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1、BS ISO 23380:2008 ICS 73.040 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BRITISH STANDARD Selection of methods for the determination of trace elements in coal Licensed Copy: London South Bank University, South Bank University, 16/11/2008 11:42, Uncontrolled Copy, (c) BSI T
2、his British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 October 2008 BSI 2008 ISBN 978 0 580 56513 7 Amendments/corrigenda issued since publication DateComments BS ISO 23380:2008 National foreword This British Standard is the UK implementation of I
3、SO 23380:2008. The UK participation in its preparation was entrusted to Technical Committee PTI/16, Solid mineral fuels. A 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 c
4、ontract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations. Licensed Copy: London South Bank University, South Bank University, 16/11/2008 11:42, Uncontrolled Copy, (c) BSI BS ISO 23380:2008 Reference number ISO 23380:
5、2008(E) ISO 2008 INTERNATIONAL STANDARD ISO 23380 First edition 2008-10-15 Selection of methods for the determination of trace elements in coal Slection des mthodes de dtermination des lments en traces dans le charbon Licensed Copy: London South Bank University, South Bank University, 16/11/2008 11:
6、42, Uncontrolled Copy, (c) BSI BS ISO 23380:2008 ISO 23380:2008(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
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9、e inform the Central Secretariat at the address given below. ISO 2008 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
10、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 Switzerland ii ISO 2008 All rights reserved Licensed Copy
11、: London South Bank University, South Bank University, 16/11/2008 11:42, Uncontrolled Copy, (c) BSI BS ISO 23380:2008 ISO 23380:2008(E) ISO 2008 All rights reserved iii Contents Page Foreword iv Introduction v 1 Scope . 1 2 Normative references. 1 3 Definitions . 1 4 Abbreviations 1 5 Discussion of
12、methods 2 6 Use of certified reference materials 4 7 Calculation of results . 4 8 Sensitivity 5 9 Reporting of results 6 10 Precision 6 11 Test report . 6 Annex A (informative) Scheme of analysis for trace elements 7 Annex B (informative) Alternative dissolution procedures for coal . 8 Bibliography.
13、 9 Licensed Copy: London South Bank University, South Bank University, 16/11/2008 11:42, Uncontrolled Copy, (c) BSI BS ISO 23380:2008 ISO 23380:2008(E) iv ISO 2008 All rights reserved Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bo
14、dies (ISO member bodies). The work of preparing International Standards is normally 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 organizatio
15、ns, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the
16、ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards 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 th
17、e member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 23380 was prepared by Technical Committee ISO/TC 27, Solid minera
18、l fuels, Subcommittee SC 5, Methods of analysis. Licensed Copy: London South Bank University, South Bank University, 16/11/2008 11:42, Uncontrolled Copy, (c) BSI BS ISO 23380:2008 ISO 23380:2008(E) ISO 2008 All rights reserved v Introduction The determination of trace elements in coal and coke is be
19、coming more important due to the considerable emphasis being placed on the effect of these elements on the environment. In order to have accurate and precise results for the analysis of trace elements, it is imperative that standard methods be available and that these methods be based on reliable pr
20、ocedures. The objective of this International Standard is to assist in the selection of the appropriate methods available to determine the common trace elements in coal. Licensed Copy: London South Bank University, South Bank University, 16/11/2008 11:42, Uncontrolled Copy, (c) BSI BS ISO 23380:2008
21、 Licensed Copy: London South Bank University, South Bank University, 16/11/2008 11:42, Uncontrolled Copy, (c) BSI BS ISO 23380:2008 INTERNATIONAL STANDARD ISO 23380:2008(E) ISO 2008 All rights reserved 1 Selection of methods for the determination of trace elements in coal 1 Scope This International
22、Standard provides guidance on the selection of methods used for the determination of trace elements in coal. The trace elements of environmental interest include antimony arsenic, beryllium, boron, cadmium, chlorine, chromium, cobalt, copper, fluorine, lead, manganese, mercury, molybdenum, nickel, s
23、elenium, thallium, vanadium and zinc. To this list can be added the radioactive trace elements, thorium and uranium. This International Standard does not prescribe the methods used for the determination of individual trace elements. The analysis of appropriate CRMs is essential to confirm the accura
24、cy of any method used (see ISO Guide 33). 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 edition of the referenced document (including any amend
25、ments) applies. ISO 1213-2, Solid mineral fuels Vocabulary Part 2: Terms relating to sampling, testing and analysis ISO 5725 (all parts), Accuracy (trueness and precision) of measurement methods and results ISO Guide 33, Uses of certified reference materials 3 Definitions For the purpose of this doc
26、ument, the definitions given in ISO 1213-2 apply. 4 Abbreviations AAS atomic absorption spectrometry AFS atomic fluorescence spectrometry CVAAS cold-vapour atomic absorption spectrometry GFAAS graphite-furnace atomic absorption spectrometry IC ion chromatography ICP-AES inductively coupled plasma at
27、omic emission spectrometryoften referred to as ICP-OES, i.e. inductively coupled plasma optical emission spectrometry ICP-MS inductively coupled plasma mass spectrometry INAA instrumental neutron activation analysis ISE ion selective electrode XRF X-ray fluorescence spectrometry Licensed Copy: Londo
28、n South Bank University, South Bank University, 16/11/2008 11:42, Uncontrolled Copy, (c) BSI BS ISO 23380:2008 ISO 23380:2008(E) 2 ISO 2008 All rights reserved 5 Discussion of methods 5.1 General A summary of techniques applicable to the determination of each of the trace elements are discussed belo
29、w. A schematic of procedures used for trace element determinations is given in Annex A. It is critical that moisture be determined on the sample to enable calculation to bases other than “air-dried”. NOTE 1 There are digestion procedures applicable to unashed coal. The application of these is discus
30、sed in Annex B. NOTE 2 Boron, chlorine, fluorine, mercury and selenium are released if coal is ashed; thus, it is not possible to estimate the concentration of these elements in coal by analysing a laboratory-prepared ash. Where digestion procedures require ashing of the coal, it is critical to dete
31、rmine the ash yield to enable calculation of trace elements content in the coal sample; see Clause 7. Ashing procedures are described in ISO 152386. Coals are ashed in silica or quartz dishes, or in platinum or platinum alloy crucibles/basins, in a conventional ashing furnace. The furnace temperatur
32、e is ramped from ambient to a maximum of 500 C over 1 h to 3 h and held at this temperature until the carbonaceous material is completely oxidized or for a maximum of 18 h. The ramp rate is selected to avoid ignition and mechanical loss of sample. 5.2 Arsenic and selenium Arsenic and selenium are de
33、termined by hydride generation/atomic absorption or atomic fluorescence techniques following the ashing of the coal at 800 C in the presence of Eschka mixture and dissolution with hydrochloric acid. ISO 117233 is the recommended method for the determination of arsenic and selenium in coal. Arsenic c
34、an be determined in coal by the analysis of ash prepared in a laboratory at a temperature no greater than 500 C. Selenium is vaporized at quite low temperatures and is not recovered in ash. There is no International Standard for the determination of arsenic in coal ash. A suitable procedure is the d
35、issolution of the ash either by lithium metaborate/tetraborate fusion or by mixed acids (nitric, hydrochloric and hydrofluoric acids) and determination of the analyte by hydride/AAS or hydride/AFS. This element can also be determined by ICP-MS if the interference caused by argon chloride is eliminat
36、ed. 5.3 Boron Boron is determined by ICP-AES following the ashing of the coal at 800 C in the presence of Eschka mixture and dissolution with hydrochloric acid; see AS 1038.10.37. This dissolution procedure is the same as that used for arsenic and selenium. The procedure is set out in ISO 117233. 5.
37、4 Antimony, beryllium, cadmium, chromium, cobalt, copper, lead, manganese, molybdenum, nickel, thallium, vanadium, zinc, thorium and uranium 5.4.1 General Antimony, beryllium, cadmium, chromium, cobalt, copper, lead, manganese, molybdenum, nickel, thallium, vanadium, zinc, thorium and uranium are de
38、termined by various spectrometric techniques (see ASTM D635710). NOTE 1 A number of these trace elements can be determined by XRF; however, in general, the sensitivity is too low to accurately determine beryllium, cadmium, thallium, thorium and uranium by XRF. Licensed Copy: London South Bank Univer
39、sity, South Bank University, 16/11/2008 11:42, Uncontrolled Copy, (c) BSI BS ISO 23380:2008 ISO 23380:2008(E) ISO 2008 All rights reserved 3 Recommended procedures are summarized below. a) The coal sample is ashed at a maximum temperature of 500 C to remove the carbonaceous matter. b) The laboratory
40、-prepared ash is dissolved either by fusion with a mixture of lithium metaborate and tetraborate (see AS 1038.14.18) or by mixed acids (nitric, hydrochloric and hydrofluoric acids). These dissolution procedures are applicable to the analysis of coal ash. Note that thorium and uranium can form insolu
41、ble fluorides and precautions shall be taken to prevent this in the presence of hydrofluoric acid. Thorium and uranium can be determined within 2 h of the preparation of a mixed acid solution of the coal ash or the fluoride can be removed by evaporation. The solution obtained by dissolution procedur
42、es in which fluoride is complexed with boric acid, can be used for the determination of trace elements by ICP-AES and ICP-MS. c) The concentrations of the analytes in solution are determined by spectrometric techniques. Traditionally, AAS has been used. This has generally been replaced by ICP-AES, w
43、hich is used to determine the majority of these elements with the exception of antimony, cadmium, lead, thallium, thorium and uranium. These latter six elements occur in coals at concentrations too low to be determined by ICP-AES but can be accurately determined by ICP-MS. NOTE 2 Cadmium (see ISO 15
44、238) and lead can also be determined by GFAAS. 5.4.2 Radionuclides Radionuclides are naturally present in coal. The radioactivity of these can be measured using high-resolution gamma spectrometry; refer to Fardy, et al.14. This radioactivity is due to the decay of 238U, 235U and 232Th and their daug
45、hters, as well as 40K and 87Rb. 5.5 Chlorine Chlorine can be determined by a number of methods, including ISO 5871 and ASTM D42089. These procedures require that the coal be burnt and the chlorine trapped either in Eschka mixture or in an alkaline solution. The methods lack sensitivity and, with the
46、se procedures, repeatability levels are high. The solution obtained by pyrohydrolysis (see 5.6) can by used for the measurement of chlorine by IC or ICP-AES. The use of XRF can provide a practical and accurate method for the determination of chlorine directly on the coal. NOTE Chlorine is generally
47、reported not as a trace element but as a minor element and expressed as a percentage. 5.6 Fluorine Fluorine is determined using ISO 117244. This method is a pyrohydrolysis/ISE or pyrohydrolysis/IC procedure. This procedure can be used for the analysis of coal ash. There is significant evidence in th
48、e scientific literature that methods based on the decomposition of coal with an oxygen bomb combustion procedure can give low results. 5.7 Mercury Mercury is determined using ISO 152375. In this procedure, coal is combusted in an oxygen bomb and the released mercury absorbed in a solution of dilute
49、nitric acid. A number of accurate alternative procedures exist for the determination of mercury. It is possible to digest coal with acids, either in a pressure vessel in a microwave oven or closed vessel in a heated water bath, or by refluxing with a mixture of nitric and sulfuric acids; see ASTM D641411. There are instrumental techniques in which the coal is combusted and the released mercury adsorbed onto a gold collector; the mercury is subsequently thermally released and the mercury concentration determined by
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