1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS EN ISO 3262-20:2000 In
2、corporating Corrigendum No. 1 The European Standard EN ISO 3262-20:2000 has the status of a British Standard ICS 87.060.10 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Extenders for paints Specifications and methods of test Part 20: Fumed silicaThis British Standard, having
3、 been prepared under the direction of the Sector Committee for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 August 2000 BSI 09-2000 ISBN 0 580 36100 4 BS EN ISO 3262-20:2000 Amendments issued since publication Amd. No. Date Comment
4、s 11074 Corrigendum No. 1 September 2000 Addition of annex ZA National foreword This British Standard is the official English language version of EN ISO 3262-20:2000. It is identical with ISO 3262-20:2000. Together with the other parts of BS EN ISO 3262, it will supersede BS 1795:1976 which is decla
5、red obsolescent. The UK participation in its preparation was entrusted to Technical Committee STI/1, Pigments and extenders, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or prop
6、osals 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 Attention is drawn to the fact that CEN and
7、 CENELEC Standards normally include an annex which lists normative references to international publications with their corresponding European publications. The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Cata
8、logue 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 provisions of a contract. Users of British Standards are responsible for their
9、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 EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii to v, a blank page, pages 1
10、to 13, the annex ZA page, an inside back cover and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued.EUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO326220 April2000 ICS87.060.10 Englishversion ExtendersforpaintsSpecificationsandmethods
11、oftestPart 20:Fumedsilica(ISO326220:2000) MatiresdechargepourpeinturesSpcificationset mthodesdessaiPartie20:Silicepyrogne(ISO3262 20:2000) ThisEuropeanStandardwasapprovedbyCENon15April2000. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope
12、an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheCentralSecretariatortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguage
13、madebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheCentralSecretariathasthesamestatusast heofficial versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands
14、,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG CentralSecretariat:ruedeStassart,36B1050Brussels 2000CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No
15、.ENISO326220:2000EForeword Thetext oftheInternationalStandar d ISO326220:2000has beenpreparedbyTechnical CommitteeISO/TC 35“Paintsandvarnishes“incollaborationwit h TechnicalCommitteeCEN/TC298“Pigmentsandextenders“, thesecretariatofwhichisheldbyDIN. ThisEuropeanStandardshallbegiventhestatusofanationa
16、lstandard,eitherbypublicationofanidentical text orby endorsement,a t thelatestby October2000 , andconflictin g nationalstandards shallbewithdrawn atthelatestbyOctober2000. AccordingtotheCEN/CENELE C InternalRegulations,thenationalstandardsorganizations ofthefollowing countriesareboundtoimplementthis
17、Europea nStandard:Austria,Belgium,CzechRepublic,Denmark, Finland,France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal, Spain,Sweden,SwitzerlandandtheUnitedKingdom. Endorsementnotice ThetextoftheInternationalStandardISO326220:2000hasbeenapprovedbyCENasaEuropean Standardw
18、ithoutanymodification. NOTE:NormativereferencestoInternationalStandardsarelistedinannexZA(normative). EN ISO 3262-20:2000Referencenumber ISO3262-20:2000(E) INTERNATIONAL STANDARD ISO 3262-20 Firstedition 2000-04-15 ExtendersforpaintsSpecifications andmethodsoftest Part20: Fumedsilica Matires de char
19、ge pour peintures Spcifications et mthodes dessai Partie 20: Silice pyrogne EN ISO 3262-20:2000ii EN ISO 3262-20:2000 iii Contents Page Foreword.iv 1 Scope1 2 Normativereferences1 3 Termanddefinition2 4 Requirementsandtestmethods.2 5 Sampling.3 6 Determinationofsilicacontent3 7 Determinationofalumin
20、iumoxide,titanium(IV)oxideandiron(III)oxidecontentsbyspectrometry.4 8 Determinationofcarboncontent.9 9 Determinationofchloridecontent.11 10 Testreport13 EN ISO 3262-20:2000iv Foreword ISO(theInternationalOrganizationforStandardization)isaworldwidefederationofnationalstandardsbodies (ISOmemberbodies)
21、.TheworkofpreparingInternationalStandardsisnormallycarriedoutthroughISOtechnical committees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhas therighttoberepresentedonthatcommittee.Internationalorganizations,governmentalandnon-governmental,in liaisonwithISO,alsotakep
22、artinthework.ISOcollaboratescloselywiththeInternationalElectrotechnical Commission(IEC)onallmattersofelectrotechnicalstandardization. InternationalStandardsaredraftedinaccordancewiththerulesgivenintheISO/IECDirectives,Part3. DraftInternationalStandardsadoptedbythetechnicalcommitteesarecirculatedtoth
23、ememberbodiesforvoting. PublicationasanInternationalStandardrequiresapprovalbyatleast75%ofthememberbodiescastingavote. AttentionisdrawntothepossibilitythatsomeoftheelementsofthispartofISO3262maybethesubjectofpatent rights.ISOshallnotbeheldresponsibleforidentifyinganyorallsuchpatentrights. Internatio
24、nalStandardISO3262-20waspreparedbyTechnicalCommitteeISO/TC35, Paints and varnishes, SubcommitteeSC2, Pigments and extenders. Togetherwiththeotherparts(seebelow),thispartofISO3262cancelsandreplacesISO3262:1975,whichhas beentechnicallyrevised.Part1comprisesthedefinitionofthetermextenderandanumberoftes
25、tmethodsthat areapplicabletomostextenders,whilstpart2andthefollowingpartsspecifyrequirementsand,whereappropriate, particulartestmethodsforindividualextenders. ISO3262consistsofthefollowingparts,underthegeneraltitle Extenders for paints Specifications and methods of test: Part 1: Introduction and gen
26、eral test methods Part 2: Barytes (natural barium sulfate) Part 3: Blanc fixe Part 4: Whiting Part 5: Natural crystalline calcium carbonate Part 6: Precipitated calcium carbonate Part 7: Dolomite Part 8: Natural clay Part 9: Calcined clay Part 10: Natural talc/chlorite in lamellar form Part 11: Natu
27、ral talc, in lamellar form, containing carbonates Part 12: Muscovite-type mica Part 13: Natural quartz (ground) EN ISO 3262-20:2000 v Part 14: Cristobalite Part 15: Vitreous silica Part 16: Aluminium hydroxides Part 17: Precipitated calcium silicate Part 18: Precipitated sodium aluminium silicate Pa
28、rt 19: Precipitated silica Part 20: Fumed silica Part 21: Silica sand (unground natural quartz) Part 22: Flux-calcined kieselguhr EN ISO 3262-20:2000EN ISO 3262-20:2000 1 ExtendersforpaintsSpecificationsandmethodsoftest Part20: Fumedsilica 1 Scope ThispartofISO3262specifiesrequirementsandcorrespondi
29、ngmethodsoftestforfumedsilica. 2 Normativereferences Thefollowingnormativedocumentscontainprovisionswhich,throughreferenceinthistext,constituteprovisionsof thispartofISO3262.Fordatedreferences,subsequentamendmentsto,orrevisionsof,anyofthesepublications donotapply.However,partiestoagreementsbasedonth
30、ispartofISO3262areencouragedtoinvestigatethe possibilityofapplyingthemostrecenteditionsofthenormativedocumentsindicatedbelow.Forundated references,thelatesteditionofthenormativedocumentreferredtoapplies.MembersofISOandIECmaintain registersofcurrentlyvalidInternationalStandards. ISO648:1977, Laborato
31、ry glassware One-mark pipettes. ISO787-2:1981, General methods of test for pigments and extenders Part 2: Determination of matter volatile at 105 C. ISO787-9:1981, General methods of test for pigments and extenders Part 9: Determination of pH value of an aqueous suspension. ISO787-11:1981, General m
32、ethods of test for pigments and extenders Part 11: Determination of tamped volume and apparent density after tamping. ISO787-18:1983, General methods of test for pigments and extenders Part 18: Determination of residue on sieve Mechanical flushing procedure. ISO1042:1998, Laboratory glassware One-ma
33、rk volumetric flasks. ISO3262-1:1997, Extenders for paints Specifications and methods of test Part 1: Introduction and general test methods. ISO3696:1987, Water for analytical laboratory use Specification and test methods. ISO3819:1985, Laboratory glassware Beakers. ISO15528: 1) , Paints, varnishes
34、and raw materials for paints and varnishes Sampling. 1)Tobepublished.(RevisionofISO842:1984andISO1512:1991) EN ISO 3262-20:20002 3 Termanddefinition ForthepurposesofthispartofISO3262,thefollowingtermanddefinitionapply: 3.1 fumedsilica amorphoussilicaproducedfromsiliconhalidesbyhigh-temperatureflameh
35、ydrolysis 4 Requirementsandtestmethods ForfumedsilicacomplyingwiththispartofISO3262,theessentialrequirementsarespecifiedinTable1andthe conditionalrequirementsarelistedinTable2. Table1Essentialrequirements Requirement Characteristic Unit GradeA GradeB Testmethod Silicacontent,min. 99,8 Seeclause6 Oxi
36、decontent Al 2 O 3 ,max. 0,05 TiO 2 ,max. 0,03 Fe 2 O 3 ,max. 0,003 Seeclause7 Carboncontent a max.0,2 min.0,3 Seeclause8 Chloridecontent,max. %(m/m) 0,025 Seeclause9 Organicsurfacecoating? No Yes Seeclause8 Residueon45msieve,max. %(m/m) 0,05 NotapplicableISO787-18 Mattervolatileat105C,max. %(m/m) 3
37、 1 ISO787-2 Lossonignition,max. %(m/m) 2,5 10 ISO3262-1 pHvalueofaqueoussuspension 3,6to4,5 3,4to8 b ISO787-9 a Thecarboncontentisalsopartofthelossonignition. b Usea1:1(m/m)mixtureofwaterandmethanol. Table2Conditionalrequirements Requirement Characteristic Unit GradeA GradeB Testmethod Apparentdensi
38、tyafter tamping g/ml ISO787-11 Specificsurfacearea m 2 /g Tobeagreedbetweentheinterested parties Tobeagreedbetweenthe interestedparties EN ISO 3262-20:2000 3 5 Sampling Takearepresentativesampleoftheproducttobetested,asdescribedinISO15528. 6 Determinationofsilicacontent 6.1 Principle Atestportionisi
39、gnited,weighedandtreatedwithsulfuricacidandhydrofluoricacid.Thesilicontetrafluoridethus formedisevaporatedoffandthesilicacontentiscalculatedfromtheresultinglossofmass. Asthesilicacontentisveryhigh,apreviousseparationfromtheimpuritiesisnotrequired. 6.2 Reagents Useonlyreagentsofrecognizedanalyticalgr
40、adeandonlywaterofatleastgrade3purityasdefinedinISO3696. 6.2.1Sulfuricacid,diluted1 1. Add1partbyvolumeofconcentratedsulfuricacid,approximately96%(m/m), 1,84g/ml,slowlyto1partby volumeofwater. 6.2.2Hydrofluoricacid,concentrated,approximately40%(m/m), 1,13g/ml. 6.3 Apparatus Useordinarylaboratoryappar
41、atusandglassware,togetherwiththefollowing: 6.3.1Platinumdish. 6.3.2Mufflefurnace,capableofbeingmaintainedat(1000 20)C. 6.3.3Infraredevaporator. 6.3.4Desiccator,containingmagnesiumperchlorateasdesiccant. 6.4 Procedure 6.4.1 Numberofdeterminations Carryoutthedeterminationinduplicate. 6.4.2 Testportion
42、 Weigh,tothenearest0,2mg,approximately1g(m 0 )ofthesample(seeclause5)intothetaredplatinumdish (6.3.1). 6.4.3 Determination Ignitethetestportioninthemufflefurnace(6.3.2)at(1000 20)Ctoconstantmass(thisshouldtake approximately2h)andallowtocoolinthedesiccator(6.3.4).Weighthetestportionagain(m 1 ). EN IS
43、O 3262-20:20004 Wettheignitedtestportionintheplatinumdishwith2mlto3mlofwater,add1mlofsulfuricacid(6.2.1)and15ml ofhydrofluoricacid(6.2.2)andevaporatetoasyrupontheinfraredevaporator(6.3.3),takingcaretoavoidlossby spitting.Allowtocoolandwashthesidesdownwithsmallquantitiesofwater.Thenaddafurther10mlof
44、hydrofluoricacidandevaporatetodryness.Iftheevaporationofthesilicontetrafluorideisnotcomplete,adda further10mlofhydrofluoricacidandevaporatetodrynessagain. Heattheresidueuntilwhitefumesarenolongerevolved,thenignitefor30mininthemufflefurnaceat (1000 20)C.Removefromthefurnace,allowtocoolinthedesiccator
45、andweightothenearest0,2mg(m 2 ). 6.5 Expressionofresults Calculatethesilicacontentw(SiO 2 ),expressedasapercentagebymass,usingtheequation w mm m (SiO)= () 100 2 12 1 where m 1 isthemass,ingrams,ofthetestportionafterignition; m 2 isthemass,ingrams,aftertreatmentwithhydrofluoricacidandignition. Calcul
46、atethemeanofthetwodeterminationsandreporttheresulttothenearest0,1%. 6.6 Precision Noprecisiondataarecurrentlyavailable. 7 Determinationofaluminiumoxide,titanium(IV)oxideandiron(III)oxidecontentsby spectrometry 7.1 Principle Atestportionistreatedwithsulfuricacidandhydrofluoricacidinaplatinumdish.Ther
47、esultingsilicontetrafluoride isvolatilizedandtheresidueisdissolvedinhydrochloricacid.Afterdilutingwithwatertoaconstant,knownvolume, theAl,TiandFeimpuritiesaredeterminedeitherbyflameatomicabsorptionspectrometry(FAAS)orbyinductively coupledplasmaatomicemissionspectrometry(ICP-AES),dependingonwhichinst
48、rumentisavailableinthe laboratory. NOTE TheadvantagesoftheICP-AESmethodincludeitswidedynamicrangeandmulti-elementcapabilities.Both methods(FAASandICP-AES)arerelativeanalyticaltechniques.Forquantitativeanalyticalresults,bothmeasurement techniquesmustbecalibratedusingstandardmatchingsolutions. 7.2 Reagentsandmaterials Useonlyreagentsofrecognizedanalyticalgradeexceptforacids,whichshallbeultrapu
