1、BRITISH STANDARD BS EN 13900-2:2003 Pigments and extenders Methods of dispersion and assessment of dispersibility in plastics Part 2: Determination of colouristic properties and ease of dispersion in plasticized polyvinyl chloride by two-roll milling The European Standard EN 13900-2:2003 has the sta
2、tus of a British Standard ICS 83.040.30 BS EN 13900-2:2003 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 21 February 2003 BSI 21 February 2003 ISBN 0 580 41285 7 National foreword This British Standard is the official English language versi
3、on of EN 13900-2:2003. 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 implem
4、ent international 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
5、 not purport 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
6、 committee 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
7、2 to 9 and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN139002 February2003 ICS83.040.30 Englishversion PigmentsandextendersMetho
8、dsofdispersionand assessmentofdispersibilityinplasticsPart2:Determinationof colouristicpropertiesandeaseofdispersioninplasticized polyvinylchloridebytworollmilling PigmentsetmatiresdechargeMthodesdedispersion etvaluationdescaractristiquesdedispersibilitdansles plastiquesPartie2:Dterminationdespropri
9、ts colorimtriquesetdelafacilitdedispersiondansle chloruredepolyvinyleplastifiparcalandragesurbicylindre PigmenteundFllstoffeDispergierverfahrenund BeurteilungderDispergierbarkeitinKunststoffenTeil2: BestimmungderkoloristischenEigenschaftenundder DispergierhrteinweichmacherhaltigenPolyvinychlorid (PV
10、CP)FormmassenimWalztest ThisEuropeanStandardwasapprovedbyCENon12December2002. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings
11、 uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesames
12、tatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,SwitzerlandandUn ited Kingdom. EUROPEANCOMMITTEEFORSTANDARDIZAT
13、ION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN139002:2003EEN139002:2003(E) 2 Foreword Thisdocument(EN139002:2003)hasbeenpreparedbyTechni
14、calCommitteeCEN/TC298,“Pigmentsand extenders“,thesecretariatofwhichisheldbyDIN. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyAugust2003,andconflictingnationalstandardsshallbewithdrawnatthelatestby August2003. AnnexAisi
15、nformative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal, S
16、lovakia,Spain,Sweden,SwitzerlandandtheUnitedKingdom.EN139002:2003(E) 3 1Scope ThispartofthisEuropeanStandardspecifiesamethodofdeterminingthecolouristicpropertiesofatestpigment relativetoastandard,andtheeaseofdispersionDH PVCP ofpigmentsfromthedifferencesincolourstrengthon dispersingcolouringmaterial
17、sundervariousconditionsinplasticizedpolyvinylchloride(PVCP)compounds. Themethodisappropriateforusewithorganicandinorganicblackandcolourpigmentsandforpigment preparations. Theeaseofdispersiondeterminedinthiswayisvalidonlyforthedispersionequipment,dispersionconditionsand dispersionmediumbeingused.Theu
18、seoftestconditionsdifferingfromthosespecifiedmaygivedifferentresults; thisappliesbothtotheabsolutemagnitudeandtotherelationbetweenvaluesoftheeaseofdispersionofvarious pigments.ThesubscriptDH PVCP isthereforeusedtodesignatethevalueobtainedasspecifiedinthispartofthis EuropeanStandard. Theprincipleofth
19、isstandardmayalsobeusedforroutinequalitycontrolpurposesbyreferencetothephotometric datageneratedfromthesheetsmilledat130 C.Forqualitycontrolpurposes,theratioofpigmenttoTiO 2 maybe agreedbetweentheinterestedparties.Ratiosof1:10fororganicpigmentsand0,2to0,5:1forinorganicpigments aresuggestedasconvenie
20、ntandwidelyusedstandardratios. AnnexAisinformativeandgivesadescriptionofasuitablebasiccompound. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelisted
21、hereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). EN128771, ColouringmaterialsinplasticsDetermin
22、ationofcolourstabilitytoheatduringprocessingofcolouring materialsinplasticsPart1:Generalintroduction. ENISO78724:1995, GeneralmethodoftestsforpigmentsandextendersPart24:Determinationofrelative tintingstrengthofcolouredpigmentsandrelativescatteringpowerofwhitepigmentsPhotometricmethods(ISO 78724:1985
23、). ENISO15528, Paints,varnishesandrawmaterialsforpaintsandvarnishesSampling(ISO15528:2000). ISO77242:1984, PaintsandvarnishesColorimetryPart2:Colourmeasurement. 3 Termanddefinition ForthepurposesofthisEuropeanStandardthefollowingtermanddefinitionapplies. 3.1 easeofdispersionDH PVCP measureoftheratea
24、twhichorthedegreetowhichapigmentorextenderachievesagivenlevelofdispersion whendispersedinaplasticsmaterial.TheDH PVCP isderivedfromtheincreaseincolourstrengthachievedbytwo rollmillingasspecifiedin8.2,relativetothecolourstrengthachievedasspecifiedin8.1 4Principle Usingatworollmill,thepigmentundertest
25、isdispersedat160 C5 Cinthebasiccompound.Themilledsheet obtainedinthiswayisthensubjectedtothehighershearingforcesresultingfromtworollmillingat130 C5 C. TheresultingincreaseincolourstrengthisameasureoftheeaseofdispersionDH PVCP.EN139002:2003(E) 4 5Material Asuitableandrecommendedbasiccompoundisdescrib
26、edinannexA.Analternativecompoundmaybeagreed betweentheinterestedpartiesandistobementionedinthetestreport. Thequantityofthepigmentusedshallbesuchthatadepthofshade(seeEN128771)ofapproximately1/25SD isachieved. 6Apparatus 6.1 Tworollmill Equippedwithheatingfacilitiesandhavingrollersadjustableforspacing
27、Therolldiametershallbebetween 80mmand200mm,andtheratioofthespeedsofrotationofthetworollersshallbebetween1:1,1and1:1,2. NOTE Ithasbeenfoundthatcomparableresultsondifferenttworollmillswillbeobtainedunderthefollowingconditions ratioofrollerdiametersofthetwomachines:between1:1and1:1,5, ratioofperiphera
28、lspeeds:between1:1and1:1,1, H k(bank)toH s(gapwidth)shouldbeH k/H s 20. Ifsmallerrollersetsareused(rollerdiametere.g.80mm),thesettingsofthethicknessofthemilledsheetfrom0,4mmto 0,5mmwiththerecommendedconditionsofsimilaritycanleadtodifficultieswithregardtotherequirementforarollingbank . 6.2 Platepress
29、 Providedwithheatingfacilitiesand,advantageously,withcoolingfacilitiesaswell. 6.3Photometer 7Sampling RepresentativesamplesofthecolouringmaterialstobetestedshallbetakenasdescribedinENISO15528. 8Procedure 8.1 Millingat160 C5 C Themixtureconsistingofthepigmentundertestandthebasiccompoundshallbeprocess
30、edtoproduceamilled sheet.Atestspecimenhavingdimensionsof1mmbyatleast50mm 50mmshallbeproducedfromaportionof themilledsheet. NOTE Inthismethodincreasedshearisobtainedbymillingthereferencesheetatalowertemperatureof130 C,asa resultofwhichthewettingoutpropertiesofthePVCPcompoundarealsochanged.Theroutineu
31、seofthismethodthus requireseitherthatthetemperatureofasinglemillisincreasedanddecreased,whichistimeconsuming,orthattwomills operatingsimultaneouslyatdifferenttemperaturesareemployed.Analternativeprinciplebywhichthemillingtemperatureis maintained,andincreasedshearisgeneratedbyreducingthegapasinEN1287
32、74,isbeinginvestigatedforcomparabilityand asapotentiallymoreefficientmethod. 8.1.1 Premixingofthetestmaterials TheprescribedquantitiesofcolouringmaterialandbasicPVCPcompoundrequiredforthetestspecimensare mixedtogetherinasuitablecontainer,forexampleusingamixingshaker,for5min.EN139002:2003(E) 5 NOTE I
33、nthecaseofcolouringmaterialsinpasteform,itisrecommendedtomixthecomponentsinapolyethyleneor polypropylenebeakerbyhandusingamixingrod(notofglass)untilthemixtureappearstobehomogeneous. 8.1.2Tworoll milling Thepremixedmaterialisaddedtotherotatingmillrollswhichhavebeenbroughttoatemperatureof 160 C5 C.Any
34、materialfallingthroughthenipshallbereturnedquicklyandcarefullyfromthetraytothe movingmillrolls. Thequantityofmixturetobeusedshallbesuchthatacontinuouslyrotationbeadisformedinthenip,oncethe sheethasbeenformed.Setthegapsothatthesheethasauniformthicknessof0,4mmto0,5mmthickness acrossitswidth. Millthema
35、terial,limitingthewidthofthesheetbyfrequentcuttingtoonehalfandbyreversalandlateralrolling,to preventthematerialfromrunningupontotherollguidesandtoachieveadequatedispersionofthecolouring material.Alternativelyitmayberemovedrepeatedlyandreturnedwithoutdelaytotherollstoensurethorough mixing.Inthiscaset
36、henumberofsuchrepetitionsshallbedefinedaspartofthemethodandrecordedinthetest report. Mixingiscarriedoutforatotalof200rotationsoftherolls.Accordingtothediameteroftherollsofthemachine beingused(see6.1)thedurationofmillingshallnotbelessthan5minbutshallnotexceed10min. Thesheetisthenremovedfromtherolls.T
37、ofacilitatethissteptherollgapand,ifnecessary,rollspeedandfriction maybeadjusted. Aftereachmillingoperationtherollsshallbecleaned. 8.1.3Pressing Forphotometricmeasurementitisadvantageoustopreparespecimenswithahighsurfaceglossandquality. Suchspecimensmaybeobtainedbypressingthesheetsinaplatepressfornol
38、ongerthat2minat165 Ctomax. 170 Cbetweenhighglosschromesteelplatesusingaspacerframeof1mmthickness.Thepressedsheetsshall becooledrapidlytoroomtemperature. 8.2 Millingat130 C5 C Theremainderofthemilledsheetpreparedasspecifiedin8.1shallbeusedforthispurpose.Therollergapshall beset,andmaintainedunchangedd
39、uringrollmilling,suchthatamilledsheethavingathicknessof0,4mmto 0,5mmisproduced.Therollertemperaturesshallbemaintainedat130 C5 C. Themilledsheetshallfirstbepassedthroughtherollergapunfolded,thenfoldedonceandpassedwithoutdelay throughthegapagain.Thisprocedure(i.e.foldedonce)shallberepeatedtentimes.Ate
40、stspecimenhaving dimensionsof1mmbyatleast50mm 50mmshallbepreparedbypressingasspecifiedin8.1.3. 9Photometric measurement Thecolourstrengthofthetestspecimenspreparedasspecifiedin8.1and8.2shallbemeasuredasspecifiedin ISO 77242 : 1984,clause9.Thesevaluesshallbeusedtodeterminethecolourstrengthasspecified
41、in ENISO78724:1995,8.1andclause9forthepurposesofthecalculationofDH PVCP . 10Evaluation 10.1 Evaluationofcolouristicpropertiesinawhitereduction Forqualitycontrolpurposesthecolouristicpropertiesandcolourdifferencesofthetestspecimensrelativetoa standardshallbemeasuredasspecifiedinclause9. NOTE Thecolou
42、risticpropertiesinafullshadesystemcanbecarriedoutinasimilarmannerbutwithoutadditionofTiO 2.EN139002:2003(E) 6 10.2 Evaluationoftheeaseofdispersion TheeaseofdispersionDH PVCP isthepercentageincreaseincolourstrengthfollowingrollmillingat130 C.It shallbecomputedfromtheFvalues,usingthefollowingequation: - = - 1 100 1 2 F F DH P PVC where F 1 isthecolourstrengthvalueofthetestspecimen,specifiedin8.1; F 2 isthecolourstrengthvalueofthetestspecimenspecifiedin8.2. 11 Testreport Thetestreportshallcontainatleastthefollowinginformation: a) alldetailsnecessarytoidentifytheproductte
