EN ISO 6427-2014 en Plastics - Determination of matter extractable by organic solvents (conventional methods)《塑料 有机溶剂萃取物的测定(常规法)(ISO 6427 2013)》.pdf

1、BSI Standards PublicationBS EN ISO 6427:2014Plastics Determination of matter extractable by organic solvents (conventional methods) BS EN ISO 6427:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 6427:2014. It is identical to ISO 6427:2013. It supersedes

2、 BS EN ISO 6427:1999 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee PRI/21, Testing of plastics.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the nece

3、ssary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2014. Published by BSI Standards Limited 2014ISBN 978 0 580 84591 8 ICS 83.080.01 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standar

4、d was published under the authority of the Standards Policy and Strategy Committee on 30 June 2014.Amendments issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 6427 June 2014 ICS 83.080.01 English Version Plastics - Determination of matter e

5、xtractable by organic solvents (conventional methods) (ISO 6427:2013) Plastiques - Dtermination des matires extractibles par des solvants organiques (Mthodes conventionnelles) (ISO 6427:2013) Kunststoffe - Bestimmung der extrahierbaren Bestandteile durch organische Lsemittel (Standardverfahren) (ISO

6、 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 bibliograph

7、ical 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 responsibilit

8、y 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

9、 Macedonia, 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. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATIO

10、N EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 6427:2014 EBS EN ISO 6427:2014BS EN ISO 6427:2014EN ISO 6427:2014 (E) 3 Fore

11、word The text of ISO 6427:2013 has been prepared by Technical Committee ISO/TC 61 “Plastics” of the International Organization 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 Sta

12、ndard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the 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

13、of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any 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 Europea

14、n Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Sloven

15、ia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 6427:2013 has been approved by CEN as EN ISO 6427:2014 without any modification. BS EN ISO 6427:2014ISO 6427:2013(E) ISO 2013 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope . 12 No

16、rmative references 13 Reagents and materials . 14 Apparatus . 25 Preparation of test sample . 46 Number of tests 47 Procedure. 48 Expression of results 59 Precision . 610 Test report . 6Annex A (normative) Procedure for casting, drying, and cutting films of cellulose acetate .10Annex B (normative) D

17、etermination of solubility of polypropylene in cold pxylene .12Bibliography .15BS EN ISO 6427:2014ISO 6427:2013(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards

18、 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 organizations, governmental and non-governmental, in liaison with ISO, also take p

19、art 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 ISO/IEC Directives, Part 2.The main task of technical committees is to p

20、repare International Standards. 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

21、 some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights.ISO 6427 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical-chemical properties.This third edition cancels and

22、 replaces the second edition (ISO 6427:1992), of which it constitutes a minor revision, the main purpose of which was to delete the second sentence in (subclause) 5.1. In addition, the minimum density for which the method is suitable for PE has been indicated directly in footnote “e” to Table 1, rat

23、her than referring the reader to ISO 1872-11and what was Table 1 in the 1992 edition has been split into two tables for ease of comprehension.iv ISO 2013 All rights reservedBS EN ISO 6427:2014ISO 6427:2013(E)IntroductionThere are several very similar national and international standards for determin

24、ation of the percentage of extractable matter, with only slight differences in the procedures. To facilitate 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. ISO 2

25、013 All rights reserved vBS EN ISO 6427:2014BS EN ISO 6427:2014Plastics Determination of matter extractable by organic solvents (conventional methods)1 ScopeThis International Standard specifies methods for the determination of components in plastics that can be extracted by hot organic liquids near

26、 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 percentage of extractable matter influence the properties of plastics.The recommended extr

27、action 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 International Standard does not apply to plastics that come into contact with food or

28、 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 are used in most cases. The methods of this International Standard are not intende

29、d 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 Normative referencesThe following documents, in whole or in part, are normatively referen

30、ced 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) applies.ISO 308, Plastics Phenolic moulding materials Determination of acetone-solubl

31、e 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 sheet Nominal sizes of openingsISO 1773, Laboratory glassware Narrow-necked boiling f

32、lasksISO 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 requirements of the plastic material being tested (see Table 1).3.2 Antibumping gra

33、nules.3.3 Glass wool, pre-extracted.INTERNATIONAL STANDARD ISO 6427:2013(E) ISO 2013 All rights reserved 1BS EN ISO 6427:2014ISO 6427:2013(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 blades is preferred.

34、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-glass neck complying w

35、ith 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 Figure 2), may be used,

36、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 dimensions as the thimble (4.

37、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 basket (4.5.2) cannot

38、 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 Reflux condenser, fit

39、ted 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 calcium chloride or silica

40、 gel.2 ISO 2013 All rights reservedBS EN ISO 6427:2014ISO 6427:2013(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

41、be 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. ISO 2013 All rights reserved 3BS EN I

42、SO 6427:2014ISO 6427:2013(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

43、 plastics product shall 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-u

44、p during grinding. The 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

45、be cut into small fragments 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.4

46、 ISO 2013 All rights reservedBS EN ISO 6427:2014ISO 6427:2013(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

47、 (4.9) and weigh in a closed weighing bottle.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), a

48、nd put it into the extraction apparatus (4.4). 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 g

49、ranules (3.2) may be added. Mount the extractor (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. Depending 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, ta