1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS 5202-1:2000 ISO 2817:1
2、999 ICS 65.160 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Methods for chemical analysis of tobacco and tobacco products Part 1:Determination of silicated residues insoluble in hydrochloric acidThis British Standard, having been prepared under the direction of the Consumer
3、 Products and Services Sector Committee, was published under the authority of the Standards Committee and comes into effect on 15 April 2000 BSI 04-2000 ISBN 0 580 32780 9 BS 5202-1:2000 Amendments issued since publication Amd. No. Date Comments National foreword This British Standard reproduces ver
4、batim ISO 2817:1999 and implements it as the UK national standard. It supersedes BS 5202-1:1975 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee AW/40, Tobacco and tobacco products, which has the responsibility to: aid enquirers to understand the text;
5、 present to the responsible international/European committee any enquiries on the interpretation, 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
6、can be obtained on request to its secretary. Cross-references The British Standards which implement international or European 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 t
7、he “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport 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 fro
8、m legal obligations. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, page ii, pages 1 to 6, an inside back cover and a back cover. The BSI copyright notice displayed in this document indicates when this document was updated.A Referencenumbe r ISO281
9、7:1999(E) INTERNATIONAL STANDARD ISO 2817 Secondedition 19990715 Tobaccoandtobaccoproducts Determinationofsilicatedresidues insolubleinhydrochloricacid TabacetproduitsdutabacDterminationdesrsidussilicatsinsoluble s danslacidechlorhydrique BS 5202-1:2000ii Foreword ISO (the InternationalOrganizationf
10、orStandardization)isaworldwidefederationofnationalstandardsbodies(ISO memberbodies).TheworkofpreparingInternationalStandardsisnormallycarriedoutthroughISOtechnical committees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhas therighttoberepresentedonthatcommittee.Int
11、ernationalorganizations,governmentalandnongovernmental,in liaisonwithISO,alsotakepartinthework.ISOcollaboratescloselywiththeInternationalElectrotechnical Commission(IEC)onallmattersofelectrotechnicalstandardization. InternationalStandardsaredraftedinaccordancewiththerulesgivenintheISO/IECDirectives,
12、Part3. DraftInternationalStandardsadoptedbythetechnicalcommitteesarecirculatedtoth ememberbodiesforvoting. PublicationasanInternationalStandardrequiresapprovalbyatleast75%ofthememberbodiescastingavote. InternationalStandardISO2817waspreparedbyTechnicalCommitteeISO/TC 126,Tobaccoandtobacco products,S
13、ubcommitteeSC1, Physicalanddimensionaltests . Thissecondeditioncancelsandreplacesthefirstedition(ISO2817:1974),whichhasbeentechnicallyrevised. AnnexAofthisInternationalStandardisforinformationonly. BS 5202-1:20001 TobaccoandtobaccoproductsDeterminationof silicatedresiduesinsolubleinhydrochloricacid
14、1Scope ThisInternationalStandardspecifiesamethodforthedeterminationofthepercentageofhydrochloricacid insolubleextraneoussilicaparticles,especiallyparticlesofsand,intobacco(wholeleaf,cuttobacco,tobacco scrapsanddust)andtobaccoproducts. Itisparticularlyusefultoknowtheproportionoftheseresidues,inthefol
15、lowingcircumstances: whenbuyingtobaccoleaves,inordertocheckthecleanness; beforeprocessingtobaccoandtobaccoproducts. 2Normativereferences The following normativedocumentscontainprovisionswhich,throughreferenceinthistext,constituteprovisionsof thisInternationalStandard.Fordatedreferences,subsequentame
16、ndmentsto,orrevisionsof ,anyofthese publications do not apply. However, partiestoagreementsbasedonthisInternationalStandardareencouragedto investigatethepossibilityofapplyingthemostrecenteditionsofth enormativedocumentsindicatedbelow.For undatedreferences,thelatesteditionofthenormativedocumentreferr
17、edtoapplies.MembersofISOandIEC maintainregistersofcurrentlyvalidInternationalStandards. ISO565,TestsievesMetalwirecloth,perforatedmetalplateandelectroformedsheetNominalsizesof openings. ISO4874, TobaccoSamplingofbatchesofrawmaterialGeneralprinciples . ISO64881, TobaccoDeterminationofwatercontentPart
18、1:KarlFischermethod . 3Termanddefinition ForthepurposesofthisInternationalStandard,thefollowingtermanddefinitionapply. 3.1 hydrochloricacidinsolublesilicatedresidues residual material ofwholeleaforcuttobacco,tobaccoscrapsanddust,obtainedafterincinerationandextractionof hydrochloricacidsolublemateria
19、lundertheconditionsspecifiedinthisInternationalStandard 4Principle Atestportionisincineratedatatemperatureof65 0 C 5 0 C.Theashesareleachedwithhydrochloric acid, then reincineratedat650C 50C.Theresidueisweighed. BS 5202-1:20002 5Reagents Useonlyreagentsofrecognizedanalyticalgradeanddistilledordemine
20、ralizedwaterorwaterofequivalentpurity. 5.1 Hydrochloricacid , c(HCl)=4moll 21 . 6Apparatus Usuallaboratoryapparatusand,inparticular,thefollowing. 6.1 Mufflefurnace ,wellventilated,capableofbeingregulatedat350C 50Cand650C 50C. 6.2 Widemouthflatbottomedcrucible ,inporcelainorplatinum,ofcapacityanddime
21、nsionsappropriatetothe volumeofthetestportion.Ingeneral,crucibleshavingadiameterof5 0 mmto70 mmandaheightof30 mmare suitable. 6.3 Screen,witha2mmsizeaperture,inaccordancewithISO565. 6.4 Rapidfilterpaper, ashless,hardened. 1) 6.5 Analyticalbalance ,witharesolutionof0,0001g. 6.6 Mixer. 7Sampling Sampl
22、ingshallhavebeencarriedoutinaccordancewithISO4874. Thesizeofthelaboratorysampleshallbesufficienttoensurethatitisrepresentativeofthebatch. 8Preparationoftestsample Ifnecessary,drythesampletofacilitatethegrinding.Themaximumwatercontentshallbe12%. Grindthelaboratorysampleuntilthewholesamplepassesthroug
23、hthescreen(6.3). Thoroughlymixthegroundsample,preferablybymechanicalmeans. Ifthesampleisnottobeanalysedwithin 4daysafterthepreparation,itshouldbestoredatatemperatureof between0 Cand 5 Cinawidemouthairtightcontainerofsuchacapacitythatth esamplemaybeadequately mixedbyinvertingthecontaineratleasttwiceb
24、eforetakinganysampleforanalysis. 9Determinationofwatercontent Take a test portion fromthepreparedtestsamplefollowingclause8,anddeterminethewatercontentasdescribed inISO64881. Expressthemassfractionofmoisture(watercontent), w 1 ,ofthesampleinpercent. 1)Ithasbeenprovedbyexperience,thatWhatmanGradeNo.5
25、40filterpaperissuitable. WhatmanfilterpaperGradeNo.540thetradenameofaproductsuppliedbyWhatman.Thisinformationisgivenfo rthe convenienceofusersofthisInternationalStandardanddoesnotconstituteanendorse mentbyISOo f this product. Equivalent productsmaybeusediftheycanbeshowntoleadtothesameresults. BS 520
26、2-1:20003 10Procedure 10.1Testportion Weigh,tothenearest0,001g,thecleancrucible(6.2)previouslydriedat650C 50C. From the containertakeapproximately1 0 gofthepreparedtestsample(claus e 8)andspreadituniformlyoverthe bottomofthecrucible. Weighthecrucibleandthetestportiontothenearest0,001g. Themass( m 1
27、)ofthetestportioncanthenbecalculatedbysubtraction. 10.2Determination Placethecruciblecontainingthetestportion(10.1)inthemufflefurnace(6.1)andheattoatemperatureof 350C 50Cuntilthetestportioniscompletelycharred,withoutanyformationofsmoke. Increase the temperature of the furnace to 650 C 5 0 Cforabout3
28、 0 min.Allowittocoolt o350 C 50C , and thenremovethecruciblefromthefurnace.Afterithascooleddowntoambienttemperature,addslowly4 0 mlof hydrochloricacid(5.1),allowingittorundownthewallofthecrucible. CAUTION:Addthefirstfewmillilitrescarefullytoavoidvigorouseffervescence. Stirgentlyfromtimetotimewithagl
29、assrodforabout1 0 min.Filterthecontentsofthecruciblethroughthefilter paper (6.4). Collect all the residueonthefilter.Usearubbertippedglassrodtoremoveanyresiduestilladheringto thesidesofthecrucible.Rinsethecruciblewithabout2 5 mlofwaterandfilter.Carefullywashtheresidueonthe filterpaperseveraltimeswit
30、habout25mlofwater,untilneutralpH. Placethefilterpapercontainingtheresidueinthecrucible(6.2)andtransferthecrucibleintothemufflefurnace (6.1),thetemperatureofwhichshallbelessthan20 0 C.Heatto65 0 C50 Cfor30min .Allowittocoolto 350 C50C .Removethecruciblefromthefurnace,transferittoadesiccatorcontaining
31、driedsilicageland allowittocooltoambienttemperature.Weighthecrucibleandresiduetothenearest0,001g. Calculatethemass( m 2 )oftheresidue. 11Expressionofresults Thehydrochloricacidinsolublesilicatedresidue,expressedas themassfraction, w,inpercent,isobtainedbythe equation: w m m w = - 2 1 1 1 100 100% wh
32、ere w 1 isthemassfractionofwater,inpercent,ofthetestportion,asdeterminedaccordingtoclause9; m 1 isthemass(expressedingrams)ofthetestportion; m 2 isthemass(expressedingrams)oftheresidue. BS 5202-1:20004 12Precision 12.1Interlaboratorytest Detailsofaninterlaboratorytestontheprecisionofthemethodaresumm
33、arizedinannex A.Thevaluesderived fromthisinterlaboratorytestmaynotbeapplicabletoconcentrationrangesandmatricesotherthanthosegiven. 12.2Repeatability (r) The absolute difference between two independent single testresults,obtainedusingthesamemethodonidentical testmaterialinthesamelaboratorybythesameop
34、eratorusingthesameequipmentwithi na short interval of time, willinnotmorethan5%ofcasesbegreaterthan: level0%: r =0,12 level5%: r =0,35 level10%: r=0,47 12.3Reproducibility (R) Theabsolutedifferencebetweentwosingletestresults,obtaine dusingthesamemethodonidenticaltestmaterial indifferentlaboratoriesw
35、ithdifferentoperatorsusingdifferentequipment,willinnotmorethan 5 %ofcasesbe greaterthan: level0%: R=0,12 level5%: R=0,83 level10%: R =1,73 13Testreport Thetestreportshallspecify: allinformationnecessaryforthecompleteidentificationofthesample; thesamplingmethodused,ifknown; thetestmethodused,withrefe
36、rencetothisInternationalStandard; alloperatingdetailsnotspecifiedinthisInternationalStandard(i n particular the temperature of incineration if it wasdifferentfrom650 C 50 C),orregardedasoptional,togetherwithdetailsofanyincidentswhichmay haveinfluencedthetestresult(s); thetestresult(s)obtained; ifthe
37、repeatabilityhasbeenchecked,thefinalquotedresultobtained. BS 5202-1:20005 AnnexA (informative) Interlaboratorytest Aninternationalcollaborativestudyinvolving12laboratories,4samplesand5repeatswasorganizedby ISO/TC126/SC1in1996.Theresultsobtainedweresubjectedtostatistica lanalysisinaccordancewith ISO5
38、72521togivetheprecisiondatashowninTableA.1. TableA.1Statisticalresultsoftheinterlaboratorytest (incinerationatthetemperatureof650C 50C) Proportionofaddedsilicaintobacco 0% 5% 10% Numberofparticipatinglaboratoriesaftereliminatingoutliers 7 9 10 Meanvalueofsilicatedresiduecontent,%,ondrymatter 0,51 5,
39、56 10,33 Repeatabilitystandarddeviation, s r 0,04 0,12 0,17 Coefficientofvariationofrepeatability,% 8,21 2,22 1,61 Repeatabilitylimit, r (2,8 s r ) 0,12 0,35 0,47 Reproducibilitystandarddeviation, s R 0,04 0,29 0,61 Coefficientofvariationofreproducibility,% 8,21 5,30 5,92 Reproducibilitylimit, R (2,
40、8 s R ) 0,12 0,83 1,73 NOTE Theresultsgivenabovewereobtainedatthetemperatureo f incineration of 650 C 5 0 Cwhichisthetemperature adoptedinthisInternationalStandard.However,comparativeinterlaboratorytestsindicatedthattheresultsobtainedatan incinerationtemperatureof850C 50Cwerenotstatisticallydifferen
41、tatthe95%probabilitylevel. BS 5202-1:20006 Bibliography 1ISO 57252:1994, Accuracy(truenessandprecision)ofmeasurementmethodsandresultsPart2:Basic methodforthedeterminationofrepeatabilityandreproducibilityofastandardmeasurementmethod . 2ISO/IE CGuide25:1990, Generalrequirementsforthecompetenceofcalibr
42、ationandtestinglaboratories . BS 5202-1:2000BS 5202-1:2000 ISO 2817:1999 BSI 389 Chiswick High Road London W4 4AL | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | |
43、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | 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 revision. 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 any
