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1、BRITISH STANDARD BS EN ISO 6321:2002 BS 684-1.3: 2002 Incorporating Corrigendum No. 1 Animal and vegetable fats and oils Determination of melting point in open capillary tubes (slip point) The European Standard EN ISO 6321:2002 has the status of a British Standard ICS 67.200.10 NO COPYING WITHOUT BS
2、I PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:26:24 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 6321:2002 This British Standard, having been prepared under the direction of the Consumer Products and Services Sector Policy and Str
3、ategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 15 April 2002 BSI 10 May 2002 ISBN 0 580 39420 4 National foreword This British Standard is the official English language version of EN ISO 6321:2002. It is identical with ISO 6321:2002. It supersede
4、s BS 684-1.3:1991 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee AW/11, Animal and vegetable fats and oils, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-refe
5、rences The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Cata
6、logue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the te
7、xt; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front co
8、ver, an inside front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii and iii, a blank page, pages 1 to 11, the Annex ZA page, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Ame
9、ndments issued since publication Amd. No. DateComments 13911 Corrigendum No. 1 10 May 2002Correction to the EN ISO foreword page and the EN ISO shoulder heads Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:26:24 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE
10、EUROPISCHE NORM EN ISO 6321 February 2002 ICS 67.200.10 English version Animal and vegetable fats and oils - Determination of melting point in open capillary tubes (slip point) (ISO 6321:2002) Corps gras dorigines animale et vgtale - Dtermination du point de fusion en tube capillaire ouvert (ISO 632
11、1:2002) Tierische und pflanzliche Fette und le - Bestimmung des Schmelzpunktes in offenen Kapillarrhrchen (ISO 6321:2002) This European Standard was approved by CEN on 14 December 2001. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for givin
12、g this European Standard the status 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 Management Centre or to any CEN member. This European Standard exists in three official versions
13、 (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech
14、Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue d
15、e Stassart, 36 B-1050 Brussels 2002 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 6321:2002 E Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:26:24 GMT+00:00 2006, Uncontrolled Copy, (c) BSI I NESO 36:1202( 20E) 2 CO
16、RRECTED 2002-04-17 Foreword This document (ISO 6321:2002) has been prepared by Technical Committee ISO/TC 34 “Agricultural food 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
17、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 2002, and conflicting national standards shall be withdrawn at the latest by August 2002. According to
18、 the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal
19、, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the International Standard ISO 6321:2002 has been approved by CEN as a European Standard without any modifications. NOTE Normative references to International Standards are listed in annex ZA (normative). EN ISO 6321
20、:2002 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:26:24 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTERNATIONAL STANDARD ISO 6321 Second edition 2002-02-15 Reference number ISO 6321:2002(E) Animal and vegetable fats and oils Determination of melting point in open capillary tubes (slip
21、 point) Corps gras dorigines animale et vgtale Dtermination du point de fusion en tube capillaire ouvert Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:26:24 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii EN ISO 6321:2002 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:26:24 GMT+
22、00:00 2006, Uncontrolled Copy, (c) BSI iii Foreword ISO (the International Organization for Standardization) 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
23、 body interested in a subject for which a technical committee has been established has the right to 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 Elect
24、rotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting.
25、 Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any
26、or all such patent rights. International Standard ISO 6321 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 11, Animal and vegetable fats and oils. This second edition cancels and replaces the first edition (ISO 6321:1991), of which it constitutes a minor revision to inc
27、orporate Amendment 1:1998. Annex A forms a normative part of this International Standard. Annex B is for information only. EN ISO 6321:2002 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:26:24 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 6321:2002 Licensed Copy: sheffieldun sheffield
28、un, na, Sun Nov 19 15:26:24 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ANRETNIITOTS LANDNADRAISO 2362002:1)E( ISO 2002 r llAithgs reservde 1 Animal and vegetable fats and oils Determination of melting point in open capillary tubes (slip point) 1Scope This International Standard specifies two methods
29、 for the determination of the melting point in open capillary tubes, commonly known as the slip point, of animal and vegetable fats and oils (referred to as fats hereinafter). Method A is only applicable to animal and vegetable fats which are solid at ambient temperature and which do not exhibit pro
30、nounced polymorphism. Method B is applicable to all animal and vegetable fats which are solid at ambient temperature, and is the method to be used for fats whose polymorphic behaviour is unknown. A method for the determination of the melting point of palm oil samples is given in annex A. NOTE 1If ap
31、plied to fats with pronounced polymorphism, method A will give different and less satisfactory results than method B. NOTE 2Fats which exhibit pronounced polymorphism are principally cocoa butter and fats containing appreciable quantities of 2-unsaturated, 1,3-saturated triacylglycerols. 2Normative
32、reference The following normative document contains provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, this publication do not apply. However, parties to agreements based on this Int
33、ernational Standard are encouraged to investigate the possibility of applying the most recent edition of the normative document indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid Inte
34、rnational Standards. ISO 661, Animal and vegetable fats and oils Preparation of test sample 3Term and definition For the purposes of this International Standard, the following term and definition apply. 3.1 melting point (in open capillary tubes) slip point temperature at which a column of fat in an
35、 open capillary tube commences to rise under the conditions specified in this International Standard 4Principle A capillary tube containing a column of the fat which has been crystallized under controlled conditions is immersed to a specified depth in water, the temperature of which is increased at
36、a specified rate. The temperature at which the column is observed to start rising in the capillary tube is recorded. 2002:1236 OSI NE 11 EN ISO 6321:2002 1 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:26:24 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 6321:2002(E) 2 ISO 2002 Ar llithg
37、r seresvde 5Apparatus Usual laboratory apparatus and, in particular, the following. 5.1Capillary tubes, having uniform walls and which are open at both ends, of internal diameter to , external diameter to , wall thickness to and length to . Check the internal and external diameters of the capillary
38、tubes using a test gauge such as that shown in Figure 1. Before use, clean the tubes thoroughly by washing them successively with a mixture of chromic acid, water and acetone, and then dry them in an oven. It is recommended that new tubes be used. 5.2Thermometer, graduated in divisions of , calibrat
39、ed over the range of melting points expected. 5.3Stirrer, electrical. 5.4Cooling bath, filled with brine or other non-freezing liquid, thermostatically maintained at a temperature of to , or filled with a mixture of flaked ice and salt (in the proportions 2 to 1 by mass) at a temperature of to . Dim
40、ensions in millimetres Figure 1 Test gauge for capillary tubes 1,0 mm1,2 mm 1,3 mm1,6 mm0,15 mm0,20 mm50 mm60 mm 0,1 C 10 C 12 C 10 C 12 C 2002:1236 OSI NE 22 EN ISO 6321:2002 2 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:26:24 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 6321:2002(E
41、) ISO 2002 r llAithgs reservde 3 5.5Heating apparatus, consisting of the following elements: a)water jacket, made of glass, provided with inlet and outlet tubes, and having the shape and dimensions shown in Figure 2; b)water heater, capable of delivering a slow stream of water, the temperature of wh
42、ich can be controlled to increase at a rate of between and , through the water jacket a). An example of a suitable heating apparatus is shown in Figure 3. Other types of heating apparatus, such as a water bath with magnetic stirrer, capable of being controlled to produce the specified temperature ri
43、se, may also be used. Dimensions in millimetres Key 1Rubber band Figure 2 Water jacket 0,5 C/min 4 C/min 2002:1236 OSI NE 33 EN ISO 6321:2002 3 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:26:24 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 6321:2002(E) 4 ISO 2002 Ar llithgr seresvde 6
44、Sampling It is important the laboratory receive a sample which is truly representative and has not 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 given in ISO 5555 1. 7Preparation of t
45、est sample Prepare the test sample in accordance with ISO 661. Key 1Heating element (coil ) 2To drain Figure 3 Example of heating apparatus (heating by natural convection) 220 W 2002:1236 OSI NE 44 EN ISO 6321:2002 4 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:26:24 GMT+00:00 2006, Unc
46、ontrolled Copy, (c) BSI ISO 6321:2002(E) ISO 2002 r llAithgs reservde 5 8Procedure 8.1Preparation of the capillary tubes for method A Melt a portion of the test sample as rapidly as possible to at least , but not more than , above the temperature at which it is completely melted. Dip two capillary t
47、ubes (5.1) into the melted test sample until columns of fat long are obtained. Immediately after filling the tubes, wipe them quickly with absorbent tissue to remove any fat adhering to the outer surfaces of the tubes. Immediately place the filled capillary tubes for a few seconds against a beaker f
48、illed with ice so that the fat solidifies. Place the tubes in the cooling bath (5.4) for . Continue in accordance with 8.3. 8.2Preparation of the capillary tubes for method B Melt a portion of the test sample as rapidly as possible to at least , but not more than , above the temperature at which it
49、is completely melted. Cool the melted test sample, with occasional stirring, until its temperature is to and then stir continuously with the stirrer (5.3), allowing the fat to cool until the first signs of cloudiness appear. Continue stirring by hand until the fat has a pasty consistency and then transfer the fat to a beaker at . Store the fat at this temperature for a minimum of . Push four capillary tubes (5.1) into the conditioned fat until a column of fat long is obtained in each tube. Wipe the tubes quickly with