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1、BS EN ISO 663:2008 ICS 67.200.10 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BRITISH STANDARD Animal and vegetable fats and oils Determination of insoluble impurities content (ISO 663:2007) Licensed Copy: London South Bank University, South Bank University, 31/01/2009 03:2
2、4, Uncontrolled Copy, (c) BSI This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 December 2008 BSI 2008 ISBN 978 0 580 58524 1 Amendments/corrigenda issued since publication DateComments BS EN ISO 663:2008 National foreword This British Stand
3、ard is the UK implementation of EN ISO 663:2008. It is identical to ISO 663:2007. It supersedes BS EN ISO 663:2001 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee AW/307, Oil seeds, animal and vegetable fats and oils and their by products. A list of o
4、rganizations represented on this committee can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obl
5、igations. Licensed Copy: London South Bank University, South Bank University, 31/01/2009 03:24, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 663 November 2008 ICS 67.200.10Supersedes EN ISO 663:2001 English Version Animal and vegetable fats and oils - Determina
6、tion of insoluble impurities content (ISO 663:2007) Corps gras dorigines animale et vgtale - Dtermination de la teneur en impurets insolubles (ISO 663:2007) Tierische und pflanzliche Fette und le - Bestimmung des Anteils an unlslichen Verunreinigungen (ISO 663:2007) This European Standard was approv
7、ed 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 European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
8、standards 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 translation under the responsibility of a CEN member into its own language and notif
9、ied to the CEN Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Mal
10、ta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2008 CENAll rights of exp
11、loitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 663:2008: E Licensed Copy: London South Bank University, South Bank University, 31/01/2009 03:24, Uncontrolled Copy, (c) BSI BS EN ISO 663:2008 EN ISO 663:2008 (E) 3 Foreword The text of ISO 663:2007
12、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 Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fats and oils and their by-products - Methods of sa
13、mpling 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 May 2009, and conflicting national standards shall be withdrawn at the latest by May
14、 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 identifying any or all such patent rights. This document supersedes EN ISO 663:2001. According to the CEN/CENELEC Internal
15、 Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
16、 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 CEN as a EN ISO 663:2008 without any modification. Licensed Copy: London South Bank University, South Bank Universi
17、ty, 31/01/2009 03:24, Uncontrolled Copy, (c) BSI BS EN ISO 663:2008BS EN ISO 663:2008 INTERNATIONAL STANDARD ISO 663:2007(E) ISO 2007 All rights reserved 1 Animal and vegetable fats and oils Determination of insoluble impurities content 1 Scope This International Standard specifies a method for the
18、determination of the insoluble impurities content of animal and vegetable fats and oils. If it is not desired to 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 agreemen
19、t is to be reached between the parties concerned. 2 Normative reference The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including an
20、y amendments) applies. ISO 661, Animal and vegetable fats and oils Preparation of test sample 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 insoluble impurities content quantity of dirt and other foreign matter insoluble in n-hexane or ligh
21、t petroleum under the conditions specified in this International Standard NOTE 1 The content is expressed as a percentage by mass. NOTE 2 These impurities include mechanical impurities, mineral substances, carbohydrates, nitrogenous substances, various resins, calcium soaps, oxidized fatty acids, fa
22、tty 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-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 weigh
23、ed. 5 Reagents WARNING Attention is drawn to the regulations which specify the handling of dangerous substances. Technical, organizational and personal safety measures shall be followed. Use only reagents of recognized analytical grade. Licensed Copy: London South Bank University, South Bank Univers
24、ity, 31/01/2009 03:24, Uncontrolled Copy, (c) BSI BS EN ISO 663:2008BS EN ISO 663:2008 ISO 663:2007(E) 2 ISO 2007 All rights reserved 5.1 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 solv
25、ent, 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) 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
26、,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, 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
27、 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-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
28、 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 Sampling A representative sample should have been sent to the laboratory. It should not have been damaged or changed during transport or storage. S
29、ampling is not part of the method specified in this International Standard. A recommended sampling method is given 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 s
30、ample (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 information is given for the convenience of users of this International Standard and does not constitute an endorsement by
31、 ISO of these products. Licensed Copy: London South Bank University, South Bank University, 31/01/2009 03:24, Uncontrolled Copy, (c) BSI BS EN ISO 663:2008BS EN ISO 663:2008 ISO 663:2007(E) ISO 2007 All rights reserved 3 9.2 Determination 9.2.1 Dry the filter paper and the vessel (6.5) with its lid,
32、 or the filter crucible (6.6), in the 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 th
33、e test portion (9.1). Stopper the flask 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 t
34、hrough the filter crucible, using suction 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 fi
35、ltrate to be free from fat or oil. Warm the 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 filte
36、r paper to evaporate in air, and complete the 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 evapo
37、rate in air under a fume hood, and complete the 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, a
38、shless filter paper is necessary. In this case, 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 th
39、is difference in mass by 100/m0, where m0 is the mass, 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.
40、1). Pour the mixture into the filter crucible under 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 deter
41、minations on test portions taken from the same test sample (Clause 8). Licensed Copy: London South Bank University, South Bank University, 31/01/2009 03:24, Uncontrolled Copy, (c) BSI BS EN ISO 663:2008BS EN ISO 663:2008 ISO 663:2007(E) 4 ISO 2007 All rights reserved 10 Expression of results The ins
42、oluble impurities content, w, expressed as a percentage by mass, is equal to 21 0 100 % mm w m - = where m0 is the mass of the test portion (9.1), in grams; m1 is the mass of the vessel with its lid and filter paper, or of the filter crucible (see 9.2.1), in grams; m2 is the mass of the vessel with
43、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. 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 A
44、nnex A. The values derived from these interlaboratory 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
45、 laboratory by the same operator using the same equipment 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
46、method on identical test material in different laboratories 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
47、complete identification of the sample; b) the sampling 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 inci
48、dents which may have influenced the test results; f) the test result obtained or, if the repeatability has been checked, the final result obtained. Licensed Copy: London South Bank University, South Bank University, 31/01/2009 03:24, Uncontrolled Copy, (c) BSI BS EN ISO 663:2008BS EN ISO 663:2008 IS
49、O 663:2007(E) ISO 2007 All rights reserved 5 Annex A (informative) Results of interlaboratory tests Interlaboratory tests on the determination of insoluble impurities in palm oil, crude palm oil and palm kernel oil were organized by the Federation of Oils, Seeds and Fats Associations (FOSFA) and carried out in accordance with ISO 5725-2. The results are shown in Table A.1. Table A.1 Results of interlaboratory tests on different oil Sample RDB palm olein RDB palm oil Crude palm kernel oil Crude palm olein Crude fish oi