DIN EN ISO 6427-2014 Plastics - Determination of matter extractable by organic solvents (conventional methods) (ISO 6427 2013) German version EN ISO 6427 2014《塑料 使用有机溶剂测定可萃取物质(标准方法.pdf

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1、August 2014Translation by DIN-Sprachendienst.English price group 12No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS

2、83.080.01!%:1-“2231410www.din.deDDIN EN ISO 6427Plastics Determination of matter extractable by organic solvents (conventionalmethods) (ISO 6427:2013);English version EN ISO 6427:2014,English translation of DIN EN ISO 6427:2014-08Kunststoffe Bestimmung der extrahierbaren Bestandteile durch organisch

3、e Lsemittel(Standardverfahren) (ISO 6427:2013);Englische Fassung EN ISO 6427:2014,Englische bersetzung von DIN EN ISO 6427:2014-08Plastiques Dtermination des matires extractibles par des solvants organiques (Mthodesconventionnelles) (ISO 6427:2013);Version anglaise EN ISO 6427:2014,Traduction anglai

4、se de DIN EN ISO 6427:2014-08SupersedesDIN EN ISO 6427:1998-10,withdrawn 2008-04www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises 23 pages07.14 2 A comma is used as the decimal marker. National foreword The text of ISO 6427:2013 has been

5、prepared by Technical Committee ISO/TC 61 “Plastics” and has been taken over as EN ISO 6427:2014 by Technical Committee CEN/TC 249 “Plastics” (Secretariat: NBN, Belgium). The responsible German body involved in its preparation was the Normenausschuss Kunststoffe (DIN Standards Committee Plastics), W

6、orking Committee NA 054-01-03 AA Physikalische, rheologische und analytische Prfungen. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 308 DIN EN ISO 308 ISO 383 DIN 12242-1 ISO 565 DIN ISO 565 ISO 1773 DIN 12347, DIN 12380, DIN ISO 177

7、3 There is no DIN Standard available which corresponds to the International Standard ISO 1875. Amendments This standard differs from DIN EN ISO 6427:1998-10 as follows: a) normative references have been updated; b) Table 2 “Further processing” has been added; c) Annex ZA has been deleted; d) the Bib

8、liography has been updated; Previous editions DIN 53738: 1972-11, 1983-10 DIN EN ISO 6427: 1998-10 DIN EN ISO 6427:2014-08 DIN EN ISO 6427:2014-08 3 National Annex NA (informative) Bibliography DIN 12242-1, Laboratory glassware Interchangeable conical ground joints Dimensions, tolerances DIN 12347,

9、Laboratory glassware Round bottom and flat bottom flasks DIN 12380, Laboratory glassware Conical flasks, narrow neck DIN EN ISO 308, Plastics Phenolic moulding materials Determination of acetone-soluble matter (apparent resin content of material in the unmoulded state) DIN ISO 565, Test sieves Metal

10、 wire cloth, perforated metal plate and electroformed sheet Nominal sizes of openings DIN ISO 1773, Laboratory glassware Narrow-necked boiling flasks DIN EN ISO 6427:2014-08 4 This page is intentionally blank EN ISO 6427 June 2014 ICS 83.080.01 English Version Plastics - Determination of matter extr

11、actable by organic solvents (conventional methods) (ISO 6427:2013) Plastiques - Dtermination des matires extractibles pardes solvan ts organiqu es (Mthod es conventionnelles) (ISO 6427:2013)Kunststoffe - Bestimmung der extrahierbaren Bestandteiledurch organisc he Lsemit tel (Standardverfahren) (ISO

12、6427:2013)This European Standard was approved by CEN on 29 May 2014. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographic

13、al references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility

14、of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of M

15、acedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2014

16、CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 6427:2014 EEUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMContents Page Foreword

17、. 3 Introduction . 4 1 Scope . 5 2 Normative references. 5 3 Reagents and materials . 5 4 Apparatus 6 5 Preparation of test sample 8 6 Number of tests 8 7 Procedure 8 8 Expression of results . 9 9 Precision . 10 10 Test report . 10 Annex A (normative) Procedure for casting, drying, and cutting films

18、 of cellulose acetate . 14 Annex B (normative) Determination of solubility of polypropylene in cold p-xylene . 16 Bibliography 19 2DIN EN ISO 6427:2014-08EN ISO 6427:2014 (E)Foreword The text of ISO 6427:2013 has been prepared by Technical Committee ISO/TC 61 “Plastics” of the International Organiza

19、tion for Standardization (ISO) and has been taken over as EN ISO 6427:2014 by Technical Committee CEN/TC 249 “Plastics” the secretariat of which is held by NBN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at t

20、he latest by December 2014, and conflicting national standards shall be withdrawn at the latest by December 2014. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any

21、 or all such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republ

22、ic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 6427:2013 has been appro

23、ved by CEN as EN ISO 6427:2014 without any modification. 3DIN EN ISO 6427:2014-08EN ISO 6427:2014 (E)IntroductionThere are several very similar national and international standards for determination of the percentage of extractable matter, with only slight differences in the procedures. To facilitat

24、e the work of the laboratory staff which has to carry out these determinations on various plastics products, the generally applicable methods are described in this International Standard.4DIN EN ISO 6427:2014-08EN ISO 6427:2014 (E)1 ScopeThis International Standard specifies methods for the determin

25、ation of components in plastics that can be extracted by hot organic liquids near their boiling points. For one special case, a so-called cold-extraction method is given in Annex B.The extractable components can be monomers, oligomers, polymers, plasticizers, stabilizers, etc. The kind and percentag

26、e of extractable matter influence the properties of plastics.The recommended extraction liquid depends on the type of plastic and on the purpose of the determination (see Table 1). The extracted amounts of special constituents are often not quantitative in the sense of analytical chemistry.This Inte

27、rnational Standard does not apply to plastics that come into contact with food or drinking water. Special regulations for those plastics are established in many countries. In order to test plastics for compliance with these regulations, methods other than those given in this International Standard a

28、re used in most cases. The methods of this International Standard are not intended to be used for migration tests.If this International Standard is used to test plastics other than those mentioned in Table 1, the operating conditions is intended to be agreed upon by the interested parties.2 Normativ

29、e referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) appl

30、ies.ISO 308, Plastics Phenolic moulding materials Determination of acetone-soluble matter (apparent resin content of material in the unmoulded state)ISO 383, Laboratory glassware Interchangeable conical ground jointsISO 565, Test sieves Metal wire cloth, perforated metal plate and electroformed shee

31、t Nominal sizes of openingsISO 1773, Laboratory glassware Narrow-necked boiling flasksISO 1875, Plastics Plasticized cellulose acetate Determination of matter extractable by diethyl ether3 Reagents and materials3.1 Extraction liquid, of recognized analytical grade, to be selected according to the re

32、quirements of the plastic material being tested (see Table 1).3.2 Antibumping granules.3.3 Glass wool, pre-extracted.5DIN EN ISO 6427:2014-08EN ISO 6427:2014 (E)4 Apparatus4.1 Mill, for reducing the sample to the required grain size.A mill in which the sample is cut between rotating and stationary b

33、lades is preferred. Large pieces can be reduced in size with a pair of shears before they are fed into the mill.4.2 Set of sieves, complying with the requirements of ISO 565.4.3 Flat-bottomed flask, of suitable capacity, for example 250 ml, complying with the requirements of ISO 1773, with ground-gl

34、ass neck complying with the requirements of ISO 383.4.4 Extraction apparatus, of such a design that the crucible or thimble is heated by the rising vapour of the extraction liquid.4.4.1 Soxhlet extractor, as shown in Figure 1.4.4.2 Other extractors, for example that designed by Twisselmann (see Figu

35、re 2), may be used, if they give the same results as the Soxhlet extractor.4.5 Container, for the test portion to be extracted: chosen from one of the following:4.5.1 Cellulose paper thimble, of suitable size, for example diameter 33 mm and length 94 mm.4.5.2 Metal wire basket, of the same dimension

36、s as the thimble (4.5.1).4.5.3 Glass-filter crucible, pore size 40 m to 100 m.NOTE The choice of a suitable container for the extraction is very important. The mass of the cellulose thimble (4.5.1) depends on its moisture content, and this can lead to variable results when weighing. The metal wire b

37、asket (4.5.2) cannot be used with a powder sample or if a chemical reaction is possible between the metal and any of the components of the plastic. Difficulties can be caused by penetration of components of the plastic into the pores of the glass-filter crucible (4.5.3) and subsequent swelling.4.6 R

38、eflux condenser, fitted with a ground-glass cone to fit the extraction apparatus (4.4), for example a Dimroth condenser.4.7 Heating device, which does not use a naked flame and is explosion-proof, suitable for use with the flask (4.3).4.8 Balance, accurate to 0,1 mg.4.9 Desiccator, containing calciu

39、m chloride or silica gel.6DIN EN ISO 6427:2014-08EN ISO 6427:2014 (E)Dimensions in millimetresKey1 extractor trap2 thimble3 solvent4 heaterFigure 1 Extraction apparatus capable of receiving the thimble (4.5.1) or other sample containers4.10 Distillation equipment.One of the following devices shall b

40、e used:4.10.1 Rotary evaporator.4.10.2 Distillation apparatus, fitted with a Vigreux or equivalent distillation column of length at least 400 mm.4.11 Vacuum oven or oven with fresh air circulation, explosion-proof, capable of maintaining a temperature of 105 C.7DIN EN ISO 6427:2014-08EN ISO 6427:201

41、4 (E)4.12 Evaporating dish, of suitable capacity, for example 200 ml.Dimensions in millimetresKey1 45/40 ground-glass socket2 vacuum jacket3 29/32 ground-glass coneFigure 2 Extractor of Twisselmann type with vacuum jacket5 Preparation of test sample5.1 The plastics material or plastics product shall

42、 be free of dust and foreign matter.5.2 The sample of plastic shall be reduced to small pieces, for example by grinding in a suitable mill (4.1), but shall not be heated more than necessary. In some cases, it may be necessary to add solid carbon dioxide to prevent heat build-up during grinding. The

43、reduction in size may also be done by the use of a razor blade or a pair of scissors, or a file for hard materials. The portion of the sample of specified granular size (see Table 1) shall be kept in a closed bottle until tested. Films with a thickness of less than 0,5 mm may be cut into small fragm

44、ents for insertion into the thimble.6 Number of testsAt least two determinations shall be made.7 Procedure7.1 The specific details of the procedure to be used depend on the material to be tested and are given in Tables 1 and 2. The general procedure is as described hereafter.8DIN EN ISO 6427:2014-08

45、EN ISO 6427:2014 (E)7.2 Dry the paper thimble (4.5.1), wire basket (4.5.2) or filter crucible (4.5.3) for 1 h in the oven (4.11) at the same temperature as used later for the drying of the plastic tested; allow to cool to room temperature in the desiccator (4.9) and weigh in a closed weighing bottle

46、.NOTE In special cases, it might be necessary to pre-extract the thimble with the extraction liquid (3.1).Weigh a test portion of the mass given in Table 1 to the nearest 1 mg in the thimble, basket or crucible, cover it with a piece of glass wool (3.3), and put it into the extraction apparatus (4.4

47、). If the expected content of extractable material is below 0,5 % (by mass), increase the mass of the test portion to obtain a residue of at least 25 mg. Pour the appropriate volume of extraction liquid (3.1) into the flask (4.3). One or two anti-bumping granules (3.2) may be added. Mount the extrac

48、tor (4.4) and the reflux condenser (4.6) on the flask and adjust the heating device (4.7) so that, when a Soxhlet-type extractor (4.4.1) is used, the extraction liquid syphons several times per hour. For the number of syphonings and the extraction time, see Table 1.7.3 Carry out the extraction. Depe

49、nding on the type of plastic extracted (see Table 2), further process the residue in accordance with 7.4 and/or the extract in accordance with 7.5.7.4 When the extraction is finished, take the thimble, basket or crucible out of the extractor, allow it to drain and air-dry, and then dry it under the conditions given in Table 2 (depending on the kind of extraction liquid). Allow it to cool to room temperature in the desiccator (4.9) and weigh the