BS ISO 15671-2000 Rubber and rubber additives - Determination of total sulfur content using an automatic analyser《橡胶和橡胶添加剂 采用自动分析仪对含硫总量的测定》.pdf

1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS ISO 15671:2000 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 sulfur content using an automatic analyserThis British Standard, having been prepared under the direction of the Sector Committee for Materials and Chemicals, was

3、published under the authority of the Standards Committee and comes into effect on 15 October 2000 BSI 10-2000 ISBN 0 580 36517 4 BS ISO 15671:2000 Amendments issued since publication Amd. No. Date Comments National foreword This British Standard reproduces verbatim ISO 15671:2000 and implements it a

4、s 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 interpr

5、etation, 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 which

6、 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 to

7、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, t

8、he 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 15671 Firstedition 2000-07-15 Referencenumber ISO15671:2000(E) Rubberandrubberadditives Determi

9、nationoftotalsulfurcontentusing anautomaticanalyser Caoutchouc et additifs pour caoutchouc Dosage du soufre total laide dun analyseur automatiqueISO15671:2000(E) ii ISO15671:2000(E)iii Foreword ISO(theInternationalOrganizationforStandardization)isaworldwidefederationofnationalstandardsbodies(ISO mem

10、berbodies).TheworkofpreparingInternationalStandardsisnormallycarriedoutthroughISOtechnicalcom- mittees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhasthe righttoberepresentedonthatcommittee.Internationalorganizations,governmentalandnon-governmental,inliai- sonwithI

11、SO,alsotakepartinthework.ISOcollaboratescloselywiththeInternationalElectrotechnicalCommission (IEC)onallmattersofelectrotechnicalstandardization. InternationalStandardsaredraftedinaccordancewiththerulesgivenintheISO/IECDirectives,Part3. DraftInternationalStandardsadoptedbythetechnicalcommitteesareci

12、rculatedtothememberbodiesforvoting. PublicationasanInternationalStandardrequiresapprovalbyatleast75%ofthememberbodiescastingavote. AttentionisdrawntothepossibilitythatsomeoftheelementsofthisInternationalStandardmaybethesubjectof patentrights.ISOshallnotbeheldresponsibleforidentifyinganyorallsuchpate

13、ntrights. InternationalStandardISO15671waspreparedbyTechnicalCommitteeISO/TC45, Rubber and rubber products, SubcommitteeSC2, Testing and analyses.INTERNATIONALSTANDARD ISO15671:2000(E)1 RubberandrubberadditivesDeterminationoftotalsulfur contentusinganautomaticanalyser WARNINGPersonsusingthisInternat

14、ionalStandardshouldbefamiliarwithnormallaboratorypractice. Thisstandarddoesnotpurporttoaddressallofthesafetyproblems,ifany,associatedwithitsuse.Itisthe responsibilityoftheusertoestablishappropriatesafetyandhealthpracticesandtoensurecompliancewith anynationalregulatoryconditions. 1Scope ThisInternati

15、onalStandardspecifiesaninstrumental(automaticanalyser)methodforthedeterminationoftotalsul- furinrubberandrubberadditives. 2Termsanddefinitions ForthepurposesofthisInternationalStandard,thefollowingtermsanddefinitionsapply. 2.1 sample unitselectedtorepresentthematerialtobeanalysed 2.2 testportion act

16、ualmaterialusedintheanalysis 2.3 controlsample materialwitharecognizedcontentofsulfur,analysedwitheachsetoftestportions 3Principle 3.1Specifiedisareliable,rapid,instrumental(automaticanalyser)methodfordeterminingtotalsulfurinrubberand rubberadditives.Thesulfurisdeterminedbyasingleinstrumentalprocedu

17、reconsistingofweighingatestportion, placingitintheinstrumentandinitiatingthe(subsequentlyautomatic)analyticalprocess.Theanalysismaybecon- trolledmanuallytoalimiteddegree,andacapabilitytoperformcomputationsautomaticallymaybeprovidedbythe instrumentusedtoperformtheanalysis. 3.2Theactualprocesscanvarys

18、ubstantiallyfrominstrumenttoinstrumentbecauseavarietyofmeanscanbe usedtomeettheprimaryrequirementsofthemethod.Themethodincludesthefollowing: a)conversionofsulfur-containingmaterialstosulfurdioxideinanoxygenstream; b)determinationofthesulfurdioxidebyoneofthreedetectionschemes,andhencethetotalsulfurco

19、ntent. 3.3Inthehydrogenperoxidedetectionconfiguration,thesulfurdioxideisabsorbedinhydrogenperoxide,con- vertingsulfurdioxidetosulfuricacidwhichissubsequentlytitratedwithstandardalkali,enablingthesulfurtobecal- culated.ISO15671:2000(E) 2 3.4Intheiodinesolutiondetectionconfiguration,thesulfurdioxideis

20、absorbedinstandardiodinesolution,re- ducingiodinetoiodidewhichissubsequentlymeasuredbyapolarizeddualplatinumelectrodesystem,enablingthe sulfurtobecalculated. 3.5Inthesulfurdioxidedetectionconfiguration,thesulfurdioxideispassedthroughaninfraredabsorptionde- tectoranddeterminedusingasulfurdioxidestand

21、ard,enablingthesulfurtobecalculated. 4Requirementsforapparatus 4.1Becauseavarietyofinstrumental(automaticanalyser)componentconfigurationscanbeusedsatisfactorilyfor thismethod,nospecificationsarepresentedwithregardtooverallsystemdesign.Functionally,however,thefollow- ingrequirementsarespecifiedforall

22、instruments. 4.2Theconditionsforcombustionofthesampleshallbesuchthat(forthefullrangeofapplicablesamples)sulfur- containingcomponentsshallbeconvertedcompletelytosulfurdioxide.Generalinstrumentalconditionsthataffect completecombustioninclude: a)availabilityoftheoxidant, b)temperature, c)time. 4.3Forth

23、econfigurationdescribedin3.3,acorrectionshallbemadeforaciditywhenchlorineispresentbytitration ofaportionoftheabsorptionsolutionforchloride,whichiscalculatedashydrochloricacidandsubtractedfromthe totalacidity. 4.4Intheiodinesolutionandsulfurdioxidedetectionmethods(3.4and3.5),thedetectionsystemshallde

24、termine sulfurwithoutinterferenceandthedetectorshouldideallyprovidealinearresponsethatcorrelatesdirectlywithsulfur concentrationoverthefullrangeofpossibleconcentrationsfromtheapplicabletestsamples. 4.5Thesystemshallincludeprovisionsforevaluatingnonlinearresponseappropriately,sothatnonlinearre- spons

25、escanbecorrelatedaccuratelywithconcentration.Suchprovisionscanbeintegralwiththeinstrumentorbe providedby(auxiliary)computationschemes. 4.6Finally,exceptforthosesystemsinwhichthesulfurconcentrationisexpressedasadirectoutput,theinstru- mentshallincludeanappropriatedetectorresponsereadoutdevice. 5Reage

26、nts Reagentgradechemicalsshallbeusedinallanalysesunlessotherwiseindicated. 5.1Oxygen,asspecifiedbytheinstrumentmanufacturer. 5.2Additionalreagentsasspecifiedbytheinstrumentmanufacturer. Thisspecificationreferstothereagentsusedtomeettherequirementscitedin3.3to3.5.Thesereagentscanvary substantiallyfor

27、differentinstruments;inallcases,however,thereagentsspecifiedbytheinstrumentmanufacturer shallbeused. 6Instrument(automaticanalyser)preparationandcalibration 6.1Assembletheinstrumental(automaticanalyser)systeminaccordancewiththemanufacturersinstructions. 6.2Fortheresponse(drift)adjustment,weighandana

28、lyse(inaccordancewiththemanufacturersinstructions)an appropriatetestportionofthesulfurcalibratingagent.Repeatthisprocedure,adjustinginstrumentresponse,asrec- ommendedbythemanufacturer,untiltheabsenceofdriftisindicated.ISO15671:2000(E)3 6.3Forthecalibration,selectcalibratingagentsandmaterialsspecifie

29、dbythemanufacturerthathavecertifiedsul- furcontentslyingwithintherangeofthoseofthesamplestobeanalysed.Atleastthreesuchcalibratingagentsare recommendedforeachrangeofsulfurcontentstobedetermined.Whenpossible,twoofthecalibratingagentsshall brackettherangeofsulfurcontentstobedetermined,withthethirdfalli

30、ngwithintherange. 6.4Forthecalibrationprocedure,analyseportionsofthecalibratingagentchosen(see6.3)torepresentthesulfur contentinthesamplestobetested.Continueanalysinguntiltheresultsfromfiveconsecutivedeterminationsfall withintherepeatabilityinterval(see9.3)ofthistestmethod.Calibratetheinstrumentinac

31、cordancewiththemanu- facturersinstructionsusingthesevalues.Theresultsobtainedshallbewithintheprecisionlimitsstatedforthecali- bratingagent,otherwisethecalibrationprocedureshallberepeated. 6.5Fortheperiodiccalibrationverificationandrecalibration,analyseacontrolsampleonaperiodicbasis.There- sultsobtai

32、nedforthecontrolsampleshallbewithinestablishedlimits.Ifnot,allresultsobtainedsincethelast successfulcontrolcheckshallberejectedandthecalibrationprocedurerepeated. 7Procedure Analyseatestportionofthesampleinaccordancewiththemanufacturersinstructions. Carryouttheanalysisinduplicate. 8Calculation Calcu

33、latethepercentsulfur asfollows: where isthedetectorresponseforsulfur; isthedetectorresponseperunitmassestablishedforsulfurduringcalibration; isthemassofthetestportion,ingrams. 9Precision 9.1Althoughtheprecisionofthistestmethodwascalculatedfromdataobtainedfromtheanalysisofbituminous coal,itisconsider

34、edtobedirectlyapplicabletotheanalysisforsulfurinrubbercompounds.Theprecisionisex- pressedintermsasspecifiedinISO/TR9272,onthebasisofa confidencelevelforthevaluesestablishedfor repeatability andreproducibility . 9.2Theprecisiondatagiveninthisclausegiveanestimateoftheprecisionofthismethodwiththemateri

35、alsused intheparticularinterlaboratorytestprogramme.Theprecisionparametersshallnotbeusedforacceptanceorrejec- tiontestingofanygroupofmaterialswithoutdocumentationthattheparametersareapplicabletotheparticular groupofmaterialsandthespecifictestprotocolsofthemethod. 9.3Therepeatability,inpercentsulfur,

36、hasbeenestablishedasthevalueinTable1.Tworesults,obtainedin onelaboratory(sameinstrument,material,operator)undernormalprocedures,thatdifferbymorethanthistabulated valueshallbeconsideredtohavecomefromdifferentornon-identicalsamplepopulations. 9.4Thereproducibility ,inpercentsulfur,hasbeenestablishedas

37、thevalueinTable1.Tworesults,obtainedin differentlaboratories(samematerial,butdifferentinstrumentanddifferentoperator)undernormalprocedures,that differbymorethanthistabulatedvalueshallbeconsideredtohavecomefromdifferentornon-identicalsamplepop- ulations. S S= B C m 100% B C m 95% rR r RISO15671:2000(

38、E) 4 9.5Biasiseliminatedwhentheapparatusiscalibratedproperlyagainstcertifiedreferencestandards.Propercali- brationincludescomparisonoftestdataoncalibratingagentsthathavecertifiedsulfurcontents. 10Testreport Thetestreportshallincludethefollowinginformation: a)areferencetothisInternationalStandard; b)

39、alldetailsnecessaryforidentificationofthesampleanalysed; c)theprocedureused(hydrogenperoxide,iodinesolutionorsulfurdioxide); d)theduplicatepercentsulfurresultstothenearest ; e)theinstrument(automaticanalyser)makeandmodel; f) anydeviationsfromthemethod; g)thedateoftheanalysis. Table1Sulfuranalysispre

40、cision Withinlab Betweenlabs 0,05 0,09 where istherepeatabilitystandarddeviation. where isthereproducibilitystandarddeviation. rR r=2,83 s r s r R=2,83 s R s R 0,1%ISO15671:2000(E)5 Bibliography 1ISO/TR9272:1986, Rubber and rubber products Determination of precision for test method standards.BS ISO

41、15671:2000 BSI 389 Chiswick High Road London W4 4AL | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | |

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