1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS EN ISO 3262-19:2000 In
2、corporating Corrigendum No. 1 The European Standard EN ISO 3262-19:2000 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 19: Precipitated silicaThis British Standard,
3、 having 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 36099 7 BS EN ISO 3262-19:2000 Amendments issued since publication Amd. No. Date
4、Comments 11073 Corrigendum No. 1 September 2000 Addition of annex ZA National foreword This British Standard is the official English language version of EN ISO 3262-19:2000. It is identical with ISO 3262-19:2000. Together with the other parts of BS EN ISO 3262, it will supersede BS 1795:1976 which i
5、s declared 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,
6、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 Attention is drawn to the fact that
7、CEN and 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 Standar
8、ds 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 provisions of a contract. Users of British Standards are responsible for
9、 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 EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii to v, a blank page, p
10、ages 1 to 9, 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 ENISO326219 April2000 ICS87.060.10 Englishversion ExtendersforpaintsSpecificationsandm
11、ethodsoftestPart 19:Precipitatedsilica(ISO326219:2000) MatiresdechargepourpeinturesSpcificationset mthodesdessaiPartie19:Siliceprcipit(ISO3262 19:2000) ThisEuropeanStandardwasapprovedbyCENon15April2000. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivi
12、ngthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheCentralSecretariatortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninany
13、otherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheCentralSecretariathasthesamestatusast heofficial versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembour
14、g,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG CentralSecretariat:ruedeStassart,36B1050Brussels 2000CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMe
15、mbers. Ref.No.ENISO326219:2000EForeword Thetext oftheInternationalStandar d ISO326219:2000has beenpreparedbyTechnical CommitteeISO/TC 35“Paintsandvarnishes“incollaborationwit h TechnicalCommitteeCEN/TC298“Pigmentsandextenders“, thesecretariatofwhichisheldbyDIN. ThisEuropeanStandardshallbegiventhesta
16、tusofanationalstandard,eitherbypublicationofanidentical text orby endorsement,a t thelatestby October2000 , andconflictin g nationalstandards shallbewithdrawn atthelatestbyOctober2000. AccordingtotheCEN/CENELE C InternalRegulations,thenationalstandardsorganizations ofthefollowing countriesareboundto
17、implementthisEuropea nStandard:Austria,Belgium,CzechRepublic,Denmark, Finland,France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal, Spain,Sweden,SwitzerlandandtheUnitedKingdom. Endorsementnotice ThetextoftheInternationalStandardISO326219:2000hasbeenapprovedbyCENasaEurop
18、ean Standardwithoutanymodification. NOTE:NormativereferencestoInternationalStandardsarelistedinannexZA(normative). EN ISO 3262-19:2000Referencenumber ISO3262-19:2000(E) INTERNATIONAL STANDARD ISO 3262-19 Firstedition 2000-04-15 ExtendersforpaintsSpecifications andmethodsoftest Part19: Precipitatedsi
19、lica Matires de charge pour peintures Spcifications et mthodes dessai Partie 19: Silice prcipite EN ISO 3262-19:2000ii EN ISO 3262-19:2000 iii Contents Page Foreword.iv 1 Scope1 2 Normativereferences1 3 Termanddefinition1 4 Requirementsandtestmethods.2 5 Sampling.2 6 Determinationofsilicacontent3 7
20、Determinationofcarboncontent.5 8 Determinationofresidueonsieve.7 9 Testreport9 EN ISO 3262-19:2000iv Foreword ISO(theInternationalOrganizationforStandardization)isaworldwidefederationofnationalstandardsbodies (ISOmemberbodies).TheworkofpreparingInternationalStandardsisnormallycarriedoutthroughISOtec
21、hnical committees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhas therighttoberepresentedonthatcommittee.Internationalorganizations,governmentalandnon-governmental,in liaisonwithISO,alsotakepartinthework.ISOcollaboratescloselywiththeInternationalElectrotechnical Co
22、mmission(IEC)onallmattersofelectrotechnicalstandardization. InternationalStandardsaredraftedinaccordancewiththerulesgivenintheISO/IECDirectives,Part3. DraftInternationalStandardsadoptedbythetechnicalcommitteesarecirculatedtothememberbodiesforvoting. PublicationasanInternationalStandardrequiresapprov
23、albyatleast75%ofthememberbodiescastingavote. AttentionisdrawntothepossibilitythatsomeoftheelementsofthispartofISO3262maybethesubjectofpatent rights.ISOshallnotbeheldresponsibleforidentifyinganyorallsuchpatentrights. InternationalStandardISO3262-19waspreparedbyTechnicalCommitteeISO/TC35, Paints and v
24、arnishes, SubcommitteeSC2, Pigments and extenders. Togetherwiththeotherparts(seebelow),thispartofISO3262cancelsandreplacesISO3262:1975,whichhas beentechnicallyrevised.Part1comprisesthedefinitionofthetermextenderandanumberoftestmethodsthat areapplicabletomostextenders,whilstpart2andthefollowingpartss
25、pecifyrequirementsand,whereappropriate, particulartestmethodsforindividualextenders. ISO3262consistsofthefollowingparts,underthegeneraltitle Extenders for paints Specifications and methods of test: Part 1: Introduction and general test methods Part 2: Barytes (natural barium sulfate) Part 3: Blanc f
26、ixe 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: Natural talc, in lamellar form, containing carbonates Part 12: Muscovite-type
27、mica Part 13: Natural quartz (ground) EN ISO 3262-19:2000 v Part 14: Cristobalite Part 15: Vitreous silica Part 16: Aluminium hydroxides Part 17: Precipitated calcium silicate Part 18: Precipitated sodium aluminium silicate Part 19: Precipitated silica Part 20: Fumed silica Part 21: Silica sand (ung
28、round natural quartz) Part 22: Flux-calcined kieselguhr EN ISO 3262-19:2000EN ISO 3262-19:2000 1 ExtendersforpaintsSpecificationsandmethodsoftest Part19: Precipitatedsilica 1 Scope ThispartofISO3262specifiesrequirementsandcorrespondingmethodsoftestforprecipitatedsilica. 2 Normativereferences Thefoll
29、owingnormativedocumentscontainprovisionswhich,throughreferenceinthistext,constituteprovisionsof thispartofISO3262.Fordatedreferences,subsequentamendmentsto,orrevisionsof,anyofthesepublications donotapply.However,partiestoagreementsbasedonthispartofISO3262areencouragedtoinvestigatethe possibilityofap
30、plyingthemostrecenteditionsofthenormativedocumentsindicatedbelow.Forundated references,thelatesteditionofthenormativedocumentreferredtoapplies.MembersofISOandIECmaintain registersofcurrentlyvalidInternationalStandards. ISO787-2:1981, General methods of test for pigments and extenders Part 2: Determi
31、nation of matter volatile at 105 C. ISO787-5:1980, General methods of test for pigments and extenders Part 5: Determination of oil absorption value. 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. 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
33、 and test methods. ISO5794-1:1994, Rubber compounding ingredients Silica, precipitated, hydrated Part 1: Non-rubber tests. ISO15528: 1) , Paints, varnishes and raw materials for paints and varnishes Sampling. 3 Termanddefinition ForthepurposesofthispartofISO3262,thefollowingtermanddefinitionapply: 3
34、.1 precipitatedsilica amorphoussilicaprecipitatedbyreactionofsodiumsilicatesolutionwithamineralacidand/orcarbondioxide 1)Tobepublished.(RevisionofISO842:1984andISO1512:1991) EN ISO 3262-19:20002 4 Requirementsandtestmethods ForprecipitatedsilicacomplyingwiththispartofISO3262,theessentialrequirements
35、arespecifiedinTable1and theconditionalrequirementsarelistedinTable2. Table1Essentialrequirements Requirement Characteristic Unit GradeA GradeB Testmethod Silicacontent,min. 95 95 Seeclause6 Carboncontent a %(m/m) max.0,2 min.0,3 Seeclause7 Organicsurfacecoating? No Yes Seeclause7 Mattervolatileat105
36、C,max. %(m/m) 8 ISO787-2 Lossonignition %(m/m) 3to8 3to15 ISO3262-1 Oilabsorptionvalue b ,min. g/100g 120 ISO787-5 pHvalueofaqueoussuspension c 3,5to9 ISO787-9 a Thecarboncontentisalsopartofthelossonignition. b AtestmethodwithhigherreproducibilityandrepeatabilityisdescribedinASTMD2414-97, Standard t
37、est method for carbon black n-Dibutyl phthalate absorption number. However, the results cannot be compared directly with oil absorption values determined in accordance withISO787-5. c Forhydrophobicsilicas,usea1:1(m/m)mixturebymassofwaterandmethanol. Table2Conditionalrequirements Requirement Charact
38、eristic Unit GradeA GradeB Testmethod Residueon45msieve, max. %(m/m) Tobeagreed betweenthe interestedparties Notapplicable Spraymethod(seeclause8) a Particlesizedistribution (instrumentalmethod) %(m/m) Tobeagreedbetweentheinterestedparties Apparentdensityafter tamping g/ml ISO787-11 Specificsurfacea
39、rea m 2 /g Tobeagreedbetweentheinterested parties ISO5794-1:1994,annexD a Onlyforhydrophylicmaterials. 5 Sampling Takearepresentativesampleoftheproducttobetested,asdescribedinISO15528. EN ISO 3262-19:2000 3 6 Determinationofsilicacontent 6.1 Principle Atestportionisrepeatedlytreatedwithhydrochlorica
40、cidandevaporatedtodryness.Torenderthedehydrated silicicacidthusformedasinsolubleaspossible,itisthenheatedfor2hat(140 5)C.Anychloridespresentare removedbyextractingtheprecipitatewithhotdilutehydrochloricacid. Theprecipitateisignitedat1000C,givingimpuresilicondioxide,whichistreatedwithsulfuricandhydro
41、fluoric acid.Thesilicontetrafluorideformedisevaporatedoffandthesilicacontentiscalculatedfromtheresultinglossin mass. 6.2 Reagents Useonlyreagentsofrecognizedanalyticalgradeandonlywaterofatleastgrade3purityasdefinedinISO3696. 6.2.1Hydrochloricacid,concentrated,approximately32%(m/m), 1,16g/ml. 6.2.2Hy
42、drochloricacid,diluted1 1. Add1partbyvolumeofconcentratedhydrochloricacid(6.2.1)to1partbyvolumeofwater. 6.2.3Sulfuricacid,diluted1 1. Add1partbyvolumeofconcentratedsulfuricacid,approximately96%(m/m), 1,84g/ml,slowlyto1partby volumeofwater. 6.2.4Hydrofluoricacid,concentrated,approximately40%(m/m), 1,
43、13g/ml. 6.3 Apparatus Useordinarylaboratoryapparatusandglassware,togetherwiththefollowing: 6.3.1Dish. 6.3.2Platinumcrucible. 6.3.3Waterbath,capableofbeingmaintainedat100C. 6.3.4Infraredevaporator. 6.3.5Mufflefurnace,capableofbeingmaintainedat(1000 20)C. 6.3.6Dryingoven,capableofbeingmaintainedat(140
44、 5)C. 6.3.7Filterpaper. Thefilterpaperusedforfiltrationofthesilicashallbeofsuchtextureastoretainthesmallestparticlesof precipitateandneverthelesspermitrapidfiltration. 2) 6.3.8Desiccator,containingmagnesiumperchlorateasdesiccant. 2)ForexampleWhatmanNo.40or41orSchleicherundSchllNo.589/2“Weiband“. EN
45、ISO 3262-19:20004 6.4 Procedure 6.4.1 Numberofdeterminations Carryoutthedeterminationinduplicate. 6.4.2 Testportion Weigh,tothenearest0,2mg,approximately1g(m 0 )ofthesample(seeclause5)intoadish(6.3.1). 6.4.3 Determination Addslowly20mlofconcentratedhydrochloricacid(6.2.1)andevaporatetodrynessunderth
46、einfraredevaporator (6.3.4).Addagain20mlofconcentratedhydrochloricacidandevaporatetodryness.Repeatthissteponcemore. Afterthethirdevaporation,placethedishinthedryingoven(6.3.6),maintainedat(140 5)C,andleavefor2h. Removethedishfromtheovenandallowtocool.Add50mlof1 1hydrochloricacid(6.2.2)totheresiduein
47、the dishandwarmitforapproximately20minonthewaterbath(6.3.3)at100C.Filterthroughasuitablefilterpaper (6.3.7)andwashtheresidueonthefilterwithhotwateruntilthewashingsareneutral. Pourthefiltrateandwashingsintotheoriginaldishandevaporatetodryness.Repeatthisevaporationstepanother twotimes,addingeachtime10
48、mlofconcentratedhydrochloricacidtotheresidue.Afterthethirdevaporation,heat at(140 5)Cfor2hinthedryingoven. Add20mlof1 1hydrochloricacidtotheresidueinthedishandwarmitforapproximately10minonthewater bathat100C.Filterthroughafreshfilterpaperandwashtheresidueonthefilterwithhotwateruntilthewashings areneutral. Ifitisfeltnecessary,checkthefiltrateforanysiliconwhichmayhavepassedthroughthefilt
