1、BS EN ISO 663:2017Animal and vegetable fatsand oils Determination ofinsoluble impurities content(ISO 663:2017)BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS EN ISO 663:2017 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO
2、663:2017. Itsupersedes BS EN ISO 663:2008 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee AW/307, Oilseeds, animal and vegetable fats and oils and their by-products.A list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
3、 secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2017.Published by BSI Standards Limited 2017ISBN 978 0 580 94414 7 ICS 67.200.10 Compliance with a British Standard
4、 cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 28 February 2017.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO
5、 663 February 2017 ICS 67.200.10 Supersedes EN ISO 663:2008English Version Animal and vegetable fats and oils - Determination of insoluble impurities content (ISO 663:2017) Corps gras dorigines animale et vgtale - Dtermination de la teneur en impurets insolubles (ISO 663:2017) Tierische und pflanzli
6、che Fette und le - Bestimmung des Anteils an unlslichen Verunreinigungen (ISO 663:2017) This European Standard was approved by CEN on 8 February 2017. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status
7、 of a national standard 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, Germ
8、an). A version in any other 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
9、, 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, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey
10、and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2017 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref.
11、 No. EN ISO 663:2017 EBS EN ISO 663:2017EN ISO 663:2017 (E) 3 European foreword This document (EN ISO 663:2017) 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
12、- 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 August 2017, and conflicting national standards shall be withdrawn at
13、 the latest by August 2017. 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 supersedes EN ISO 663:2008. According to the
14、 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 Republic of Macedonia, France, Germany, Greece, Hu
15、ngary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 663:2017 has been approved by CEN as EN ISO 663:2017 without
16、 any modification. BS EN ISO 663:2017ISO 663:2017(E)Foreword iv1 Scope . 12 Normative reference . 13 Terms and definitions . 14 Principle 15 Reagents 16 Apparatus . 27 Sampling 28 Preparation of test sample . 29 Procedure. 29.1 Test portion 29.2 Determination . 310 Expression of results 411 Precisio
17、n . 411.1 Interlaboratory tests 411.2 Repeatability . 411.3 Reproducibility . 412 Test report . 4Annex A (informative) Results of interlaboratory tests 5Bibliography 6 ISO 2017 All rights reserved iiiContents PageBS EN ISO 663:2017ISO 663:2017(E)ForewordISO (the International Organization for Standa
18、rdization) is a worldwide federation of national 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 t
19、o 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 International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures use
20、d to develop this document and those intended for 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 o
21、f the ISO/IEC Directives, Part 2 (see www .iso .org/ 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 identif
22、ied during the development of the document will be in 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
23、on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www .iso .org/ iso/ foreword .htmlThis document was prep
24、ared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 11, Animal and vegetable fats and oils.This fifth edition cancels and replaces the fourth edition (ISO 663:2007), of which it constitutes a minor revision to exclude fat coming from milk and milk products.iv ISO 2017 All rights re
25、servedBS EN ISO 663:2017INTERNATIONAL STANDARD ISO 663:2017(E)Animal and vegetable fats and oils Determination of insoluble impurities content1 ScopeThis document specifies a method for the determination of the insoluble impurities content of animal and vegetable fats and oils.If it is not desired t
26、o include soaps (particularly calcium soaps) or oxidized fatty acids in the insoluble impurities content, it is necessary to use a different solvent and procedure. In this case, an agreement is to be reached between the parties concerned.Milk and milk products (or fat coming from milk and milk produ
27、cts) are excluded from the scope of this document.2 Normative referenceThe following documents are referred to in the text in such a way that some or all of their content constitutes requirements of this document. For dated references, only the edition cited applies. For undated references, the late
28、st edition of the referenced document (including any amendments) applies.ISO 661, Animal and vegetable fats and oils Preparation of test sample3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.ISO and IEC maintain terminological databases for use in
29、standardization at the following addresses: IEC Electropedia: available at h t t p :/ www .electropedia .org/ ISO Online browsing platform: available at h t t p :/ www .iso .org/ obp3.1insoluble impurities contentquantity of dirt and other foreign matter insoluble in n-hexane or light petroleum unde
30、r the conditions specified in this documentNote 1 to entry: The content is expressed as a percentage by mass.Note 2 to entry: These impurities include mechanical impurities, mineral substances, carbohydrates, nitrogenous substances, various resins, calcium soaps, oxidized fatty acids, fatty acid lac
31、tones, and (in part) alkali soaps, hydroxy-fatty acids and their glycerides.4 PrincipleA test portion is treated with an excess of n-hexane or light petroleum, then the solution obtained is filtered. The filter and residue are washed with the same solvent, then dried at 103 C and weighed.5 ReagentsW
32、ARNING Attention is drawn to the regulations which specify the handling of dangerous substances. Technical, organizational and personal safety measures shall be followed. ISO 2017 All rights reserved 1BS EN ISO 663:2017ISO 663:2017(E)Use only reagents of recognized analytical grade.5.1 n-Hexane, or
33、in the absence of this, light petroleum, having a distillation range between 30 C and 60 C and having a bromine value of less than 1.For either solvent, the residue on complete evaporation shall not exceed 0,002 g per 100 ml.5.2 Kieselgur, purified, calcinated, with loss in mass at 900 C (red heat)
34、of less than 0,2 % by mass.6 ApparatusUsual laboratory apparatus and, in particular, the following.6.1 Analytical balance, with an accuracy of 0,001 g.6.2 Electric drying oven, capable of operating at 103 C 2 C.6.3 Conical flask, of 250 ml capacity, with ground glass stopper.6.4 Desiccator, containi
35、ng an efficient desiccant.6.5 Ashless filter paper (maximum ash content 0,01 %, by mass), retention value of 98 %, by mass, for particles of size greater than 2,5 m1), or an equivalent glass-fibre filter, of diameter 120 mm, together with a metal (preferably aluminium) or glass vessel with a well-fi
36、tting lid.These are alternatives to the filter (6.6) for all products except acid oils.6.6 Filter crucible, glass, of grade P16 (pore size 10 m to 16 m), diameter 40 mm, of capacity 50 ml, together with a suction bottle.This is an alternative to 6.5 for all products including acid oils.7 SamplingA r
37、epresentative 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 document. A recommended sampling method is given in ISO 5555.8 Preparation of test samplePrepare the test sample i
38、n accordance with ISO 661.9 Procedure9.1 Test portionWeigh, to the nearest 0,01 g, approximately 20 g of the test sample (Clause 8) into a conical flask (6.3).1) Whatman 42 (2,5 m) filter paper or Whatman GF/D glass-fibre filter are examples of suitable products available commercially. This informat
39、ion is given for the convenience of users of this document and does not constitute an endorsement by ISO of these products.2 ISO 2017 All rights reservedBS EN ISO 663:2017ISO 663:2017(E)9.2 Determination9.2.1 Dry the filter paper and the vessel (6.5) with its lid, or the filter crucible (6.6), in th
40、e oven (6.2) set at 103 C. Allow to cool in the desiccator (6.4) then weigh to the nearest 0,001 g. For acid oils, prepare the crucible as described in 9.2.7 and continue as in 9.2.2.9.2.2 Add 200 ml of n-hexane or light petroleum (5.1) to the flask containing the test portion (9.1). Stopper the fla
41、sk and shake.For castor oil, the quantity of solvent may be increased to facilitate the operation and this may necessitate the use of a larger flask.Leave to stand at about 20 C for about 30 min.9.2.3 Filter through the filter paper in a suitable funnel or through the filter crucible, using suction
42、if necessary. Rinse the flask to ensure that all impurities are washed into the filter/crucible.Wash the filter paper or filter crucible by pouring through it small amounts of the same solvent as used in 9.2.2, but no more than is necessary for the final filtrate to be free from fat or oil. Warm the
43、 solvent, if necessary, to a maximum temperature of 60 C in order to dissolve any solidified fats retained on the filter.9.2.4 If a filter paper is used, remove it from the funnel and place it in the vessel. Allow most of the solvent remaining in the filter paper to evaporate in air and complete the
44、 evaporation in the oven set at 103 C. Then remove from the oven, close the vessel with its lid, allow to cool in the desiccator (6.4) and weigh to the nearest 0,001 g.9.2.5 If a filter crucible is used, allow most of the solvent remaining in it to evaporate in air under a fume hood and complete the
45、 evaporation in the oven set at 103 C. Then remove from the oven, allow to cool in the desiccator (6.4) and weigh to the nearest 0,001 g.9.2.6 If it is desired to determine the content of organic impurities, the use of a previously dried and weighed, ashless filter paper is necessary. In this case,
46、the filter paper containing the insoluble impurities shall be ignited and the mass of ash obtained subtracted from the mass of insoluble impurities.The organic impurities content, expressed as a percentage by mass, is then calculated by multiplying this difference in mass by 100/m0, where m0is the m
47、ass, in grams, of the test portion.9.2.7 If analysing acid oils, coat the glass filter crucible with kieselgur (5.2) as follows. In a 100 ml glass beaker, prepare a slurry consisting of 2 g of kieselgur and approximately 30 ml of light petroleum (5.1). Pour the mixture into the filter crucible under
48、 reduced pressure in order to obtain a layer of kieselgur on the glass filter.Dry the prepared glass filter crucible for 1 h in the oven (6.2) set at 103 C. Allow to cool in the desiccator (6.4) and weigh to the nearest 0,001 g.Carry out two determinations on test portions taken from the same test s
49、ample (Clause 8). ISO 2017 All rights reserved 3BS EN ISO 663:2017ISO 663:2017(E)10 Expression of resultsThe insoluble impurities content, w, expressed as a percentage by mass, is equal towmmm=210100%wherem0is the mass of the test portion (9.1), in grams;m1is the mass of the vessel with its lid and filter paper, or of the filter crucible (see 9.2.1), in grams;m2is the mass of the vessel with its lid and filter paper containing the dry residue (see 9.2.4), or of the filter crucible and dry residue (see 9.2.5), in grams.Repo