwithoutinterference. 4.8Thedetectorshouldideallyprovidealinearresponsethatco

29、rrelatesdirectlywithnitrogenconcentrationover thefullrangeofpossibleconcentrationsfromtheapplicabletestsamples. 4.9Thesystemshallincludeprovisionsforevaluatingnonlinearresponseappropriately,sothatnonlinearre- sponsescanbecorrelatedaccuratelywithconcentration.Suchprovisionscanbeintegralwiththeinstrum

30、entorbe providedby(auxiliary)computationschemes. 4.10Finally,exceptforthosesystemsinwhichthenitrogenconcentrationisexpressedasadirectoutput,thein- strumentshallincludeanappropriatedetectorresponsereadoutdevice.ISO15672:2000(E)3 5Reagents Reagentgradechemicalsshallbeusedinallanalyses,unlessotherwisei

31、ndicated. 5.1Helium,carriergas,asspecifiedbytheinstrumentmanufacturer. 5.2Oxygen,asspecifiedbytheinstrumentmanufacturer. 5.3Additionalreagents,asspecifiedbytheinstrumentmanufacturer. Thisspecificationreferstothereagentsusedtomeettherequirementscitedin3.3to3.5.Thesereagentscanvary substantiallyfordif

32、ferentinstruments;inallcases,however,thereagentsspecifiedbythemanufacturershallbe used. 6Instrument(automaticanalyser)preparationandcalibration 6.1Assembletheinstrumental(automaticanalyser)systeminaccordancewiththemanufacturersinstructions. 6.2Fortheresponse(drift)adjustment,weighandanalyse(inaccord

33、ancewiththemanufacturersinstructions)an appropriatetestportionofthenitrogencalibratingagent.Repeatthisprocedure,adjustinginstrumentresponseas recommendedbythemanufacturer,untiltheabsenceofdriftisindicated. 6.3Forthecalibration,selectcalibratingagentsandmaterialsspecifiedbythemanufacturerthathavecert

34、ified nitrogencontentslyingwithintherangeofthoseofthesamplestobeanalysed.Atleastthreesuchcalibratingagents arerecommendedforeachrangeofnitrogencontentstobedetermined.Whenpossible,twoofthecalibratingagents shallbrackettherangeofnitrogencontentstobedetermined,withthethirdfallingwithintherange. 6.4Fort

35、hecalibrationprocedure,analyseportionsofthecalibratingagentchosen(see6.3)torepresentthe nitrogencontentinthesamplestobetested.Continueanalysinguntiltheresultsfromfiveconsecutivedetermina- tionsfallwithintherepeatabilityinterval(see9.3)ofthismethod.Calibratetheinstrumentinaccordancewiththe manufactur

36、ersinstructionsusingthesevalues.Theresultsobtainedshallbewithintheprecisionlimitsstatedforthe calibratingagent,otherwisethecalibrationprocedureshallberepeated. 6.5Fortheperiodiccalibrationverificationandrecalibration,analyseacontrolsampleonaperiodicbasis.There- sultsobtainedforthecontrolsampleshallb

37、ewithinestablishedlimits.Ifnot,allresultsobtainedsincethelast successfulcontrolcheckshallberejectedandthecalibrationprocedurerepeated. 7Procedure Analyseatestportionofthesampleinaccordancewiththemanufacturersinstructions. Carryouttheanalysisinduplicate. 8Calculation Calculatethepercentnitrogen asfol

38、lows: where isthedetectorresponsefornitrogen; isthedetectorresponseperunitmassestablishedfornitrogenduringcalibration; N N= B C m 100% B CISO15672:2000(E) 4 isthemassofthetestportion,ingrams. 9Precision 9.1Althoughtheprecisionofthismethodwascalculatedfromdataobtainedfromtheanalysisofbituminouscoal t

39、hatcontainednitrogenintherange to ,itisconsideredtobedirectlyapplicabletotheanalysisfor nitrogeninrubbercompounds.TheprecisionisexpressedintermsasspecifiedinISO/TR9272,onthebasisofa confidencelevelforthevaluesestablishedforrepeatability andreproducibility . 9.2Theprecisiondatagiveninthisclausegivean

40、estimateoftheprecisionofthismethodwiththematerialsused intheparticularinterlaboratorytestprogramme.Theprecisionparametersshallnotbeusedforacceptanceorrejec- tiontestingofanygroupofmaterialswithoutdocumentationthattheparametersareapplicabletotheparticular groupofmaterialsandthespecifictestprotocolsof

41、themethod. 9.3Therepeatability,inpercentnitrogen,hasbeenestablishedasthevalueinTable1.Tworesults,obtainedin onelaboratory(sameinstrument,material,operator)undernormalprocedures,thatdifferbymorethanthistabulated valueshallbeconsideredtohavecomefromdifferentornon-identicalsamplepopulations. 9.4Therepr

42、oducibility ,inpercentnitrogen,hasbeenestablishedasthevalueinTable1.Tworesults,obtained indifferentlaboratories(samematerial,butdifferentinstrumentanddifferentoperator)undernormalprocedures,that differbymorethanthistabulatedvalueshallbeconsideredtohavecomefromdifferentornon-identicalsamplepop- ulati

43、ons. 9.5Biasiseliminatedwhentheapparatusiscalibratedproperlyagainstcertifiedreferencestandards.Propercali- brationincludescomparisonoftestdataoncalibratingagentsthathavecertifiednitrogencontents. 10Testreport Thetestreportshallincludethefollowinginformation: a)areferencetothisInternationalStandard;

44、b)alldetailsnecessaryforidentificationofthesampleanalysed; c)theprocedureused(thermalconductivitydetection,combinedabsorbance/conductivitydetectionormodified chromatographicdetection); d)theduplicatepercentnitrogenresultstothenearest ; e)theinstrument(automaticanalyser)makeandmodel; f) anydeviations

45、fromthemethod; g)thedateoftheanalysis. Table1Nitrogenanalysisprecision Withinlabs Betweenlabs 0,11 0,17 where istherepeatabilitystandarddeviation. where isthereproducibilitystandarddeviation. m 0,69% 1,57% 95% rR r R rR r=2,83 s r s r R=2,83 s R s R 0,1%ISO15672:2000(E)5 Bibliography 1ISO/TR9272:198

46、6, Rubber and rubber products Determination of precision for test method standards.BS ISO 15672:2000 BSI 389 Chiswick High Road London W4 4AL | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | |

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