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 | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | |
42、| | | BSI British Standards Institution BSI is the independent national body responsible for preparing British Standards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Revisions British Standards are updated by amendment or revisi
43、on. Users of British Standards should make sure that they possess the latest amendments or editions. It is the constant aim of BSI to improve the quality of our products and services. We would be grateful if anyone finding an inaccuracy or ambiguity while using this British Standard would inform the
44、 Secretary of the technical committee responsible, the identity of which can be found on the inside front cover. Tel: 020 8996 9000. Fax: 020 8996 7400. BSI offers members an individual updating service called PLUS which ensures that subscribers automatically receive the latest editions of standards
45、. Buying standards Orders for all BSI, international and foreign standards publications should be addressed to Customer Services. Tel: 020 8996 9001. Fax: 020 8996 7001. In response to orders for international standards, it is BSI policy to supply the BSI implementation of those that have been publi
46、shed as British Standards, unless otherwise requested. Information on standards BSI provides a wide range of information on national, European and international standards through its Library and its Technical Help to Exporters Service. Various BSI electronic information services are also available w
47、hich give details on all its products and services. Contact the Information Centre. Tel: 020 8996 7111. Fax: 020 8996 7048. Subscribing members of BSI are kept up to date with standards developments and receive substantial discounts on the purchase price of standards. For details of these and other
48、benefits contact Membership Administration. Tel: 020 8996 7002. Fax: 020 8996 7001. Copyright Copyright subsists in all BSI publications. BSI also holds the copyright, in the UK, of the publications of the international standardization bodies. Except as permitted under the Copyright, Designs and Pat
49、ents Act 1988 no extract may be reproduced, stored in a retrieval system or transmitted in any form or by any means electronic, photocopying, recording or otherwise without prior written permission from BSI. This does not preclude the free use, in the course of implementing the standard, of necessary details such as symbols, and size, type or grade designations. If these details are to be used for any other purpose than implementation then the prior written permission of BSI must be obtained. If permission is granted, the terms may include royalty payment
