1、May 2016 English price group 9No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 67.200.20!%SM7“2484220www.din.deDIN E
2、N ISO 22630Oilseed meals Determination of oil content Rapid extraction method (ISO 22630:2015);English version EN ISO 22630:2015,English translation of DIN EN ISO 22630:2016-05lsamenschrote Bestimmung des lgehaltes Schnellextraktionsverfahren (ISO 22630:2015);Englische Fassung EN ISO 22630:2015,Engl
3、ische bersetzung von DIN EN ISO 22630:2016-05Tourteaux de graines olagineuses Dtermination de la teneur en huile Mthode dextraction rapide (ISO 22630:2015);Version anglaise EN ISO 22630:2015,Traduction anglaise de DIN EN ISO 22630:2016-05SupersedesDIN EN ISO 734-2:2010-08www.beuth.deDocument compris
4、es 14 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.04.16 DIN EN ISO 22630:2016-05 2 A comma is used as the decimal marker. National foreword This document (EN ISO 22630:2015) has been prepared by Technical Committee ISO/TC 3
5、4 “Food products” (Secretariat: AFNOR, France) in collaboration with Technical Committee CEN/TC 307 “Oil seeds, vegetable and animal fats and oils and their by-products Methods of sampling and analysis” (Secretariat: AFNOR, France). The responsible German bodies involved in its preparation were DIN-
6、Normenausschuss Lebensmittel und landwirtschaftliche Produkte (DIN Standards Committee Food and Agricultural Products) and the Deutsche Gesellschaft fr Fettwissenschaft (German Fat Research Society), Joint Committee NA 057-05-05 AA Gemeinschaftsausschuss fr die Analytik von Fetten, len, Fettprodukte
7、n, verwandten Stoffen und Rohstoffen. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 5725-1 DIN ISO 5725-1 ISO 5725-2 DIN ISO 5725-2 Amendments This standard differs from DIN EN ISO 734-2:2010-08 as follows: a) the standard has been ed
8、itorially revised and brought in line with the current rules of presentation. Previous editions DIN EN ISO 734-2: 2001-02, 2008-10, 2010-08 National Annex NA (informative) Bibliography DIN ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and
9、 definitions DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 22630 December 2015 ICS 67.200.2
10、0 Supersedes EN ISO 734-2:2010English Version 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 - Schnellex
11、traktionsverfahren (ISO 22630:2015) This European 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
12、-to-date lists and bibliographical references 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 trans
13、lation under the responsibility of a CEN member 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, Finlan
14、d, Former Yugoslav Republic of Macedonia, 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
15、COMIT EUROPEN DE NORMALISATION EUROPISCHES 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 EEuropean foreword .31 Scope . 52 No
16、rmative references 53 Terms and definitions . 54 Principle 55 Reagents and materials . 56 Apparatus . 67 Sampling 78 Preparation of test sample . 79 Procedure. 89.1 General . 89.2 Test portion 89.3 Determination . 810 Expression of results 911 Precision . 911.1 Interlaboratory test. 911.2 Repeatabil
17、ity . 911.3 Reproducibility . 912 Test report 10Annex A (informative) Results of interlaboratory test . 11Bibliography . 12Contents PageDIN EN ISO 22630:2016-05 EN ISO 22630:2015 (E) 2Foreword .4European foreword This document (EN ISO 22630:2015) has been prepared by Technical Committee ISO/TC 34 “F
18、ood 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 secretariat of which is held by AFNOR. This European Standard shall be given the status of a national standard, either by pub
19、lication of an identical text or by endorsement, at the latest by June 2016, and conflicting national standards shall be withdrawn at the latest by June 2016. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shal
20、l not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 734-2:2010. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bul
21、garia, 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, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, T
22、urkey 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. DIN EN ISO 22630:2016-05 EN ISO 22630:2015 (E) 3 ForewordISO (the International Organization for Standardization) is a worldwide federation of national
23、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
24、 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.The procedures used to develop this document and those intended for
25、 its further maintenance 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
26、/directives).Attention is 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 i
27、n the Introduction and/or 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 re
28、lated to conformity assessment, 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
29、 seeds and fruits and oilseed meals.This first edition cancels and replaces ISO 734-2:2008, which has been renumbered and editorially revised.DIN EN ISO 22630:2016-05 EN ISO 22630:2015 (E) 4 1 ScopeThis International Standard specifies an extraction method which may be used to assess the efficiency
30、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 734 is applicable.It is applicable to oilseed meals obtained from oilseeds by expel
31、ling 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 indispensable for its application. For dated references, only the edition cited applies. For
32、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 Preparation of test samples3 Terms and definitionsFor the purposes of this document, the foll
33、owing 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 1 to entry: The mass fraction is expressed as a percentage.Note 2 to entry: On req
34、uest, 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 apparatus. The solvent is removed from the extract by distillation, then the residue is
35、 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 with six carbon atoms, of which less than 5 % distils below 50 C and more than 95 %
36、 distils between 50 C and 70 C.For either solvent, the residue on complete evaporation shall not exceed 2 mg per 100 ml.DIN EN ISO 22630:2016-05 EN ISO 22630:2015 (E) 5 The solvent recovered from the extract by distillation should not be used for further determinations.5.2 Cotton wool, fat-free.EXAM
37、PLE 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 oven, capable of being maintained at 103 C 2 C.6.3 Mechanical microgrinder, capable of wet grinding in t
38、he 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 polytetrafluoroethylene, cooling is obligatory. A suitable cooling jacket is shown in Figure 1.Figure
39、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.The stem shall just reach into the extraction thimble on placing the funnel in the extraction apparatus
40、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 commercially and has been studied in a ring test (Annex A). This information is given for the convenience of use
41、rs 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.DIN EN ISO 22630:2016-05 EN ISO 22630:2015 (E) 6 Dimensions in millimetresFigure 2 Funnel with stanced metal pin6.5 Contin
42、uous 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 a reflux condenser.The apparatus should include a suitable heating element for boiling technical hexane under reflux co
43、nditions. 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 material of known oil content to confirm the suitability of the apparatus.6.6 Extraction thimbles, of dimensions 25 mm
44、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 during transport or storage.Sampling is not part of the method specified in this International Standard. A recommended s
45、ampling 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 products available commercially. This information is given for the convenience of users of this International Standard
46、and does not constitute an endorsement by ISO of these products. The Butt-type extractor is described in AOCS Official method Aa 4-38.4DIN EN ISO 22630:2016-05 EN ISO 22630:2015 (E) 7 9 Procedure9.1 GeneralIf it is required to check whether the repeatability limit (11.2) is met, carry out two single
47、 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).9.3 Determination9.3.1 Transfer the contents of the thimble to the beaker or tube of the mechanical microgrinder (6.3) containing all stain
48、less-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 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
