1、BS EN ISO663:2008ICS 67.200.10NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDAnimal and vegetablefats and oils Determination ofinsoluble impuritiescontent (ISO 663:2007)Copyright European Committee for Standardization Provided by IHS under license with CENNot f
2、or ResaleNo reproduction or networking permitted without license from IHS-,-,-This British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on 31 December2008 BSI 2008ISBN 978 0 580 58524 1Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 663:2
3、008National forewordThis British Standard is the UK implementation of EN ISO 663:2008. Itis identical to ISO 663:2007. It supersedes BS EN ISO 663:2001 which iswithdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee AW/307, Oil seeds, animal and vegetable fats and oils
4、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 responsible for its correct application.Compliance with a British Standard cannot co
5、nfer immunityfrom legal obligations.Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 663November 2008ICS 67.200.10 Supersedes
6、 EN ISO 663:2001 English VersionAnimal and vegetable fats and oils - Determination of insolubleimpurities content (ISO 663:2007)Corps gras dorigines animale et vgtale - Dterminationde la teneur en impurets insolubles (ISO 663:2007)Tierische und pflanzliche Fette und le - Bestimmung desAnteils an unl
7、slichen Verunreinigungen (ISO 663:2007)This European Standard was approved by CEN on 23 October 2008.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-
8、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 Standard exists in three official versions (English, French, German). A version in any other language made by translationunder
9、 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 standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hung
10、ary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: ru
11、e de Stassart, 36 B-1050 Brussels 2008 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 663:2008: ECopyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking
12、permitted without license from IHS-,-,-BS EN ISO 663:2008EN ISO 663:2008 (E) 3 Foreword The text of ISO 663:2007 has been prepared by Technical Committee ISO/TC 34 “Agricultural food products” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 663:2008 by T
13、echnical 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 publication of an identical text or by e
14、ndorsement, at the latest by May 2009, and conflicting national standards shall be withdrawn at the latest by May 2009. 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 identifyi
15、ng any or all such patent rights. This document supersedes EN ISO 663:2001. 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, Cyprus, Czech Republic, Denmark, E
16、stonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 663:2007 has been approved by CE
17、N as a EN ISO 663:2008 without any modification. Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 663:2008INTERNATIONAL STANDARD ISO 663:2007(E) ISO 2007 All rights rese
18、rved 1Animal and vegetable fats and oils Determination of insoluble impurities content 1 Scope This International Standard specifies a method for the determination of the insoluble impurities content of animal and vegetable fats and oils. If it is not desired to include soaps (particularly calcium s
19、oaps) 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. 2 Normative reference The following referenced documents are indispensable for the application of th
20、is document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 661, Animal and vegetable fats and oils Preparation of test sample 3 Terms and definitions For the purposes of this documen
21、t, the following terms and definitions apply. 3.1 insoluble impurities content quantity of dirt and other foreign matter insoluble in n-hexane or light petroleum under the conditions specified in this International Standard NOTE 1 The content is expressed as a percentage by mass. NOTE 2 These impuri
22、ties include mechanical impurities, mineral substances, carbohydrates, nitrogenous substances, various resins, calcium soaps, oxidized fatty acids, fatty acid lactones, and (in part) alkali soaps, hydroxy-fatty acids and their glycerides. 4 Principle A test portion is treated with an excess of n-hex
23、ane 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 Reagents WARNING Attention is drawn to the regulations which specify the handling of dangerous substances. Technical, organizational and persona
24、l safety measures shall be followed. Use only reagents of recognized analytical grade. Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 663:2008ISO 663:2007(E) 2 ISO 200
25、7 All rights reserved5.1 n-Hexane, or 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
26、, with loss in mass at 900 C (red heat) of less than 0,2 % by mass. 6 Apparatus Usual 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
27、ground glass stopper. 6.4 Desiccator, containing 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 (prefe
28、rably aluminium) or glass vessel with a well-fitting 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
29、for all products including acid oils. 7 Sampling A 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 sampling method is give
30、n in ISO 5555. 8 Preparation of test sample Prepare the test sample in accordance with ISO 661. 9 Procedure 9.1 Test portion Weigh, 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
31、 are examples of suitable 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. Copyright European Committee for Standardization Provided by IHS under license with CENNot
32、 for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 663:2008ISO 663:2007(E) ISO 2007 All rights reserved 39.2 Determination 9.2.1 Dry the filter paper and the vessel (6.5) with its lid, or the filter crucible (6.6), in the oven (6.2) set at 103 C. Allow to cool
33、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 flask and shake. For castor oil, the quanti
34、ty 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 if necessary. Rinse the flask to en
35、sure 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 solvent, if necessary, to a maxim
36、um 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 evaporation in the oven set at
37、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 evaporation in the oven set a
38、t 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, the filter paper containing t
39、he 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 mass, in grams, of the test p
40、ortion. 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 reduced pressure in order
41、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 sample (Clause 8). Copyrig
42、ht European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 663:2008ISO 663:2007(E) 4 ISO 2007 All rights reserved10 Expression of results The insoluble impurities content, w, expressed a
43、s a percentage by mass, is equal to 210100 %mmwm-= where m0 is 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 residu
44、e (see 9.2.4), or of the filter crucible and dry residue (see 9.2.5), in grams. Report the result to the second decimal place. 11 Precision 11.1 Interlaboratory tests Details of interlaboratory tests on the precision of the method are summarized in Annex A. The values derived from these interlaborat
45、ory tests may not be applicable to concentration ranges and matrices other than those given. 11.2 Repeatability The absolute difference between two independent single test results, obtained using the same method on identical test material in the same laboratory by the same operator using the same eq
46、uipment within a short interval of time, will in not more than 5 % of the cases exceed the value of the repeatability limit, r, given in Table A.1. 11.3 Reproducibility The absolute difference between two single test results, obtained using the same method on identical test material in different lab
47、oratories with different operators using different equipment, will in not more than 5 % of cases exceed the value of the reproducibility limit, R, given in Table A.1. 12 Test report The test report shall specify: a) all information necessary for the complete identification of the sample; b) the samp
48、ling method used, if known; c) the test method used, with reference to this International Standard; d) the solvent used; e) any operating details not specified in this International Standard, or regarded as optional, together with details of any incidents which may have influenced the test results;
49、f) the test result obtained or, if the repeatability has been checked, the final result obtained. Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 663:2008ISO 663:2007(E)
