EN ISO 659-2009 en Oilseeds - Determination of oil content (Reference method)《油料种子 油含量的测定(参考方式)》.pdf

1、BS EN ISO 659:2009ICS 67.200.20NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDOilseeds Determination of oil content (Reference method) (ISO 659:2009)This British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on 31 July 20

2、09 BSI 2009ISBN 978 0 580 62165 9Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 659:2009National forewordThis British Standard is the UK implementation of EN ISO 659:2009. Itsupersedes BS EN ISO 659:1999 which is withdrawn.The UK participation in its preparation was entrusted t

3、o TechnicalCommittee AW/307, Oil seeds, animal and vegetable fats and oils andtheir by products.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsib

4、le for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 659July 2009ICS 67.200.20 Supersedes EN ISO 659:1998 English VersionOilseeds - Determination of oil content (Reference method) (ISO659:

5、2009)Graines olagineuses - Dtermination de la teneur en huile(Mthode de rfrence) (ISO 659:2009)lsamen - Bestimmung des lgehaltes(Referenzverfahren) (ISO 659:2009)This European Standard was approved by CEN on 3 June 2009.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which

6、stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN Management Centre or to any CEN member.This European Standar

7、d exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standard

8、s bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.

9、EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: Avenue Marnix 17, B-1000 Brussels 2009 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 659:2009: EBS EN ISO 659:

10、2009EN ISO 659:2009 (E) 3 Foreword This document (EN ISO 659:2009) has been prepared by Technical Committee ISO/TC 34 “Food products“ in collaboration with Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fats and oils and their by-products - Methods of sampling and analysis” the secre

11、tariat 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 2010, and conflicting national standards shall be withdrawn at the latest by January 2010. Attention is dr

12、awn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 659:1998. According to the CEN/CENELEC Internal Regulations, the nati

13、onal standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

14、Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 659:2009 has been approved by CEN as a EN ISO 659:2009 without any modification. BS EN ISO 659:2009ISO 659:2009(E) ISO 2009 All rights reserved iiiContents Page Forewo

15、rd iv 1 Scope . 1 2 Normative references . 1 3 Terms and definitions. 1 4 Principle. 1 5 Reagent 2 6 Apparatus 2 7 Sampling 3 8 Preparation of test sample. 3 8.1 Reduction of laboratory sample 3 8.2 Predrying . 3 8.3 Test sample . 4 9 Procedure 5 9.1 General. 5 9.2 Test portion . 5 9.3 Determination

16、 6 9.4 “Oil content” of impurities. 7 10 Expression of results . 7 10.1 Method of calculation. 7 11 Precision 10 11.1 Interlaboratory test programme 10 11.2 Repeatability 10 11.3 Reproducibility 10 12 Test report . 10 Annex A (informative) Results of interlaboratory tests on the determination of oil

17、 content . 11 Bibliography . 12 BS EN ISO 659:2009ISO 659:2009(E) iv ISO 2009 All rights reservedForeword 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 car

18、ried 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.

19、 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 2. The main task of technical committees is to prepare Interna

20、tional 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

21、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 659 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 2, Oleaginous seeds and fruits and oilseed meals. This fourth edition

22、cancels and replaces the third edition1)(ISO 659:1998), which has been technically revised. The main change is the inclusion of an additional subclause (Subclause 8.3.5) for the preparation of the test sample in the case of sunflower seed. This different procedure for sunflower seed includes an extr

23、a step, viz measurement of the moisture content after grinding the seed. This is necessary to correct for the loss of moisture caused by the heating of the seed which occurs during grinding due to the particular physical nature of sunflower seed. 1) Users should note that the front cover and forewor

24、d of ISO 659:1998 indicate erroneously that it is the second edition, whereas it is in fact the third. BS EN ISO 659:2009INTERNATIONAL STANDARD ISO 659:2009(E) ISO 2009 All rights reserved 1Oilseeds Determination of oil content (Reference method) 1 Scope This International Standard specifies a refer

25、ence method for the determination of the hexane extract (or light petroleum extract), called the “oil content”, of oilseeds used as industrial raw materials. The procedure for sunflower seed is different from those for other seeds as it includes an additional moisture content determination after the

26、 seed has been ground to prepare the test sample. The method has been tested on rapeseed, soya beans and sunflower seed. This does not, however, preclude its applicability to other commercial seeds. If required, the pure seeds and the impurities (see 9.4) can be analysed separately. In the case of g

27、roundnuts (see 10.1.6), the pure seeds, the total fines, the non-oleaginous impurities and the oleaginous impurities can be analysed separately. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition ci

28、ted applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 658, Oilseeds Determination of content of impurities ISO 664, Oilseeds Reduction of laboratory sample to test sample ISO 665, Oilseeds Determination of moisture and volatile mat

29、ter content 3 Terms and definitions For the purposes of this International Standard, the following terms and definitions apply. 3.1 hexane extract “oil content” all the substances extracted under the operating conditions specified in this International Standard, expressed as a percentage by mass of

30、the product as received, or on the cleaned seed NOTE On request, it may be expressed relative to the dry matter. 4 Principle The oil is extracted from a test portion, in a suitable apparatus, with hexane or light petroleum. The solvent is removed from the extract and the extract weighed. Due to the

31、varied nature of seeds, there are some variations in the procedure for different seeds. BS EN ISO 659:2009ISO 659:2009(E) 2 ISO 2009 All rights reserved5 Reagent 5.1 Technical hexane, n-hexane or light petroleum, essentially composed of hydrocarbons with six carbon atoms, of which less than 5 % dist

32、ils below 40 C and more than 95 % distils between 40 C and 60 C or between 50 C and 70 C, and which has a bromine value of less than 1. 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 balan

33、ce, with an accuracy of 0,001 g. 6.2 Mechanical mill, easy to clean, appropriate for the nature of the oilseeds and allowing the oilseeds to be ground to a uniform particle size without appreciable heating or change in moisture, volatile-matter or oil content. NOTE The following mills have been foun

34、d to give satisfactory results: the Christy see 8.3.2, 8.3.3 and 8.3.4); the Retsch ZM 200 ultra-centrifugal mill2), with a 1 mm screen for sunflower seed or with other screens depending on seed type. Other mills may be satisfactory, provided they conform to the criteria given above. 6.3 Mechanical

35、microgrinder, capable of producing a fineness of grind of the oilseeds of less than 160 m, with the exception of the “shell”, particles of which may reach 400 m. Coffee grinders and similar cutting-action mechanical grinders shall not be used as microgrinders. NOTE A ball mill comprising a stainless

36、-steel tube of volume approximately 120 ml and 1 cm, 2 cm and 3 cm diameter steel balls (weighing approximately 7 g, 30 g and 130 g), depending on the sample being ground, and utilizing extremely rapid shaking, has been found to be suitable. If the microgrinder and its closure are designed for use w

37、ith solvents, a small amount (approximately 20 ml) of solvent may be added to the cylinder in order to increase the speed of the extraction. 6.4 Extraction thimble (cellulose) and cotton wool, free from matter soluble in hexane or light petroleum. 6.5 Suitable extraction apparatus, fitted with a fla

38、sk of capacity 200 ml to 250 ml. Straight-through extractors, for example the Butt, Smalley or Bolton-Williams type, are preferred for safety reasons and have been found to give a more efficient extraction. The use of other extractors is conditional upon the results of a test on a standard material

39、of known oil content to confirm the suitability of the apparatus. If a Soxhlet syphoning-type extractor is used then, for safety reasons, a 250 ml flask should be utilized and the volume of solvent used shall be at least 150 ml. This should prevent rapid boiling on syphoning, which could otherwise c

40、ause loss of solvent and/or part of the test portion. 6.6 Pumice stone, in small particles, or other anti-bumping granules, previously dried in an oven at (130 2) C and cooled in a desiccator. 2) The Christy for shell and dirt: grind for 10 min in a microgrinder (6.3) using a 3 cm steel ball. 8.3.3

41、Copra (and coconut) Freeze the entire sample before milling in the mechanical mill (6.2). A mechanical mill with a 6 mm screen has been found to be satisfactory. The length of the particles shall be approximately 2 mm but shall not be greater than 5 mm. Mix the particles carefully and carry out the

42、determination without delay. Care shall be taken to avoid condensation of moisture onto the seeds during and after grinding. 8.3.4 Large- and medium-sized seeds (illipe nuts, shea nuts, groundnuts, soya, etc., but NOT sunflower seed or cottonseed) Grind the test sample in the mechanical mill (6.2) u

43、ntil the major dimension of the particles obtained is not greater than 2 mm. Reject the first particles (about one-twentieth of the sample), collect the rest, mix carefully and carry out the determination without delay. The following milling techniques have been found to be satisfactory: for soya: a

44、 mechanical mill with a 0,8 mm perforated plate or with a 1 mm screen; for groundnuts: a mechanical mill with a 3 mm bar screen (with samples containing a mass fraction of more than about 45 % of oil, care shall be taken to avoid, as far as possible, the formation of a pasty mass); other seeds: a me

45、chanical mill with a 6 mm bar screen. BS EN ISO 659:2009ISO 659:2009(E) ISO 2009 All rights reserved 5The grinding of very oily seeds can often be improved if the seeds are first frozen at 10 C to 20 C, but great care shall be taken to avoid condensation of moisture onto the seeds during and after g

46、rinding. 8.3.5 Sunflower seed Determine the moisture and volatile-matter content of the sunflower seed (as received) on the whole seed in accordance with ISO 665, taking care to observe strictly the drying periods laid down in the method specified in ISO 665. Record the result of this moisture and v

47、olatile-matter determination (U1). Grind the test sample in a mechanical mill (6.2). During grinding, the mill shall be fed slowly with the sunflower seeds to prevent a paste being formed. A mechanical mill with a 1 mm screen has been found to be suitable. If a screen-type mill is not used, sieve th

48、rough a 2 mm sieve and regrind the material which does not pass through the sieve until the major dimension of the particles is not greater than 2 mm. Collect all the sievings, mix carefully and, without delay, determine the moisture and volatile-matter content in accordance with ISO 665, taking car

49、e to observe strictly the drying periods laid down in ISO 665. Record the result of the moisture and volatile-matter determination on the ground seed (U2) and carry out the oil extraction on the ground seed as specified in Clause 9. 8.3.6 Cottonseed Weigh, to the nearest 1 mg, into a tared metal dish (6.12) about 15 g of the sample as received. Place the dish and seeds in the oven (6.11), previously heated to 130 C, and leave to dry for 2 h at (130 2) C. Then remove the dish from the oven and allow to cool in