[BS 1016-104.2-1991] -- Methods for analysis and testing of coal and coke..pdf

BRITISH STANDARDMethods for Analysis and testing of coal and coke — Part 104: Proximate analysis — Section 104.2 Determination of moisture content of the general analysis sample of coke BS 1016-104.2: 1991 ) This British Standard. was published under the authority of the Standards Board and comes into effect on 30 April 1991 © BSI 07-1999 First published as BS 1016-4. No.) Institute of British Foundrymen Institute of Petroleum Power Generation Contractors’ Association (BEAMA Ltd. Quality. Design and Education Division) Electricity Supply Industry in United Kingdom GAMBICA (BEAMA Ltd.2:1991 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Solid Mineral Fuels Standards Policy Committee (SFC/-) to Technical Committee SFC/3. March 1942 Second edition May 1957 Third edition October 1965 Fourth edition October 1973 Fifth edition as BS 1016-104. upon which the following bodies were represented: British Cement Association British Coal Corporation British Gas plc British Steel Industry Department of Trade and Industry (Standards and Quality Policy Unit. April 1991 The following BSI references relate to the work on this standard: Committee reference SFC/3 Draft for comment 90/53515 DC ISBN 0 580 19470 1 Amendments issued since publication Amd.2. having been prepared under the direction of the Solid Mineral Fuels Standards Policy Committee.BS 1016-104. Date Comments . BS 1016-104.2:1991 Contents Committees responsible Foreword 0 Introduction 1 Scope 2 Definitions 3 Principle 4 Reagent 5 Apparatus 6 Preparation of test sample 7 Procedure 8 Expression of results 9 Precision 10 Test report Publication(s) referred to © BSI 07-1999 Page Inside front cover ii 1 1 1 1 1 1 1 1 2 2 2 Inside back cover i . BS 1016-104. The following Parts in the new series have been published.1: Determination of moisture content of the general analysis sample of coal.2:1991 Foreword This Section of BS 1016 has been prepared under the direction of the Solid Mineral Fuels Standards Policy Committee.3) by heating in air and then cooling in nitrogen. Determination of volatile matter content. — Part 6: Ultimate analysis of coal (Part 106). when complete. — Part 21: Determination of moisture-holding capacity of hard coal (Part 103). — Part 15: Fusibility of coal ash and coke ash (Part 113). with the new Part numbers (which will be given to revisions when they are published) in parentheses. The principal difference is that in the method described in ISO 687 the weighing dish is cooled in a desiccator instead of in an atmosphere of nitrogen. — Section 104. — Part 1: Total moisture of coal (Part 101). ii © BSI 07-1999 . — Part 111: Determination of abrasion index of coal. — Part 5: Gross calorific value of coal and coke (Part 105). Part 104 is a further Part numbered under a scheme for rationalizing and restructuring BS 1016. — Part 8: Chlorine in coal and coke (Part 106). which will include a general introduction. from which the principal changes are the omission of the direct gravimetric method (in 4. published by the International Organization for Standardization (ISO). — Section 104.2: Determination of moisture content of the general analysis sample of coke. Part 104 is a revision of the 1973 editions of BS 1016-3 and BS 1016-4.3. The earlier series of Parts is as follows. — Part 14: Analysis of coal ash and coke ash (Part 114). — Part 9: Phosphorus in coal and coke (Part 106). will begin with Part 100. — Part 2: Total moisture of coke (Part 102). — Part 7: Ultimate analysis of coke (Part 106).2) and the replacement of drying in nitrogen (in 4. — Part 20: Determination of Hardgrove grindability index of hard coal (Part 112). This Section is related to ISO 687:1974. Part 104 is divided into four Sections as follows. — Section 104. which are superseded and withdrawn. — Part 18: Size analysis of coke (Part 110).4: Determination of ash. — Part 17: Size analysis of coal (Part 109). — Part 10: Arsenic in coal and coke (Part 106). — Part 12: Caking and swelling properties of coal (Part 107). — Section 104. — Part 16: Methods for reporting results (Part 100). — Part 104: Proximate analysis. This Section replaces clause 4 in BS 1016-4:1973. — Part 11: Forms of sulphur in coal (Part 106). The new series. — Part 13: Tests special to coke (Part 108). Act 1974 or the Control of Substances Hazardous to Health Regulations 1988. WARNING NOTE. pages 1 and 2. Attention should be paid to any appropriate precautions and the method should be operated only by trained personnel.2:1991 There may be alternative methods for carrying out this determination which are more rapid and/or less labour-intensive than the reference method described in this Section of BS 1016. This British Standard does not necessarily detail all the precautions necessary to comply with the requirements of the Health and Safety at Work etc. and will give a level of repeatability which is the same as or better than that quoted for the reference method (see clause 9). pages i to iv. This will be indicated in the amendment table on the inside front cover.BS 1016-104. It is important to demonstrate that an alternative method is free from bias when compared to this reference method. This standard has been updated (see copyright date) and may have had amendments incorporated. an inside back cover and a back cover. Users of British Standards are responsible for their correct application. A British Standard does not purport to include all the necessary provisions of a contract. an inside front cover. Compliance with a British Standard does not of itself confer immunity from legal obligations. Work is in hand on the preparation of a standard for the validation of such alternative methods. Summary of pages This document comprises a front cover. © BSI 07-1999 iii . iv blank . 1 Balance.1). Transfer the dish to the cooling vessel (5.2) and maintained at this temperature until constant in mass. and weigh the dish. moisture in the general analysis sample 7.BS 1016-104. with provision for the nitrogen to pass through it at about 15 volumes per hour.4) through which the nitrogen (4. NOTE 3 Heating for 4 h is normally sufficient if the mass of coke per unit area does not exceed 0. 4 Reagent 4. one test for moisture content should suffice. 6 Preparation of test sample The coke used for the determination of moisture content is the general analysis sample. If all the portions taken for analysis are weighed out on the same day and at about the same time. then cool and reweigh it with its cover to the nearest 0.2 Air oven.1 mg. ground to pass a sieve of 212 Èm aperture (see BS 1017-2). reheat the dish without its cover at the same temperature as before.15 g/cm2 (see note 2 to 7. to the nearest 0.2:1991 0 Introduction As coke is hygroscopic.1 mg. capable of maintaining a temperature within the range 190 °C to 210 °C (see note 1 to 7. calorific value. Immediately before weighing out the test portion (see 7. dry. 5. 1 Scope This Section of BS 1016 describes a reference method for determining the moisture content of the general analysis sample of coke. the moisture in the general analysis sample has to be determined whenever portions are weighed out for other analytical determinations (for example. to the nearest 0. and heat the dish at that temperature for a minimum of 60 min (see notes 2 and 3). 5.15 g/cm2. to the oven (5. NOTE The provision of a metal plate. 7 Procedure 7.3) with its cover.1 mg. 6 h will probably be required. © BSI 07-1999 NOTE 1 The time taken for the determination can be considerably shortened if drying is carried out at a temperature of 320 °C in an atmosphere of nitrogen.25 g/cm2. of such a size that the mass of coke per unit area does not exceed 0. Add 1 g to 2 g of the test sample to the dish in an even layer and reweigh the dish.2).25 g/cm2. cover and test portion to the nearest 0. Remove the dish from the oven and replace its cover. shallow. but if the mass per unit area is 0. 1 . Weigh.1 Nitrogen.1) is passing at about 15 volumes per hour. a clean. NOTE 2 The mass per unit area of the coke layer may be increased up to 0. NOTE The titles of the publications referred to in this standard are listed on the inside back cover. 5. preferably by mechanical means.4 Cooling vessel. dry and containing less than 10 ÈL of oxygen per litre. Expose the sample in a thin layer for the minimum time required for the moisture content to reach approximate equilibrium with the laboratory atmosphere.1).1 Test portion For the purposes of this Section of BS 1016. together with the following. when heating for 1 h will usually suffice. provided that the heating time is increased sufficiently (see note 3). 2 Definitions 3 Principle A known mass of the coke is heated in air at between 190 °C and 210 °C (see note 1 to 7. volatile matter content. empty weighing dish (5.1 mg. without its cover. For further periods each of at least 10 min. preheated to a temperature within the range 190 °C to 210 °C (see note 1).2 Determination moisture content of the general analysis sample of a solid mineral fuel after it has attained approximate equilibrium with the atmosphere in the laboratory and which is removable under specified conditions Transfer the dish containing the test portion (see 7. the definitions given in BS 1017-2 apply. capable of weighing to the nearest 0. of glass with ground-on covers or of corrosion-resistant metal with well-fitting covers. when cool. until any further change in mass on successive weighings does not exceed 1 mg. The moisture content is calculated from the loss in mass of the coke.2). inside the vessel will increase the rate of cooling.1 mg. cabon and hydrogen content) and when results are required on a dry basis. preferably of aluminium.2) and in which the atmosphere changes from 3 times to 8 times per hour.3 Weighing dishes. mix the test sample for not less than 1 min. Therefore. its moisture content will vary with change of humidity of the atmosphere. 5 Apparatus 5. b) the reference to the method used. carried out in the same laboratory by the same operator with the same apparatus on representative portions weighed out at the same time from the same test sample.´ 100 m 2 – m1 where m1 is the mass of the empty dish plus cover (in g).2 Reproducibility Since the humidity conditions in different laboratories will vary. m3 is the mass of the dish plus cover plus coke after heating (in g). is given by the formula: The test report shall include the following: a) the identification of the sample.1 % (m/m). m2 is the mass of the dish plus cover plus coke before heating (in g). expressed as a percentage by mass. 9. e) any operations not specified in this standard or regarded as optional. d) any unusual features noted during the determination.1 % (m/m).2:1991 8 Expression of results 10 Test report The moisture content of the coke.2:1991. BS 1016-104.1 Repeatability The results of duplicate determinations. NOTE It is recommended that the result is calculated as the mean of duplicate determinations. 2 © BSI 07-1999 .BS 1016-104.e. i. 9 Precision 9. c) the results expressed in accordance with clause 8. Report the result to the nearest 0. m 2 – m3 ---------------------. should not differ by more than 0. it is not practical to quote a limiting value for reproducibility. Sampling of coal and coke. Methods for sampling of coke.2:1991 Publication(s) referred to BS 1017. BS 1017-2. ISO 687. © BSI 07-1999 . 1) Referred to in the foreword only. Coke — Determination of moisture in the analysis sample1).BS 1016-104. Designs and Patents Act 1988 no extract may be reproduced. It presents the UK view on standards in Europe and at the international level. and size. Users of British Standards should make sure that they possess the latest amendments or editions. type or grade designations. Fax: 020 8996 7400. Tel: 020 8996 7070. 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