BS-EN-ISO-11337-2004.pdf

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 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 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-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 Electronic 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 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 comprises a front cover, an inside 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. DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:45:12 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM EN ISO 11337 May 2004 ICS 83.080.20 English version Plastics - Polyamides - Determination of e-caprolactam and w- laurolactam by gas chromatography (ISO 11337:2004) Plastiques - Polyamides - Détermination 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 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 national 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 notified 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, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels © 2004 CEN All rights of exploitation in any form 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 “Plastics“ 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 national 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, France, 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 any 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 -laurolactam by gas chromatography Plastiques Polyamides Détermination 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 emdebt dedyfepcaes. 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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 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 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 prepare 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 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 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 INTENRATIONAL 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 its 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 chromatography. 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 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 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 amendments) 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: sheffieldun 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 separate 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, plus 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 µm and 500 µm 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 or 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 sides 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 µm to 50 µm, capacity 30 ml; porcelain filter-plate of slightly smaller diameter than the crucible, with holes 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 µm to 50 µm, capacity 30 ml, 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. 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), packed 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 µm; a megabore carbowax column (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 results. 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