1、BRITISH STANDARD BS 6043-1.5: 1983 ISO 6791:1981 Methods of sampling and test for Carbonaceous materials used in aluminium manufacture Part 1: Electrode pitch Section 1.5 Determination of content of quinoline-insoluble material ISO title: Carbonaceous materials for the production of aluminium Pitch
2、for electrodes Determination of content of quinoline-insoluble material UDC 665.775:669.713.7:543.868BS6043-1.5:1983 This British Standard, having been prepared under the directionof the Chemicals Standards Committee, was published under the authority ofthe Board of BSI and comes intoeffect on 31May
3、1983 BSI 10-1999 The following BSI references relate to the work on this standard: Committee reference CIC/24 Draft for comment 80/50463 DC ISBN 0 580 11910 6 Cooperating organizations The Chemicals Standards Committee, under whose direction this British Standard was prepared, consists of representa
4、tives from the following: Association of Fatty Acid Distillers British Tar Industry Association* Chemical Industries Association Consumer Standards Advisory Committee of BSI Department of Health and Social Security Department of Industry (Laboratory of the Government Chemist) Fertiliser Manufacturer
5、s 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 Royal Society of Chemistry Soap and Detergent Industry Association Standardization of Tar
6、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 Institute of Pet
7、roleum Amendments issued since publication Amd. No. Date of issue CommentsBS6043-1.5:1983 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 Reagents and materials 1 5 Apparatus 1 6 Sample pre
8、paration 1 7 Procedure 1 8 Expression of results 2 9 Test report 2 Figure Details of Hartley funnel 3 Publications referred to Inside back coverBS6043-1.5:1983 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; Part 2: Electrode coke. Initially, it is proposed that Part1 will comprise the
10、 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 ISO6791:1981 “Carbonaceous materials for the production of aluminium Pitch f
11、or electrodes Determination of content of quinoline-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. S
12、ome 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 baseline as the decimal marker. Wherever
13、 the words “International Standard” appear, referring to this standard, they should be read as “British Standard”. 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 this Section should sta
14、te that the method of test used is in accordance with BS6043-1.5:1982. Section Subject Identical with 1.1 Sampling ISO 6257 1.2 Water content (Dean and Stark method) ISO 5939 1.3 Softening point (ring and ball method) ISO 5940 1.4 Content of toluene-insoluble material ISO 6376 1.5 Content of quinoli
15、ne-insoluble material ISO 6791 1.6 Coking value ISO a 1.7 Density ISO a 1.8 Ash content ISO a 1.9 Sulphur content ISO a a In course of preparation and referred to for information purposes only. Cross-reference International Standard Corresponding British Standard ISO 6257:1980 BS 6043 Methods of sam
16、pling and test for carbonaceous materials used in aluminium manufacture Part 1 Electrode pitch Section 1.1:1981 Sampling (Identical)BS6043-1.5:1983 BSI 10-1999 iii A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible fo
17、r 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 to iv, pages1to 4, an inside back cover and a back cover. This standard has been updated (
18、see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.iv blankBS6043-1.5:1983 BSI 10-1999 1 1 Scope and field of application This International Standard specifies a conventional gravimetric method for the determination o
19、f the content of quinoline-insoluble material in pitch used in the production of aluminium. 2 Reference ISO 6257, Carbonaceous materials used in the production of aluminium Pitch for electrodes Sampling. 3 Principle Extraction of a test portion with quinoline, at a specified temperature and for a sp
20、ecified period. Filtration and weighing of the residue. 4 Reagents and materials During the analysis, use only reagents of recognized analytical grade. 4.1 Quinoline, freshly distilled, boiling between235 and237 C at1013 mbar 1) . WARNING Risk of poisoning by inhalation or swallowing. Irritating to
21、skin and eyes. Prevent inhalation of vapour and contact with skin, eyes and clothing. 4.2 Toluene WARNING Highly flammable. Harmful by inhalation. Keep away from sources of ignition. No smoking. Do not empty into drains. Take precautionary measures against static discharges. 4.3 Filter aid, diatomac
22、eous silica type, free from organic compounds, and chemically neutral. The particle sizes shall be within the range1 to404m and the average particle size shall be within the range6 to104m. Dry the material in the oven (5.4), controlled at105 to110 C, for1h. Allow to cool in a desiccator and weigh. R
23、epeat the process of heating, cooling and weighing until the difference between two consecutive weighings does not exceed0,005g. Store the dried material in a desiccator. 5 Apparatus Ordinary laboratory apparatus and 5.1 Water bath, capable of being controlled at70to80 C. 5.2 Hartley funnel, or equi
24、valent, having a disc diameter of70mm (a suitable type is shown in theFigure). 5.3 Glass fibre filter pads, of diameter70mm, with retention equal to98% for particles of size1,24m. NOTEA larger funnel (5.2) and pad (5.3), for example of diameter120mm, may be used, if available, as this largely obviat
25、es the need to transfer any residue from the walls of the funnel to the pad during the determination (7.3). 5.4 Electric oven, capable of being controlled at105 to110 C. 6 Sample preparation Sample in accordance with ISO6257. Prepare the test sample immediately before the determination. If it is suf
26、ficiently hard, grind the whole of the test sample, using a mortar and pestle, to a particle size not exceeding2004m. If the pitch is too soft for grinding, melt and mix the sample, ensuring that its temperature does not exceed150 C and that the melting period does not exceed10min. NOTEFor soft pitc
27、hes, the material for the test portion may be taken from the molten sample. 7 Procedure WARNING Attention is drawn to the dangers involved in the use of quinoline and toluene (see WARNINGS to clauses4.1 and4.2). Carry out all operations involving the use of these products in an efficiently ventilate
28、d fume cupboard. 7.1 Test portion Weigh, to the nearest0,005g, approximately1g of the test sample. 7.2 Filter preparation Heat one of the filter pads (5.3) in the oven (5.4), controlled at105to110 C, for1h. Transfer the pad to a desiccator, allow to cool to ambient temperature and weigh to the neare
29、st0,005g. Repeat the process of heating, cooling and weighing until the difference between two consecutive weighings does not exceed0,005g. Fit the pad into the clean and dry Hartley funnel (5.2). 1) 1 mbar = 100 PaBS6043-1.5:1983 2 BSI 10-1999 7.3 Determination Transfer the test portion (7.1) quant
30、itatively to a100ml beaker. Add approximately1g of the dried filter aid (4.3), weighed to the nearest0,005g, and25ml of the quinoline (4.1). Stir the contents of the beaker to break up any lumps and cover the beaker with a watch glass. Partially immerse the beaker in the water bath(5.1), controlled
31、at70 to80 C, together with another suitable beaker containing about100ml of the quinoline. Bring the temperature of the contents of each beaker to70 to80 C and continue heating for15 to20min, occasionally stirring the contents of the beaker containing the test portion. Fit the assembled Hartley funn
32、el and filter pad (see7.2) into the neck of a filter flask. Moisten the pad with a little of the hot quinoline and apply suction. As soon as filtration is complete, start filtering the dissolved test portion and any residue without unduly disturbing the solution, transferring about2ml of this suspen
33、sion at a time to the filter pad and allowing each portion to filter completely before making the next addition. Between each addition, maintain the temperature of the solution remaining in the beaker at70 to80 C by means of the heated water bath. When filtration is complete, rinse the beaker five t
34、imes with approximately5ml portions of the hot quinoline from the other beaker, so as to transfer all remaining insoluble matter to the pad. Wash the residue on the filter pad with further5ml portions of the hot quinoline until the washings are clear. About ten washings are usually necessary. Wash t
35、he beaker which had contained the test portion with ten approximately5ml portions of the toluene (4.2), allowing each washing to pass completely through the filter pad before making the next addition. During the entire filtering operation, ensure that as little as possible of the solution and residu
36、e is allowed to come into contact with the walls of the funnel. Release the suction, remove the filter pad with the residue and, after transferring to it any solid remaining on the walls of the funnel, place in the oven (5.4), controlled at105 to110 C, for about1h. Transfer from the oven to the desi
37、ccator and allow to cool to ambient temperature. Weigh to the nearest0,005g. Repeat the operations of heating, cooling and weighing until the difference between two consecutive weighings does not exceed0,005g. A drying time of2 to3h is usually sufficient. 8 Expression of results 8.1 Method of calcul
38、ation The content of quinoline-insoluble material, expressed as a percentage by mass, is given by the formula where 8.2 Precision Repeatability: 1 % Reproducibility: 1,50% 9 Test report The test report shall include the following particulars: a) an identification of the sample; b) the reference of t
39、he 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, or regarded as optional. m 0is the mass, in grams, of th
40、e test portion(7.1); m 1is the mass, in grams, of the dried filter pad(5.3); m 2is the mass, in grams, of the filter aid (4.3) added; m 3is the mass, in grams, of the dried filter pad, the filter aid and the residue. m 3 m 2 m 1 m 0 -100 BS6043-1.5:1983 BSI 10-1999 3 Figure Details of Hartley funnel
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