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
