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

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1、BSI Standards PublicationBS ISO 602:2015Coal Determination ofmineral matterBS ISO 602:2015 BRITISH STANDARDNational forewordThis 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 list o

2、f 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 Standards Limi

3、ted 2015ISBN 978 0 580 88406 1ICS 73.040Compliance 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 publicationDate T e x t

4、a f f e c t e dBS ISO 602:2015 ISO 2015Coal Determination of mineral matterCharbon Dtermination du taux de matires minralesINTERNATIONAL STANDARDISO602Third edition2015-04-15Reference numberISO 602:2015(E)BS ISO 602:2015ISO 602:2015(E)ii ISO 2015 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2

5、015All 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. Permission can be reques

6、ted from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 602:2015ISO 602:2015(E)Foreword iv1 Scope

7、. 12 Normative references 13 Principle 14 Reagents 15 Apparatus . 16 Preparation of sample 27 Procedure. 28 Expression of results 39 Precision of the method 39.1 Repeatability . 49.2 Reproducibility . 410 Test report . 4Annex A (normative) Example of calculation 6Bibliography 7 ISO 2015 All rights r

8、eserved iiiContents PageBS ISO 602:2015ISO 602:2015(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. E

9、ach 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 work. ISO collaborates closely with the Internati

10、onal 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 different approval criteria needed for the differen

11、t 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 document may be the subject of patent rights. ISO shall no

12、t 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/patents).Any trade name used in this document is inf

13、ormation 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 principles in the Technical Barriers to Trade (TBT), see

14、 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 602:1983), which constitutes a minor revision.iv ISO 2015 All

15、 rights reservedBS ISO 602:2015Coal Determination of mineral matter1 ScopeThis International Standard specifies a method of determining the amount of mineral matter in all types of coal, including brown coals and lignites.2 Normative referencesThere are no normative references cited in this document

16、.3 PrincipleThe 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 loss in mass of the coal due to the acid treatment and determinat

17、ion 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; andd) determination of the amount of hydrochloric acid absorbed by the coal substance.4 Re

18、agentsDuring 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 Hydrofluoric acid, 1,13 g/ml.WARNING Very toxic by inhalation, in contact with skin,

19、 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 and gloves. In case of accident or feeling unwell, seek medical advice immed

20、iately (show the label where possible).5 ApparatusAll 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, with a cover slip.INTERNATIONAL STANDARD ISO 602:2015(E) ISO 2015 All rights res

21、erved 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 alumina filter plate, as shown in Figure 1.5.6 Filter flask.5.7 Balance, accurate to 0,1 m

22、g.6 Preparation of sampleThe 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 required for the moisture content to reach approximate equilibrium with the laboratory atm

23、osphere (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 means.NOTE Alternatively, the coal sample can be dried at 105 C to 110 C before carrying out

24、 the procedure.7 ProcedureWeigh, 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 tube (5.2) carrying a thermometer and place the cover slip over the beaker. Place the beaker in a

25、 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. Filter the solution through the filter (5.5) under suction.Wash the coal retained on the fil

26、ter 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 acid (4.3) to the beaker and repeat the heat treatment and filtration as previously described. Ri

27、nse 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 previously described. Filter and wash the coal three times, decanting each time. Transfer the coal enti

28、rely 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 5 min to 10 min.Dismantle the filter, break up the wet coal, and dry the filter and coal in a va

29、cuum oven at 50 C and a pressure of 3,5 kPa1)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 possible to a glass stoppered bottle. Brush the filter top and filter paper free from coal and reweigh.

30、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 ash), and chlorine (see ISO 587 for determination of chlorine), as well as the total iron content o

31、f 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 rights reservedBS ISO 602:2015ISO 602:2015(E)out according to the appropriate International Standards

32、(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 lignites, the acids can be placed in the beaker before adding the sample to avoid local overheating.NOTE 2

33、The first hydrochloric acid extraction is unnecessary for coals having a carbon dioxide content of less than 0,5 % (m/m).8 Expression of resultsAll results used in the calculation shall be on the dry basis. The mineral matter, MM, expressed as a percentage by mass, is given by Formula (1)2).mmmm mm1

34、234 5111100+,(1)wherem1is the mass, in grams, of the test portion taken;m2is the mass, in grams, of the test portion after extraction;m3is the mass, in grams, of pyrites in the extracted coal;m4is the mass, in grams, of hydrochloric acid in the extracted coal;m5is the mass, in grams, of ash, less ir

35、on oxide from the pyrites in the extracted coalThe mineral matter factor, FMM, is given by Formula (2):MMA(2)where A is the percentage of ash in the original coal.An example of the calculation is given in Annex A.The result (preferably the mean of two determinations, see Clause 9) shall be reported

36、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 approximately for the water of hydration of the aluminium and silicon compounds in the demineralized coal. In most cases, t

37、he correction is small and can be ignored.9 Precision of the methodMineral matterMaximum acceptable difference between results obtainedIn the same laboratory(repeatability)In different laboratories(reproducibility)0,4 % absolute (see 9.2)2) See the notes. ISO 2015 All rights reserved 3BS ISO 602:201

38、5ISO 602:2015(E)9.1 RepeatabilityThe result of duplicate determinations, carried out at different times in the same laboratory by the same operator with the same apparatus on the same analysis sample, should not differ by more than the above value.9.2 ReproducibilityNo value for reproducibility can

39、be quoted for determinations carried out in different laboratories, since insufficient data are available.10 Test reportThe test report shall include the following information:a) an identification of the product tested;b) the reference of the method used;c) the results and the method of expression u

40、sed;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 reservedBS ISO 602:2015ISO 602:2015(E)12345Key1 paper filter, connected to the upper cylinder with an adhesive substance2 plate of si

41、ntered alumina3 rubber ring4 cylinder of acid resistant material (for example, polyvinyl chloride)5 cylinder of acid resistant material (for example, polyvinyl chloride)Figure 1 Filtering device (Left half shown in section) ISO 2015 All rights reserved 5BS ISO 602:2015ISO 602:2015(E)Annex A (normati

42、ve) Example of calculationThe following example illustrates the method of calculation. All results are quoted on the dry basis.% (m/m) g 1 Mass of original coal = 6,836 (m1)2 Ash content of original coal = 52,8 (A)3 Mass of extracted coal = 3,205 (m2)4 Ash content of extracted coal = 6,03 (A1)5 Amou

43、nt of hydrochloric acid absorbed by the extracted coal = 1,06 (P1)6 Amount of iron oxide in the ash of the extracted coal = 4,2 (P2)7 Loss in mass of the sample (m1 m2) = 3,631 8 Mass of hydrochloric acid absorbed (P1m2/100) = 0,034 (m4)9 Mass of the pyrites in the extracted coal (1,5 P2m2/100) = 0,

44、202 (m3)10 Mass of the residual ash 1,1 m2(A1 P2)/100) = 0,065 (1,1 m5)11 Total mass of mineral matter (m1 m2+ m3+ m4+ 1,1 m5) = 3,932 (m6)12 Percentage of mineral matter (100 m6/m1) = 57,5 (MM)13 Mineral matter factor (MM/A) = 1,09 (FMM)6 ISO 2015 All rights reservedBS ISO 602:2015ISO 602:2015(E)Bi

45、bliography1 ISO 157, Coal Determination of forms of sulfur2 ISO 587, Solid mineral fuels Determination of chlorine using Eschka mixture3 ISO 1170, Coal and coke Calculation of analyses to different bases4 ISO 1171, Solid mineral fuels Determination of ash5 ISO 11722, Solid mineral fuels Hard coal De

46、termination of moisture in the general analysis test sample by drying in nitrogen ISO 2015 All rights reserved 7BS ISO 602:2015ISO 602:2015(E) ISO 2015 All rights reservedICS 73.040Price based on 7 pagesThis page deliberately left blankBSI is the national body responsible for preparing British Stand

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