BS-EN-ISO-734-2-2001.pdf

BRITISH STANDARD BS EN ISO 734-2:2001 Incorporating Amendment No. 1 to BS 4325-13:1999 (renumbers the BS as BS EN ISO 734-2:2001) Oilseed residues Determination of oil Content Part 2: Rapid extraction method The European Standard EN ISO 734-2:2000 has the status of a British Standard ICS 67.200.20 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:53:41 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 734-2:2001 This British Standard, having been prepared under the direction of the Consumer Products and Services Sector Committee, was published under the authority of the Standards Committee and comes into effect on 15 March 1999 © BSI 03-2001 ISBN 0 580 30542 2 National foreword This British Standard is the official English language version of EN ISO 734-2:2000. It is identical with ISO 734-2:1998. The UK participation in its preparation was entrusted to Technical Committee AW/2, Oilseeds and residues, which has the responsibility to: 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. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references Attention is drawn to the fact that CEN and CENELEC Standards normally include an annex which lists normative references to international publications with their corresponding European publications. The British Standards which implement these international or European publications may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct applica- tion. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the EN ISO title page, the EN ISO foreword page, the ISO title page, the ISO foreword page, pages 1 to 5 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 11090March 2001 Implementation of the European Standard Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:53:41 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 734-2:2001 © BSI 03-2001 i Contents Page National forewordInside front cover Forewordii 1Scope1 2Normative references1 3Definition1 4Principle1 5Reagents1 6Apparatus1 7Sampling2 8Preparation of test sample2 9Procedure2 10Expression of results2 11Precision2 12Test report3 Annex A (informative) Results of an interlaboratory test5 Annex B (informative) Bibliography5 Figure 1 Grinding beaker with cooling mantle3 Figure 2 Funnel with stanced metal pin3 Figure 3 Extraction apparatus according to Twisselmann4 Table A.1 Results of interlaboratory test5 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:53:41 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii blank Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:53:41 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM EN ISO 734-2 August 2000 ICS 67.200.20 English version Oilseed residues Determination of oil content Part 2: Rapid extraction method (ISO 734-2:1998) Tourteaux de graines oléagineuses Détermination de la teneur en huile Partie 2: Méthode rapide par extraction (ISO 734-2:1998) Ölsamenrückstände Bestimmung des Ölgehaltes Teil 2: Schnellextraktionsverfahren (ISO 734-2:1998) This European Standard was approved by CEN on 5 August 2000. 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, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European Committee for Standardization Comité Européen de Normalisation Europäisches Komitee für Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels © 2000 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 734-2:2000 E Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:53:41 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 734-2:2000 © BSI 03-2001 Foreword The text of the International Standard from Technical Committee ISO/TC 34, Agricultural food products of the International Organization for Standardization (ISO) has been taken over as an European Standard 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 February 2001, and conflicting national standards shall be withdrawn at the latest by February 2001. 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, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:53:41 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:53:41 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 734-2:2000 © BSI 03-2001 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 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. 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. International Standard ISO 734-1 was prepared by Technical Committee ISO/TC 34, Agricultural food products, Subcommittee SC 2, Oleaginous seeds and fruits. This first edition of ISO 734-2, together with ISO 734-1, cancels and replaces ISO 734:1979, which has been technically revised. ISO 734 consists of the following parts, under the general title Oilseed residues Determination of oil content: Part 1: Extraction method with hexane (or light petroleum); Part 2: Rapid extraction method. Annexes A and B of this part of ISO 734 are for information only. Descriptors: Agricultural products, plant products, oilseeds, oilseed residues, determination of content, oils, extraction methods Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:53:41 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 734-2:2000 © BSI 03-2001 1 1 Scope This part of ISO 734 specifies an extraction method which may be used to assess the efficiency of a de-oiling process by comparing the oil content of the oilseed with the residual oil content of the corresponding extraction meals, pellets and expeller cakes. It is applicable to oilseed residues obtained from oilseeds by expelling or by extraction with a solvent, as well as to the pellets made from the residues. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this part of ISO 734. At the time of the publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this part of ISO 734 are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 771:1977, Oilseed residues Determination of moisture and volatile matter content. ISO 5502:1992, Oilseed residues Preparation of test samples. 3 Definition For the purposes of this part of ISO 734, the following definition applies. 3.1 oil content whole of the substances extracted under the operating conditions specified in this part of ISO 734, and expressed as a percentage by mass of the product as received NOTEOn request the oil content may be expressed relative to dry matter. 4 Principle Pulverization of the sample in a micro-ball mill in the presence of a solvent and subsequent extraction with the same solvent in a suitable apparatus. Removal of the solvent from the extract by distillation, then weighing of the residue after drying. 5 Reagents Use only reagents of recognized analytical grade, unless otherwise specified. 5.1 Technical hexane, n-hexane or light petroleum, essentially composed of hydrocarbons with 6 carbon atoms, of which less than 5 % distils below 50?C and more than 95 % distils between 50?C and 70?C. For either solvent, the residue on complete evaporation shall not exceed 2 mg per 100 ml. NOTEThe solvent recovered from the extract by distillation should not be used for further determinations. 6 Apparatus Usual laboratory apparatus and, in particular, the following. 6.1 Analytical balance, capable of weighing to an accuracy of?0,001 g. 6.2 Drying oven, capable of being maintained at 103?C?2?C. 6.3 Micro-ball mill, of the Dangoumau type1). 6.4 Grinding beaker, made of stainless steel or polytetrafluoroethylene, and of capacity 65 ml (see Figure 1), with stainless-steel balls. The grinding beaker can (as depicted in Figure 1) be surrounded by a cooling mantle through which water circulates during grinding. When using grinding beakers made of polytetrafluoroethylene, cooling is obligatory. 6.5 Funnel, made of light-petroleum-resistant plastic, with a diameter of 70 mm, a stem external diameter of 10 mm and stem length of 100 mm to 150 mm. The stem shall just reach into the extraction thimble on placing the funnel in the extraction apparatus as described in 9.2.4. There is a fixed metal pin in the funnel to retain the stainless-steel balls (see Figure 2). 6.6 Continuous extraction apparatus, of the Twisselmann type2) with ground joints, consisting of a flat-bottomed flask of 100 ml to 200 ml capacity, a connecting tube (extractor) to hold the extraction thimble, and a reflux condensor (see Figure 3). NOTEThe use of other extractors is conditional upon the results of a test on a standard material of known oil content to confirm the suitability of the apparatus. 6.7 Extraction thimbles, of dimensions 25 mm?100 mm, with wall strength 1,5 mm and reinforced bottom part. 6.8 Water bath, electrically heated and explosion-proof. 1)The Dangoumau mill is an example of a suitable product available commercially. 2)Twisselmann continuous extraction apparatus is an example of a suitable apparatus available commercially. This information is given for the convenience of users of this part of ISO 734 and does not constitute an endorsement by ISO of these products. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:53:41 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 734-2:2000 2© BSI 03-2001 6.9 Steam bath. 6.10 Cotton wool, fat-free. NOTEFor example, defatted cotton wool for ophthalmic use. 7 Sampling Sampling is not part of the method specified in this part of ISO 734. A recommended sampling method is given in ISO 55001. It is important that the laboratory receives a sample which is truly representative and has not been damaged or changed during transport or storage. 8 Preparation of test sample Prepare the test sample in accordance with ISO 5502. 9 Procedure NOTEIf it is required to check whether the repeatability limit (11.2) is met, carry out two single determinations in accordance with 9.1 to 9.2.11. 9.1 Test portion Weigh, to the nearest 0,001 g, 5 g of the well-mixed test sample in an extraction thimble (6.7). 9.2 Determination 9.2.1 Transfer the contents of the thimble to the grinding beaker (6.4) of the micro-ball mill containing all the stainless-steel balls. 9.2.2 Add about 20 ml of solvent (5.1). Close the grinding beaker and shake in the ball mill (6.3) for 10 min. (See 6.4 for warning about cooling.) 9.2.3 Place the thimble in the connecting tube (extractor) of the extraction apparatus (6.6) and connect this to a dried and weighed flask. 9.2.4 Place the funnel (6.5) in the connecting tube in such a manner that the stem of the funnel reaches into the upper quarter of the thimble. 9.2.5 Then pour the contents of the grinding beaker through the funnel into the extraction thimble in such a manner that the balls remain on the metal pin in the funnel. Carefully rinse the grinding beaker, its lid and the balls with solvent in order to transfer all sample particles quantitatively into the extraction thimble. This requires about 50 ml of solvent, the total volume of which is therefore about 70 ml. 9.2.6 Cover the contents of the extraction thimble with a wad of cotton wool (6.10). Connect the flask and connecting tube (extractor) to the condenser and place the whole apparatus in a boiling water bath (6.8) or steam bath (6.9). 9.2.7 Extract for 1 h, calculated from when the solvent begins to boil, while maintening a reflux rate of least 5 ml/min. 9.2.8 Then close the cock of the Twisselmann condenser and collect the bulk of the solvent in the collecting vessel of the extraction apparatus. (See note in 5.1.) 9.2.9 Remove the flask from the extraction apparatus and leave for about 5 min on the boiling water bath to evaporate any residual solvent. 9.2.10 Dry the flask containing the oil for 1,5 h in the drying oven (6.2) set at 103?C, and weig