BS EN ISO 22630-2015 Oilseed meals Determination of oil content Rapid extraction method《含油种子 油含量的测定 快速萃取法》.pdf

1、BSI Standards PublicationBS EN ISO 22630:2015Oilseed meals Determinationof oil content Rapidextraction methodBS EN ISO 22630:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 22630:2015. It supersedes BS EN ISO 734-2:2010 which iswithdrawn.The UK particip

2、ation in its preparation was entrusted to Technical Committee AW/307, Oilseeds, animal and vegetable fats and oils and their by-products.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary pr

3、ovisions of a contract. Users are responsible for its correct application. The British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 86666 1 ICS 67.200.20 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was pub

4、lished under the authority of the Standards Policy and Strategy Committee on 31 December 2015.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 22630 December 2015 ICS 67.200.20 Supersedes EN ISO 734-2:2010English Versi

5、on Oilseed meals - Determination of oil content - Rapid extraction method (ISO 22630:2015) Tourteaux de graines olagineuses - Dtermination de la teneur en huile - Mthode dextraction rapide (ISO 22630:2015) lsamenschrote - Bestimmung des lgehaltes - Schnellextraktionsverfahren (ISO 22630:2015) This E

6、uropean Standard was approved by CEN on 26 September 2015. 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 referen

7、ces concerning such national standards may be obtained on application to the CEN-CENELEC 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 m

8、ember into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,

9、France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES

10、 KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 22630:2015 EBS EN ISO 22630:2015EN ISO 22630:2015 (E) 3 European foreword This document (

11、EN ISO 22630:2015) has been prepared by Technical Committee ISO/TC 34 “Foodproducts“ in collaboration with Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fatsand oils and their by-products - Methods of sampling and analysis” the secretariat of which is held byAFNOR. This European Sta

12、ndard shall be given the status of a national standard, either by publication of anidentical text or by endorsement, at the latest by June 2016, and conflicting national standards shall bewithdrawn at the latest by June 2016. Attention is drawn to the possibility that some of the elements of this do

13、cument may be the subject ofpatent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patentrights. This document supersedes EN ISO 734-2:2010. According to the CEN-CENELEC Internal Regulations, the national standards organizations of thefollowing countries are

14、bound to implement this European Standard: Austria, Belgium, Bulgaria,Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,Netherlands, Norway, Poland, Portuga

15、l, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland,Turkey and the United Kingdom. Endorsement notice The text of ISO 22630:2015 has been approved by CEN as EN ISO 22630:2015 without any modification. BS EN ISO 22630:2015ISO 22630:2015(E)Foreword iv1 Scope . 12 Normative references 13 Terms a

16、nd definitions . 14 Principle 15 Reagents and materials . 16 Apparatus . 27 Sampling 38 Preparation of test sample . 39 Procedure. 49.1 General . 49.2 Test portion 49.3 Determination . 410 Expression of results 511 Precision . 511.1 Interlaboratory test. 511.2 Repeatability . 511.3 Reproducibility .

17、 512 Test report . 6Annex A (informative) Results of interlaboratory test 7Bibliography 8 ISO 2015 All rights reserved iiiContents PageBS EN ISO 22630:2015ISO 22630:2015(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO mem

18、ber 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, governmen

19、tal 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.The procedures used to develop this document and those intended for its further maintenance

20、are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).Attention is

21、 drawn to the possibility that some of the 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. Details of any patent rights identified during the development of the document will be in the Introduction and/or

22、 on the ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity asses

23、sment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 34, Food products, Subcommittee SC 2, Oleaginous seeds and fruits and oil

24、seed meals.This first edition cancels and replaces ISO 734-2:2008, which has been renumbered and editorially revised.iv ISO 2015 All rights reservedBS EN ISO 22630:2015INTERNATIONAL STANDARD ISO 22630:2015(E)Oilseed meals Determination of oil content Rapid extraction method1 ScopeThis International

25、Standard 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 not applicable to disputed cases, for which ISO

26、734 is applicable.It is applicable to oilseed meals obtained from oilseeds by expelling or by extraction with a solvent, as well as to the pellets made from the residues.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensa

27、ble for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 771, Oilseed residues Determination of moisture and volatile matter contentISO 5502, Oilseed residues Preparatio

28、n of test samples3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1oil contentsum of the mass fractions of the substances extracted under the operating conditions specified in this International Standard on the basis of the product as receivedNote

29、 1 to entry: The mass fraction is expressed as a percentage.Note 2 to entry: On request, the oil content may be expressed relative to dry matter.4 PrincipleThe test portion is ground in a micro-ball mill in the presence of a solvent and subsequently extracted with the same solvent in a suitable appa

30、ratus. The solvent is removed from the extract by distillation, then the residue is weighed after drying.5 Reagents and materialsUse only reagents of recognized analytical grade, unless otherwise specified.5.1 Technical hexane, n-hexane or light petroleum ether, essentially composed of hydrocarbons

31、with six 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. ISO 2015 All rights reserved 1BS EN ISO 22630:2015ISO 22630:2015(E)The solvent recovered from th

32、e extract by distillation should not be used for further determinations.5.2 Cotton wool, fat-free.EXAMPLE Defatted cotton wool for ophthalmic use.6 ApparatusUsual laboratory apparatus and, in particular, the following.6.1 Analytical balance, capable of being read to the nearest 0,001 g.6.2 Drying ov

33、en, capable of being maintained at 103 C 2 C.6.3 Mechanical microgrinder, capable of wet grinding in the presence of light petroleum ether and reducing the test portion to an average particle size of less than 10 m. A commercially available ball mill1)is suitable.When using grinding beakers made of

34、polytetrafluoroethylene, cooling is obligatory. A suitable cooling jacket is shown in Figure 1.Figure 1 Grinding beaker with cooling mantle6.4 Funnel, made of light petroleum ether-resistant plastic, with a diameter of 70 mm, a stem external diameter of 10 mm and a stem length of 100 mm to 150 mm.Th

35、e stem shall just reach into the extraction thimble on placing the funnel in the extraction apparatus as described in 9.3.4. There is a fixed metal pin in the funnel to retain the stainless steel balls (see Figure 2).1) The Dangoumau ball mill is an example of a suitable product available commercial

36、ly and has been studied in a ring test (Annex A). This information is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of this product. Equivalent products may be used if they can be shown to lead to the same results.2 ISO 2015 All right

37、s reservedBS EN ISO 22630:2015ISO 22630:2015(E)Dimensions in millimetresFigure 2 Funnel with stanced metal pin6.5 Continuous extraction apparatus2), with ground joints, consisting of a flat bottomed flask of capacity 100 ml to 200 ml, a connecting tube (extractor) to hold the extraction thimble, and

38、 a reflux condenser.The apparatus should include a suitable heating element for boiling technical hexane under reflux conditions. This might be a water bath, steam bath or safety-approved electrical heating unit.NOTE The use of other extractors is conditional upon the results of a test on a standard

39、 material of known oil content to confirm the suitability of the apparatus.6.6 Extraction thimbles, of dimensions 25 mm 100 mm, of wall thickness 1,5 mm and a reinforced bottom part.7 SamplingA representative sample should have been sent to the laboratory. It should not have been damaged or changed

40、during transport or storage.Sampling is not part of the method specified in this International Standard. A recommended sampling method is given in ISO 5500.18 Preparation of test samplePrepare the test sample in accordance with ISO 5502.2) The Twisselmann and Butt extractors are examples of suitable

41、 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. The Butt-type extractor is described in AOCS Official method Aa 4-38.4 ISO 2015 All rights reserved 3BS EN ISO 2263

42、0:2015ISO 22630:2015(E)9 Procedure9.1 GeneralIf it is required to check whether the repeatability limit (11.2) is met, carry out two single determinations in accordance with 9.2 to 9.3.11.9.2 Test portionWeigh, to the nearest 0,001 g, 5 g of the well-mixed test sample in an extraction thimble (6.6).

43、9.3 Determination9.3.1 Transfer the contents of the thimble to the beaker or tube of the mechanical microgrinder (6.3) containing all stainless-steels balls.9.3.2 Add about 20 ml of solvent (5.1). Close the grinding beaker or tube and shake in the microgrinder (6.3) for 10 min or shake the stainless

44、 steel tubes on a flat bed shaker for 45 min horizontally at a frequency of 240 min1, with a horizontal displacement of 35 mm.9.3.3 Place the thimble (6.6) in the connecting tube (extractor) of the extraction apparatus (6.5) and connect this to a dried and weighed flask.9.3.4 Place the funnel (6.4)

45、in the connecting tube in such a manner that the stem of the funnel reaches into the upper quarter of the thimble.9.3.5 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

46、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.9.3.6 Cover the contents of the extraction thimble with a wad of cott

47、on wool (5.2). Connect the flask and connecting tube (extractor) to the condenser and place the whole apparatus on the heating apparatus.9.3.7 Extract for 1 h, calculated from when the solvent begins to boil, while maintaining a reflux rate of at least 5 ml/min.9.3.8 Collect the bulk of the solvent

48、in the collecting vessel of the extraction apparatus using the appropriate actions. Discard recovered solvent.9.3.9 Remove the flask from the extraction apparatus and leave for about 5 min on the boiling water bath to evaporate any residual solvent.9.3.10 Dry the flask containing the oil for 1,5 h i

49、n the drying oven (6.2) maintained at 103 C, and weigh after cooling to room temperature.CAUTION Drying of highly unsaturated oils (e.g. flaxseed oils) may cause the oils to start oxidizing. This might require special attention if the oils are required for other tests.9.3.11 Dry the flask for a further 10 min at the same temperature and weigh after cooling. The difference between the two weighings shall not exceed 0,01 g. If this is not the case, repeat the drying and weighing procedures.4 ISO 2015 All rights reservedBS E