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1、BRITISH STANDARD BS EN ISO 659:1999 BS 4289-4: 1999 Oilseeds Determination of oil content (Reference method) The European Standard EN ISO 659:1998 has the status of a British Standard ICS 67.200.20 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:01:03 GMT+00:00 2006, Uncontrolled Copy, (c)
2、 BSI BS EN ISO 659:1999 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 April 1999 BSI 02-2000 ISBN 0 580 29872 8 National foreword This Br
3、itish Standard is the English language version of EN ISO 659:1998. It is identical with ISO 659:1998. It supersedes BS 4289-4:1989 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee AW/2, Oilseeds and residues, which has the responsibility to: aid enquir
4、ers 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 rep
5、resented 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
6、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
7、 to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. 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 cove
8、r, pages i and ii, the EN ISO title page, page 2, the ISO title page, pages ii to iv, pages 1 to 8 and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Amendments issue
9、d since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:01:03 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 659:1999 BSI 02-2000i Contents Page National forewordInside front cover Foreword2 Forewordiii Text of ISO 6591 Licensed Copy: sheffieldun shef
10、fieldun, na, Sun Nov 19 14:01:03 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii blank Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:01:03 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 659 June 1998 ICS 67.200.20 Descriptors: See ISO do
11、cument English version Oilseeds Determination of oil content (Reference method) (ISO 659:1998) Graines olagineuses Dtermination de la teneur en huile (Mthode de rfrence) (ISO 659:1998) lsamen Bestimmung des lgehaltes (Referenzverfahren) (ISO 659:1998) This European Standard was approved by CEN on 9
12、April 1998. 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 o
13、btained 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 S
14、ecretariat 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. CE
15、N European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1998 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 659:1998 E Lic
16、ensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:01:03 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 659:1998 BSI 02-2000 2 Foreword The text of the International Standard ISO 659:1998 has been prepared by Technical Committee ISO/TC 34 “Agricultural food products” in collaboration with Tec
17、hnical 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 endo
18、rsement, at the latest by December 1998, and conflicting national standards shall be withdrawn at the latest by December 1998. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Be
19、lgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the International Standard ISO 659:1998 was approved by CEN as a European Standard w
20、ithout any modification. NOTENormative references to International Standards are listed in Annex ZA (normative). Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:01:03 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:01:03 GMT+00:00 2006,
21、Uncontrolled Copy, (c) BSI EN ISO 659:1998 ii BSI 02-2000 Contents Page Forewordiii 1Scope1 2Normative references1 3Definition1 4Principle1 5Reagent1 6Apparatus1 7Sampling2 8Preparation of test sample2 9Procedure3 10Expression of results4 11Precision5 12Test report6 Annex A (informative) Results of
22、interlaboratory tests on the determination of oil content7 Annex B (informative) Bibliography8 Annex ZA (normative) Normative references to international publications with their relevant European publications8 Table A.1 Results of interlaboratory tests on rapeseeds7 Table A.2 Results of interlaborat
23、ory tests on soyabeans7 Table A.3 Results of interlaboratory tests on sunflower seeds8 Descriptors: Agricultural products, plant products, oilseeds, chemical analysis, determination of content, oils, extraction methods. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:01:03 GMT+00:00 2006,
24、Uncontrolled Copy, (c) BSI EN ISO 659:1998 BSI 02-2000iii 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 committe
25、es. 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 Inte
26、rnational 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
27、bodies casting a vote. International Standard ISO 659 was prepared by Technical Committee ISO/TC 34, Agricultural food products, Subcommittee SC 2, Oleaginous seeds and fruits. This second edition cancels and replaces the first edition (ISO 659:1988), which has been technically revised. Annex A and
28、Annex B of this International Standard are for information only. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:01:03 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv blank Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:01:03 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 659:1
29、998 BSI 02-20001 1 Scope This International Standard specifies a reference method for the determination of the hexane extract (or light petroleum extract), called “oil content”, of oil seeds used as industrial raw materials. NOTEIf required, the following may be analysed separately: the pure seeds a
30、nd the impurities (see 9.3); in the case of groundnuts, the pure seeds, the total fines, the non-oleaginous impurities and the oleaginous impurities. The method has been tested on rapeseed, soya beans and sunflower seeds. This does not, however, preclude its applicability to other commercial seeds.
31、2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of the publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on
32、the International Standard 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 658:1988, Oilseeds Determination of impurities. ISO 664:1990, Oils
33、eeds Reduction of laboratory sample to test sample. ISO 665:1977, Oilseeds Determination of moisture and volatile matter content. 3 Definition For the purposes of this International Standard, the following definition applies. 3.1 hexane extract, called “oil content” all the substances extracted unde
34、r the operating conditions specified in this International Standard, expressed as a percentage by mass of the product as received tale quale or on the cleaned seed NOTEOn request, it may be expressed relative to the dry matter. 4 Principle Extraction of a test portion, in a suitable apparatus, with
35、technical hexane or light petroleum. Elimination of the solvent and weighing of the extract obtained. 5 Reagent 5.1 Technical hexane, n-hexane or light petroleum, essentially composed of hydrocarbons with 6 carbon atoms, of which less than 5 % distils below 40 C and more than 95 % distils between 40
36、 C and 60 C or between 50 C and 70 C. The residue on complete evaporation shall not exceed 2 mg per 100 ml. 6 Apparatus Usual laboratory apparatus and, in particular, the following. 6.1 Analytical balance 6.2 Mechanical mill, easy to clean, appropriate for the nature of the oilseeds, and allowing th
37、e oilseeds to be ground to a uniform particle size without heating or appreciable change in moisture, volatile matter or oil content. NOTEThe following mills have been found to give satisfactory results: the Christy Norris 8 Laboratory Mill1) with perforated plate of bar-type screens depending on se
38、ed type (e.g. 0,8 mm perforated plate, 3 mm and 6 mm bar screens; see 8.3.2, 8.3.3 and 8.3.4); the Ultra Centrifugal Mill (UCM) (Glen Creston)1) with 1 mm screen for sunflower seeds and other screens according to seed type. Other mills may be satisfactory, provided they conform to the criteria given
39、 above. 6.3 Mechanical micro-grinder, capable of producing a fineness of grinding of the oilseeds of less than 160 4m, with the exception of the “shell”, particles of which may reach 400 4m. NOTEA “Dangoumau” type analytical grinder2) with a 150 ml cylinder and 1 cm, 2 cm and 3 cm diameter steel bal
40、ls (approximately 7 g, 30 g and 130 g) according to the sample being ground, has been found to be suitable. The following microgrinders have also been found to be suitable: Retsch2), IE Retsch2), Planetary Ball Mill2), S1 and S2 Centrifugal Ball Mill2), Batam Mikro Pulverizer Hammer Mill2), IKA Mill
41、2), Fritch Pulverisette 5 Planetary Ball Mill2) and Steam Mill2). 6.4 Extraction thimble and cotton wool, free from matter soluble in hexane or light petroleum. 6.5 Suitable extraction apparatus, fitted with a flask of capacity 200 ml to 250 ml. 1) The Christy Norris 8 Laboratory Mill and the Ultra
42、Centrifugal Mill (UCM) (Glen Creston) are examples of suitable products available commercially. This information is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of these products. 2) The above-mentioned microgrinders are examples of
43、suitable products available commercially. This information is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of these products. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 14:01:03 GMT+00:00 2006, Uncontrolled Copy, (c) BSI
44、EN ISO 659:1998 2 BSI 02-2000 NOTEStraight-through extractors, for example the Butt, Smalley or Bolton-Williams type3), are suitable. The 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. 6.6 Pum
45、ice stone, in small particles, or other anti-bumping granules, previously dried in an oven at (130 2) C and cooled in a desiccator. 6.7 Apparatus for safely removing solvent from extraction thimble (for example in a current of warm air). 6.8 Electric heating bath (sand bath, water bath, heating mant
46、el, etc.) or hot-plate. 6.9 Electrically heated oven, with thermostatic control, capable of being maintained at (103 2) C. The oven should be capable of being used at either atmospheric or reduced pressure (see 9.2.3). 6.10 Desiccator, containing an efficient desiccant (e.g. silica gel with blue ind
47、icator, or P2O5). 6.11 Electrically heated oven, capable of being maintained at (130 2) C (for cottonseed, see 8.3.5). 6.12 Metal dish, flat-bottomed, of diameter 100 mm and height approx. 40 mm. 7 Sampling Sampling is not part of the method specified in this International Standard. A recommended sa
48、mpling method is given in ISO 542. It is important that the laboratory receive a sample which is truly representative and has not been damaged or changed during transport and storage. 8 Preparation of test sample 8.1 Reduction of laboratory sample Prepare the test sample in accordance with ISO 664.
49、If large non-oleaginous foreign bodies have been separated before reduction of the laboratory sample, make allowance for this in the calculation (see 10.1.3). According to the requirements of the contract, take a sample as received or after separation of the impurities. 8.2 Predrying 8.2.1 The moisture content of the test portion (9.1) shall be less than 10 % (m/m) when extraction of the oil (9.2) is commenced. NOTEFailure to observe this may result in an incorrect result and invalidate the analysis. Use a rap