EN 13900-3-2003 en Pigments and extenders - Methods of dispersion and assessment of dispersibility in plastics - Part 3 Determination of colouristic properties and ease of dispersi.pdf

1、BRITISH STANDARD BS EN 13900-3:2003 Pigments and extenders Methods of dispersion and assessment of dispersibility in plastics Part 3: Determination of colouristic properties and ease of dispersion of black and colour pigments in polyethylene by two-roll milling The European Standard EN 13900-3:2003

2、has the status of a British Standard ICS 83.040.30 BS EN 13900-3:2003 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 41286 5 National foreword This British Standard is the official English lan

3、guage version of EN 13900-3:2003. 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 w

4、hich implement 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 publi

5、cation does 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 internation

6、al/European 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 p

7、age, pages 2 to 7 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 EN139003 February2003 ICS83.040.30 Englishversion Pigmentsandext

8、endersMethodsofdispersionand assessmentofdispersibilityinplasticsPart3:Determinationof colouristicpropertiesandeaseofdispersionofblackandcolour pigmentsinpolyethylenebytworollmilling PigmentsetmatiresdechargeMthodesdedispersion etvaluationdescaractristiquesdedispersibilitdansles plastiquesPartie3:Dt

9、erminationdesproprits colorimtriquesetdelafacilitdedispersiondespigments noirsetcolorsdanslepolythylneparcalandragesur bicylindre PigmenteundFllstoffeDispergierverfahrenund BeurteilungderDispergierbarleitinKunststoffenTeil3: BestimmungderkoloristischenEigenschaftenundder DispergierhrtevonSchwarzundB

10、untpigmentenin PolyethylenimWalztest ThisEuropeanStandardwasapprovedbyCENon12December2002. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferenc

11、esconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCent

12、rehasthesamestatusasthe 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. EUROPEANCOMMITTEEFO

13、RSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN139003:2003EEN139003:2003(E) 2 Foreword Thisdocument(EN139003:2003)hasbeenpre

14、paredbyTechnicalCommitteeCEN/TC298“Pigmentsand extenders“,thesecretariatofwhichisheldbyDIN. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyAugust2003,andconflictingnationalstandardsshallbewithdrawnatthelatestby August200

15、3. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal, Slovakia,S

16、pain,Sweden,SwitzerlandandtheUnitedKingdom.EN139003:2003(E) 3 1Scope ThispartofthisEuropeanStandardspecifiesamethodofdetermininginpolyethylene(PE)thecolouristicproperties ofatestpigmentrelativetoastandard,andtheeaseofdispersionDH PE ofpigmentsfromthedifferencesincolour strengthondispersingcolouringm

17、aterialsundervariousconditions. MethodAisappropriateforusewithorganicpowderpigmentsandcarbonblackpigmentsinpowderform,manyof whicharesubjecttocompaction(reagglomerationunderpressure),forinorganicpigmentsinpowderformandfor pigmentpreparationsinpowderorflakeform. MethodBisappropriatefortestingpigments

18、andpigmentpreparationsingranularformandforinorganicpigments inanyform. Theeaseofdispersiondeterminedinthiswayisvalidonlyforthedispersionequipment,dispersionconditionsand dispersionmediumbeingused.Theuseoftestconditionsdifferingfromthosespecifiedmaygivedifferentresults;this appliesbothtotheabsolutema

19、gnitudeandtotherelationbetweenvaluesoftheeaseofdispersionofvarious pigments.ThesubscriptDH PE isthereforeusedtodesignatethevalueobtainedasspecifiedinthispartofthis EuropeanStandard. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications.These

20、normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publication

21、referredtoapplies(includingamendments). EN128771, ColouringmaterialsinplasticsDeterminationofcolourstabilitytoheatduringprocessingofcolouring materialsinplasticsPart1:Generalintroduction. ENISO78724:1995, GeneralmethodoftestsforpigmentsandextendersPart24:Determinationofrelative tintingstrengthofcolo

22、uredpigmentsandrelativescatteringpowerofwhitepigmentsPhotometricmethods(ISO 78724:1985). ENISO15528, Paints,varnishesandrawmaterialsforpaintsandvarnishesSampling(ISO15528:2000). ISO77242:1984, PaintsandvarnishesColorimetryPart2:Colourmeasurement. 3 Termanddefinition ForthepurposesofthisEuropeanStand

23、ardthefollowingtermanddefinitionapplies. 3.1 easeofdispersionDH PE measureoftherateatwhichorthedegreetowhichapigmentorextenderachievesagivenlevelofdispersion whendispersedinaplasticsmaterial.TheDH PE isderivedfromtheincreaseincolourstrengthachievedbytworoll millingasspecifiedin8.2,relativetothecolou

24、rstrengthachieved asspecifiedin8.1 4Principle Usingatworollmill,thepigmentundertestisdispersedatanappropriatetemperatureinthepolymer.Thecooled milledsheetobtainedinthiswayisthensubjectedtothehighershearingforcesresultingfromtworollmillingata narrowergapwidth.Theresultingincreaseincolourstrength(seeE

25、N128771)isameasureoftheeaseofdispersion DH PE.EN139003:2003(E) 4 5Materials 5.1 MaterialsformethodA 5.1.1 Testmedium Polyethylene,inpowderorflakeform;ofatypeandgradetobeagreedbetweentheinterestedparties. NOTE WhereHDPEisused,aphenolicantioxidantcanbeusedtofacilitateprocessing. 5.1.2 Titaniumdioxidep

26、igment Easilydispersingpowdergradeofatyperecommendedforuseinpolyethylene. 5.2 MaterialsformethodB 5.2.1 Testmedium Polyethylene,ingranularform;ofatypeandgradetobeagreedbetweentheinterestedparties. NOTE WhereHDPEisused,aphenolicantioxidantcanbeusedtofacilitateprocessing. 5.2.2 Titaniumdioxidepigment

27、Asin5.1.2orasawelldispersedpolyethylenemasterbatch. 6Apparatus 6.1 Tworollmill Equippedwithheatingfacilitiesandhavingrollersadjustableforspacing.Therolldiametershallbebetween 80mmand200mm,andtheratioofthespeedsofrotationofthetworollersshallbebetween1:1,1and1:1,2. NOTE Ithasbeenfoundthatcomparableres

28、ultsondifferenttworollmillscanbeobtainedunderthefollowingconditions ratioofrollerdiametersofthetwomachines:between1:1and1:1,5; ratioofperipheralspeeds:between1:1and1:1,1; H k(bank)toH s(gapwidth)shouldbeH k/H s 20. Ifsmallerrollersetsareused(rollerdiametere.g.80mm),thesettingsofthethicknessofthemill

29、edsheetfrom0,4mmto 0,5mmwiththerecommendedconditionsofsimilaritycanleadtodifficultieswithregardtotherequirementforarollingbank . 6.2Plate press Providedwithheatingfacilitiesand,advantageously,alsowithcoolingfacilities. 6.3Photometer 7Sampling Representativesamplesofthecolouringmaterialstobetestedsha

30、llbetakenasdescribedinENISO15528.EN139003:2003(E) 5 8Procedure 8.1 Testingofcolouristicpropertiesinwhitereduction 8.1.1 Preparationofthemixtures 8.1.1.1 PreparationofthemixtureformethodA Inaplasticbeakerpreblendgently100partsofpolyethylenepowder,1,0partstitaniumdioxidepigment(5,0partsin thecaseofcar

31、bonblack)andwhereappropriate0,1partsantioxidant.Add0,1partsofcarbonblackororganictest pigmentor0,2partsto0,5partsofinorganictestpigmentaccordingtotype.Mixusingaspatulasothatnotest pigmentremainsonthebeakerwalls. NOTE1 Itcanbeadvantageoustopreparealargequantityofahomogeneouspreblendofpolymerpowder,an

32、tioxidantand titaniumdioxidepigmentforexamplebymixingfor5mininalaboratoryhighspeedmixerat1800min 1 followedbyextrusion andgrindingintoasuitablyfineforminordertoimprovereproducibility. 8.1.1.2 PreparationofthemixtureformethodB Prepareamixtureof100partsofPEgranulate(5.2.1)with1,0partstitaniumdioxidepi

33、gment(5,0partsinthecase ofcarbonblack)oranequivalentquantityoftitaniumdioxidemasterbatch(5.2.2)inaplasticbeakerorother suitablecontainer. 8.1.2Tworoll milling 8.1.2.1Method A Themixtureisaddedtotherotatingmillrollswhichhavebeenbroughttoadefinedtemperature,previously establishedasallowingeasyhandling

34、ofthepolymeronthemill.Temperaturesofbetween140 Cand160 C havebeenfoundsuitableformosttypesofpolymer. Withagapwidthsetat0,4mmto0,5mmasheetisformedwithinapproximately1mininsuchawaythatthe wholeofthematerialformsacontinuoussheetonthefrontroll.Anymaterialfallingthroughthenipshallbe returnedquicklyandcar

35、efullyfromthetraytotherotatingmillrolls.Thequantityofmixturetobeusedshallbesuch thatacontinuouslyrotationbeadisformedinthenip,oncethesheethasbeenformed. NOTE Aquantityoftestmixturebasedon100gpolymershouldgenerallybeadequateformosttworollmills.Itcanif necessaryincreasedaccordingtothesizeofthemillinor

36、dertofacilitatehandling. Thedispersionofthepigmentisobtainedbycuttingandfoldingofthesheet,onceformed,every30swhilstmilling withagapwidthsetat0,5mmforatotalof200rotationsoftherolls,countingfromthepointatwhichthemixtureis addedtothemill.Accordingtothediameteroftherollsofthemachinebeingused(see6.1)thed

37、urationofmilling shallnotbelessthan5minbutshallnotexceed10min. 8.1.2.2Method B Placethemixtureonthestatic,previouslyheatedtworollmillusingthegapwidthandtemperaturesasdescribed in8.1.2.1andallowtopreheatfor1min.Startthetworollmillandprepareamillsheetinabout1min.Addthetest pigmentorpigmentpreparations

38、lowlyandevenlytotherotatingsheetacrossthewidthofthemill.Thedispersion ofthepigmentthenproceedsasin8.1.2.1. Aftereachmillingoperationtherollsshallbecleaned.EN139003:2003(E) 6 8.1.3Pressing Forphotometricmeasurementitisadvantageoustopreparespecimenswithahighsurfaceglossandquality. Suchspecimensmaybeob

39、tainedbypressingthesheetsinaplatepressfornolongerthat2minat160 Ctomax. 170 Cbetweenhighglosschromesteelplatesusingaspacerframeof1mmthickness.Thepressedsheetsshall becooledrapidlytoroomtemperature. 8.1.4Photometric measurement Thecolourstrengthandcolouristicpropertiesofthetestspecimenspreparedasspeci

40、fiedin8.1.2and8.1.3shallbe measuredasspecifiedinISO77242:1984,clause9.Thesevaluesshallbeusedtodeterminethecolourstrengthas specifiedinENISO78724:1995,8.1andclause9forthepurposesofthecalculationofDH PE . 8.2 Testingofeaseofdispersion 8.2.1 Preparationofthetestsamples Therollgapofthemillisreducedto0,3

41、mmandonehalfofthesheetpreparedunder8.1.2isreturnedtotherollers maintainedatthesametemperatureasusedin8.1.2at25min 1 .Millingiscontinuedfor200revolutionsoftherolls withcuttingandfoldingevery30s.Thesheetisthenremovedandcooledbetweenmetalplates. Thisprocedureiscarriedoutforeachsheetcontainingthetestpig

42、ments. Aftereachmillingoperationtherollsshallbecleaned. 8.2.2Pressing and photometric measurement Pressingandphotometricmeasurementarecarriedoutasdescribedin8.1.3and8.1.4. 9Evaluation TheeaseofdispersionDH PE isexpressedasthepercentageincreaseincolourstrengthfollowingrollmillingat 0,3mmgapwidthrelat

43、ivetothatobtainedfollowingmillingat0,5mm(see8.1). ItshallbecomputedfromtheFvalues,usingthefollowingequation: - = 1 100 1 2 PE F F DH where F 1 isthecolourstrengthvalueofthetestspecimen,specifiedin8.1; F 2 isthecolourstrengthvalueofthetestspecimen,specifiedin8.2. 10 Testreport Thetestreportshallcontainatleastthefollowinginform