BS-EN-ISO-9832-2003.pdf

BRITISH STANDARD BS EN ISO 9832:2003 Animal and vegetable fats and oils Determination of residual technical hexane content The European Standard EN ISO 9832:2003 has the status of a British Standard ICS 67.200.10 ? Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:54:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 9832:2003 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 6 August 2003 © BSI 6 August 2003 ISBN 0 580 42396 4 National foreword This British Standard is the official English language version of EN ISO 9832:2003. It is identical with ISO 9832:2002. It supersedes BS EN ISO 9832:2000 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee AW/307, Oil seeds, animal and vegetable fats and oils, 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 and iii, a blank page, pages 1 to 10, the Annex ZA page 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, Sun Nov 19 14:54:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM EN ISO 9832 July 2003 ICS 67.200.10Supersedes EN ISO 9832:2000 English version Animal and vegetable fats and oils - Determination of residual technical hexane content (ISO 9832:2002) Corps gras d'origines animale et végétale - Dosage de l'hexane technique résiduel (ISO 9832:2002) Tierische und pflanzliche Fette und Öle - Bestimmung des Gehaltes an technischem Resthexan (ISO 9832:2002) This European Standard was approved by CEN on 10 July 2003. 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 Management Centre 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 Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, 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 © 2003 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 9832:2003 E Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:54:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Foreword The text of ISO 9832:2002 has been prepared by Technical Committee ISO/TC 34 “Agricultural food products” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 9832:2003 by Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fats and oils and their by-products - Methods of sampling and analysis“, the secretariat of which is held by AFNOR. 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 January 2004, and conflicting national standards shall be withdrawn at the latest by January 2004. This document supersedes EN ISO 9832:2000. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 9832:2002 has been approved by CEN as EN ISO 9832:2003 without any modifications. NOTE Normative references to International Standards are listed in annex ZA (normative). EN ISO 9832:2003 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:54:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Reference number ISO 9832:2002(E) INTERNATIONAL STANDARD ISO 9832 Second edition 2002-02-15 Animal and vegetable fats and oils Determination of residual technical hexane content Corps gras d'origines animale et végétale Dosage de l'hexane technique résiduel EN ISO 9832:2003 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:54:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI lcsid FDParemi ihTs PDF file mc yatnoaie nmt deddebyfepca.se Icca ncnadrow eitA h'ebods licsneilop gnic,y tihs file mirp eb yatniv ro deewb detu slahl ton ide ebtlnu desse tt ehyfepacse wihce era hml era deddebicsnede to i dnasntlalde t noeh comtupfrep remroign tide ehti.gn Iwod nnlidaogn tihs fil,e trapies ccatpe tiereht nsnopser ehiiblity fo ton ifnriignA gn'ebods licnesilop gnic.y I ehTStneC Oarl Scerteiraat cacpets l oniibality it nihs .aera Ai ebods a tedarmfo kra Aebod SystemI snctaropro.de teDials fo ts ehfotworp eracudts ust dec ortaet eihs PDF filc eeb na fi dnuot nlareneG eh Ifnler otait evt of ehil;e tP ehD-Fcrtaeiarap nomtesre wretpo eimizf deirp rotni.gn Evyre csah era t neebkat nesne ot eruaht tf ehili es siutlbaf esu roI yb eSO memidob rebse. 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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 3. 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 International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 9832 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 11, Animal and vegetable fats and oils. This second edition cancels and replaces the first edition (ISO 9832:1992), of which it constitutes a minor revision to incorporate Amendment 1:1998. Annex A of this International Standard is for information only. EN ISO 9832:2003 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:54:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:54:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTENRATIONAL TSANDADR IS:2389 O2002(E) 1 Animal and vegetable fats and oils Determination of residual technical hexane content 1 Scope This International Standard specifies a method for the determination of the residual technical hexane content of animal and vegetable fats and oils (referred to as fats hereinafter). The method is suitable for the determination of hexane contents between 10 mg and 1 500 mg per kilogram of fat. The method is not applicable to marine oils 2 Normative reference The following normative document contains provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent edition of the normative document indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 661:1989, 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 residual technical hexane content content of volatile hydrocarbons such as those remaining in fats following processing involving the use of hydrocarbon solvents, when determined by the method specified in this International Standard NOTE The content is expressed as milligrams of hexane per kilogram of sample. 4 Principle Desorption of volatile hydrocarbons by heating at 80 °C in a closed vessel after addition of an internal standard. Determination of the particular volatile hydrocarbons content of the headspace by gas chromatography using packed or capillary columns. 5 Reagents Use only reagents of recognized analytical grade, unless otherwise stated, and distilled or demineralized water or water of equivalent purity. EN ISO 9832:2003 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:54:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 2 5.1 Technical hexane, with a composition similar to that of hexane used in industrial processing or, if this is not available, n-hexane. It is recommended that technical hexane be used for the calibration. This reagent usually has an n-hexane content of 50 % (by mass) and consists mainly of C6 isomers but may include C5 and C7 hydrocarbons. 5.2 Internal standard, n-heptane. If this is not available, cyclohexane may be used, provided that the solvent (5.1) used for the extraction or calibration has a negligible content of cyclohexane and/or n-heptane or components with similar retention times. 5.3 Carrier gas, e.g. hydrogen, nitrogen or helium, etc., thoroughly dried and with an oxygen content of less than 10 mg/kg. 5.4 Auxiliary gases, hydrogen (99,9 % pure, free from organic impurities) and air (free from organic impurities). 5.5 Calibration fat, freshly refined and deodorized vegetable fat, the technical hexane content of which is negligible. This material should be free from peroxides or other components likely to decompose with the formation of volatile material which could be confused with hydrocarbons during the test. 6 Apparatus Usual laboratory equipment and, in particular, the following. 6.1 Septum vials, of 20 ml capacity. 6.2 Septa, inert to fats and solvents, made of a material such as butyl rubber or red rubber free from hydrocarbon solvent residues and of a suitable quality that they will not swell under the conditions of use, aluminium caps suitable for use with the vials (6.1) and crimping pliers. 6.3 Tongs, suitable for holding the vials (6.1). 6.4 Syringes, of 10 µl capacity, used only for the analysis of residual technical hexane. They shall not be cleaned with hydrocarbon solvent. 6.5 Syringes, of 1 µl capacity, used only for the analysis of residual technical hexane. They shall not be cleaned with hydrocarbon solvent. 6.6 Syringes, of 1 000 µl capacity, gas-tight, used only for the analysis of residual technical hexane. They shall not be cleaned with hydrocarbon solvent. 6.7 Gas chromatograph, with a flame ionization detector and an integrator and/or recorder, equipped with either a) a packed glass column, 2 m to 4 m long and of internal diameter 3,2 mm approximately, packed with an acid- washed and silanized diatomaceous earth support of particle size 150 µm to 180 µm (Chromosorb P NAW 60-80 mesh1) is suitable), and coated with 10 % squalane or any other phase permitting the chromatographic separation required, or b) a glass capillary column, approximately 30 m long and of 0,3 mm internal diameter, coated with methylpolysiloxane of film thickness 0,2 µm. 1) Chromosorb P NAW 60-80 is an example of a suitable product available commercially. This information is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of this product. EN ISO 9832:2003 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:54:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 3 The injector and detector temperature shall be set at 100 °C and the oven temperature at 50 °C. If a capillary column see b) is used, the apparatus shall have a 1/100 split injection system. NOTE For analyses in series, a headspace gas chromatograph with automatic sample injection and tempering bath has been shown to be satisfactory. In this case, manual injection is not necessary. 6.8 Heating bath, equipped with clamps for holding septum vials, regulated thermostatically at 80 °C ± 2 °C. NOTE For