1、BRITISH STANDARD BS 6043-1.4: 1981 ISO 6376:1980 Methods of sampling and test for Carbonaceous materials used in aluminium manufacture Part 1: Electrode pitch Section 1.4 Determination of content of toluene-insoluble material ISO title: Carbonaceous materials for the production of aluminium Pitch fo
2、r electrodes Determination of content of toluene-insoluble material UDC 665.775:669.713.7:543.86BS6043-1.4:1981 This British Standard, having been prepared under the directionof the Chemicals Standards Committee, was published under the authority ofthe Executive Board and comesinto effect on 30 Octo
3、ber 1981 BSI 10-1999 The following BSI references relate to the work on this standard: Committee reference CLC/24 Draft for comment 79/54055 DC ISBN 0 580 12338 3 Cooperating organizations The Chemicals Standards Committee, under whose direction this British Standard was prepared, consists of repres
4、entatives from the following: Association of Fatty Acid Distillers British Tar Industry Association* Chemical Industries Association* Chemical Society, Analytical Division* Consumer Standards Advisory Committee of BSI Department of Health and Social Security Department of Industry (Laboratory of the
5、 Government Chemist) Fertiliser Manufacturers Association Ltd. Ministry of Agriculture, Fisheries and Food Ministry of Defence National Sulphuric Acid Association Paintmakers Association of Great Britain Ltd. Royal Institute of Public Health and Hygiene Soap and Detergent Industry Association Standa
6、rdization of Tar Products Tests Committee* The organizations marked with an asterisk in the above list, together with the following, were directly represented on the Technical Committee entrusted with the preparation of this British Standard: Aluminium Federation British Ceramic Research Association
7、 Institute of Petroleum Royal Society of Chemistry Amendments issued since publication Amd. No. Date of issue CommentsBS6043-1.4:1981 BSI 10-1999 i Contents Page Cooperating organizations Inside front cover National foreword ii 1 Scope and field of application 1 2 Reference 1 3 Principle 1 4 Reagent
8、s and materials 1 5 Apparatus 1 6 Sampling 1 7 Procedure 1 8 Expression of results 2 9 Test report 2 Publications referred to Inside back coverBS6043-1.4:1981 ii BSI 10-1999 National foreword This British Standard has been prepared under the direction of the Chemicals Standards Committee to provide
9、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” and Part 2 “Electrode coke”. Initially, it is proposed that Part 1 will comprise
10、 the following Sections: Other international methods of test for electrode pitch are under consideration and, subject to approval by the United Kingdom, will be published as they become available. This Section is identical with ISO 6376:1980 “Carbonaceous materials for the production of aluminium Pi
11、tch for electrodes Determination of content of toluene-insoluble material”, 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 British Standard without deviation
12、. 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 throughout as a decimal marker. In British Standards it is current practice to use a full point on the baseline as the decimal ma
13、rker. Wherever the words “International Standard” appear, referring to this standard, they should be read as “British Standard”. The Technical Committee has reviewed the provisions of ISO383, ISO565 and ISO4793, to which reference is made in clauses5 and6, and has decided that they are acceptable fo
14、r use in conjunction with this standard. Related British Standards for ISO383, ISO565 and ISO4793 are BS572, BS410 and BS1752 respectively. ISO4797, to which reference is made in5.1, is in course of preparation and, subject to approval by the UK, will be published as a British Standard without devia
15、tion. Section Subject Identical with 1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.8 1.9 Sampling Water content (Dean and Stark method) Softening point (Ring and ball method) Content of toluene-insoluble material Content of quinoline-insoluble material Coking value Density Ash content Sulphur content ISO 6257 ISO 5
16、939 ISO 5940 ISO 6376 ISO 6791 aISO aISO aISO aISO aa In course of preparation. Cross-references International Standard Corresponding British Standard ISO 6257:1980 BS 6043 Methods of sampling and test for carbonaceous materials used in aluminium manufacture Part 1 Electrode pitch Section 1.1:1981 S
17、ampling (Identical)BS6043-1.4:1981 BSI 10-1999 iii Additional information. This standard prescribes methods of test only, and should not be used or quoted as a specification defining limits of purity. Reference to this Section should state that the method of test used is in accordance with BS6043-1.
18、4:1981. 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. Summary of pages This document co
19、mprises a front cover, an inside front cover, pages i to iv, pages1and 2, 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 front cover.iv blankBS6043-1.4:19
20、81 BSI 10-1999 1 1 Scope and field of application This International Standard specifies a gravimetric method for the determination of the content of toluene-insoluble material in pitch used for the production of aluminium. NOTEThe content of toluene-insoluble material is commonly called “sum of resi
21、ns ! + “”. 2 Reference ISO 6257, Carbonaceous materials for the production of aluminium Pitch for electrodes Sampling. 3 Principle Determination by weighing of the fraction of a test portion of pitch which is insoluble in toluene after boiling for a specified period. 4 Reagents and materials During
22、the analysis, use only reagents of recognized analytical grade. 4.1 Toluene 4.2 Acetone 5 Apparatus Ordinary laboratory apparatus and 5.1 Conical flask, of capacity500ml, of borosilicate glass, fitted with a ground glass socket (seeISO4797). 5.2 Reflux condenser, effective length300mm, having a grou
23、nd glass cone (seeISO383) at its lower end, by means of which it can be fitted to the socket of the conical flask (5.1). 5.3 Filter crucible, of glass, of capacity about30ml, fitted with a sintered glass disc (seeISO4793) of porosity grade P16 (pore size index 10 to 164m) and having the following ap
24、proximate principal dimensions: disc diameter: 30mm height (disc to upper rim): 35mm. 5.4 Electric oven, capable of being controlled at a temperature between 105 and 110 C. 6 Sampling See ISO 6257. In the case of hard pitches, grind the sample so that it passes through a sieve of nominal aperture si
25、ze2004m (seeISO565). In the case of soft pitches, use the sample as received. 7 Procedure WARNING Toluene is toxic and highly flammable. Carry out all operations involving its use in an efficiently ventilated fume cupboard. 7.1 Test portion Weigh, to the nearest0,001g, approximately 1g of the sample
26、 (see clause6). 7.2 Determination Prepare the filter crucible (5.3) for the determination by heating it for about 1h in the oven (5.4) controlled at a temperature between 105 and110 C, allowing it to cool to ambient temperature in a desiccator and weighing it to the nearest 0,001g. Place the test po
27、rtion (7.1) in the conical flask (5.1). Add about 100ml of hot (approximately 80 C) toluene (4.1) and swirl to dissolve the test portion. NOTEDissolution before boiling of soft pitches that are liquid on transfer to the flask is particularly necessary to prevent the formation of droplets of pitch wh
28、ich are subsequently not readily soluble in the boiling toluene. Fit the condenser (5.2) to the flask and start the water circulation. Bring the contents of the flask to a steady boil and continue boiling under reflux for about 30min. Stop the heating and remove the condenser. Using gentle suction,
29、immediately filter the contents of the flask through the dried and weighed filter crucible(5.3). Rinse the flask (5.1) with about 10ml of the hot (approximately 80 C) toluene (4.1) and filter the washings through the filter crucible (5.3). When filtration is complete, repeat the rinsing and filterin
30、g operations with further 10ml portions of the hot toluene until any residue in the flask is transferred to the filter crucible and the filtrate is colourless. Wash the filter crucible and its contents with approximately10ml of the acetone (4.2) and, when filtration is complete, repeat the operation
31、 with a further 10 ml portion of the acetone (4.2). Treat the filter crucible and its contents as follows: Heat for approximately 1h in the oven (5.4), maintained at a temperature between 105 and110 C, allow to cool to ambient temperature in a desiccator and weigh to the nearest0,001g.BS6043-1.4:198
32、1 2 BSI 10-1999 8 Expression of results 8.1 Method of calculation The quantity of toluene-insoluble material, expressed as a percentage by mass, is given by the formula where 8.2 Precision Repeatability: 0,5% Reproducibility: 1% 9 Test report The test report shall contain the following information:
33、a) identification of the sample; b) the reference of the method used; 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 Standard to which reference is made, o
34、r regarded as optional. m 0 is the mass, in grams, of the test portion(7.1); m 1 is the mass, in grams, of the crucible containing the insoluble material; m 2 is the mass, in grams, of the empty crucible. m 1 m 2 () m 0 -100 BS6043-1.4:1981 BSI 10-1999 Publications referred to See national foreword.
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