1、BRITISH STANDARD BS EN 13900-4:2004 Pigments and extenders Methods of dispersion and assessment of dispersibility in plastics Part 4: Determination of colouristic properties and ease of dispersion of white pigments in polyethylene by two-roll milling The European Standard EN 13900-4:2004 has the sta
2、tus of a British Standard ICS 83.040.30 BS EN 13900-4:2004 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 11 May 2004 BSI 11 May 2004 ISBN 0 580 43763 9 National foreword This British Standard is the official English language version of EN 1
3、3900-4:2004. The UK participation in its preparation was entrusted to Technical Committee STI/1, Pigments, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement intern
4、ational or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purpo
5、rt to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee
6、 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. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 6, an
7、 inside back cover and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN139004 April2004 ICS83.040.30 Englishversion Pigmentsandext
8、endersMethodsofdispersionand assessmentofdispersibilityinplasticsPart4:Determinationof colouristicpropertiesandeaseofdispersionofwhitepigments inpolyethylenebytworollmilling PigmentsetmatiresdechargeMthodesdedispersion etvaluationdelaptitudeladispersiondansles plastiquesPartie4:Dterminationdespropri
9、ts colorimtriquesetdelafacilitdedispersiondespigments blancsdanslepolythylneparcalandragesurbicylindre PigmenteundFllstoffeDispergierverfahrenund BeurteilungderDispergierbarkeitinKunststoffenTeil4: BestimmungderkoloristischenEigenschaftenundder DispergierhrtevonWeipigmenteninPolyethylenim Walztest T
10、hisEuropeanStandardwasapprovedbyCENon2February2004. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmayb
11、eobtainedonapplicationtotheCentralSecretariatortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheCentralSecretariathasthesamestatusast heofficial ve
12、rsions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,Cyprus,CzechRepublic,Denmark,Estonia,Finland,France, Germany,Greece,Hungary,Iceland,Ireland,Italy,Latvia,Lithuania,Luxembourg,Malta,Netherlands,Norway,Poland,Portugal, Slovakia, Slovenia,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPE
13、ANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2004CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN139004:2004:EEN139004:2004(E) 2 Foreword Thisdocument(EN139004:2
14、004)hasbeenpreparedbyTechnicalCommitteeCEN/TC298“Pigmentsand extenders”,thesecretariatofwhichisheldbyDIN. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyOctober2004,andconflictingnationalstandardsshallbewithdrawnatthelat
15、est byOctober2004. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,Cyprus,CzechRepublic,Denmark, Estonia,Finland,France,Germany,Greece,Hungary,Iceland,Ireland,Italy,Latvia,Lithuania,Luxembou
16、rg,Malta, Netherlands,Norway,Poland,Portugal,Slovakia,Slovenia,Spain,Sweden,SwitzerlandandUnitedKingdom.EN139004:2004(E) 3 1Scope ThisPartofEN13900specifiesamethodofdeterminingthecolouristicpropertiesofatestpigmentinpolyethylene (PE)relativetoastandard,andtheeaseofdispersionDH PE ofpigmentsfromthedi
17、fferencesintintingstrengthof dispersingcolouringmaterialsundervariousconditions. Themethodisappropriateforusewithwhitepigments. Theeaseofdispersiondeterminedinthiswayisvalidonlyforthedispersionequipment,dispersionconditionsand dispersionmediumbeingused.Theuseoftestconditionsdifferingfromthosespecifi
18、edcangivedifferentresults;this appliesbothtotheabsolutemagnitudeandtotherelationbetweenvaluesoftheeaseofdispersionofvarious pigments.ThesubscriptDH PE isthereforeusedtodesignatethevalueobtainedasspecifiedinthisPartofEN13900. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedrefer
19、ence,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundated
20、referencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). EN ISO78724:1995, GeneralmethodoftestsforpigmentsandextendersPart24:Determinationofrelative tintingstrengthofcolouredpigmentsandrelativescatteringpowerofwhitepigmentsPhotometricmethods(ISO 78724:1985). ENISO15528, Pai
21、nts,varnishesandrawmaterialsforpaintsandvarnishesSampling(ISO15528:2000). ISO77242:1984, PaintsandvarnishesColorimetryPart2:Colourmeasurement . 3 Termsanddefinitions ForthepurposesofthisEuropeanStandard,thefollowingtermanddefinitionapplies. 3.1 easeofdispersion (DH PE) measureoftherateatwhichorthede
22、greetowhichapigmentorextenderachievesagivenlevelofdispersion whendispersedinaplasticsmaterial. TheDH PE isderivedfromtheincreaseintintingstrengthachievedbytworollmillingasspecifiedin8.2,relativeto thetintingstrengthachievedasspecifiedin8.1. 4Principle Usingatworollmill,thepigmentundertestisdispersed
23、atanappropriatetemperatureinthepolymer.Thecooled milledsheetobtainedinthiswayisthensubjectedtothehighershearingforcesresultingfromtworollmillingata narrowergapwidth.TheresultingincreaseintintingstrengthisameasureoftheeaseofdispersionDH PE.EN139004:2004(E) 4 5Materials 5.1Polyethylene ofaform,gradean
24、dtypetobeagreedbetweentheinterestedparties. NOTE WhereHDPEisused,aphenolicantioxidantcanbeusedasaslipagenttofacilitateprocessing. 5.2 Carbonblackpolyethylenemasterbatch basedonaneasilydispersingtypeofcarbonblackasrecommendedforuseinpolyethylene. 6Apparatus 6.1 Tworollmill equippedwithheatingfaciliti
25、esandhavingrollersadjustableforspacing.Therolldiametershallbebetween80mmand 200mm,andtheratioofthespeedsofrotationofthetworollersshallbebetween1:1,1and1:1,2. NOTE Ithasbeenfoundthatcomparableresultsondifferenttworollmillswillbeobtainedunderthefollowingconditions ratioofrollerdiametersofthetwomachine
26、s:between1:1and1:1,5, ratioofperipheralspeeds:between1:1and1:1,1, H k (bank)toH s (gapwidth)shouldbeH k /H s 20. Ifsmallerrollersetsareused(rollerdiametere.g.80mm),thesettingsofthethicknessofthemilledsheetto0,4mmto 0,5mmwiththerecommendedconditionsofsimilaritycanleadtodifficultieswithregardtotherequ
27、irementforarolling bank. 6.2Plate press providedwithheatingfacilitiesand,preferably,alsowithcoolingfacilities. 6.3Photometer 7Sampling RepresentativesamplesofthecolouringmaterialstobetestedshallbetakenasdescribedinENISO15528. 8Procedure 8.1 TestingofcolouristicpropertiesinPolyethyleneinadmixturewith
28、carbonblack 8.1.1 Preparationofthemixture Inaplasticbeakerpreblendgently100partsofpolyethyleneand0,05partscarbonblackinpreparedform(5.2).Add 5partsoftitaniumdioxidetestpigment.Mixusingaspatulasothatnotestpigmentremainsonthebeakerwalls. NOTE Themasterbatchshouldbedilutedinthetestpolymertofacilitatein
29、corporationandhandling. Aquantityoftestmixturebasedon100gpolymerwillgenerallybeadequateformosttworollmills.Itmayif necessarybeincreasedordecreasedaccordingtothesizeofthemillinordertofacilitatehandling.EN139004:2004(E) 5 8.1.2 Preparationofthetestsample Themixtureisaddedtotherotatingrollsofthetworoll
30、millpreviouslyheatedtoadefinedtemperatureestablishedas beingappropriateforthepolymerbeingused.Theratioofthespeedsofrotationofthetworollersshallbebetween 1:1,1and1:1,2. NOTE Atemperaturebetween140 Cand160 Chasbeenfoundsuitableformosttypesofpolymer. Asheetisformedwithin1mininsuchawaythatthewholeofthem
31、aterialformsacontinuoussheetonthefrontroll. Thedispersionofthepigmentisobtainedbycuttingandfoldingofthesheetevery30swhilstmillingforafurther 7minat25min 1 withthegapwidthmaintainedat0,5mm.Afterthefull8minmillingthesheetisremovedand allowedtocooltoroomtemperature,unlessphotometricmeasurementiscarried
32、outdirectlyontherotatingsheet. Aftereachmillingoperationtherollsshallbecleaned. 8.1.3Pressing Sufficientlylargepiecesarecutoutofthesheetspreparedfromthestandardandthetestsampleandpressedina spacingframebetweenpolishedchromedpressplatessoastoensureasurfacesuitableforphotometric measurement. NOTE Phot
33、ometricmeasurementcanalsobecarriedoutdirectlyontherotatingsheet. 8.1.4Photometric measurement Thetintingstrengthofthetestspecimenspreparedasspecifiedin8.1.2and8.1.3shallbemeasuredasspecifiedin ISO77242:1984,clause9.ThesevaluesshallbeusedtodeterminethetintingstrengthasspecifiedinENISO787 24:1995,8.1a
34、ndclause9forthepurposesofthecalculation. 8.2 Testingofeaseofdispersion 8.2.1 Preparationofthetestsamples Therollgapofthemillisreducedto0,3mmandonehalfofthesheetpreparedunder8.1.2isreturnedtotherollers maintainedatthesametemperatureasusedin8.1.2at25min 1 .Millingiscontinuedfor7minwithcuttingand foldi
35、ngevery30s.Thenthesheetisremovedandcooledbetweenmetalplates,unlessphotometricmeasurementis carriedoutdirectlyontherotatingsheet. Thisprocedureiscarriedoutforeachsheetcontainingthetestpigments,therollsbeingcleanedaftereachmilling operation. 8.2.2 Pressingandphotometricmeasurement Pressingandphotometr
36、icmeasurementarecarriedoutasdescribedin8.1.3and8.1.4.EN139004:2004(E) 6 9Evaluation TheeaseofdispersionDH PE isexpressedasthepercentageincreaseintintingstrengthfollowingrollmillingat 0,3mmgapwidthrelativetothatobtainedfollowingmillingat0,5mm(see8.1). ItshallbecomputedfromtheFvalues,usingthefollowing
37、equation: - = 1 F F 100 DH 1 2 PE (1) where: F 1 isthetintingstrengthofthetestspecimenspecifiedin8.1; F 2 isthetintingstrengthofthetestspecimenspecifiedin8.2. 10 Testreport Thetestreportshallcontainatleastthefollowinginformation: a)alldetailsnecessarytoidentifytheproducttested; b)areferencetothisPar
38、tofEN13900(EN139004); c)designationofthetestspecimensandtheirpreparation,includingthetemperatureofmilling; d)typeandconcentrationofthecarbonblackpigmentinthemasterbatch; e)type,gradeandformofthetestpolymerused; f)photometricdataobtained,howobtainedandtheeaseofdispersionDH PE ; g)methodoftintingstren
39、gthdetermination; h)anydeviationfromthetestmethodspecified; i)dateofthetest. 11Precision Thisstandarddefinestheprinciplesofthemethodandtheprocedurestobeused,butallowsvariationasregards thedimensionsofthemachineryusedandthetypeandgradeofpolyethyleneused.Precisiondatathuscannotbe establishedforthemeth
40、oditself,precisionshouldbedeterminedbyrepeatabilityandreproducibilitystudies accordingtotheequipmentandcompoundusedinthetestinglaboratory,andaccordingtothepigmentundertest.blankBS EN 13900-4:2004 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent nation
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