BS ISO 602-2015 en_5161 Coal Determination of mineral matter《煤 矿物质的测定》.pdf

1、BSI Standards Publication BS ISO 602:2015 Coal Determination of mineral matterBS ISO 602:2015 BRITISH STANDARD National foreword This British Standard is the UK implementation of ISO 602:2015. The UK participation in its preparation was entrusted to Technical Committee PTI/16, Solid mineral fuels. A

2、 list of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2015. Published by BSI Stand

3、ards Limited 2015 ISBN 978 0 580 88406 1 ICS 73.040 Compliance with a British Standard cannot confer immunity from legal obligations. This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 April 2015. Amendments/corrigenda issued since publicatio

4、n Date T e x t a f f e c t e dBS ISO 602:2015 ISO 2015 Coal Determination of mineral matter Charbon Dtermination du taux de matires minrales INTERNATIONAL STANDARD ISO 602 Third edition 2015-04-15 Reference number ISO 602:2015(E)BS ISO 602:2015ISO 602:2015(E)ii ISO 2015 All rights reserved COPYRIGHT

5、 PROTECTED DOCUMENT ISO 2015 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission

6、. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in SwitzerlandBS ISO 602:2015I

7、SO 602:2015(E)Foreword iv 1 Scope . 1 2 Normative references 1 3 Principle 1 4 Reagents 1 5 Apparatus . 1 6 Preparation of sample 2 7 Procedure. 2 8 Expression of results 3 9 Precision of the method 3 9.1 Repeatability . 4 9.2 Reproducibility . 4 10 Test report . 4 Annex A (normative) Example of cal

8、culation 6 Bibliography 7 ISO 2015 All rights reserved iii Contents PageBS ISO 602:2015ISO 602:2015(E) Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normal

9、ly carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the

10、 work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the

11、different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives). Attention is drawn to the possibility that some of the elements of this docume

12、nt may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/

13、patents). Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement. For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO pr

14、inciples in the Technical Barriers to Trade (TBT), see the following URL: Foreword Supplementary Information. The committee responsible for this document is ISO/TC 27, Solid mineral fuels, Subcommittee SC 05, Methods of analysis. This third edition cancels and replaces the second edition ( ISO 602:1

15、983), which constitutes a minor revision.iv ISO 2015 All rights reservedBS ISO 602:2015Coal Determination of mineral matter 1 Scope This International Standard specifies a method of determining the amount of mineral matter in all types of coal, including brown coals and lignites. 2 Normative referen

16、ces There are no normative references cited in this document. 3 Principle The following principle applies: a) partial demineralization of a sample of the coal by treatment with hydrochloric and hydrofluoric acids under such conditions that the coal substance remains unaffected; b) recording of the l

17、oss in mass of the coal due to the acid treatment and determination of the undissolved part of the mineral matter by ashing the partially demineralized coal; c) determination of the iron content of the ash so that the pyrites present in the extracted coal can be calculated; and d) determination of t

18、he amount of hydrochloric acid absorbed by the coal substance. 4 Reagents During the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. 4.1 Hydrochloric acid, 1,18 g/ml. 4.2 Hydrochloric acid, solution, c(HCI) 5 mol/l. 4.3 Hy dr ofluori

19、c acid, 1,13 g/ml. WARNING Very toxic by inhalation, in contact with skin, and if swallowed. Causes severe burns. Keep container tightly closed in a well-ventilated place. In case of contact with eyes, rinse immediately with plenty of water and seek medical advice. Wear suitable protective clothing

20、and gloves. In case of accident or feeling unwell, seek medical advice immediately (show the label where possible). 5 Apparatus All the apparatus listed below shall be resistant to acids, especially hydrofluoric acid. A suitable material is polyvinyl chloride (PVC). 5.1 Beaker, of capacity 200 ml, w

21、ith a cover slip. INTERNATIONAL ST ANDARD ISO 602:2015(E) ISO 2015 All rights reserved 1BS ISO 602:2015ISO 602:2015(E) 5.2 Thermometer pocket: a tube, sealed at one end, to carry a thermometer. 5.3 Stirrer. 5.4 Wash-bottle. 5.5 Filter, quantitative filter paper with 1 m aperture and a sintered alumi

22、na filter plate, as shown in Figure 1. 5.6 Filt er flask. 5.7 Balance, accurate to 0,1 mg. 6 Preparation of sample The coal used for determination of mineral matter is the analysis sample, ground to pass a sieve of 200 m aperture. If necessary, expose the sample in a thin layer for the minimum time

23、required for the moisture content to reach approximate equilibrium with the laboratory atmosphere (see ISO 11722 for moisture in the analysis sample). Before starting the determination, mix the air-dried analysis sample of coal (see the note) thoroughly for at least 1 min, preferably by mechanical m

24、eans. NOTE Alternatively, the coal sample can be dried at 105 C to 110 C before carrying out the procedure. 7 Procedure Weigh, to the nearest 0,1 mg, about 6 g of the sample into the beaker (5.1) and add 40 ml of the hydrochloric acid solution (4.2) (see Note 1). Insert the stirrer (5.3) and the tub

25、e (5.2) carrying a thermometer and place the cover slip over the beaker. Place the beaker in a water-bath adjusted to maintain the temperature of the solution between 55 C to 60 C. Stir the contents at 5 min intervals, remove the beaker after 45 min and allow the coal suspension to settle for 10 min

26、. Filter the solution through the filter (5.5) under suction. Wash the coal retained on the filter with water, drain and transfer the coal back to the beaker with the aid of not more than 5 ml of water. Care is required to avoid loss of coal by splashing (see Note 2). Add 40 ml of the hydrofluoric a

27、cid (4.3) to the beaker and repeat the heat treatment and filtration as previously described. Rinse the coal retained on the filter into the beaker with not more than 5 ml of water. Add 50 ml of hydrochloric acid (4.1) to the beaker, replace it in the water-bath and repeat the heat treatment previou

28、sly described. Filter and wash the coal three times, decanting each time. Transfer the coal entirely to the filter and wash 20 times with 25 ml portions of hot water each time. Recover any residual coal from the beaker by means of a rubber tipped rod and cold water. Drain the coal under suction for

29、5 min to 10 min. Dismantle the filter, break up the wet coal, and dry the filter and coal in a vacuum oven at 50 C and a pressure of 3,5 kPa 1)absolute for about 1,5 h. Remove and allow to cool in air for about 1 h to attain equilibrium and then weigh. Recover the coal and transfer as much as possib

30、le to a glass stoppered bottle. Brush the filter top and filter paper free from coal and reweigh. Obtain the mass of extracted coal by difference. Mix the extracted coal thoroughly and determine its moisture (see ISO 11722 for moisture in the analysis sample), ash (see ISO 1171 for determination of

31、ash), and chlorine (see ISO 587 for determination of chlorine), as well as the total iron content of the ash (see ISO 157 for determination of forms of sulphur); determine also the moisture and ash content of the original sample, each determination being carried 1) 1 kPa = 10 mbar.2 ISO 2015 All rig

32、hts reservedBS ISO 602:2015ISO 602:2015(E) out according to the appropriate International Standards (see Bibliography). Calculate the hydrochloric acid equivalent to the chlorine content and the pyrites equivalent to the total iron content. NOTE 1 For reactive coals, including brown coals and lignit

33、es, the acids can be placed in the beaker before adding the sample to avoid local overheating. NOTE 2 The first hydrochloric acid extraction is unnecessary for coals having a carbon dioxide content of less than 0,5 % (m/m). 8 Expression of results All results used in the calculation shall be on the

34、dry basis. The mineral matter, MM, expressed as a percentage by mass, is given by Formula (1) 2) . mmmm m m (1) wherem 1 is the mass, in grams, of the test portion taken;m 2 is the mass, in grams, of the test portion after extraction;m 3 is the mass, in grams, of pyrites in the extracted coal;m 4 is

35、 the mass, in grams, of hydrochloric acid in the extracted coal;m 5 is the mass, in grams, of ash, less iron oxide from the pyrites in the extracted coal The mineral matter factor, F MM , is given by Formula (2): (2) where A is the percentage of ash in the original coal. An example of the calculatio

36、n is given in Annex A. The result (preferably the mean of two determinations, see Clause 9) shall be reported to the nearest 0,1 %. NOTE 1 If it is required to derive the mineral matter from the percentage of ash by the application of a formula, see ISO 1170. NOTE 2 The factor 1,1 allows approximate

37、ly for the water of hydration of the aluminium and silicon compounds in the demineralized coal. In most cases, the correction is small and can be ignored. 9 Precision of the method Mineral matter Maximum acceptable difference between results obtained In the same laboratory (repeatability) In differe

38、nt laboratories (reproducibility) 0,4 % absolute (see 9.2) 2) See the notes. ISO 2015 All rights reserved 3BS ISO 602:2015ISO 602:2015(E) 9.1 Repeatability The result of duplicate determinations, carried out at different times in the same laboratory by the same operator with the same apparatus on th

39、e same analysis sample, should not differ by more than the above value. 9.2 Reproducibility No value for reproducibility can be quoted for determinations carried out in different laboratories, since insufficient data are available. 10 Test report The test report shall include the following informati

40、on: a) an identification of the product tested; 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 regarded as optional.4 ISO 2015 All rights r

41、eservedBS ISO 602:2015ISO 602:2015(E) 1 2 3 4 5 Key 1 paper filter, connected to the upper cylinder with an adhesive substance 2 plate of sintered alumina 3 rubber ring 4 cylinder of acid resistant material (for example, polyvinyl chloride) 5 cylinder of acid resistant material (for example, polyvin

42、yl chloride) Figure 1 Filtering device (Left half shown in section) ISO 2015 All rights reserved 5BS ISO 602:2015ISO 602:2015(E) Annex A (normative) Example of calculation The following example illustrates the method of calculation. All results are quoted on the dry basis.% (m/m) g 1 Mass of origina

43、l coal = 6,836 (m 1 ) 2 Ash content of original coal = 52,8 (A) 3 Mass of extracted coal = 3,205 (m 2 ) 4 Ash content of extracted coal = 6,03 (A 1 ) 5 Amount of hydrochloric acid absorbed by the extracted coal = 1,06 (P 1 ) 6 Amount of iron oxide in the ash of the extracted coal = 4,2 (P 2 ) 7 Loss

44、 in mass of the sample (m 1 m 2 ) = 3,631 8 Mass of hydrochloric acid absorbed (P 1 m 2 /100) = 0,034 (m 4 ) 9 Mass of the pyrites in the extracted coal (1,5 P 2 m 2 /100) = 0,202 (m 3 ) 10 Mass of the residual ash 1,1 m 2(A 1 P 2 )/100) = 0,065 (1,1 m 5 ) 11 Total mass of mineral matter (m 1 m 2+ m

45、 3+ m 4+ 1,1 m 5 ) = 3,932 (m 6 ) 12 Percentage of mineral matter (100 m 6 /m 1 ) = 57,5 (MM) 13 Mineral matter factor (MM/A) = 1,09 (F MM )6 ISO 2015 All rights reservedBS ISO 602:2015ISO 602:2015(E) Bibliography 1 ISO 157, Coal Determination of forms of sulfur 2 ISO 587, Solid mineral fuels Determ

46、ination of chlorine using Eschka mixture 3 ISO 1170, Coal and coke Calculation of analyses to different bases 4 ISO 1171, Solid mineral fuels Determination of ash 5 ISO 11722, Solid mineral fuels Hard coal Determination of moisture in the general analysis test sample by drying in nitrogen ISO 2015 A

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