BS 6043-2 8-1987 Methods of sampling and test for carbonaceous materials used in aluminium manufacture - Electrode coke - Determination of oil content by solvent extraction of calc.pdf

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1、BRITISH STANDARD BS 6043-2.8: 1987 ISO 8723:1986 Methods of sampling and test for Carbonaceous materials used in aluminium manufacture Part 2: Electrode coke Section 2.8 Determination of oil content by solvent extraction of calcined coke ISO title: Carbonaceous materials for the production of alumin

2、ium Calcined coke Determination of oil content Method by solvent extraction UDC 669.713.7:665.777:543.383:542.61BS6043-2.8:1987 This British Standard, having been prepared under the directionof the Chemical Standards Committee, was published under the authority ofthe Board of BSI and comesintoeffect

3、 on 30 September 1987 BSI 10-1999 The following BSI references relate to the work on this standard: Committee reference CIC/24 Draft for comment 85/55641 DC ISBN 0 580 16111 0 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Chemicals Sta

4、ndards 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 A

5、mendments issued since publication Amd. No. Date of issue CommentsBS6043-2.8:1987 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 Solvent 1 5 Apparatus 1 6 Sampling and sampl

6、e 1 7 Procedure 1 8 Expression of results 2 9 Test report 2 Figure Extraction apparatus 3 Publications referred to Inside back coverBS6043-2.8:1987 ii BSI 10-1999 National foreword This British Standard has been prepared under the direction of the Chemicals Standards Committee to provide methods of

7、sampling and test for carbonaceous materials used in the production of aluminium. The standard is being 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 Part2will comprise the following S

8、ections 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 ISO8723:1986 “Carbonaceous material

9、s for the production of aluminium Calcined coke Determination of oil content Method by solvent extraction”, published by the International Organization for Standardization (ISO). Terminology and conventions. The text of the International Standard has been approved as suitable for publication as a Br

10、itish 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 a full point on the basel

11、ine as the decimal marker. The symbol “ml” has been used to denote millilitre. In British Standards it is current practice to use the symbol “mL”. Wherever the words “International Standard” appear, referring to this standard, they should be read as “Section of BS6043”. Section Subject Identical wit

12、h 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) b ISO 8004 2.7 Oil content (gravimetric method) b ISO 6997 2.8 Oil content (extraction

13、 method) b ISO 8723 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 preparation.BS6043-2.8:1987 BSI 10-1999 iii The Technical Committee has reviewed the provisi

14、ons 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 ISO565:1983is BS410:1976 “Specification for test sieves”. A related British Standard for ISO5725:1981is BS54

15、97 “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 defining limits of purity. Reference to

16、this Section should state that the method of test used is in accordance with BS6043-2.8:1987. 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 n

17、ot of itself confer immunity from legal obligations. Cross-references International Standards Corresponding British Standards 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) ISO 4

18、793:1980 BS 1752:1983 Specification for laboratory sintered or fritted filters including porosity grading (Identical) Summary of pages This document comprises a front cover, an inside front cover, pages i to iv, pages1 to 4, an inside back cover and a back cover. This standard has been updated (see

19、copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.iv blankBS6043-2.8:1987 BSI 10-1999 1 0 Introduction Calcined coke may be treated with different types of oil in order to limit the formation of a dust cloud during loadi

20、ng and transportation. The method specified in this International Standard permits the determination of the loss of mass in calcined coke after elimination of oil adhering to the particles, by extraction with a suitable solvent. 1 Scope and field of application This International Standard specifies

21、a method for the determination, by solvent extraction, of the oil content of calcined coke in the production of aluminium. 2 References ISO 5725, Precision of test methods Determination of repeatability and reproducibility by inter-laboratory tests. ISO 6375, Carbonaceous materials for the productio

22、n of aluminium Cokes for electrodes Sampling. 3 Principle Treatment of a test portion in an extraction apparatus with dichloromethane (methylene chloride) to remove the oil, and determination of oil removed in terms of the loss of mass of the test portion. NOTEThe small quantities of water which may

23、 still be present in the dried test portion are considered to be oil. 4 Solvent Dichloromethane (methylene chloride), of purity at least99%, boiling point39to40 C. WARNING Dangerous when inhaled. Avoid contact with the skin. Carry out work in a fume cupboard. NOTEThe methylene chloride used may be r

24、ecovered by filtration on activated carbon or by distillation. However, the presence of a yellow colour after distillation indicates the presence of hydrochloric acid and, in this case, the product should be discarded. 5 Apparatus Ordinary laboratory apparatus and 5.1 Electric oven, capable of being

25、 controlled at110 2 C. 5.2 Extraction apparatus, as shown in the Figure, and comprising the following items: 5.2.1 Cylindrical glass funnel, of capacity approximately1000ml, fitted with a glass fritted disk of porosity P250(pore diameter between160and 2504m see ISO4793) of effective diameter45to50mm

26、. The fritted disk is fitted with an internal tube to permit evacuation of air. 5.2.2 Glass extraction crucible, vacuum-resistant, of inner effective diameter45to50mm, fitted with a glass fritted disk of porosity P4(pore diameter between1,6and44m see ISO4793). 5.2.3 Glass adapter, provided with a4mm

27、 polytetrafluorethylene (PTFE) stopcock. 5.2.4 Glass Bchner flask, of capacity approximately2000ml. 5.3 Glass jar, for supporting the crucible (5.2.2) during drying and weighing. 5.4 PTFE cuffs, for sealing joints. 5.5 Vacuum device (water pump for example). 5.6 Drying device, for drying the crucibl

28、e (5.2.2) and jar (5.3), containing silica gel or activated alumina. 6 Sampling and sample 6.1 Sampling Sampling shall be carried out according to the procedure specified in ISO6375. 6.2 Preparation of test sample Crush in a mortar approximately200g of the laboratory sample to pass a nominal4mm mesh

29、 sieve (see ISO565). Dry the crushed and sieved product in the electric oven (5.1), maintained at110 2 C, for2h and then allow to cool in a desiccator for1h. 7 Procedure 7.1 Test portion Wash the crucible (5.2.2) with the methylene chloride (clause4), dry for30min in the oven (5.1), maintained at110

30、 2 C, using the jar (5.3). Allow to cool to ambient temperature in the drying device(5.6), and weigh the crucible with the jar to the nearest0,001g.BS6043-2.8:1987 2 BSI 10-1999 Introduce into the crucible approximately100g of the test sample (6.2) and weigh the crucible with the jar and the test po

31、rtion to the nearest0,001g. The difference between the two weighings represents the mass of the test portion. 7.2 Determination Assemble the extraction apparatus (5.2). Use the PTFE cuffs (5.4) to seal the joints. Close the stopcock and add the methylene chloride (clause4) to the crucible (5.2.2) th

32、rough the funnel (5.2.1) to a level2cm above the test portion (approximately100ml). Wait until all effervescence ceases (approximately5min), open the stopcock and turn on the vacuum device (5.5). When the methylene chloride level reaches the stopcock, close the stopcock. Repeat this procedure10times

33、 with1min extraction time before each drainage. Close the stopcock, remove the crucible and wipe off the moisture from the outside of the crucible. Place the crucible with the jar in the oven, maintained at110 2 C, and leave for30min. Remove the crucible and the jar from the oven, transfer to the dr

34、ying device and allow them to cool to ambient temperature. Weigh the crucible, its contents and the jar to the nearest0,001g. 8 Expression of results 8.1 Method of calculation The oil content, expressed as a percentage by mass, is given by the formula where Carry out at least two determinations and

35、report the mean value. 8.2 Precision (see ISO 5725, sub-clause 3.1) Nine laboratories from nine different countries have carried out the inter-laboratory tests. 9 Test report The test report shall include the following particulars: a) an identification of the sample; b) the reference of the method u

36、sed; c) the results and the method of expression used; d) any unusual features noted during the determination; e) any operations 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 the test p

37、ortion(7.1); m 1 is the mass, in grams, of the crucible supported by the jar, containing the test portion before extraction; m 2 is the mass, in grams, of the crucible supported by the jar, containing the test portion after extraction and drying. m 1 m 2 m 0 -100 m (mean) :0,60 % (m/m) r (repeatabil

38、ity) :0,023 % (m/m) R (reproducibility) :0,050 % (m/m)BS6043-2.8:1987 BSI 10-1999 3 Figure Extraction apparatus4 blankBS6043-2.8:1987 BSI 10-1999 Publications referred to See national foreword.BS 6043-2.8: 1987 ISO 8723:1986 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI

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