BS 684-0 1-1996 Methods of analysis of fats and fatty oils - General introduction - General procedures and list of determinations in BS 684《脂肪和脂肪油分析方法 一般说明 通用程序和BS 684标准中的检测表》.pdf

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1、BRITISH STANDARD BS 684-0.1: 1995 Methods of analysis of Fats and fatty oils Part 0: General introduction Section 0.1 General procedures and list of determinations in BS684 UDC 665.1.014:543BS684-0.1:1995 This British Standard, having been prepared under the directionof the Consumer Products and Ser

2、vices Sector Board, was published under theauthority of the Standards Board and comes into effect on 15February 1996 BSI 07-1999 First published as BS 684-0 October 1976 Second edition November 1982 Third edition January 1990 First published as BS 684-0.1 February 1996 The following BSI references r

3、elate to the work on this standard: Committee reference AW/11 Draft announced in BSI News November 1995 ISBN 0 580 25395 3 Committees responsible for this British Standard The preparation of this British Standard was entrusted to Technical Committee AW/11, Animal and vegetable fats and oils, upon wh

4、ich the following bodies were represented: Association of Public Analysts Department of Trade and Industry (Laboratory of the Government Chemist) Feed Fat Association FOSFA International Institute of Biology International Federation of Inspection Agencies Lard Association Leatherhead Food Research A

5、ssociation Margarine and Shortening Manufacturers Association Ministry of Agriculture, Fisheries and Food National Edible Oil Distributors Association Natural Resources Institute Royal Society of Chemistry Seed Crushers and Oil Processors Association Soap and Detergent Industry Association Society o

6、f Chemical Industry Tropical Growers Association United Kingdom Renderers Association Ltd. Amendments issued since publication Amd. No. Date CommentsBS684-0.1:1995 BSI 07-1999 i Contents Page Committees responsible Inside front cover Foreword ii 1 Scope 1 2 References 1 3 Determinations in BS684 1 4

7、 Determinations supplementary to those in BS684 2 5 Laboratory sample 2 6 Preparation of test sample 3 7 Reagents 3 8 Apparatus 3 9 Test report 3 Annex A (informative) Alphabetical index of determinations and associated methods contained in BS684 4 Table 1 Determinations supplementary to those in BS

8、684 2 List of references Inside back coverBS684-0.1:1995 ii BSI 07-1999 Foreword This Section of BS684 has been prepared by Technical Committee AW/11. It supersedes BS684-0:1989, which is withdrawn. Appendix B of BS684-0:1989 has been published separately as BSENISO661:1995. BS684, which was first p

9、ublished in 1936, was revised in 1950 and 1958. In 1976 the standard was divided into a series of Parts and Sections, published separately to facilitate revision and the inclusion of methods of analysis published by the International Organization for Standardization (ISO), some of which have now bee

10、n implemented as European standards by the European Committee for Standardization (CEN). It is essential that this Section be read in conjunction with the individual Sections of Parts 1 and 2. A British Standard does not purport to include all the necessary provisions of a contract. Users of British

11、 Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, pages1to 6, an inside back cover and a back cover. Th

12、is standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.BS684-0.1:1995 BSI 07-1999 1 1 Scope This Section of BS684 gives general procedures relating to the methods of analysis for fats given i

13、n other Sections of BS684. These other Sections are listed in clause 3. Unless stated otherwise in the particular Section, the methods are applicable to most fats. The term “fat” denotes both fats and fatty oils (the phrase used traditionally in BS684) and animal and vegetable fats and oils (the ter

14、m introduced through the International Organization for Standardization). Relevant methods given in other British Standards are listed in clause 4. The guidance and requirements given in clauses5 to9 apply to all Sections of Parts 1 and 2 of BS684, except when otherwise stated in the individual Sect

15、ions. Annex A is an alphabetical index to the determinations given in Parts 1 and 2 of BS684. 2 References 2.1 Normative references This Section of BS684 incorporates, by dated or undated reference, provisions from other publications. These normative references are made at the appropriate places in

16、the text and the cited publications are listed on the inside back cover. For dated references, only the edition cited applies; any subsequent amendments to or revisions of the cited publication apply to this Section of BS684 only when incorporated in the reference by amendment or revision. For undat

17、ed references, the latest edition of the cited publication applies, together with any amendments. 2.2 Informative references This Section of BS684 refers to other publications that provide information or guidance. Editions of these publications current at the time of issue of this standard are liste

18、d on the inside back cover, but reference should be made to the latest editions. 3 Determinations in BS684 The following list shows the number and title of each Section of BS684. Annex A gives an alphabetical index to these Sections. The numbering of the Sections is not intended to indicate the orde

19、r of publication nor does it have any technical significance. Not all the listed Sections have been published and others may be added. Part 0 General introduction Part 1 Physical methods Part 2 Other methods Section Title 0.1 General procedures and list of determinations in BS684 0.2 Preparation of

20、test sample (BSENISO661) Section Title 1.1 Determination of litre weight in air 1.2 Determination of refractive index 1.3 Determination of melting point (slip point) 1.4 Determination of flow and drop points 1.5 Determination of cloud point 1.6 a Determination of titre 1.7 Determination of surface-d

21、rying time 1.8 Determination of smoke point 1.9 Determination of water-insoluble solvents 1.10 Determination of moisture and other volatile matter 1.11 Determination of penetration value 1.12 Determination of dilatation 1.13 Determination of cooling curve 1.14 Determination of colour 1.15 Determinat

22、ion of ultraviolet absorbance 1.16 Determination of water content: entrainment method a The method for the preparation of fatty acids described in Section 1.6 may be used when the method of analysis requires the use of fatty acids derived from the sample. Section Title 2.1 Determination of water by

23、the Karl Fischer method 2.2 Determination of ash 2.3 Determination of insoluble impurities content (BS EN ISO 663) 2.4 Calculation of total fatty matter 2.5 Determination of alkalinity 2.6 Determination of saponification value 2.7 Determination of unsaponifiable matter 2.8 Determination of total neu

24、tral oil 2.9 Determination of the hydroxyl value and the acetyl value 2.10 Determination of acidityBS684-0.1:1995 2 BSI 07-1999 4 Determinations supplementary to those in BS684 Methods of determination supplementary to those in BS684 are listed in Table 1 for reference. Although suitable for fats, t

25、hese methods have been standardized for other or wider purposes. Table 1 Determinations supplementary to those in BS684 5 Laboratory sample 5.1 General If the sample cannot be taken in accordance with5.2 or 5.3, the method of sampling agreed between the parties concerned shall be stated in the infor

26、mation accompanying the sample and in the test report. 5.2 Non-emulsified fats The sample shall be taken in accordance with BSENISO5555. 5.3 Emulsified fats The sample shall be taken in accordance with BS809. Section Title 2.11 Determination of volatile acids (Reichert, Polenske and Kirschner values

27、) 2.12 Determination of oxidized fatty acids 2.13 Determination of iodine value 2.14 Determination of peroxide value 2.15 Calculation of total saponifiable matter 2.16 Determination of copper colorimetric method 2.17 Determination of iron colorimetric method 2.18 Determination of copper, iron and ni

28、ckel content graphite furnace atomic absorption method 2.19 a Determination of phosphorus 2.20 Determination of carotene in vegetable oils 2.21 Determination of lead content graphite furnace atomic absorption method 2.22 Determination of solid fat content (pulsed NMR method) (BS EN ISO 8292) 2.23 b

29、Determination of Bmer value 2.24 Determination of anisidine value 2.25 c Determination of oxidative stability value 2.26 Determination of polyethylene-type plastics 2.27 Determination of bleachability 2.28 2.29 Cottonseed oil test (Halphen) 2.30 d Sesame oil test (Baudouin) 2.31 d Arachis oil test (

30、Evers) 2.32 Determination of rancidity index 2.33 Detection and identification of antioxidants 2.34 Preparation of methyl esters of fatty acids 2.35 Analysis by gas chromatography of methyl esters of fatty acids (BS EN ISO 5508) 2.36 Determination of butylhydroxyanisole (BHA) and butylhydroxytoluene

31、 (BHT) 2.37 Determination of residual technical hexane content 2.38 Determination of the proportions of individual sterols in the sterol fraction Section Title 2.39 Determination of the composition of fatty acids in the 2-position 2.40 a Determination of tocopherols and tocotrienols 2.41 e Determina

32、tion of erucic acid 2.42 Determination of 1-monoglycerides and free glycerol contents 2.43 Determination of polyunsaturated fatty acids with a cis, cis 1,4-diene structure 2.44 Determination of gallates 2.45 Determination of polar compounds content (BSENISO8420) a In preparation. b The 1989 edition

33、has been withdrawn and is not being replaced. c The 1979 edition has been withdrawn and a revision is in preparation. d The 1978 edition has been withdrawn and is not being replaced. e The 1987 edition has been withdrawn and is not being replaced. Determination Relevant British Standard Determinatio

34、n of viscosity Determination of pour point Determination of PAT value Determination of flash point BS 188 BS 2000-15 BS 6900 BS EN 22719BS684-0.1:1995 BSI 07-1999 3 6 Preparation of test sample 6.1 Non-emulsified fats The sample shall be prepared in accordance with BSENISO661. 6.2 Emulsified fats Th

35、e method of preparation agreed between the parties concerned shall be fully documented. The method used shall ensure thorough mixing and shall be stated in the test report. 7 Reagents Reagents of recognized analytical quality shall be used and, unless otherwise stated, water conforming to the approp

36、riate grade of BSENISO3696 shall be used. Specific details are given in each Section of BS684-1andBS684-2. WARNING. Many reagents are hazardous. Warnings are given in the individual Sections about particularly hazardous reagents. Statutory and general precautions need to be followed at all times and

37、 protective measures such as the use of fume cupboards, gloves and goggles should be taken. 8 Apparatus The items of apparatus described in the individual Sections are items that are not commonly available in a laboratory, or which have features critical to a particular method of test. Further items

38、 of ordinary laboratory apparatus should be used as appropriate. 9 Test report The test report shall show the method used and the result obtained. It shall also mention any operating conditions not specified, or regarded as optional, as well as any circumstances that may have influenced the result.

39、If only a single determination was carried out, this shall be indicated. The report shall include all details required for complete identification of the sample and shall state any variations from the specified methods of sampling or preparation of the sample.BS684-0.1:1995 4 BSI 07-1999 Annex A (in

40、formative) Alphabetical index of determinations and associated methods contained in BS684 Section accelerated oxidation test acetyl value acid(s) (see also fatty acids): erucic value volatile (Reichert, Polenske and Kirschner values) 2.25 2.9 2.41 2.10 2.11 acidity alkalinity anisidine value antioxi

41、dants: detection and identification BHA or BHT gallates apparent density ash 2.10 2.5 2.24 2.33 2.36 2.44 1.1 2.2 bleachability Bmer value butylhydroxyanisole (BHA) butylhydroxytoluene (BHT) 2.27 2.23 2.36 2.36 carotene content cloud point colour cooling curve copper content: graphite furnace atomic

42、 absorption method colorimetric method cottonseed oil test (Halphen) 2.20 1.5 1.14 1.13 2.18 2.16 2.29 density dilatation drop point drying time, surface 1.1 1.12 1.4 1.7 erucic acid fatty acids: cis, cis 1,4-dienepolyunsaturated free individual, identification and determination of by gas-liquid chr

43、omatography in 2-position oxidized preparation of methyl esters of fatty matter, total, calculation of flash point: seeTable 1 flow point 2.41 2.43 2.10 2.35 2.39 2.12 2.34 2.4 1.4 Section gallates glycerol 2.44 2.42 Halphen test for cottonseed oil hydroxyl value 2.29 2.9 insoluble impurities iodine

44、 value iron content: graphite furnace atomic absorption method colorimetric method 2.3 2.13 2.18 2.17 Karl Fischer determination of water Kirschner value Kreis test for rancidity 2.1 2.11 2.32 lead (graphite furnace atomic absorption method) litre weight in air 2.21 1.1 melting point methyl esters o

45、f fatty acids, preparation of moisture and other volatile matter monoglycerides 1.3 2.34 1.10 2.42 neutral oils, total nickel content (graphite furnace atomic absorption method) oxidation test, accelerated oxidative stability: see oxidation test, accelerated oxidized fatty acids 2.8 2.18 2.25 2.12 P

46、AT value: seeTable 1 penetration value peroxide value phosphorus plastics, polyethylene-type Polenske value pour point: seeTable 1 polar compounds 1.11 2.14 2.19 2.26 2.11 2.45 rancidity index refractive index Reichert value residual hexane 2.32 1.2 2.11 2.37BS684-0.1:1995 BSI 07-1999 5 Section sapo

47、nifiable matter, total of saponification value slip point soap dissolved in fats solid fat content pulsed NMR method solvent(s): residual water-insoluble smoke point stability, oxidative sterols, individual surface-drying time 2.15 2.6 1.3 2.5 2.22 2.37 1.9 1.8 2.25 2.38 1.7 titre tocopherols tocotr

48、ienols total fatty matter, calculation of total neutral oils 1.6 2.40 2.40 2.4 2.8 unsaponifiable matter ultraviolet 2.7 1.15 viscosity: seeTable 1 volatile: acids (Reichert, Polenske and Kirschner values) matter 2.11 1.10 water: azeotropic distillation Karl Fischer water-insoluble solvents 1.16 2.1

49、 1.96 blankBS684-0.1:1995 BSI 07-1999 List of references (seeclause2) Normative references BSI publications BRITISH STANDARDS INSTITUTION, London BS 809:1985, Methods for sampling of milk and milk products. BS EN ISO 661:1995, Animal and vegetable fats and oils Preparation of test sample. BS EN ISO 3696:1995, Specification for water for laboratory use. BS EN ISO 5555:1995, Animal and vegetable fats and oils Sampling. Informative references BSI publications BRITISH STANDARDS INSTITUTION, London BS 188:1977, Methods for determination of the visco