BS 4325-3-1978 Methods for analysis of oilseed residues - Determination of ash insoluble in hydrochloric acid《油料种子残留物分析方法 第3部分 盐酸不溶灰分测定》.pdf

1、BRITISH STANDARD BS 4325-3: 1978 ISO 735:1977 Methods for Analysis of oilseed residues Part 3: Determination of ash insoluble in hydrochloric acid ISO title: Oilseed residues Determination of ash insoluble in hydrochloric acid UDC 633.85:665.3.002.68:543.822:543.832BS4325-3:1978 This British Standar

2、d, having been prepared under the directionof the Oil and Fats Standards Committee was published under the authority ofthe Executive Board on 29 December 1978 BSI10-1999 First published July 1968 First revision December 1978 The following BSI references relate to the work on this standard: Committee

3、 reference OFC/24 Draft for approval 78/50360 ISBN 0 580 10438 9 Cooperating organizations The Oils and Fats Standards Committee, under whose direction this British Standard was prepared, consists of representatives from the following Government department and scientific and industrial organizations

4、: Chemical Industries Association Chemical Society, Analytical Division* Department of Industry, Laboratory of the Government Chemist* Greater London Council Lard Association Margarine and Shortening Manufacturers Association* Overseas Development Administration Tropical Products Institute* Royal In

5、stitute of Public Health and Hygiene Seed Crushers and Oil Processors Association* Soap and Detergent Industry Association* United Kingdom Renderers Association Ltd. The organizations marked with an asterisk in the above list, together with the following, were directly represented on the committee e

6、ntrusted with the preparation of this British Standard: Association of Fatty Acid Distillers British Food Manufacturing Industries Research Association British Resin Manufacturers Association Co-operative Wholesale Society Ltd. Federation of Gelatine and Glue Manufacturers Limited Federation of Oils

7、, Seeds and Fats Association Ltd. Ministry of Agriculture Fisheries and Food National Linseed Oil Processors Association Oil and Colour Chemists Association Rubber Growers Association Society of Chemical Industry United Kingdom Glycerine Producers Association Amendments issued since publication Amd.

8、 No. Date of issue CommentsBS4325-3:1978 BSI 10-1999 i Contents Page Cooperating organizations Inside front cover National foreword ii 1 Scope and field of application 1 2 References 1 3 Definition 1 4 Principle 1 5 Reagents 1 6 Apparatus 1 7 Procedure 1 8 Expression of results 1 9 Test report 2 Pub

9、lications referred to Inside back coverBS4325-3:1978 ii BSI 10-1999 National foreword This Part of BS 4325 is identical with ISO735 “Oilseed residues Determination of ash insoluble in hydrochloric acid” and constitutes the first revision of BS4325-3:1968. Terminology and conventions. The text of the

10、 International Standard has been approved as suitable for publication, without deviation, as a British Standard. Some terminology and certain conventions are not identical with those used in British Standards; attention is especially drawn to the following. The comma has been used as a decimal marke

11、r. In British Standards it is current practice to use a full point on the baseline as the decimal marker. Where the words “International Standard” appear, referring to this standard, they should be interpreted as “British Standard”. Important note. Attention is drawn to Statutory Instrument1973 No15

12、21 (Agriculture. The Fertilisers and Feeding Stuffs Regulations1973) and to Statutory Instrument1976 No840 (Agriculture. The Fertilisers and Feeding Stuffs (Amendment) Regulations1976), which control the sale of oilseed residues and compound cakes or meals intended for animal feeding purposes in the

13、 United Kingdom and prescribe methods for determining specified analytical characteristics. Where differences exist between these methods and those given in this British Standard the latter may be used only for purposes which do not fall within the scope of the Statutory Instruments. A British Stand

14、ard 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. Cross-references International Standard Corresponding Br

15、itish Standard ISO 749:1977 BS 4325 Methods for the analysis of oilseed residues Part 2:1978 Determination of total ash (Technically equivalent) ISO 771:1977 BS 4325 Methods for the analysis of oilseed residues Part 1:1978 Determination of moisture and volatile matter content (Technically equivalent

16、) Summary of pages This document comprises a front cover, an inside front cover, pagesi andii, pages1 and2, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside

17、 front cover.BS4325-3:1978 BSI 10-1999 1 1 Scope and field of application This International Standard specifies a method for the determination of the ash insoluble in hydrochloric acid, from residues (excluding compounded products) obtained by the extraction of oil from oilseeds by pressure or solve

18、nt. 2 References ISO 749, Oilseed residues Determination of total ash. ISO 771, Oilseed residues Determination of moisture and volatile matter content. 3 Definition ash insoluble in hydrochloric acid the fraction of the total ash which remains undissolved after treatment with hydrochloric acid under

19、 the operating conditions specified below 4 Principle Treatment of the total ash with hydrochloric acid, to remove the portion soluble in this reagent, then incineration and weighing of the insoluble residue. 5 Reagents 5.1 Hydrochloric acid, 3 N solution. 5.2 Silver nitrate, 10 g/l solution. 6 Appa

20、ratus 6.1 Analytical balance 6.2 Flat-bottomed incineration dish, of diameter about60mm and height not exceeding25mm, of platinum, platinum-plated gold, silica or, if not available, porcelain. 6.3 Hardened filter paper, of medium porosity, ash-free. 6.4 Electrically heated muffle furnace, with air c

21、irculation and capable of being controlled at550 15 C. 6.5 Desiccator, containing an efficient desiccant. 7 Procedure Make all weighings to the nearest0,001g. 7.1 Test portion and incineration See ISO749. 7.2 Determination Moisten the total ash obtained with10ml of the hydrochloric acid solution (5.

22、1), covering the incineration dish containing the ash with a watch-glass. Heat gently and, by several washes with hydrochloric acid solution (5.1), using about50ml of acid solution in all and washing the watch-glass as well as the dish, transfer the contents of the dish quantitatively to a beaker of

23、 about250ml capacity. Heat to boiling and keep gently boiling for about10min, then filter through hardened filter paper (6.3) and wash with boiling water until chloride ions are removed test with the silver nitrate solution (5.2). Place the filter paper and the residue in the incineration dish (6.2)

24、, previously heated for15min in the furnace (6.4) at550 15 C, allowed to cool in the desiccator (6.5) to laboratory temperature and weighed. Heat the dish containing the filter paper and residue progressively on an electric hot-plate or over a gas flame until the filter paper is carbonized, then pla

25、ce in the furnace controlled at550 15 C. Continue heating until a residue visibly free from carbon particles is obtained (generally1h). Allow the dish to cool in the desiccator and weigh when it has reached laboratory temperature. Replace the dish in the furnace and continue heating for another30min

26、 at550 15 C. Allow the dish to cool and re-weigh, as before. If the difference between the two weighings is less than or equal to0,001g, consider the determination as finished. If not, continue with periods of30min in the furnace until the difference between two successive weighings is less than or

27、equal to0,001g. Carry out two determinations, starting from the same test sample. 8 Expression of results 8.1 Method of calculation and formulae 8.1.1 The ash insoluble in hydrochloric acid, expressed as a percentage by mass of the sample as received, is equal to where m 0is the mass, in grams, of t

28、he test portion taken for the determination of the total ash; m 1is the mass, in grams, of the tared dish (6.2); m 2is the mass, in grams, of the dish containing the residue obtained by calcination. m 1 m 2 () 100 m 0 - BS4325-3:1978 2 BSI 10-1999 Take as the result the arithmetic mean of the two de

29、terminations, provided that the requirement concerning repeatability (see8.2) is satisfied. Other wise, repeat the determination on two other.test portions. If this time the difference again exceeds0,2g per100g of sample, take as the result the arithmetic mean of the four determinations carried out,

30、 provided that the maximum difference between the individual results does not exceed0,5g per100g of sample. Report the result to one decimal place. 8.1.2 If requested, the ash insoluble in hydrochloric acid may be expressed in relation to the dry matter by multiplying the result obtained in accordan

31、ce with8.1.1 by where U is the percentage by mass of moisture and volatile matter determined as specified in ISO771. 8.2 Repeatability The difference between the results of two determinations carried out simultaneously or in rapid succession by the same analyst should not exceed0,2g of ash insoluble

32、 in hydrochloric acid per100g of sample. 9 Test report The test report shall show the method used and the result obtained, indicating clearly whether the result is expressed in relation to the product as received or in relation to the dry matter. It shall also mention any operating conditions not sp

33、ecified in this International Standard, or regarded as optional, as well as any circumstances that may have influenced the result. The report shall include all details required for complete identification of the sample. 100 100U -BS4325-3:1978 BSI 10-1999 Publications referred to See national forewo

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