BS ISO 562-2010 Hard coal and coke Determination of volatile matter《硬煤和焦炭 易挥发物质测定》.pdf

1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 562:2010Hard coal and coke Determination of volatilematterBS ISO 562:2010 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 562:2010.

2、Itsupersedes BS 1016-104.3:1998 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee PTI/16, Solid mineral fuels.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all

3、 the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2010ISBN 978 0 580 70435 2ICS 73.040; 75.160.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy

4、and Strategy Committee on 30 November 2010.Amendments issued since publicationDate Text affectedBS ISO 562:2010Reference numberISO 562:2010(E)ISO 2010INTERNATIONAL STANDARD ISO562Third edition2010-06-15Hard coal and coke Determination of volatile matter Houille et coke Dtermination des matires volat

5、iles BS ISO 562:2010ISO 562:2010(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the

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8、t at the address given below. COPYRIGHT PROTECTED DOCUMENT ISO 2010 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing fr

9、om 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 Switzerland ii ISO 2010 All rights reservedBS ISO 562:2010I

10、SO 562:2010(E) ISO 2010 All rights reserved iiiContents Page Foreword iv Introduction.v 1 Scope1 2 Normative references1 3 Principle1 4 Reagents and materials 1 5 Apparatus.1 6 Preparation of the test sample.6 7 Procedure.6 8 Expression of results6 9 Precision.7 10 Test report7 Bibliography8 BS ISO

11、562:2010ISO 562:2010(E) iv ISO 2010 All rights reservedForeword ISO (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.

12、 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 work. ISO collaborates closely with the Interna

13、tional Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Stan

14、dards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subje

15、ct of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 562 was prepared by Technical Committee ISO/TC 27, Solid mineral fuels, Subcommittee SC 5, Methods of analysis. This third edition cancels and replaces the second edition (ISO 562:1998), of whic

16、h it constitutes a minor revision. BS ISO 562:2010ISO 562:2010(E) ISO 2010 All rights reserved vIntroduction In this International Standard the volatile matter is determined as the loss in mass, less that due to moisture, when coal or coke is heated out of contact with air under standardized conditi

17、ons. The test is empirical and, in order to ensure reproducible results, it is essential that the rate of heating, the final temperature and the overall duration of the test be carefully controlled. It is also essential to exclude air from the coal or coke during heating to prevent oxidation. The fi

18、t of the crucible lid is, therefore, critical. The moisture content of the sample is determined at the same time as the volatile matter so that the appropriate correction can be made. Mineral matter associated with the sample can also lose mass under the conditions of the test, the magnitude of the

19、loss being dependent on both the nature and the quantity of the minerals present. NOTE When applying this International Standard for classification purposes, to samples obtained directly from coal seams, it is required to give special care to the ash. The apparatus and procedure are specified so tha

20、t one or more determinations can be performed simultaneously in the furnace. BS ISO 562:2010BS ISO 562:2010INTERNATIONAL STANDARD ISO 562:2010(E) ISO 2010 All rights reserved 1Hard coal and coke Determination of volatile matter 1 Scope This International Standard specifies a method of determining th

21、e volatile matter of hard coal and of coke. It is not applicable to brown coals and lignites. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edi

22、tion of the referenced document (including any amendments) applies. ISO 687, Solid mineral fuels Coke Determination of moisture in the general analysis test sample ISO 11722, Solid mineral fuels Hard coal Determination of moisture in the general analysis test sample by drying in nitrogen 3 Principle

23、 A portion of the sample is heated out of contact with air at 900 C for 7 min. The percentage mass fraction of volatile matter is calculated from the loss in mass of the test portion after deducting the loss in mass due to moisture. 4 Reagents and materials 4.1 Cyclohexane, of recognized analytical

24、grade. 5 Apparatus 5.1 Furnace, heated by electricity, in which a zone of uniform temperature of 900 C 5 C can be maintained. It may be of the stop-ended type or fitted at the back with a flue approximately 25 mm in diameter and 150 mm long (see Figure 1). It is important for furnaces with flues tha

25、t the furnace door seal well. The flue should not reach far out of the oven and should be fitted with a butterfly valve to restrict airflow through the furnace. Its heat capacity shall be such that, with an initial temperature of 900 C, the temperature is regained within 4 min after insertion of a c

26、old stand and its crucibles. The temperature is measured with a thermocouple (5.2). Normally, the furnace is designed specifically either for multiple determinations using a number of crucibles in one stand or for receiving one crucible and its stand. In the first case, the zone of uniform temperatu

27、re shall be at least 160 mm 100 mm; in the latter case, a zone with a diameter of 40 mm is sufficient. BS ISO 562:2010ISO 562:2010(E) 2 ISO 2010 All rights reservedA position for the crucible stand shall be chosen within the zone of uniform temperature and this position shall be used for all determi

28、nations. The temperature of 900 C shall be attained as closely as possible with a specified tolerance of 5 C in order to compensate for inherent errors in the temperature measurement and lack of uniformity in the temperature distribution. 5.2 Thermocouple, unsheathed, of wire no thicker than 1 mm. I

29、t should be long enough to reach the centre of the underside of each crucible when placed in the zone of uniform temperature on being inserted through the front or rear of the furnace. The thermojunction shall be placed midway between the base of the crucible in its stand and the floor of the furnac

30、e. If the stand holds more than one crucible, the temperature under each crucible shall be checked in the same manner. If desired, a sheathed thermocouple may be permanently installed in the furnace (see Figure 1) with its thermojunction as close as possible to the centre of the zone of uniform temp

31、erature; in this case furnace temperature readings shall be correlated at frequent intervals with those of the unsheathed thermocouple, which is thus inserted only when necessary. NOTE The temperature/electromotive force relationship of a thermojunction maintained at elevated temperatures gradually

32、changes with time. 5.3 Crucible, cylindrical, with a well-fitting lid, both of fused silica. The crucible with lid shall have a mass between 10 g and 14 g and dimensions approximating to those shown in Figure 2. The fit of the lid on the crucible is critical to the determination and a lid shall be s

33、elected to match the crucible so that the horizontal clearance between them is no greater than 0,5 mm. After selection, the crucible and the lid shall be ground together to give smooth surfaces and then be given a common distinguishing mark. When performing multiple determinations on highly swelling

34、 coals, it can be necessary to use taller crucibles. These may be up to 45 mm in height without affecting the determined volatile matter, provided that the specified rate of temperature recovery be maintained. 5.4 Crucible stand, on which the crucible is placed in the furnace, such that the appropri

35、ate rate of heating can be achieved. For example, it may consist of the following: a) for single determinations, a ring of heat-resistant steel wire as shown in Figure 3 a) with ceramic discs, 25 mm in diameter and 2 mm thick, resting on the inner projection of its legs; or b) for multiple determina

36、tions, a tray of heat-resistant steel wire as shown in Figure 3 b), of appropriate size, with ceramic plates 2 mm thick supporting the crucibles. 5.5 Balance, capable of reading to the nearest 0,1 mg. BS ISO 562:2010ISO 562:2010(E) ISO 2010 All rights reserved 3Dimensions in millimetres Key 1 zone o

37、f uniform temperature 2 check thermocouple 3 chamber (width 200 mm) 4 heating system 5 flue 6 valve 7 thermocouple Figure 1 Example of a suitable furnace BS ISO 562:2010ISO 562:2010(E) 4 ISO 2010 All rights reservedDimensions in millimetres Figure 2 Silica crucible and lid BS ISO 562:2010ISO 562:201

38、0(E) ISO 2010 All rights reserved 5Dimensions in millimetres a) Suitable for a single determination b) Suitable for multiple determinations Key 1 three legs separated by 120 3 handle 2 ring 4 ceramic plates Figure 3 Crucible stands BS ISO 562:2010ISO 562:2010(E) 6 ISO 2010 All rights reserved6 Prepa

39、ration of the test sample The coal or coke used for the determination of volatile matter is the general analysis test sample (ground to pass a sieve of 212 m aperture). The sample shall be well mixed and in moisture equilibrium with the laboratory atmosphere. A test portion from the same test sample

40、 is separated for determination of moisture in parallel with the determination of volatile matter. 7 Procedure 7.1 Furnace temperature checking Adjust the temperature of the zone in the furnace (5.1), containing either a stand with one crucible and lid Figure 3 a) or a stand with the requisite numbe

41、r of crucibles and lids Figure 3 b), to 900 C 5 C as indicated by the correctly located thermocouple (5.2). Check that the temperature under each crucible, at the same height, lies within the temperature tolerance of the uniform zone. Temperature checking should be made before starting determination

42、s. However, in routine operation when several analyses are performed per day, a monthly temperature check is sufficient. The check of the temperature recovery criterion (5.1) should be dealt with in a similar way. 7.2 Volatile matter determination Fill either a stand with one empty crucible and lid

43、Figure 3 a) or a stand with the requisite number of empty crucibles and lids Figure 3 b) and insert in the oven. Maintain at 900 C 5 C for 7 min. Remove the crucible(s) from the furnace and allow to cool to room temperature on a thick metal plate. As soon as they are cool, weigh each empty crucible

44、and lid and weigh into each crucible, to the nearest 0,1 mg, 1 g 0,1 g of test sample. Replace the lid and tap each crucible on a clean hard surface until the test portion forms a layer of even thickness on the bottom of the crucible. If the sample is coke, remove the lid of the charged crucible, ad

45、d 2 drops to 4 drops of cyclohexane (4.1) and replace the lid. NOTE 1 The addition of cyclohexane prevents the oxidation of the coke but does not prevent adsorption of gases, e.g. nitrogen. Place the charged crucible(s) in a cold stand, transfer to the furnace, close the door and leave for 7 min 5 s

46、. If multiple determinations are being made, any vacant places in the stand should be filled with empty crucibles. Remove and allow to cool to room temperature. When cool, weigh the crucible(s) to the nearest 0,1 mg in the same manner as for the empty crucible(s). NOTE 2 The same treatment of the cr

47、ucible before and after the determination minimizes the effect of any film of water adsorbed on its surface, while the rapid cooling reduces absorption of moisture by the coal or coke residue. 8 Expression of results The volatile matter, V, in the sample as analysed, expressed as a percentage mass f

48、raction, is given by Equation (1): 223HO21100 mmVmm=()(1) BS ISO 562:2010ISO 562:2010(E) ISO 2010 All rights reserved 7where m1is the mass, expressed in grams, of the empty crucible and lid; m2is the mass, expressed in grams, of the crucible and lid and test portion before heating; m3is the mass, ex

49、pressed in grams, of the crucible and lid and contents after heating; H2Ois the moisture, expressed as a percentage mass fraction, in the sample as analysed, determined in accordance with the method specified in ISO 11722 for coal or ISO 687 for coke. Report the result, as the mean of duplicate determinations, to the nearest 0,1 % mass fraction. The results of the determination described in this International Standard are reported on the “air-dried” basis. Calculation of the re