BS ISO 5796-2000 Rubber compounding ingredients - Natural calcium carbonate - Test methods《橡胶配合剂 天然碳酸钙 试验方法》.pdf

1、 | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS ISO 5796:2000 ICS 83.0

2、40.20 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Rubber compounding ingredients Natural calcium carbonate Test methodsThis British Standard, having been prepared under the direction of the Sector Committee for Materials and Chemicals, was published under the authority of

3、the Standards Committee and comes into effect on 15 November 2000 BSI 11-2000 ISBN 0 580 36694 4 BS ISO 5796:2000 Amendments issued since publication Amd. No. Date Comments National foreword This British Standard reproduces verbatim ISO 5796:2000 and implements it as the UK national standard. The UK

4、 participation in its preparation was entrusted to Technical Committee PRI/50, Rubber raw, natural and synthetic, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for c

5、hange, 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 implement international pu

6、blications 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 include all the necessary p

7、rovisions 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, the ISO title page, pages ii

8、 to iv, pages 1 to 20, an inside back cover and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued.Referencenumber ISO5796:2000(E) INTERNATIONAL STANDARD ISO 5796 Secondedition 2000-09-01 Rubbercompoundingingredients NaturalcalciumcarbonateT

9、estmethods IngrdientsdemlangeducaoutchoucCarbonatedecalciumnaturel MthodesdessaiISO5796:2000(E) ii ISO5796:2000(E)iii Contents Page Foreword.iv 1 Scope1 2 Normativereferences1 3 Sampling.2 4 Methodsoftest2 5 Testreport10 AnnexA(normative)DeterminationoftotalcoppercontentAtomicabsorptionmethod11 Anne

10、xB(normative)DeterminationoftotalmanganesecontentAtomicabsorptionmethod14 AnnexC(normative)DeterminationoftotalironcontentAtomicabsorptionmethod.17 AnnexD(informative)Classificationofnaturalcalciumcarbonateandtypicalphysicalandchemical properties.20ISO5796:2000(E) iv Foreword ISO(theInternationalOrg

11、anizationforStandardization)isaworldwidefederationofnationalstandardsbodies(ISO memberbodies).TheworkofpreparingInternationalStandardsisnormallycarriedoutthroughISOtechnical committees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhas therighttoberepresentedonthatcom

12、mittee.Internationalorganizations,governmentalandnon-governmental,in liaisonwithISO,alsotakepartinthework.ISOcollaboratescloselywiththeInternationalElectrotechnical Commission(IEC)onallmattersofelectrotechnicalstandardization. InternationalStandardsaredraftedinaccordancewiththerulesgivenintheISO/IEC

13、Directives,Part3. DraftInternationalStandardsadoptedbythetechnicalcommitteesarecirculatedtothememberbodiesforvoting. PublicationasanInternationalStandardrequiresapprovalbyatleast75%ofthememberbodiescastingavote. AttentionisdrawntothepossibilitythatsomeoftheelementsofthisInternationalStandardmaybethe

14、subjectof patentrights.ISOshallnotbeheldresponsibleforidentifyinganyorallsuchpatentrights. InternationalStandardISO5796waspreparedbyTechnicalCommitteeISO/TC45,Rubberandrubberproducts, SubcommitteeSC3,Rawmaterials(includinglatex)foruseintherubberindustry. Thissecondeditioncancelsandreplacesthefirsted

15、ition(ISO5796:1990),ofwhichitconstitutesatechnical revision. AnnexesA,BandCformanormativepartofthisInternationalStandard.AnnexDisforinformationonly.INTERNATIONALSTANDARD ISO5796:2000(E)1 RubbercompoundingingredientsNaturalcalciumcarbonate Testmethods WARNINGPersonsusingthisInternationalStandardshoul

16、dbefamiliarwithnormallaboratorypractice. Thisstandarddoesnotpurporttoaddressallofthesafetyproblems,ifany,associatedwithitsuse.Itis theresponsibilityoftheusertoestablishappropriatesafetyandhealthpracticesandtoensurecompliance withanynationalregulatoryconditions. 1 Scope 1.1 ThisInternationalStandards

17、pecifiesthemethodstobeusedfortheevaluationofnaturalcalciumcarbonate (chalkorlimestone)groundtoadrypowderforuseintherubberindustry. NOTE1 Classificationofnaturalcalciumcarbonateaccordingtofinenessandchemicalpurityandtypicalphysicaland chemicalpropertiesforuseintherubberindustryaregivenininformativean

18、nexD. NOTE2 ThisInternationalStandarddoesnotcovercalciumcarbonatespreparedbyprecipitationfromsolution. 1.2 TherearetwosetsofanalyticalmethodslistedinthisInternationalStandard.Inthebodyofthetext(4.8.2to 4.8.4),thetraditionalspectrophotometricmethodsaregiven;theseareobsolescent,time-consumingandusea c

19、hlorinatedsolvent.Itisrecommendedthatthesemethodsbephasedoutandreplacedbytheatomicabsorption methodslistedinannexesA,BandC. 2 Normativereferences Thefollowingnormativedocumentscontainprovisionswhich,throughreferenceinthistext,constituteprovisionsof thisInternationalStandard.Fordatedreferences,subseq

20、uentamendmentsto,orrevisionsof,anyofthese publicationsdonotapply.However,partiestoagreementsbasedonthisInternationalStandardareencouragedto investigatethepossibilityofapplyingthemostrecenteditionsofthenormativedocumentsindicatedbelow.For undatedreferences,thelatesteditionofthenormativedocumentreferr

21、edtoapplies.MembersofISOandIEC maintainregistersofcurrentlyvalidInternationalStandards. ISO565:1990,TestsievesMetalwirecloth,perforatedmetalplateandelectroformedsheetNominalsizesof openings. ISO787-2:1981,GeneralmethodsoftestforpigmentsandextendersPart2:Determinationofmattervolatileat 105C. ISO787-1

22、0:1993,GeneralmethodsoftestforpigmentsandextendersPart10:Determinationofdensity Pyknometermethod. ISO3262-1:1997ExtendersforpaintsSpecificationsandmethodsoftestPart1:Introductionandgeneraltest methods. ISO4793:1980,Laboratorysintered(fritted)filtersPorositygrading,classificationanddesignation. ISO15

23、528:2000,Paints,varnishesandrawmaterialsforpaintsandvarnishesSampling.ISO5796:2000(E) 2 3 Sampling SamplingshallbecarriedoutinaccordancewithISO15528. 4 Methodsoftest 4.1 General Duringtheanalysis,allreagentsusedshallbeofrecognizedanalyticalreagentquality.Distilledwaterorwaterof equalpurityshallbeuse

24、dthroughoutthetests. 4.2 Residueonsieve DeterminethesieveresidueinaccordancewithISO3262-1,using45 mand125 mopeningtestsievesas definedbyISO565. 4.3 Calciumcarbonate(ondrysample) DeterminethecalciumcarbonatecontentinaccordancewithISO3262-1. 4.4 Lossonheatingat105C Determinethelossonheatingat105Cinacc

25、ordancewithISO787-2. 4.5 Lossonignitionat1000C(ondrysample) Determinethelossonignitionat1000CinaccordancewithISO3262-1. 4.6 Matterinsolubleinhydrochloricacid 4.6.1 Reagent 4.6.1.1 Hydrochloricacid,73g/dm 3 solution. Dilute170cm 3 ofconcentrated(35%bymass)hydrochloricacid( =1,18g/cm 3 )to1dm 3 withwa

26、terandmix. 4.6.2 Apparatus 4.6.2.1 Beaker,ofcapacity250cm 3 ,watchglass,suitableforcoveringthebeaker,andglassrodsuitablefor stirring. 4.6.2.2 Analyticalbalance,accurateto0,1mg. 4.6.2.3 Sintered-glasscrucible,porositygradeP40,inconformitywiththerequirementsofISO4793. 4.6.2.4 Oven,capableofbeingmainta

27、inedatatemperatureof105C 2C. 4.6.2.5 Desiccator. 4.6.3 Procedure 4.6.3.1 Weigh,tothenearest1mg,approximately2gofsampleintothebeaker(4.6.2.1). 4.6.3.2 Pour100cm 3 ofhydrochloricacid(4.6.1.1)intothebeakerandcoverwithawatch-glass.ISO5796:2000(E)3 4.6.3.3 Swirlthemixturegentlyatroomtemperature,avoidingt

28、heformationoffoam.Boilthemixturegentlyfor 5minto10min,thenleavetocoolfor30minto60min,stirringfromtimetotime. 4.6.3.4 Filterofftheinsolublematterthroughthecrucible(4.6.2.3)whichhaspreviouslybeenwashed,driedat 105Candweighed.Washwithwateruntilthewashingsarefreefromchloride.Discardthefiltrateandthe was

29、hings. 4.6.3.5 Drythecruciblecontainingtheinsolubleresidueintheoven(4.6.2.4),maintainedat105C 2C, untilconstantmassisachieved,i.e.untilfurtheroven-drying,coolingandweighingyieldsamasschangeofless than1mg. 4.6.3.6 Coolinthedesiccator(4.6.2.5). 4.6.3.7 Weightothenearest1mg. 4.6.4 Expressionofresults T

30、hematterinsolubleinhydrochloricacid,M is ,isgiven,asapercentagebymass,bythefollowingequation: M mm m is 21 0 100 where m 0 isthemass,ingrams,ofthetestportion; m 1 isthemass,ingrams,oftheemptydriedcrucible; m 2 isthemass,ingrams,ofthecruciblecontainingtheinsolublematter. Expresstheresulttothenearest0

31、1%bymass. 4.7 Alkalinity 4.7.1 Reagents 4.7.1.1 Distilledwater,boiledtoremovecarbondioxide. 4.7.1.2 Phenolphthalein,0,5%bymasssolutionin95%byvolumeethanol. 4.7.1.3 Hydrochloricacid,standardvolumetricsolution,c(HCI)=0,01mol/dm 3 . 4.7.2 Apparatus 4.7.2.1 Analyticalbalance,accurateto0,1mg. 4.7.2.2 Co

32、nicalflask,narrow-mouth,ofcapacity250cm 3 . 4.7.2.3 Filterpaper,finegrade. 4.7.2.4 Burette,accurateto0,1cm 3 . 4.7.3 Procedure 4.7.3.1 Weigh,tothenearest1mg,about10gofsampleandplacethistestportionintheflask(4.7.2.2).Add 150cm 3 ofdistilledwater(4.7.1.1).Leavethemixturefor1h,shakingitfromtimetotime.I

33、SO5796:2000(E) 4 4.7.3.2 Filterthemixturethroughthefilterpaper(4.7.2.3)andkeepalltheresidueonthefilter.Washthree timeswithaminimumamountofdistilledwater,addingthewashingstothefiltrate. 4.7.3.3 Addafewdropsofphenolphthaleinsolution(4.7.1.2)asindicatortothefiltrateandtitratewith hydrochloricacid(4.7.1

34、3)untilcolourless.Readthevolumeusedforthetitrationtothenearest0,1cm 3 . 4.7.4 Expressionofresults Thealkalinity,w,expressedingramsofsodiumcarbonate(Na 2 CO 3 )per100gofsample,isgivenbythefollowing equation: w Vc m 0,00053 100 where V isthevolumeofHCl,incubiccentimetres,usedforthetitration; c isthea

35、ctualconcentration,expressedinmolesofHCIpercubicdecimetreofhydrochloricacid (4.7.1.3); m isthemass,ingrams,ofthetestportion; 0,00053 isthemass,ingrams,ofsodiumcarbonatecorrespondingto100cm 3 ofhydrochloricacid, c(HCI)=0,010mol/dm 3 . 4.8 Determinationoftotalcopper,totalmanganeseandtotaliron 4.8.1 Pr

36、eparationofstocktestsolution 4.8.1.1 Reagents 4.8.1.1.1 Nitricacid, =1,42g/cm 3 . 4.8.1.1.2 Hydrofluoricacid,40%bymasssolution. 4.8.1.1.3 Sulfuricacid,50%byvolumesolution. 4.8.1.1.4 Octylalcohol(octan-1-ol). 4.8.1.1.5 Hydrochloricacid, =1,18g/cm 3 (35%bymass). 4.8.1.2 Apparatus 4.8.1.2.1 Beaker,ofca

37、pacity250cm 3 . 4.8.1.2.2 Volumetricflask,ofcapacity250cm 3 . 4.8.1.2.3 Platinumcrucible,ofcapacity20cm 3 . 4.8.1.2.4 Mufflefurnace. 4.8.1.2.5 Fumecupboard. 4.8.1.2.6 Quartztriangle. 4.8.1.2.7 Analyticalbalance,accurateto0,1mg.ISO5796:2000(E)5 4.8.1.3 Procedure 4.8.1.3.1 Weigh,tothenearest1mg,about5

38、gofsampleintothebeaker(4.8.1.2.1).Dissolvethistestportion carefullyin25cm 3 ofwaterand15cm 3 ofnitricacid(4.8.1.1.1)andheattoboiling.Iffoamtendstoriseduringthe dissolutionofthetestportion,breakthefoambyaddingadropofoctylalcohol(4.8.1.1.4). 4.8.1.3.2 Filterthroughamediumfilterpaper,washthepaperwithho

39、twaterandallowthecombinedfiltrateplus washingstocool.Thentransferthesolutionintothevolumetricflask(4.8.1.2.2)andretainfor4.8.1.3.7. 4.8.1.3.3 Liftoutthefilterpaper,folditcarefullytoencloseanyresidueandplaceintheplatinumcrucible (4.8.1.2.3).Heatgentlyuntildry,thenheatmoretocharthepaper.Thenplacethecr

40、ucibleinthemufflefurnace (4.8.1.2.4)at1000C 50Cfor30mintooxidizeandtoremoveallchar. 4.8.1.3.4 Coolthecrucibleandadd2cm 3 ofhydrofluoricacid(4.8.1.1.2),dropbydrop,tothecrucibleinsucha waythatallthecontentsarewetted.Thenadd0,5cm 3 ofsulfuricacid(4.8.1.1.3)dropbydrop. Placethecrucibleonahotplateinthefu

41、mecupboard(4.8.1.2.5)andevaporatetodryness,takingcaretoavoid overheatingandconsequentbumpingorspitting.Thencontinueheatinguntilwhitefumesappear. 4.8.1.3.5 Transferthecrucible,stillinthefumecupboard,toaquartztriangleonastandandheattoadullred heatuntilallwhitefumeshavebeendrivenoff. 4.8.1.3.6 Allowthe

42、crucibletocool.Add5cm 3 ofwaterand1cm 3 ofnitricacid(4.8.1.1.1)andwarmona hotplate.Stirwithaglassrodtodissolveallsalts. 4.8.1.3.7 Coolandtransferthesolutionquantitativelytotheflaskcontainingtheoriginalacid-solubleportion(see 4.8.1.3.2),rinsingthecruciblethoroughlywithwaterintotheflask. 4.8.1.3.8 Fin

43、ally,dilutewithwatertothe250cm 3 mark. Theflasknowcontainsthestocktestsolution,aliquotsofwhichwillberequiredfordeterminationofcopper, manganeseandiron. 4.8.2 Copper(total)Spectrophotometricmethod 4.8.2.1 Reagents 4.8.2.1.1 Biquinolylreagent,solution. Dissolve0,03gof2,2-biquinolinein100cm 3 ofn-hexan

44、ol(4.8.2.1.8)thathasbeenfreshlydistilledfromsolid sodiumhydroxide. 4.8.2.1.2 Hydroxylammoniumchloride,solution. Dissolve25gofhydroxylammoniumchlorideinabout80cm 3 ofwater.Filter,ifnecessary,anddiluteto100cm 3 withwater. Ifanyappreciableamountsofcopperarepresentinthesolution,extractwithsuccessive10cm

45、 3 portionsofa 0,01%bymasssolutionofdithizoneincarbontetrachlorideuntilthereisnomorevioletcolorationduetocopper, hencenochangeinthegreencolourofthedithizonesolution.Thenextractthesolutionwithcarbontetrachloride untilallcolourhasbeenremovedfromtheaqueoussolution. 4.8.2.1.3 Sodiumacetatebuffersolution

46、 Dissolve136gofsodiumacetatetrihydrateinwateranddiluteto1dm 3 withwater.Ifthereagentcontainsmore thanatraceofcopper,purifythissolutionbyextractionwith0,01%bymassdithizonesolutionincarbon tetrachlorideasforthehydroxylammoniumchloridesolution(4.8.2.1.2).ISO5796:2000(E) 6 4.8.2.1.4 Hydroquinone,soluti

47、on. Dissolve1gofhydroquinonein100cm 3 ofredistilledethanol. 4.8.2.1.5 Copper,standardstocksolution. Dissolveexactly0,1gofpurecopperin3cm 3 ofnitricacid(4.8.1.1.1),add1cm 3 ofsulfuricacid(4.8.1.1.3)and evaporateinthefumecupboarduntilwhitefumesappear.Allowtocool,dissolvetheresidueinwateranddiluteto 50

48、0cm 3 . 1cm 3 ofthissolutioncontains200 gofCu. 4.8.2.1.6 Copper,4 g/cm 3 standardworkingsolution. Diluteexactly5cm 3 ofthestocksolution(4.8.2.1.5)to250cm 3 withwater. 1cm 3 ofthissolutioncontains4gofCu.Thissolutionisusedforthecalibrationofthe1cmspectrometercells. 4.8.2.1.7 Copper,1 g/cm 3 standardwo

49、rkingsolution. Forthecalibrationof4cmcells,diluteexactly5cm 3 ofthestocksolution(4.8.2.1.5)to1000cm 3 withwater,to giveasolutioncontaining1 gofcopperpercubiccentimetre. 4.8.2.1.8 n-hexylalcohol(hexan-1-ol). 4.8.2.2 Apparatus Ordinarylaboratoryapparatus,plusthefollowing: 4.8.2.2.1 Analyticalbalance,accurateto0,1mg. 4.8.2.2.2 Spectrometer,capableofbeingoperatedat540nm,with1cmand/or4cmcells. 4.8.2.2.3 Separatingfunnels,ofcapacity250cm 3 . 4.8.2.2.4 One-markvolumetricflask,ofcapacity10cm 3 . 4.8.2.3 Procedure 4.8.2.3.1 Transf