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1、BRITISH STANDARD BS EN ISO 11337:2004 Plastics Polyamides Determination of ( (-caprolactam and 6 6-laurolactam by gas chromatography The European Standard EN ISO 11337:2004 has the status of a British Standard ICS 83.080.20 ? Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:45:12 GMT+00:00
2、2006, Uncontrolled Copy, (c) BSI BS EN ISO 11337:2004 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 10 June 2004 BSI 10 June 2004 ISBN 0 580 43874 0 National foreword This British Standard is the official English language version of EN ISO
3、11337:2004. It is identical with ISO 11337:2004. The UK participation in its preparation was entrusted to Technical Committee PRI/21, Testing of Plastics, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-referen
4、ces 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 Electronic Catalogue or of British S
5、tandards 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 understand the text; present to
6、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 comprises a front cover, an inside
7、front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii to iv, pages 1 to 14, an inside back cover and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateCo
8、mments Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:45:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11337 May 2004 ICS 83.080.20 English version Plastics - Polyamides - Determination of e-caprolactam and w- laurolactam by gas chr
9、omatography (ISO 11337:2004) Plastiques - Polyamides - Dtermination du e- caprolactame et du w-laurolactam par chromatographie en phase gazeuse (ISO 11337:2004) Kunststoffe - Polyamide - Gaschromatographische Bestimmung von e-Caprolactam und w-laurolactam (ISO 11337:2004) This European Standard was
10、approved by CEN on 13 May 2004. 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 bibliographical references concerning such nationa
11、l standards may be obtained on application to the Central Secretariat 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 of a CEN member into its own language and notif
12、ied to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherla
13、nds, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2004 CEN All rights of exploitation in any for
14、m and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 11337:2004: E Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:45:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Foreword This document (EN ISO 11337:2004) has been prepared by Technical Committee ISO/TC 61 “Plas
15、tics“ in collaboration with Technical Committee CEN/TC 249 “Plastics“, the secretariat of which is held by IBN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by November 2004, and conflicting natio
16、nal standards shall be withdrawn at the latest by November 2004. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, Fran
17、ce, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 11337:2004 has been approved by CEN as EN ISO 11337:2004 without a
18、ny modifications. EN ISO 11337:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:45:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Reference number ISO 11337:2004(E) INTERNATIONAL STANDARD ISO 11337 First edition 2004-05-15 Plastics Polyamides Determination of -caprolactam and -laurolact
19、am by gas chromatography Plastiques Polyamides Dtermination du -caprolactame et du -laurolactame par chromatographie en phase gazeuse EN ISO 11337:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:45:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI DPlcsid Fremia ihTs PDF file mya ctnoian
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24、ce saCe tsopale 65 eneG 1121-HC 02 av leT. 4 + 10 947 22 1 11 xaF0 947 22 14 + 9 74 E-mial coirypthgis.o gro We bwww.is.o gro Pulbisdehi n Switlrez dna ii EN ISO 11337:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:45:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iii Contents Page Fo
25、rewordiv 1 Scope1 2 Normative references .1 3 Terms and definitions.1 4 Method A: Extraction method2 4.1 Principle.2 4.2 Reagents2 4.3 Apparatus and materials2 4.4 Preparation of test sample.4 4.5 Procedure.4 4.6 Expression of results5 4.7 Precision6 4.8 Test report6 5 Method B: Dissolution method6
26、5.1 Principle.6 5.2 Reagents7 5.3 Apparatus.7 5.4 Preparation of internal-standard solutions8 5.5 Procedure.10 5.6 Expression of results11 5.7 Precision11 5.8 Test report12 EN ISO 11337:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:45:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv
27、 Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (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
28、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 part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matter
29、s 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 prepare International Standards. Draft International Standards adopted by the technical committees are circulat
30、ed 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 some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible
31、 for identifying any or all such patent rights. ISO 11337 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical- chemical properties. EN ISO 11337:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:45:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTENRATIO
32、NAL TSANDADR IS:73311 O4002(E) 1 Plastics Polyamides Determination of -caprolactam and -laurolactam by gas chromatography WARNING This International Standard may involve hazardous chemicals, materials or operations. It does not purport to address all of the safety problems, if any, associated with i
33、ts use. It is the responsibility of the user to establish appropriate safety and health practices and to determine the applicability of regulatory limitations prior to use. 1 Scope This International Standard specifies a method for determining -caprolactam and -laurolactam in polyamides by gas chrom
34、atography. It is suitable particularly for the determination of -caprolactam in polyamide 6 and -laurolactam in polyamide 12. Bearing in mind that gas chromatography offers a wide range of possible conditions, the method specified is that shown to have been suitable in practice. Two variants of the
35、basic method are specified: Method A is an extraction method with boiling methanol, and the extract is injected into a gas chromatograph. Method B is a method using a solvent, and the solution is injected into a gas chromatograph. Method A is suitable for the determination of -caprolactam and method
36、 B for -caprolactam and -laurolactam. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendment
37、s) applies. ISO 472, Plastics Vocabulary ISO 565, Test sieves Metal wire cloth, perforated metal plate and electroformed sheet Nominal sizes of openings 3 Terms and definitions For the purposes for this document, the terms and definitions given in ISO 472 apply. EN ISO 11337:2004 Licensed Copy: shef
38、fieldun sheffieldun, na, Mon Nov 20 02:45:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 2 4 Method A: Extraction method 4.1 Principle A test portion is extracted with boiling methanol and a small volume of the extract injected into a gas chromatograph equipped with a flame-ionization detector to sep
39、arate and detect the volatile components. The extract contains 1-dodecanol as an internal standard. 4.2 Reagents During the analysis, use only reagents of recognized analytical grade. 4.2.1 Methanol. 4.2.2 1-Dodecanol. 4.2.3 -Caprolactam. 4.3 Apparatus and materials Ordinary laboratory apparatus, pl
40、us the following: 4.3.1 Mill, for reducing the sample to the required grain size. A mill in which the sample is ground at a low temperature is preferred. Large pieces can be reduced in size with a pair of scissors before they are fed to the mill. 4.3.2 Two sieves, with aperture sizes of 710 m and 50
41、0 m respectively, complying with the requirements of ISO 565. 4.3.3 Extraction apparatus, that will accommodate an extraction crucible or porous ceramic thimble containing the test portion. The apparatus shall be of such a design that the crucible or thimble is heated by the rising methanol vapour o
42、r the apparatus shall be constructed of an extraction flask with a Soxhlet-type reflux condenser. Examples of suitable extraction apparatus designed along these lines are: EXAMPLE 1 250 ml extraction flask; extraction chamber to accommodate the extraction crucible so that it is enveloped on all side
43、s by the rising methanol vapour and the condensed methanol drips through it continuously; glass triangle to support the crucible; reflux condenser; sintered-glass filter crucible, pore size 40 m to 50 m, capacity 30 ml; porcelain filter-plate of slightly smaller diameter than the crucible, with hole
44、s of diameter 0,4 mm. EXAMPLE 2 250 ml extraction flask; jacketed Soxhlet extractor; EN ISO 11337:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:45:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 3 reflux condenser; sintered-glass filter crucible, pore size 40 m to 50 m, capacity 30 ml
45、, or a porous ceramic thimble of similar capacity (the dimensions shall be such that the crucible or thimble can be satisfactorily accommodated in the Soxhlet apparatus); porcelain filter-plate of slightly smaller diameter than the crucible or thimble, as appropriate, with holes of diameter 0,4 mm.
46、4.3.4 Suitable heating device for extraction apparatus. 4.3.5 Analytical balance, accurate to 0,000 2 g. 4.3.6 Liquid nitrogen or solid carbon dioxide, if necessary. 4.3.7 Gas chromatograph, with flame-ionization detector. a) Column The following columns are suitable: a glass column (3 mm 1,6 m), pa
47、cked with acid-washed Chromosorb W of particle diameter 0,149 mm to 0,177 mm (80 mesh to 100 mesh) coated with 10 % (by mass) poly(ethylene glycol) 20M; a fused-silica capillary column (0,31 mm 30 m), liquid phase 95 % dimethyl, 5 % diphenyl polysiloxane, film thickness 0,25 m; a megabore carbowax c
48、olumn (0,53 mm 15 m) of corresponding separation efficiency. The method of packing is not specified but shall be such as to obtain satisfactory separation efficiency. The capillary column is preferred. Other column dimensions are permissible, but only if they have been proved to give the same result
49、s. Suggested operating conditions are shown in Table 1. Table 1 Operating conditions for gas chromatograph Item Value Column temperature 200 C Injector temperature 250 C Detector temperature 250 C Carrier gas Helium or nitrogen Carrier gas flow rate 20 ml/min b) Detector Use a flame-ionization detector in which the hydrogen and air flow rates can be adjusted so t