EN ISO 734-2015 en Oilseed meals - Determination of oil content - Extraction method with hexane (or light petroleum)《油籽粕 油含量的测定 正己烷萃取法(或石油醚)(ISO 734 2015)》.pdf

1、BSI Standards PublicationOilseed meals Determination of oil content Extraction method with hexane (or light petroleum)BS EN ISO 734:2015National forewordThis British Standard is the UK implementation of EN ISO 734:2015.It supersedes BS EN ISO 734-1:2006 which is withdrawn.The UK participation in its

2、 preparation was entrusted to TechnicalCommittee AW/307, Oilseeds, animal and vegetable fats and oils and theirby-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 provisions ofa co

3、ntract. Users are responsible for its correct application. The British Standards Institution 2016.Published by BSI Standards Limited 2016ISBN 978 0 580 86665 4ICS 67.200.20Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the au

4、thority of theStandards Policy and Strategy Committee on 31 January 2016. Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS EN ISO 734:2015EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 734 December 2015 ICS 67.200.20 Supersedes EN ISO 734-1:2006English Ver

5、sion Oilseed meals - Determination of oil content - Extraction method with hexane (or light petroleum) (ISO 734:2015)Tourteaux de graines olagineuses - Dtermination de la teneur en huile - Mthode par extraction lhexane (ou lther de ptrole) (ISO 734:2015) lsamenschrote - Bestimmung des lgehaltes - Ex

6、traktionsverfahren mit Hexan (oder Petrolether) (ISO 734:2015) 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

7、 without any alteration. Up-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 o

8、ther language made by translation 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 Republi

9、c, 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, Turkey and United Kingdom. EUROPEAN CO

10、MMITTEE FOR STANDARDIZATION 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 734:2015 EBS EN ISO

11、 734:2015EN ISO 734:2015 (E) 2 Contents Page European foreword . 3 BS EN ISO 734:2015EN ISO 734:2015 (E) 3 European foreword This document (EN ISO 734:2015) has been prepared by Technical Committee ISO/TC 34 “Food products“ in collaboration with Technical Committee CEN/TC 307 “Oilseeds, vegetable an

12、d 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 June 2016, and conflicti

13、ng 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 shall not be held responsible for identifying any or all such patent rights. This document sup

14、ersedes EN ISO 734-1:2006. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republi

15、c of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 734:2015 has been approve

16、d by CEN as EN ISO 734:2015 without any modification. BS EN ISO 734:2015ISO 734:2015(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 15 Reagents 16 Apparatus . 17 Sampling 28 Preparation of test sample . 29 Procedure. 39.1 Number of determinations

17、 . 39.2 Test portion 39.3 Pre-drying . 39.4 Determination . 39.4.1 Preparation of the flask 39.4.2 First extraction 39.4.3 Second extraction 39.4.4 Elimination of solvent and weighing of the extract . 410 Expression of results 411 Precision . 511.1 Interlaboratory test. 511.2 Repeatability . 511.3 R

18、eproducibility . 512 Test report . 5Annex A (informative) Results of an interlaboratory test 6Bibliography 7 ISO 2015 All rights reserved iiiContents PageBS EN ISO 734:2015ISO 734:2015(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards

19、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 organizat

20、ions, 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 its furth

21、er 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/directive

22、s).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 in the Intr

23、oduction 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 related to c

24、onformity 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 seeds and

25、 fruits and oilseed meals.This second edition cancels and replaces ISO 734-1:2006, which has been renumbered and editorially revised.iv ISO 2015 All rights reservedBS EN ISO 734:2015ISO 734:2015(E)IntroductionA method for the determination of the oil content of oilseeds has been specified in ISO 659

26、. It is therefore necessary to provide for control of oil production by establishing a reference method for the determination of the oil content of oilseed meals in the same way. ISO 2015 All rights reserved vBS EN ISO 734:2015Oilseed meals Determination of oil content Extraction method with hexane

27、(or light petroleum)1 ScopeThis International Standard specifies a method for the determination of the hexane extract (or light-petroleum extract), called “oil content”, of meals (excluding compounded products) obtained by the extraction of oil from oilseeds by pressure or solvents.2 Normative refer

28、encesThe 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 undated references, the latest edition of the referenced document (including any amendments) applies. IS

29、O 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 following terms and definitions apply.3.1oil contentall of the substances extracted under the operating con

30、ditions specified in this International Standard, and expressed as a mass fraction, in percent, of the product as receivedNote 1 to entry: The oil content may also be expressed relative to dry matter.4 PrincipleA test portion of the product is extracted in a suitable apparatus, with technical hexane

31、 or, failing this, light petroleum. The solvent is eliminated and the extract obtained is weighed.5 ReagentsUse only reagents of recognized analytical grade, unless otherwise specified.5.1 Technical hexane, n-hexane or light petroleum, essentially composed of hydrocarbons with six carbon atoms.Less

32、than 5 % shall distil below 50 C and more than 95 % between 50 C and 70 C.For any of these solvents, the residue on complete evaporation shall not exceed 2 mg per 100 ml.6 ApparatusUsual laboratory apparatus and, in particular, the following.INTERNATIONAL STANDARD ISO 734:2015(E) ISO 2015 All rights

33、 reserved 1BS EN ISO 734:2015ISO 734:2015(E)6.1 Mechanical grinder, easy to clean and allowing the meals to be ground, without heating and without appreciable change in moisture, volatile matter and oil content, to obtain particles which pass completely through a sieve of aperture size 1 mm.6.2 Mech

34、anical microgrinder, of the Dangoumau type1)capable of producing a fineness of grinding of oilseed meals of less than 160 m, with the exception of the “shell” whose particles may reach 400 m.In laboratories where a microgrinder is not available, microgrinding of the ground sample (see 9.4.3) may be

35、replaced by trituration with a pestle and mortar, in the presence of about 10 g of sand that has been washed with hydrochloric acid and then calcined. However, grinding in a mortar cannot be applied in the case of multiple analyses because operator fatigue prevents sufficiently efficient grinding of

36、 numerous samples, and the extraction of oil from a coarsely ground sample can never be complete.6.3 Extraction thimble and cotton wool, or filter paper, free from matter soluble in hexane or light petroleum.6.4 Suitable extraction apparatus, fitted with a flask of capacity 200 ml to 250 ml.NOTE Str

37、aight-through extractors, for example the Butt, Smalley, Twisselmann and Bolton-Williams2)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.6.5 Electric heating bath (e.g. sand b

38、ath, water bath) or hot plate.6.6 Electrically heated oven, with thermostatic control, permitting ventilation or obtaining reduced pressure, capable of being maintained at 103 C 2 C.6.7 Desiccator, containing an efficient desiccant.6.8 Pumice stone, in small particles, previously dried in an oven at

39、 103 C 2 C and cooled in a dessicator.6.9 Analytical balance, capable of weighing to an accuracy of 0,001 g.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 i

40、n this International Standard. A recommended sampling method is given in ISO 5500.8 Preparation of test sample8.1 Prepare the test sample in accordance with ISO 5502.1) The Dangoumau mechanical microgrinder is an example of suitable apparatus available commercially. This information is given for the

41、 convenience or users of this International Standard and does not constitute an endorsement by ISO of this apparatus.2) The Butt, Smalley, Twisselmann or Bolton-Williams straight-through extractors are examples of suitable apparatus available commercially. This information is given for the convenien

42、ce of users of this International Standard and does not constitute an endorsement by ISO of this apparatus.2 ISO 2015 All rights reservedBS EN ISO 734:2015ISO 734:2015(E)8.2 If necessary, grind the test sample in the previously well-cleaned mechanical mill (6.1). First, use about one-twentieth of th

43、e sample to complete the cleaning of the mill, and reject these grindings. Then grind the rest, collect the grindings, mix carefully and carry out the analysis without delay.9 Procedure9.1 Number of determinationsIf it is required to check whether the repeatability (11.2) is met, carry out two singl

44、e determinations in accordance with 9.2 to 9.4.4.9.2 Test portion9.2.1 Weigh, to the nearest 0,001 g, about 10 g of the test sample (8.2).9.2.2 Transfer this test portion to the extraction thimble (6.3) and close the latter with a wad of cotton wool (6.3). If a filter paper is used, wrap the test po

45、rtion in it.9.3 Pre-dryingIf the test portion is very moist moisture and volatile matter content more than 10 % (mass fraction), leave the filled thimble for some time in an oven, maintained at a temperature not higher than 80 C, to reduce the moisture and volatile matter content to less than 10 % (

46、mass fraction).As an alternative to the pre-drying procedure described above, the test portion (9.2.1) may be mixed in a suitable vessel with 2 g to 3 g of analytical quality anhydrous sodium sulfate per 5 g of grindings. Continue as indicated in 9.2.2 and 9.4.9.4 Determination9.4.1 Preparation of t

47、he flaskWeigh, to the nearest 1 mg, the flask of the extraction apparatus (6.4) containing one or two particles of pumice stone (6.8).9.4.2 First extractionPlace the thimble (6.3) containing the test portion in the extraction apparatus (6.4). Pour into the flask the necessary quantity of solvent (5.

48、1). Fit the flask to the extraction apparatus on the electric heating bath or hot-plate (6.5). Carry out the heating so that the rate of reflux is at least 3 drops per second (boiling moderately, not violently).After extracting for 4 h, allow to cool. Remove the thimble from the extraction apparatus

49、 and place it in a current of air in order to expel the greater part of the residual solvent.9.4.3 Second extractionEmpty the thimble into the microgrinder (6.2) and grind as finely as possible. Put the mixture back into the thimble and put the latter back into the extraction apparatus. Re-extract for a further 2 h, using the same flask containing the first extract.The solution obtained in the extraction flask shall be clear. If it is not, filter it through a filter paper, collecting the filtrate in another previo