1、BRITISH STANDARD BS EN ISO 3451-5:2002 Plastics Determination of ash Part 5: Poly(vinyl chloride) The European Standard EN ISO 3451-5:2002 has the status of a British Standard ICS 83.080.20 BS EN ISO 3451-5:2002 This British Standard, having been prepared under the direction of the Materials and Che
2、micals Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 30 August 2002 BSI 30 August 2002 ISBN 0 580 40321 1 National foreword This British Standard is the official English language version of EN ISO 3451-5:2002. It is identica
3、l with ISO 3451-5:2002. It supersedes BS EN ISO 3451-5:1997 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee PRI/21, Plastics test methods, which has the responsibility to: A list of organizations represented on this committee can be obtained on reques
4、t to its secretary. Cross-references The British Standards which 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 Ele
5、ctronic Catalogue or of British Standards Online. This publication 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
6、 understand 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. Summary of pages This document co
7、mprises a front cover, an inside 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 date displayed in this document indicates when the document was
8、 last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO34515 July2002 ICS83.080.20 SupersedesENISO34515:1996 Englishversion PlasticsDeterminationofashPart5:Poly(vinylchloride)(ISO 34515:2002) PlastiquesDterminationdutauxdecendresPa
9、rtie5: Poly(chloruredevinyle)(ISO34515:2002) KunststoffeBestimmungderAscheTeil5: Poly(vinylchlorid)(ISO34515:2002) ThisEuropeanStandardwasapprovedbyCENon24June2002. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofana
10、tionalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation underthe
11、responsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,
12、Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2002CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO34515:2002ECORRECTE
13、D20020724 Foreword Thisdocument(ENISO34515:2002)hasbeenpreparedbyTechnicalCommitteeISO/TC61 “Plastics“incollaborationwithTechnicalCommitteeCEN/TC249“Plastics“,thesecretariatof whichisheldbyIBN. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublication ofanidenticaltextorbyendo
14、rsement,atthelatestbyJanuary2003,andconflictingnational standardsshallbewithdrawnatthelatestbyJanuary2003. ThisdocumentsupersedesENISO34515:1996. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsof thefollowingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belg
15、ium, CzechRepublic,Denmark,Finland,France,Germany,Greece,Iceland,Ireland,Italy, Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,Switzerlandandthe UnitedKingdom. Endorsementnotice ThetextoftheInternationalStandardISO34515:2002hasbeenapprovedbyCENasa EuropeanStandardwithoutanymodifications.
16、NOTENormativereferencestoInternationalStandardsarelistedinannexZA(normative). ENISO34515:2002 INTERNATIONAL STANDARD ISO 3451-5 Second edition 2002-07-01 Reference number ISO 3451-5:2002(E) Plastics Determination of ash Part 5: Poly(vinyl chloride) Plastiques Dtermination du taux de cendres Partie 5
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20、 erom teh tneCS larterceratai ta thserdda es igvne olebw. ISO 2002 Ar llieser sthgrvsselnU .de torehceps esiwfi,dei rap ont iht fos bupliactim noarper eb yro decudo tuzilina ni dey from b roy nasnaem y, tcelernahcem ro cinoicla, inclidung tohppocoying m dnaicrfomli, tiwtuoh permini noiss wrtif gnirm
21、o ietI rehSO ta tserdda eheb slow or SIsO memreb ydob in toc ehtnury fo tr ehtseuqeer. ISO copyrithg fofiec tsop esaCela 65 G 1121-HCeneva 02 T.le + 22 14 10 947 11 ENISO34515:2002 iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards b
22、odies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizati
23、ons, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the
24、 ISO/IEC Directives, Part 3. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that s
25、ome of the elements of this part of ISO 3451 may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 3451-5 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical-chemical propertie
26、s. This second edition cancels and replaces the first edition (ISO 3451-5:1989), which has been technically revised. ISO 3451 consists of the following parts, under the general title Plastics Determination of ash: Part 1: General methods Part 2: Poly(alkylene terephthalate) materials Part 3: Unplast
27、icized cellulose acetate Part 4: Polyamides Part 5: Poly(vinyl chloride) ENISO34515:2002 1 Plastics Determination of ash Part 5: Poly(vinyl chloride) WARNING The use of this part of ISO 3451 may involve hazardous chemicals, materials, operations or equipment. This standard does not purport to addres
28、s the safety problems associated with its use. It is the responsibility of the user of this standard to establish proper safety and health practices and determine the application of regulatory limitations prior to use. Poly(vinyl chloride) evolves hydrogen chloride on thermal decomposition and preca
29、utions should be taken to avoid inhalation of these or other fumes. 1 Scope This part of ISO 3451 specifies three methods for the determination of the ash of poly(vinyl chloride). The general procedures given in ISO 3451-1 are followed. For ash, method A is used. For sulfated ash, methods B and C ar
30、e used. All three methods are applicable to resins, compounds and finished products. Methods B and C are applicable when lead-containing compounds are present. 2 Normative reference The following normative document contains provisions which, through reference in this text, constitute provisions of t
31、his part of ISO 3451. For dated references, subsequent amendments to, or revisions of, this publication do not apply. However, parties to agreements based on this part of ISO 3451 are encouraged to investigate the possibility of applying the most recent edition of the normative document indicated be
32、low. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 3451-1:1997, Plastics Determination of ash Part 1: General methods 3 Principle 3.1 Method A (direct calcination) Th
33、e organic matter in a test portion is burnt off and the residue is heated at until constant mass is reached. 3.2 Method B (calcination, with sulfuric acid treatment after combustion) The organic matter in a test portion is burnt off, the residue is converted into sulfates using concentrated sulfuric
34、 acid and, finally, the residue is heated at until constant mass is reached. 3.3 Method C (calcination, with sulfuric acid treatment before combustion) The organic matter in a test portion is burnt off after adding concentrated sulfuric acid and the residue is heated atuntil constant mass is reached
35、. This method is recommended over method B because of the better reproducibility of the results. 950 C 950 C 950 C ENISO34515:2002 2 Method B or method C should be used if lead-containing compounds are present. 4 Reagents (for methods B and C only) 4.1 Sulfuric acid, density , analytical grade. 4.2
36、Acetic acid, , analytical grade. WARNING Care should be taken in handling sulfuric acid and acetic acid. 5 Apparatus Apparatus as specified in ISO 3451-1, and in particular: 5.1 Crucible of silica, platinum or porcelain with lid, diameter of upper part to , height equal to the diameter. The size sha
37、ll be such that the crucible is not more than half-filled by the test portion. 5.2 Bunsen burner, with silica triangle and tripod, or other suitable heating device. 5.3 Muffle furnace or microwave furnace, capable of being controlled thermostatically at . 5.4 Pipettes, of appropriate capacity (for m
38、ethods B and C only). WARNING In 7.3.4 and 7.4.3, it is required to use a pipette for the addition of concentrated sulfuric acid. The acid must be introduced into the pipette using a suitable device (e.g. a rubber-bulb pipette filler) and must never be sucked up by mouth. 5.5 Desiccator, containing
39、an effective drying agent that does not react chemically with the ash components. NOTE In some cases, the affinity of ash for water can be greater than that of drying agents commonly used. 5.6 Analytical balance, accurate to . 5.7 Weighing bottles. 6 Safety precautions 6.1 Always wear safety glasses
40、 when working in the laboratory. 6.2 Exercise all normal safety precautions when working with an open flame or at high temperatures. Use insulated gloves and long crucible tongs when putting samples in the muffle furnace or taking them out of it. 6.3 Carry out the heating of the sample in a fume cup
41、board, and for calcination use an appropriately vented muffle furnace. 6.4 Read carefully and follow strictly the instructions in the warnings at the beginning of the text and in clause 4 and subclauses 5.4 and 7.4.3. 7 Procedure 7.1 Test portion The recommended test portion size is given in Table 1
42、. 1,84 g/ml 100 % 45 mm 75 mm 950 C 50 C 0,1 mg ENISO34515:2002 3 7.2 Method A (determination of unsulfated ash) 7.2.1 Heat the clean crucible and lid (5.1) in the muffle furnace (5.3) at for and cool in the desiccator (5.5) to room temperature. Weigh the crucible with lid to the nearest . 7.2.2 Int
43、roduce into the crucible a suitable quantity of sample (see Table 1) (finished product samples should preferably be cut into small pieces). Weigh the crucible with lid and test portion to the nearest and calculate the mass of the test portion ( ). 7.2.3 Heat the crucible directly on the heating devi
44、ce (5.2) so that the test portion burns slowly and loss of ash is avoided. Continue this operation until no more smoke is evolved. In the event of violent burning, the test portion may be added in successive portions. 7.2.4 Partially close the crucible with the lid so that the volatile matter evolve
45、d does not carry away particles of ash. Place the crucible at the entrance of the muffle furnace maintained at (the temperature in the entrance zone is about to ), then advance the crucible slowly into the furnace. Calcinate for at . It is recommended that the design of the lid be such that, when pl
46、aced on the crucible, the lid fits well but does not close the crucible completely. 7.2.5 Remove the crucible with lid from the furnace, place it in the desiccator, allow to cool to room temperature and weigh to the nearest ( ). 7.2.6 Calcinate again, under the same conditions, until constant mass i
47、s reached; i.e. until the results of two consecutive weighings do not differ by more than . The total duration of heating in the furnace shall however not exceed . If constant mass is not attained after this time, the mass after shall be used for calculating the test results. 7.3 Method B (determina
48、tion of sulfated ash) 7.3.1 Proceed as detailed in 7.2.1. 7.3.2 Proceed as detailed in 7.2.2. 7.3.3 Proceed as detailed in 7.2.3. 7.3.4 After allowing the crucible and contents to cool, add concentrated sulfuric acid (4.1) dropwise by means of a pipette (5.4) of suitable capacity until the residue is soaked completely. Heat carefully on a suitable heating dev
