07-30163272-DC.pdf

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1、a Date: 5 March 2007 Origin: International Latest date for receipt of comments: 30 June 2007 Project no.: 2007/00557 Responsible committee: AW/5 Chemical analysis of milk and milk products Interested committees: Title: Draft BS ISO 8260 Milk and milk products Determination of organochlorine pesticid

2、es and polychlorobiphenyls Method using capillary gas-liquid chromatography with electron-capture detection Supersession information: If this document is published as a standard, the UK implementation of it will supersede NONE and partially supersede NONE . If you are aware of a current national sta

3、ndard which may be affected, please notify the secretary (contact details below). WARNING: THIS IS A DRAFT AND MUST NOT BE REGARDED OR USED AS A BRITISH STANDARD. THIS DRAFT IS NOT CURRENT BEYOND 30 June 2007. This draft is issued to allow comments from interested parties; all comments will be given

4、 consideration prior to publication. No acknowledgement will normally be sent. See overleaf for information on commenting. No copying is allowed, in any form, without prior written permission from BSI except as permitted under the Copyright, Designs and Patent Act 1988 or for circulation within a no

5、minating organization for briefing purposes. Electronic circulation is limited to dissemination by e-mail within such an organization by committee members. Further copies of this draft may be purchased from BSI Customer Services, Tel: +44(0) 20 8996 9001 or email ordersbsi-. British, International a

6、nd foreign standards are also available from BSI Customer Services. British Standards on CD or Online are available from British Standards Publishing Sales Limited. Tel: 01344 404409 or email bsonlinetechindex.co.uk. Information on the co-operating organizations represented on the committees referen

7、ced above may be obtained from the responsible committee secretary. Cross-references The British Standards which implement International or European publications referred to in this draft may be found via the British Standards Online Service on the BSI web site http:/www.bsi-. Direct tel: 020 8996 7

8、009 Responsible Committee Secretary: Committee Service Centre (BSI) E-mail: cscbsi- Draft for Public Comment Head Office 389 Chiswick High Road London W4 4AL Telephone: +44(0)20 8996 9000 Fax: +44(0)20 8996 7001 Form 36 Version 6.1 DPC: 07/30163272 DC Licensed Copy: London South Bank University, Lon

9、don South Bank University, Sat Mar 17 04:03:38 GMT+00:00 2007, Uncontrolled Copy, (c) BSI b Introduction This draft standard is based on international discussions in which the UK has taken an active part. Your comments on this draft are invited and will assist in the preparation of the consequent st

10、andard. Comments submitted will be reviewed by the relevant BSI committee before sending the consensus UK vote and comments to the international secretariat, which will then decide appropriate action on the draft and the comments received. If no comments are received to the contrary, then the UK wil

11、l approve this draft. If the international standard is approved, it is possible the text will be published as an identical British Standard. UK Vote Please indicate whether you consider the UK should submit a negative (with reasons) or positive vote on this draft. Submission The guidance given below

12、 is intended to ensure that all comments receive efficient and appropriate attention by the responsible BSI committee. Annotated drafts are not acceptable and will be rejected. All comments must be submitted, preferably electronically, to the Responsible Committee Secretary at the address given on t

13、he front cover. Comments should be compatible with Version 6.0 or Version 97 of Microsoft Word for Windows, if possible; otherwise comments in ASCII text format are acceptable. Any comments not submitted electronically should still adhere to these format requirements. All comments submitted should b

14、e presented as given in the example below. Further information on submitting comments and how to obtain a blank electronic version of a comment form are available from the BSI web site at:http:/www.bsi- Template for comments and secretariat observations Date: xx/xx/200x Document: ISO/DIS xxxxx 1 2 (

15、3) 4 5 (6) (7) MB Clause No./ Subclause No./ Annex (e.g. 3.1) Paragraph/ Figure/Table/ Note (e.g. Table 1) Type of com- ment Comment (justification for change) by the MB Proposed change by the MB Secretariat observations on each comment submitted 3.1 Definition 1 ed Definition is ambiguous and needs

16、 clarifying. Amend to read . so that the mains connector to which no connection . 6.4 Paragraph 2 te The use of the UV photometer as an alternative cannot be supported as serious problems have been encountered in its use in the UK. Delete reference to UV photometer. Microsoft and MS-DOS are register

17、ed trademarks, and Windows is a trademark of Microsoft Corporation. Licensed Copy: London South Bank University, London South Bank University, Sat Mar 17 04:03:38 GMT+00:00 2007, Uncontrolled Copy, (c) BSI THIS DOCUMENT IS A DRAFT CIRCULATED FOR COMMENT AND APPROVAL. IT IS THEREFORE SUBJECT TO CHANG

18、E AND MAY NOT BE REFERRED TO AS AN INTERNATIONAL STANDARD UNTIL PUBLISHED AS SUCH. IN ADDITION TO THEIR EVALUATION AS BEING ACCEPTABLE FOR INDUSTRIAL, TECHNOLOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT INTERNATIONAL STANDARDS MAY ON OCCASION HAVE TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL TO B

19、ECOME STANDARDS TO WHICH REFERENCE MAY BE MADE IN NATIONAL REGULATIONS. DRAFT INTERNATIONAL STANDARD ISO/DIS 8260 DRAFT INTERNATIONAL STANDARD ISO/IDF 130 International Organization for Standardization and International Dairy Federation, 2007 INTERNATIONAL ORGANIZATION FOR STANDARDIZATION ORGANISATI

20、ON INTERNATIONALE DE NORMALISATION ISO/TC 34/SC 5 Voting begins on: 2007-02-28 Secretariat: NEN Voting terminates on: 2007-07-28 Milk and milk products Determination of organochlorine pesticides and polychlorobiphenyls Method using capillary gas-liquid chromatography with electron-capture detection

21、Lait et produits laitiers Dosage des pesticides organochlors et des diphnyles polychlors Mthode par chromatographie en phase gazeuse avec dtection capture dlectrons ICS 67.100.01 To expedite distribution, this document is circulated as received from the committee secretariat. ISO Central Secretariat

22、 work of editing and text composition will be undertaken at publication stage. Pour acclrer la distribution, le prsent document est distribu tel quil est parvenu du secrtariat du comit. Le travail de rdaction et de composition de texte sera effectu au Secrtariat central de lISO au stade de publicati

23、on. Licensed Copy: London South Bank University, London South Bank University, Sat Mar 17 04:03:38 GMT+00:00 2007, Uncontrolled Copy, (c) BSI ISO/DIS 8260|IDF 130 ii ISO and IDF 2007 All rights reserved PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing

24、policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In downloading this file, parties accept therein the responsibility of not infringing Adobes licensing policy. The ISO Cent

25、ral Secretariat accepts no liability in this area. Adobe is a trademark of Adobe Systems Incorporated. Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation parameters were optimized for printing. Every care has been tak

26、en to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. Copyright notice This ISO|IDF document is a Draft International Standard and is copyright-protected by

27、ISO and IDF. Except as permitted under the applicable laws of the users country, neither this ISO|IDF draft nor any extract from it may be reproduced, stored in a retrieval system or transmitted in any form or by any means, electronic, photocopying, recording or otherwise, without prior written perm

28、ission being secured. Requests for permission to reproduce should be addressed to ISO or IDF at the respective address below. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org International Dairy Federation Dia

29、mant Building Bd Auguste Reyers 80 B-1030 Brussels Tel. + 32 2 733 98 88 Fax + 32 2 733 04 13 E-mail infofil-idf.org Web www.fil-idf.org Reproduction may be subject to royalty payments or a licensing agreement. Violators may be prosecuted. Licensed Copy: London South Bank University, London South Ba

30、nk University, Sat Mar 17 04:03:38 GMT+00:00 2007, Uncontrolled Copy, (c) BSI ISO/DIS 8260 | IDF 130 ISO 2006 All rights reserved iii Contents Page Introduction ii 1 Scope . 1 2 Normative references. 1 3 Terms and definitions. 1 4 Principle. 1 5 Reagents 2 6 Apparatus 4 7 Sampling 4 8 Preparation of

31、 test sample. 4 8.1 Milk. 4 8.2 Evaporated milk 5 8.3 Sweetened condensed milk. 5 8.4 Powdered milk products 5 8.5 Butter and butterfat 5 8.6 Cheese . 5 8.7 Other milk products 5 9 Preparation of test portion. 5 9.1 Extraction of milk 5 9.2 Extraction of (sweetened) condensed milk, powdered milk pro

32、ducts, butter, butter fat and cheese 6 10 Procedure 6 10.1 Blank test. 6 10.2 Cryogenic extraction 6 10.3 Clean-up. 6 10.4 Gas chromatography 7 10.5 Blank results . 7 11 Calculation and expression of results 8 11.1 Calculation of the response factor 8 11.2 Expression of the response factor 8 11.3 Ca

33、lculation of the compound content 8 11.4 Expression of result . 8 11.5 Relative retention time . 8 11.6 Expression of the retention time. 9 12 Precision 9 12.1 General. 9 12.2 Repeatability 9 12.3 Reproducibility 9 13 Test report . 9 Annex A (informative) Interlaboratory trial 10 Annex B (informativ

34、e) Chromatogram . 11 Bibliography. 13 DRAFT 2007 Licensed Copy: London South Bank University, London South Bank University, Sat Mar 17 04:03:38 GMT+00:00 2007, Uncontrolled Copy, (c) BSI ISO/DIS 8260 | IDF 130 iv ISO 2006 All rights reserved Foreword ISO (the International Organization for Standardi

35、zation) 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 technical committee has been established has the right to b

36、e 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 Electro technical Commission (IEC) on all matters of electro technical standardization. International Stan

37、dards 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 Int

38、ernational 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 8260

39、| IDF 130 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 5, Milk and milk products and the International Dairy Federation (IDF). It is being published jointly by ISO and IDF. DRAFT 2007 Licensed Copy: London South Bank University, London South Bank University, Sat Mar

40、17 04:03:38 GMT+00:00 2007, Uncontrolled Copy, (c) BSI ISO/DIS 8260 | IDF 130 ISO 2006 All rights reserved v Foreword IDF (the International Dairy Federation) is a worldwide federation of the dairy sector with a National Committee in every member country. Every National Committee has the right to be

41、 represented on the IDF Standing Committees carrying out the technical work. IDF collaborates with ISO in the development of standard methods of analysis and sampling for milk and milk products. Draft International Standards adopted by the Action Teams and Standing Committees are circulated to the N

42、ational Committees for voting. Publication as an International Standard requires approval by at least 50 % of IDF National Committees casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. IDF shall not be held responsibl

43、e for identifying any or all such patent rights. ISO 8260 | IDF 130 was prepared by the International Dairy Federation (IDF) and Technical Committee ISO/TC 34, Food products, Subcommittee SC 5, Milk and milk products. It is being published jointly by ISO and IDF. All work was carried out by the Join

44、t IDF-ISO Action Team on Organic contaminants of the Standing Committee on Analytical methods for additives and contaminants under the aegis of its project leader, Mr. R. de Knegt (NL). This first edition of ISO 8260 | IDF 130 cancels and replaces the first edition of IDF 130A:1991, which has been t

45、echnically revised. DRAFT 2007 Licensed Copy: London South Bank University, London South Bank University, Sat Mar 17 04:03:38 GMT+00:00 2007, Uncontrolled Copy, (c) BSI ISO/DIS 8260 | IDF 130 vi ISO 2006 All rights reserved Introduction This document is intended for research, monitoring, and control

46、 purposes of organochlorine compounds in milk and milk products by isolation of these compounds. Generally, polychlorinated biphenyls (PCB) have been determined in the past by “empirical methods“. Mostly this was done by “peak pattern comparison“ using gas-liquid chromatography with electron capture

47、 detection (GLCECD) on packed columns. Reference was made to higher chlorinated technical mixtures, by perchlorination to decachlorobiphenyl (and GLCECD determination) or dechlorination to biphenyl. The determination was done by high-performance liquid chromatography with ultraviolet detection (HPLC

48、UV) or by gas liquid chromatography with flame ionisation detection (GLCFID) (see part 2 of ISO 8260, Bibliography, for example, 2-8). These techniques have three important drawbacks in principle: 1. By reducing the information of the PCB pattern to only one figure (the “PCB-content“) the informatio

49、n of the pattern of distribution of isomers is lost. This information would, however, be extremely useful to indicate the sources of contamination and to differentiate between background and recent contamination. 2. “PCB-contents“ determined by these techniques are arrived at in many different ways and for most PCB data the definition of the “PCB-content“ is not clearly

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