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
