BS 6043-2 7-1986 Methods of sampling and test for carbonaceous materials used in aluminium manufacture - Electrode coke - Determination of the apparent oil content of calcined coke.pdf

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1、BRITISH STANDARD BS 6043-2.7: 1986 ISO 6997:1985 Methods of sampling and test for Carbonaceous materials used in aluminium manufacture Part 2: Electrode coke Section 2.7 Determination of the apparent oil content of calcined cokes (gravimetric method) ISO title: Carbonaceous materials for the product

2、ion of aluminium Calcined coke Determination of apparent oil content Heating method UDC 665.777:669.713.7:543.824.2BS6043-2.7:1986 This British Standard, having been prepared under the directionof the Chemicals Standards Committee, was published under the authority ofthe Board of BSI and comes intoe

3、ffect on 28February1986 BSI 10-1999 The following BSI references relate to the work on this standard: Committee reference CIC/24 Draft for comment 82/54156 DC ISBN 0 580 14975 7 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Chemicals S

4、tandards Committee (CIC/-) to Technical Committee CIC/24 upon which the following bodies were represented: Aluminium Federation British Ceramic Research Association British Tar Industry Association Chemical Industries Association Institute of Petroleum Standardization of Tar Products Tests Committee

5、 Amendments issued since publication Amd. No. Date of issue CommentsBS6043-2.7:1986 BSI 10-1999 i Contents Page Committees responsible Inside front cover National foreword ii 0 Introduction 1 1 Scope and field of application 1 2 References 1 3 Principle 1 4 Apparatus 1 5 Sampling and sample 1 6 Proc

6、edure 1 7 Expression of results 2 8 Test report 2 Figure Arrangement of the crucibles in the heat-resistant steel box 3 Publications referred to Inside back coverBS6043-2.7:1986 ii BSI 10-1999 National foreword This British Standard has been prepared under the direction of the Chemicals Standards Co

7、mmittee to provide methods of sampling and test for carbonaceous materials used in the production of aluminium. The standard will be published in two Parts, each Part being divided into Sections. The two Parts are: Part 1: Electrode pitch; Part 2: Electrode coke. Initially, it is proposed that Part

8、2 will comprise the following Sections applicable to green and/or calcined coke as indicated: Other international methods of test for electrode coke are under consideration and, subject to approval by the United Kingdom, will be published as they become available. This Section is identical with ISO6

9、997:1985 “Carbonaceous materials for the production of aluminium Calcined coke Determination of apparent oil content Heating method”, published by the International Organization for Standardization (ISO). Terminology and conventions. The text of the International Standard has been approved as suitab

10、le for publication as a British Standard without deviation. Some terminology and certain conventions are not identical with those used in British Standards; attention is drawn especially to the following. The comma has been used as a decimal marker. In British Standards it is current practice to use

11、 a full point on the baseline as the decimal marker. Wherever the words “International Standard” appear, referring to this standard, they should be read as “British Standard”. In British Standards it is current practice to use the symbol “L” for litre (and its submultiples) rather than “l” and to us

12、e the spelling “sulphur”, etc., instead of “sulfur”, etc. Section Subject Identical with 2.1 Sampling ab ISO 6375 2.2 Ash content ab ISO 8005 2.3 Ash analysis (AAS) ab ISO . . . . c 2.4 Ash analysis (XRF) ab ISO . . . . c 2.5 Apparent density and porosity ab ISO . . . . c 2.6 Density (xylene method)

13、 b ISO 8004 2.7 Oil content (gravimetric method) b ISO 6997 2.8 Oil content (extraction method) b ISO . . . . c 2.9 Sieve analysis b ISO . . . . c 2.10 Electrical resistivity b ISO . . . . c 2.11 Volatile matter content a ISO . . . . c a Applicable to green coke. b Applicable to calcined coke. c In

14、preparation. Cross-references International Standard Corresponding British Standard ISO 6375:1980 BS 6043 Methods of sampling and test for carbonaceous materials used in aluminium manufacture Part 2: Electrode coke Section 2.1:1985 Sampling (Identical)BS6043-2.7:1986 BSI 10-1999 iii The Technical Co

15、mmittee has reviewed the provisions of ISO565:1983 and ISO5725:1981, to which reference is made in the text, and has decided that they are acceptable for use in conjunction with this standard. A related British Standard for ISO565:1983 is BS410:1976 “Specification for test sieves”. A related British

16、 Standard for ISO5725:1981 is BS5497 “Precision of test methods” Part 1:1979 “Guide for the determination of repeatability and reproducibility for a standard test method”. Additional information. This standard describes methods of test only, and should not be used or quoted as a specification defini

17、ng limits of purity. Reference to this Section should state that the method of test used is in accordance with BS6043-2.7:1986. 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. Complia

18、nce 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 to iv, pages1to 4, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had

19、 amendments incorporated. This will be indicated in the amendment table on the inside front cover.iv blankBS6043-2.7:1986 BSI 10-1999 1 0 Introduction Calcined coke may be treated with different types of oil in order to avoid the formation of dust during loading and transportation. The method specif

20、ied in this International Standard allows the determination of loss in mass of calcined coke resulting from the elimination by heating of oil adhering to the particles. However, loss of mass determined in this way does not give the true oil content of the coke, but rather a useful indication of the

21、loss of mass which may occur during use. 1 Scope and field of application This International Standard specifies a conventional heating gravimetric method for the determination of the apparent oil content of the calcined coke used in the production of aluminium. The method provides two ways of determ

22、ination: A: normal and reference determination (6.2.1); B: simplified determination (6.2.2); 2 References ISO 565, Test sieves Woven metal wire cloth, perforated plate and electroformed sheet Nominal sizes of openings. ISO 5725, Precision of test methods Determination of repeatability and reproducib

23、ility by inter-laboratory tests. ISO 6375, Carbonaceous materials for the production of aluminium Cokes for electrodes Sampling. 3 Principle Heating of a test portion in a non-oxidizing atmosphere at a fixed temperature and determination of the loss in mass. Calculation of the apparent oil content i

24、n terms of loss of mass. To ensure a non-oxidizing atmosphere, add some drops of toluene to the crucibles. 4 Apparatus Ordinary laboratory apparatus and 4.1 Porcelain crucibles, capacity approximately150ml, fitted with lids. 4.2 Electric oven, capable of being controlled between105 and110 C. 4.3 Ele

25、ctric furnace, capable of being controlled up to800 C. 4.4 Steel box, resistant at550 C, with lid, of dimensions200mm 100mm 100mm. 5 Sampling and sample 5.1 Sampling Sampling shall be carried out according to the procedure specified in ISO6375. 5.2 Preparation of test sample Using a mortar and pestl

26、e, crush approximately200g of the laboratory sample (seeISO6375) sufficiently to pass through a sieve of nominal mesh apertures4mm (seeISO565). Dry the crushed and sieved product in the electric oven(4.2), controlled at a temperature between105 and110 C, for1h, or a longer period, until two successi

27、ve weighings do not differ by more than0,01g. 6 Procedure 6.1 Test portion Heat two of the crucibles, with their lids (4.1), for about1h in the electric furnace (4.3) at a temperature of about800 C. Allow them to cool to ambient temperature in a desiccator and weigh each of them, without their lids,

28、 to the nearest0,001g. Weigh into each crucible, to the nearest0,001g, a test portion of approximately75g from the test sample (5.2). Add a few drops of toluene to the crucibles to ensure a non-oxidizing atmosphere. 6.2 Determination 6.2.1 A: Normal and reference determination Put the lids on each o

29、f the porcelain crucibles containing the test portion (6.1) and place them in the steel box (4.4). Embed the crucibles into screened petroleum coke of a particle size of0,25 to2mm, as indicated in the Figure. Cover the steel box and place it in the cold electric furnace (4.3). Heat up the furnace to

30、 a temperature of550 10 C and maintain this temperature for2h. After this period, shut down the furnace and let it cool. Remove the steel box from the furnace and take out the porcelain crucibles. Take care to avoid contamination of the samples with petroleum coke particles of the packing material.

31、Brush and wipe away adhering dust from the still covered crucibles and place them in a desiccator to cool to room temperature. Remove the lids and weigh each crucible with its contents, to the nearest0,001g. NOTEThe determination may be also carried out introducing directly the steel box containing

32、the crucibles in the furnace heated to550 10 C. In this case, the box should be left in the furnace for2,5h. After this period remove the box from the hot furnace and let it cool covered on a refractory plate. Then proceed as indicated above.BS6043-2.7:1986 2 BSI 10-1999 6.2.2 B: Simplified determin

33、ation Put the lids on each of the porcelain crucibles containing the test portion (6.1) and place them in the electric furnace, previously heated to500 10 C. Wait until the temperature of the furnace, which falls, returns to the value indicated, and maintain the crucibles at this temperature for20mi

34、n. After this period, remove the crucibles from the furnace and allow them to cool slightly on a refractory plate. Transfer them to a desiccator and allow to cool to ambient temperature. Remove the lids, and weigh each crucible with its contents, to the nearest0,001g. 7 Expression of results 7.1 Met

35、hod of calculation The apparent oil content, expressed as a percentage by mass, is given by the formula where Report the mean value to the nearest0,01% of two simultaneous determinations. 7.2 Precision (according to ISO 5725) 7.2.1 A: Normal determination (six laboratories) 7.2.2 B: Simplified deter

36、mination (same sample; three laboratories) The results are rounded to the third decimal place. 8 Test report The test report shall include the following particulars: a) an identification of the sample; b) the reference of the method used normal reference determination (6.2.1) or simplified determina

37、tion (6.2.2); c) the results and the method of expression used; d) any unusual features noted during the determination; e) any operation not included in this International Standard or in the International Standards to which reference is made, or regarded as optional. m 0 is the mass, in grams, of th

38、e test portion(6.1); m 1 is the mass, in grams, of the crucible containing the test portion before heating; m 2 is the mass, in grams, of the crucible containing the test portion after heating. m (mean) = 0,256 % r (repeatability) = 0,050 R (reproducibility) = 0,078 m (mean) = 0,237 % r (repeatabili

39、ty) = 0,036 R (reproducibility) = r (because of the negative value of the variance of reproducibility)BS 6043-2.7:1986 BSI 10-1999 3 Figure Arrangement of the crucibles in the heat-resistant steel box4 blankBS6043-2.7:1986 BSI 10-1999 Publications referred to See national foreword.BS 6043-2.7: 1986

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