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1、a Date: 28 January 2008 Origin: European Latest date for receipt of comments: 30 April 2008 Project no.: 2008/00232 Responsible committee: AW/307 Oil seeds, animal and vegetable fats and oils and their by products Interested committees: Title: Draft BS ISO 16931 Animal and vegetable fats and oils De
2、termination of polymerized triglycerides content by high-performance size-exclusion chromatography (HPSEC) Supersession information: If this document is published as a standard, the UK implementation of it will supersede BSENISO16931 : 2001 and partially supersede. NONE If you are aware of a current
3、 national standard 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 April 2008. This draft is issued to allow comments from interested parties; all comments
4、 will be given 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 circulati
5、on within a nominating 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, I
6、nternational and foreign standards are also available from BSI Customer Services. Information on the co-operating organizations represented on the committees referenced above may be obtained from the responsible committee secretary. Cross-references The British Standards which implement Internationa
7、l 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: 0207 283 5511 Responsible Committee Secretary: Mr John Hancock (BSI) E-mail: john.hancockfosfa.org Draft for Public Comment Head Office 389 Chisw
8、ick High Road London W4 4AL Telephone: +44(0)20 8996 9000 Fax: +44(0)20 8996 7001 Form 36 Version 7.0 DPC: 08/30176577 DC Licensed Copy: London South Bank University, London South Bank University, Fri Feb 15 07:01:32 GMT+00:00 2008, Uncontrolled Copy, (c) BSI b Introduction This draft standard is ba
9、sed on European discussions in which the UK has taken an active part. Your comments on this draft are welcome and will assist in the preparation of the consequent British Standard. If no comments are received to the contrary, then the UK will approve this draft and implement it as a British Standard
10、. Comment is particularly welcome on national, legislative or similar deviations that may be necessary. Even if this draft standard is not approved by the UK, if it receives the necessary support in Europe, the UK will be obliged to publish the official English Language text unchanged as a British S
11、tandard and to withdraw any conflicting 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 is intended to ensure that all comments receive efficient and appropriate attention by the
12、 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 the front cover. Comments should be compatible with Version 6.0 or Version 97 of Microsoft W
13、ord 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 be presented as given in the example below. Further information on submitting comments and h
14、ow 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 (3) 4 5 (6) (7) MB Clause No./ Subclause No./ Annex (e.g. 3.1) Paragraph/ Figure/Table/ Not
15、e (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 clarifying. Amend to read . so that the mains connector to which no connection . 6.4 Para
16、graph 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 registered trademarks, and Windows is a trademark of Microsoft Corporation. Licensed Copy: London
17、South Bank University, London South Bank University, Fri Feb 15 07:01:32 GMT+00:00 2008, Uncontrolled Copy, (c) BSI THIS DOCUMENT IS A DRAFT CIRCULATED FOR COMMENT AND APPROVAL. IT IS THEREFORE SUBJECT TO CHANGE AND MAY NOT BE REFERRED TO AS AN INTERNATIONAL STANDARD UNTIL PUBLISHED AS SUCH. IN ADDI
18、TION 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 BECOME STANDARDS TO WHICH REFERENCE MAY BE MADE IN NATIONAL REGULATIONS. RECIPIENTS OF THIS
19、 DRAFT ARE INVITED TO SUBMIT, WITH THEIR COMMENTS, NOTIFICATION OF ANY RELEVANT PATENT RIGHTS OF WHICH THEY ARE AWARE AND TO PROVIDE SUPPORTING DOCUMENTATION. DRAFT INTERNATIONAL STANDARD ISO/DIS 16931 International Organization for Standardization, 2008 INTERNATIONAL ORGANIZATION FOR STANDARDIZATIO
20、N ORGANISATION INTERNATIONALE DE NORMALISATION ISO/TC 34/SC 11 Voting begins on: 2008-01-24 Secretariat: BSI Voting terminates on: 2008-06-24 Animal and vegetable fats and oils Determination of polymerized triglycerides by high-performance size-exclusion chromatography (HPSEC) Corps gras dorigines a
21、nimale et vgtale Dtermination des triglycrides polymriss par chromatographie liquide dexclusion haute performance (CLHP dexclusion) Revision of first edition (ISO 16931:2001) ICS 67.200.10 ISO/CEN PARALLEL ENQUIRY The CEN Secretary-General has advised the ISO Secretary-General that this ISO/DIS cove
22、rs a subject of interest to European standardization. In accordance with the ISO-lead mode of collaboration as defined in the Vienna Agreement, consultation on this ISO/DIS has the same effect for CEN members as would a CEN enquiry on a draft European Standard. Should this draft be accepted, a final
23、 draft, established on the basis of comments received, will be submitted to a parallel two-month FDIS vote in ISO and formal vote in CEN. To expedite distribution, this document is circulated as received from the committee secretariat. ISO Central Secretariat work of editing and text composition wil
24、l 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 publication. Licensed Copy: London South Bank Univ
25、ersity, London South Bank University, Fri Feb 15 07:01:32 GMT+00:00 2008, Uncontrolled Copy, (c) BSI ISO/DIS 16931 ii ISO 2008 All rights reserved PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not
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28、mber 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 document is a Draft International Standard and is copyright-protected by ISO. Except as permitted under the applicable laws of the us
29、ers country, neither this ISO 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 permission being secured. Requests for permission to reproduce should be add
30、ressed to either ISO at the address below or ISOs member body in the country of the requester. 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 Reproduction may be subject to royalty payments or a licensing ag
31、reement. Violators may be prosecuted. Licensed Copy: London South Bank University, London South Bank University, Fri Feb 15 07:01:32 GMT+00:00 2008, Uncontrolled Copy, (c) BSI ISO/DIS 16931 ISO 2007 All rights reserved iii Contents Page Foreword iv 1 Scope1 2 Normative reference1 3 Term and definiti
32、on.1 4 Principle .1 5 Reagents 2 6 Apparatus.2 7 Sampling 3 8 Preparation of test sample .3 9 Procedure.3 9.1 Starting up the HPLC equipment.3 9.2 Preparation of test portion and analysis.4 10 Expression of results4 10.1 Qualitative analysis.4 10.2 Quantitative analysis.4 11 Precision 4 11.1 Interla
33、boratory tests4 11.2 Repeatability4 11.3 Reproducibility 5 12 Test report5 Annex A (informative) Chromatogramms.6 Annex B (informative) Results of interlaboratory tests 8 Bibliography9 DRAFT 2008 Licensed Copy: London South Bank University, London South Bank University, Fri Feb 15 07:01:32 GMT+00:00
34、 2008, Uncontrolled Copy, (c) BSI ISO/DIS 16931 iv ISO 2007 All rights reserved 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
35、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
36、 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.
37、 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
38、document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 16931 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 11, Animal and vegetable fats and oils. This second/third/. edition cancels and repla
39、ces the first/second/. edition (ISO 16931:2001), clause(s) / subclause(s) / table(s) / figure(s) / annex(es) of which has / have been technically revised. DRAFT 2008 Licensed Copy: London South Bank University, London South Bank University, Fri Feb 15 07:01:32 GMT+00:00 2008, Uncontrolled Copy, (c)
40、BSI DRAFT INTERNATIONAL STANDARD ISO/DIS 16931 ISO 2007 All rights reserved 1 Animal and vegetable fats and oils Determination of polymerized triglycerides content by high-performance size- exclusion chromatography (HPSEC) 1 Scope This International Standard specifies a method using HPSEC to determi
41、ne the contents of polymerized triglycerides in oils and fats which contain at least 3 % (from peak areas) of these polymers. Polymerized triglycerides (strictly speaking dimeric and oligomeric triglycerides) are formed during the heating of fats and oils, thus the method serves to assess the therma
42、l deterioration of used frying fats. This method is applicable to frying fats, and fats and oils that have been thermally treated, provided that the content of polymerized triglycerides is at least 3 %. It can also be applied to the determination of polymers in fats for animal feedstuffs. In this ca
43、se the extraction method used can have an influence on the result (see ISO 6492). 2 Normative reference 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 r
44、eferenced document (including any amendments) applies. ISO 661, Animal and vegetable fats and oils Preparation of test sample 3 Term and definition For the purposes of this International Standard, the following term and definition applies. 3.1 polymerized triglycerides constituents of heated fats an
45、d oils that are determined by HPSEC under the conditions specified in this International Standard NOTE The content is expressed as a percentage of all peaks from eluted acylglycerides (PTAGs, TAGs, DAGs and MAGs). 4 Principle The sample is dissolved in tetrahydrofuran and the polymerized triglycerid
46、es are separated by gel permeation chromatography according to molecular size. The compounds are detected by means of a refractive index detector. NOTE For a better resolution two columns in series (2 x 300 mm) are used. DRAFT 2008 Licensed Copy: London South Bank University, London South Bank Unive
47、rsity, Fri Feb 15 07:01:32 GMT+00:00 2008, Uncontrolled Copy, (c) BSI ISO/DIS 16931 2 ISO 2007 All rights reserved 5 Reagents Use only reagents of recognized analytical grade. WARNING Attention is drawn to the regulations which specify the handling of hazardous substances. Technical, organizational
48、and personal safety measures must be followed. 5.1 Tetrahydrofuran (THF), for HPLC, possibly with BHT, degassed, free of water. NOTE It is important that the tetrahydrofuran used to dissolve the sample has the same water content as the eluent, otherwise a negative peak can be observed. 5.2 Toluene,
49、for HPLC 5.3 Reference oil, extra virgin olive oil: dissolve 100 mg to 300 mg in 10 ml THF. NOTE The extra virgin olive oil does not contain polymerized triglycerides and can be used to determine the retention time of the monomeric triglycerides. 6 Apparatus Usual laboratory apparatus and, in particular, the following. 6.1 Solvent reservoir, 500 ml to 1000 ml of capacity, with a polytetra