BS-ISO-15033-2007.pdf
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1、BRITISH STANDARD BS ISO 15033:2007 Plastics Determination of caprolactam and its cyclic and linear oligomers by HPLC ICS 83.080.01 ? Licensed Copy: London South Bank University, London South Bank University, Tue Jul 03 01:12:00 GMT+00:00 2007, Uncontrolled Copy, (c) BSI BS ISO 15033:2007 This Britis
2、h Standard was published under the authority of the Standards Policy and Strategy Committee on 29 June 2007 BSI 2007 ISBN 978 0 580 53017 3 National foreword This British Standard was published by BSI. It is the UK implementation of ISO 15033:2007. It supersedes BS ISO 15033:2000 which is withdrawn.
3、 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 necessary provisions of a contract. Users
4、 are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations. Amendments issued since publication Amd. No. DateComments Licensed Copy: London South Bank University, London South Bank University, Tue Jul 03 01:12:00 GMT+00:00 2007, Unc
5、ontrolled Copy, (c) BSI Reference number ISO 15033:2007(E) INTERNATIONAL STANDARD ISO 15033 Second edition 2007-03-15 Plastics Determination of caprolactam and its cyclic and linear oligomers by HPLC Plastiques Dtermination du caprolactame et de ses oligomres cycliques et linaires par CLHP BS ISO 15
6、033:2007 Licensed Copy: London South Bank University, London South Bank University, Tue Jul 03 01:12:00 GMT+00:00 2007, Uncontrolled Copy, (c) BSI ii Licensed Copy: London South Bank University, London South Bank University, Tue Jul 03 01:12:00 GMT+00:00 2007, Uncontrolled Copy, (c) BSI iii Contents
7、 Page Foreword iv Introduction v 1 Scope . 1 2 Normative references. 1 3 Terms and definitions. 1 4 Principle. 1 5 Reagents 1 6 Apparatus 3 7 Test sample . 4 8 Procedure 4 8.1 Calibration . 4 8.2 Determination 4 9 Calculations. 6 9.1 Calculation of calibration factors 6 9.2 Test sample . 7 10 Precis
8、ion 7 11 Test report . 8 Annex A (normative) HPLC parameters and injector programme 9 Annex B (informative) Schematic diagram of HPLC apparatus. 10 Bibliography. 11 BS ISO 15033:2007 Licensed Copy: London South Bank University, London South Bank University, Tue Jul 03 01:12:00 GMT+00:00 2007, Uncont
9、rolled Copy, (c) BSI iv 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
10、 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 Commiss
11、ion (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
12、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
13、not be held responsible for identifying any or all such patent rights. ISO 15033 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical-chemical properties. This second edition cancels and replaces the first edition (ISO 15033:2000), which has been technically revised.
14、BS ISO 15033:2007 Licensed Copy: London South Bank University, London South Bank University, Tue Jul 03 01:12:00 GMT+00:00 2007, Uncontrolled Copy, (c) BSI v Introduction The basic method specified in this International Standard can be used for HPLC determination of the cyclic oligomers of caprolact
15、am up to and including the hexamer (n = 6), using UV detection. If desired, after post- column reaction of the primary amine with 1,2-phthalic dicarboxaldehyde, on-line determination of the linear oligomers up to and including the hexamer can also be carried out. The determination is not quantitativ
16、e for oligomers higher than the hexamer (n 6). In the determination of cyclic oligomers the sensitivity for the tetramer and higher oligomers is constant, which means that calibration should take place up to and including the tetramer (n = 4). The linear oligomers are determined by the fluorescence
17、of the iso-indole group, which is a product of the reaction between the primary amino group, 1,2-phthalic dicarboxaldehyde and 3-mercaptopropionic acid. The calibration with the linear oligomers should be carried out up to and including the hexamer (n = 6). BS ISO 15033:2007 Licensed Copy: London So
18、uth Bank University, London South Bank University, Tue Jul 03 01:12:00 GMT+00:00 2007, Uncontrolled Copy, (c) BSI blank Licensed Copy: London South Bank University, London South Bank University, Tue Jul 03 01:12:00 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 1 Plastics Determination of caprolactam an
19、d its cyclic and linear oligomers by HPLC SAFETY STATEMENT Persons using this document should be familiar with normal laboratory practice, if applicable. This document does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user to est
20、ablish appropriate safety and health practices and to ensure compliance with any regulatory requirements. 1 Scope This International Standard describes an HPLC (high-performance liquid chromatography) method for determining the concentrations of cyclic oligomers of caprolactam, from 0,01 % by mass u
21、pwards, and linear oligomers of caprolactam, from 5 mg/kg upwards, both up to and including the hexamer of caprolactam (n = 6), in samples of polyamide 6, caprolactam and mixtures of rearrangement products in water. 2 Normative references The following referenced documents are indispensable for the
22、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 3 Terms and definitions For the purposes of this document, the terms and definiti
23、ons given in ISO 472 apply. 4 Principle A test sample is dissolved in, or diluted with, formic acid and the oligomers separated in the presence of a low-pH mobile phase using a column filled with reversed-phase packing material. The cyclic oligomers are detected by UV absorption at 200 nm. If desire
24、d, the linear oligomers can be detected by fluorescence after post-column reaction of the primary amino group with 1,2-phthalic dicarboxaldehyde and 3-mercaptopropionic acid. The concentrations are calculated by comparison of the measured values with those of calibration solutions. 5 Reagents During
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