1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS EN ISO 3451-4:2000 The
2、 European Standard EN ISO 3451-4:2000 has the status of a British Standard ICS 83.080.20 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Plastics Determination of ash Part 4: PolyamidesThis British Standard, having been prepared under the direction of the Sector Committee for
3、Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 November 2000 BSI 11-2000 ISBN 0 580 36678 2 BS EN ISO 3451-4:2000 Amendments issued since publication Amd. No. Date Comments National foreword This British Standard is the official Engl
4、ish language version of EN ISO 3451-4:2000. It is identical with ISO 3451-4:1998. It supersedes BS EN ISO 3451-4:1996 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee PRI/21, Testing of plastics, which has the responsibility to: aid enquirers to unders
5、tand the text; present to the responsible international/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. A list of organizations represented on t
6、his committee can be obtained on request to its secretary. Cross-references Attention is drawn to the fact that CEN and CENELEC Standards normally include an annex which lists normative references to international publications with their corresponding European publications. The British Standards whi
7、ch implement international or European publications referred to in this document may be found in the BSI Standards 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 n
8、ot purport to include all the necessary provisions of a contract. Users of British Standards are responsible for 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
9、front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii and iii, a blank page, pages 1 to 5, 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 N
10、ORMEEUROPENNE EUROPISCHENORM ENISO34514 September2000 ICS83.080.20 SupersedesENISO34514:1995 Englishversion PlasticsDeterminationofashPart4:Polyamides(ISO3451 4:1998) PlastiquesDterminationdutauxdecendresPartie4: Polyamides(ISO34514:1998) KunststoffeBestimmungderAscheTeil4:Polyamide (ISO34514:1998)
11、ThisEuropeanStandardwasapprovedbyCENon8September2000. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsma
12、ybeobtainedonapplicationtotheCentralSecretariatortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheCentralSecretariathasthesamestatusast heofficial
13、versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKO
14、MITEEFRNORMUNG CentralSecretariat:ruedeStassart,36B1050Brussels 2000CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO34514:2000EForeword ThetextoftheInternationalStandardfromTechnicalCommitteeISO/TC61“Plastics“ofthe International OrganizationforSt
15、andardization(ISO)hasbeentakenoverasanEuropeanStandardby TechnicalCommitteeCEN/TC249“Plastics“,thesecretariatofwhichisheldbyIBN. ThisEuropeanStandardshallbegive nthestatusofanationalstandard,either bypublicationofan identicaltextorbyendorsement,a tthelatestbyMarch2001 ,andconflictingnationalstandard
16、sshall bewithdrawnatthelatestbyMarch2001. ThisEuropeanStandardsupersedesENISO34514:1995. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationso f the followingcountriesar e boundtoimplemen t thisEuropeanStandard : Austria,Belgium,Czech Republic, Denmark,Finland,France , Germ
17、any,Greece,Iceland , Ireland,Italy,Luxembourg , Netherlands,Norway, Portugal,Spain,Sweden,SwitzerlandandtheUnitedKingdom. Endorsementnotice ThetextoftheInternationalStandardISO34514:1998hasbeenapprovedbyCENasaEuropean Standardwithoutanymodification. NOTE:NormativereferencestoInternationalStandardsar
18、elistedinannexZA(normative). ENISO34514:2000 A Referencenumbe r ISO34514:1998 (E) INTERNATIONAL STANDARD ISO 34514 Secondedition 19981215 PlasticsDeterminationofash Part4: Polyamides PlastiquesDterminationdutauxdecendres Partie4:Polyamides ENISO34514:2000 ii Contents 1Scop e1 2Normativereferenc e1 3
19、Principl e1 3.1Unfilledmaterial s1 3.2Filledandglassfibrereinforcedmaterial s1 3.3Flameretardantmaterialsreinforcedwithglassfibr e2 4Reagents (methodCormethodAinthepresenceofDBB ).2 5Apparatu s.2 6Procedur e.2 6.1Testportio n.2 6.2Unfilledmaterial s3 6.3Filledandglassfibrereinforcedmaterial s3 6.4Ma
20、terialsreinforcedwithglassfibrecontainingflameretardantantimonytrioxideand/orother volatilizableadditive s.3 7Expressionofresult s4 8Precisio n.4 9Testrepor t4 ENISO34514:2000 iii Foreword ISO (the InternationalOrganizationforStandardization)isaworldwidefederationofnationalstandardsbodies(ISO member
21、bodies).TheworkofpreparingInternationalStandardsisnormallycarriedoutthroughISOtechnical committees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhas therighttoberepresentedonthatcommittee.Internationalorganizations,governmentalandnongovernmental,in liaisonwithISO,als
22、otakepartinthework.ISOcollaboratescloselywiththeInternationalElectrotechnical Commission(IEC)onallmattersofelectrotechnicalstandardization. DraftInternationalStandardsadoptedbythetechnicalcommitteesarecirculatedtoth ememberbodiesforvoting. PublicationasanInternationalStandardrequiresapprovalbyatleas
23、t75%ofthememberbodiescastingavote. InternationalStandardISO34514waspreparedbyTechnicalCommitteeISO/TC61, Plastics, SubcommitteeSC5, Physicalchemicalproperties . Thissecondeditioncancelsandreplacesthefirstedition(ISO34514:1986),whichhasbeentechnicallyrevised. ISO3451consistsofthefollowingparts,undert
24、hegeneraltitle PlasticsDeterminationofash : Part1:Generalmethods Part2:Poly(alkyleneterephthalate)materials Part3:Unplasticizedcelluloseacetate Part4:Polyamides Part5:Poly(vinylchloride) ENISO34514:2000 ENISO34514:2000 1 PlasticsDeterminationofash Part4: Polyamides WARNING This part ofISO 3451mayinv
25、olvehazardouschemicals,materialsandoperations.Thispart of ISO 3451doesnotpurporttoaddressthesafetyproblemsassociatedwithitsuse.Itistheresponsibility oftheusertoestablishpropersafetyandhealthpracticesanddeterminetheapplicabilityofregulatory limitationspriortouse. 1Scope ThispartofISO 3451specifiesmet
26、hodsfordeterminationoftheashofpolyamides,bothfilledandunfilled.The generalproceduresgiveninISO34511arefollowed.For unfilledmaterialsmethodA ormethodCof ISO34511:1997isused.ForfilledandglassfibrereinforcedmaterialsmethodAofISO34511:1997isused. Forglassfibrefilledmaterialscontainingflameretardant,anti
27、monytrioxide,and/orother,volatilizable,additives suchaspigmentzincsulfide,amodificationisincorporatedtoremovetheseasvolatilebrominecomponent(s). 2Normativereference The following standard contains provisions which,throughreferenceinthistext,constituteprovisionsofthispartof ISO3451.Atthetimeofpublica
28、tion,theeditionindicatedwasvalid.Allstandardsaresubjecttorevision,and partiestoagreementsbasedonthispartofISO 3451areencouragedt oinvestigatethepossibilityofapplyingthe mostrecenteditionofthestandardindicatedbelow.MembersofIECan dISOmaintainregistersofcurrentlyvalid InternationalStandards. ISO34511:
29、1997, PlasticsDeterminationofashPart1:Generalmethods. 3Principle 3.1Unfilledmaterials Directcalcinationbyburningtheorganicmatterandtreatingtheresidueatahightemperatureuntilconstan t mass is reached(ISO34511:1997,methodA). Ifthematerialcontainsmetalhalidesand/ormetals(especiallyi nthepresenceofhaloge
30、natedmaterial)whichare liabletoevaporateduringburningoftheorganicmatter,calcinationaftersulfatio n can be applied (ISO 34511:1997, methodC).Thisprocedureiscarriedoutbyheatingtheorganicmattertogetherwithconcentrate d sulfuric acid up to a temperature where fuming and subsequent burningoftheorganicmat
31、teroccurs,andfinallytreatingtheresidueat ahightemperatureuntilconstantmassisreached. 3.2Filledandglassfibrereinforcedmaterials Direct calcination, by burning the organic matterandtreatingtheresidueatahightemperatureuntilconstantmass isreached(ISO34511:1997,methodA)(seenote1in3.3). ENISO34514:2000 2
32、3.3Flameretardantmaterialsreinforcedwithglassfibre Calcinationbyburningtheorganicmatterinthepresenceofdecabromobiphenyl(DBB)andfinallytreatingthe residueatahightemperatureuntilconstantmassisreached(ISO34511:1997,methodA). NOTE 1 Someadditives,forinstancezincsulfide,arealsocompletelyvolatilizedasbrom
33、idesbyburnin g the organic matter in contact with decabromobiphenyl (DBB).Informationwithrespecttotheadditive(s)presentinthematerialandthepotentia l to evaporateduringburningincontactwithDBBshouldberequestedfromthesupplierorobtainedbytestingonthepure chemical. NOTE2 Flameretardantswithahighbromineco
34、ntent,forinstanceethylenebis(tetrabromophthalimide)orbrominated polystyrenemayalsobeused.Theapplicabilityandamountofchemicaltobeusedca nbedeterminedbycarryingoutash determinationsinaccordancewith6.4withincreasingamountsofflameretardantuntilaconstantresultisobtained.The chemicalshouldbeappliedasapowd
35、er. 4Reagents (methodCormethodAinthepresenceofDBB) Duringtheanalysis,useonlyreagentsofanalyticalgradeorspecifiedgradeandonlydistilledwaterorwaterof equivalentpurity. 4.1 Ammoniumcarbonate, anhydrous. 4.2 Ammoniumnitrate, approximately10% (m/m)solution. 4.3 Sulfuricacid, r1,84g/ml. 4.4 Decabromobiphe
36、nyl(DBB) ,powder,technicalgradeorhigherpurity. WARNING Theuseofdecabromobiphenylmayresultinth e formation of dioxins. Temperatures in the orderof600 Cto850 Caregenerallyknownasidealtemperaturesfortheformationofdioxins. 5Apparatus Apparatusspecifiedinclause4ofISO34511:1997,andinparticular: 5.1 Crucib
37、lesofsilica,porcelainorplatinum, inerttothematerialtested,an dtypicallyofdiameter(upperpart) 50mmto60mmandheightequaltothediameter(seenote2in3.3). 5.2 Mufflefurnace, capableofbein gmaintainedat(600 25)C ,(850 50) Corataminimumtemperatureof 850 C. 5.3 Fumecupboard. 6Procedure Thematerialshallbeinthef
38、ormofsmallpiecesof 1 cm 0,5cm 0,2 cm or smaller, granulesorpowder.Filledor reinforcedmaterialsshallbedriedbeforecalcination,i.e.byheatingat100 Cuntilconstantmassisreached. 6.1Testportion Takeaquantityofthetestsamplesufficienttoyield 5 mgto20 0 mgofash(seetabl e 1).Inthecase ofreinforced materials,ta
39、keatestportionof 2 gormore.Ifthelikelyquantityofashisunknown,carryout apreliminaryash determination.Accordingtotheapproximateashcontent,choosethesizeofthetestportiontobeusedfrom table1. ENISO34514:2000 3 Table1Massoftestportion Approximateash Testportion Massofashobtained %gmg 200 5to10 .0,01to0,05
40、100 10to50 .0,05to0,1 50 25to50 .0,1to0,2 25 25to50 .0,2to1 10 20to100 .1to10 5 50to500 .10 2 200 6.2Unfilledmaterials FollowtheproceduredescribedinISO34511:1997,methodA,applyingacalcinationtemperatureof(85 0 50)C. Ifthematerialcontainsmetalhalidesormetalsinthepresenceofhalogenatedmaterial,liabletoe
41、vaporateduring thecalcinationprocedure,orinthosecaseswhere“sulfatedash”isrequired,methodCshal lbeapplied (ISO34511:1997,methodC). 6.3Filledandglassfibrereinforcedmaterials FollowtheproceduredescribedinISO34511:1997,methodA,applyingacalcinationtemperatur e of (850 50)C. Ifatthattemperatureglassfibres
42、presentbecomemoltenan d thus prevent further calcination of the polymer, lower thetemperatureofcalcinationto(600 25)Candrepeattheprocedurewithafreshtestportion. 6.4Materialsreinforcedwithglassfibrecontainingflameretardantantimonytrioxideand/or othervolatilizableadditives Thesampleshallbegroundorcutt
43、opiecesof 1 cm 0,5cm 0,2 cmorsmaller.Proceedasi n 5.3.1 and 5.3.2 of ISO34511:1997,methodA. AddtothesampleaquantityofDBB(4.4)equaltohalfthemassofthesamplei ngramsandmixwellinthe crucible.Placethecrucibleinthemufflefurnace,applyingacalcinationtemperatur eofatleast850 C.Themuffle furnaceshallbeplacedinafumecupboard.ContinueasdirectedinISO34511:1997,from5.3.4ofmethodA. Directlyplacingthecrucibleintothemufflefurnaceispreferred.Ifdirectcalcinationleadstolargedifferences betweenrepeatedtests,forinstanceduetolossofashcontainingmaterial,gentlyheatthecrucibleover
