1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 29541:2010Solid mineral fuels Determination of total carbon,hydrogen and nitrogen content Instrumental methodBS ISO 29541:2010 BRITISH STANDARDNational forewordThis Britis
2、h Standard is the UK implementation of ISO 29541:2010. Itsupersedes DD ISO/TS 12902:2002 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee PTI/16, Solid mineral fuels.A list of organizations represented on this committee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 s
3、ecretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2010ISBN 978 0 580 62894 8ICS 73.040; 75.160.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard
4、was published under the authority of theStandards Policy and Strategy Committee on 30 November 2010.Amendments issued since publicationDate Text affectedBS ISO 29541:2010Reference numberISO 29541:2010(E)ISO 2010INTERNATIONAL STANDARD ISO29541First edition2010-10-01Solid mineral fuels Determination o
5、f total carbon, hydrogen and nitrogen content Instrumental method Combustibles minraux solides Dosage du carbone, de lhydrogne et de lazote totaux Mthode instrumentale BS ISO 29541:2010ISO 29541:2010(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing
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9、publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing 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
10、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 29541:2010ISO 29541:2010(E) ISO 2010 All rights reserved iiiContents Page Foreword iv Introduction.v 1 Scope1 2 Normative references1 3 Terms
11、and definitions .1 4 Principle2 5 Reagents.2 6 Apparatus.3 7 Preparation of the test sample.3 8 Procedure.3 8.1 Instrument set-up 3 8.2 Blank analyses.3 8.3 Conditioning and instrument stability check .3 8.4 Calibration3 8.5 Verification of calibration .4 8.6 Analysis of test samples.4 9 Expression
12、of results4 10 Precision.5 10.1 Repeatability limit5 10.2 Reproducibility limit 5 11 Test report6 Annex A (informative) Recommendations for calibration 7 Bibliography10 BS ISO 29541:2010ISO 29541:2010(E) iv ISO 2010 All rights reservedForeword ISO (the International Organization for Standardization)
13、 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. Each member body interested in a subject for which a technical committee has been established has the right to be repre
14、sented on that committee. International organizations, 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
15、 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 Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an Internationa
16、l 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 subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 29541 was prep
17、ared by Technical Committee ISO/TC 27, Solid mineral fuels, Subcommittee SC 5, Methods of analysis. This first edition of ISO 29541 cancels and replaces ISO/TS 12902:2001, which has been technically revised. BS ISO 29541:2010ISO 29541:2010(E) ISO 2010 All rights reserved vIntroduction The reliable d
18、etermination of total carbon, hydrogen and nitrogen is important for engineering calculations applied to the combustion of coal. The precise and accurate determination of the carbon content of coal is essential for carbon accounting purposes. BS ISO 29541:2010BS ISO 29541:2010INTERNATIONAL STANDARD
19、ISO 29541:2010(E) ISO 2010 All rights reserved 1Solid mineral fuels Determination of total carbon, hydrogen and nitrogen content Instrumental method WARNING The use of this International Standard can involve hazardous materials, operations and equipment. This International Standard does not purport
20、to address all of the safety problems associated with its use. It is the responsibility of the user of this International Standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 1 Scope This International Standard specifie
21、s a method for the determination of total carbon, hydrogen and nitrogen in coal and coke by instrumental methods. NOTE This International Standard has been validated for coal only in accordance with the principles of ISO 5725-1. 2 Normative references The following referenced documents are indispens
22、able 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 amendments) applies. ISO 687, Solid mineral fuels Coke Determination of moisture in the general analysis test sample I
23、SO 1213-2, Solid mineral fuels Vocabulary Part 2: Terms relating to sampling, testing and analysis ISO 5068-2, Brown coals and lignites Determination of moisture content Part 2: Indirect gravimetric method for moisture in the analysis sample ISO 5069-2, Brown coals and lignites Principles of samplin
24、g Part 2: Sample preparation for determination of moisture content and for general analysis ISO 11722, Solid mineral fuels Hard coal Determination of moisture in the general analysis test sample by drying in nitrogen ISO 13909-4, Hard coal and coke Mechanical sampling Part 4: Coal Preparation of tes
25、t samples ISO 13909-6, Hard coal and coke Mechanical sampling Part 6: Coke Preparation of test samples ISO 18283, Hard coal and coke Manual sampling 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 1213-2 apply. BS ISO 29541:2010ISO 29541:2010(E) 2 IS
26、O 2010 All rights reserved4 Principle Carbon, hydrogen and nitrogen are determined concurrently in a single instrumental procedure. The quantitative conversion of the carbon, hydrogen and nitrogen into their corresponding gases (CO2, H2O, N2/NOx) occurs during combustion of the sample at an elevated
27、 temperature in an atmosphere of oxygen. Combustion products which would interfere with the subsequent gas analysis are removed. Oxides of nitrogen (NOx) produced during the combustion are reduced to N2before detection. The carbon dioxide, water vapour and elemental nitrogen in the gas stream are th
28、en determined quantitatively by appropriate instrumental gas analysis procedures. 5 Reagents Unless otherwise specified, all reagents shall be of analytical reagent grade. 5.1 Carrier gas, helium or other suitable gas as specified by the instrument manufacturer. 5.2 Oxygen, as specified by the instr
29、ument manufacturer. 5.3 Additional reagents, of types and qualities specified by the instrument manufacturer. 5.4 Calibration materials: see Table 1. Table 1 Examples of suitable calibration materials and their stoichiometric contents of C, H and N Mass fraction % Name Formula Carbon Hydrogen Nitrog
30、en EDTA (ethylene diamine tetra-acetic acid) C10H16N2O841,1 5,5 9,6 Phenylalanine C9H11NO265,4 6,7 8,5 Acetanilide C8H9NO 71,1 6,7 10,4 BBOT (CAS-No 7128-64-5) 2,5-bis (5-tert-butyl-2-benzoxazolyl) thiophene C26H26N2O2S 72,5 6,1 6,5 If these materials are accompanied by a traceable certificate of an
31、alysis that includes the uncertainty of the assigned carbon, hydrogen and nitrogen values, then use the certificate values for calibration purposes. If pure compounds ( 99,5 % purity) are available, use the stoichiometric values. Store these substances in a desiccator under conditions that maintain
32、the compounds in a dry state. Table 1 lists those pure substances that were included in the interlaboratory study (ILS) to determine the calibration requirements and precision of this International Standard. The ILS indicated benzoic acid is not suitable for calibration. Pure substances other than t
33、hose listed in Table 1 can be used for calibration provided the substances meet the purity and calibration requirements of this International Standard. 5.5 Reference materials. Reference material coal(s) with a certified composition and uncertainty for carbon, hydrogen and nitrogen may be used as a
34、check to monitor changes in instrument response, which can be affected by constituents not present in the calibration materials, and to verify the acceptability of nitrogen results. Alternatively, coal of a known composition can also be used as a check sample. As the bulk composition of coal can cha
35、nge during storage, coals shall not be used for calibration. BS ISO 29541:2010ISO 29541:2010(E) ISO 2010 All rights reserved 36 Apparatus 6.1 Analytical instrument, consisting of a furnace, gas handling and detection system capable of analysing a test portion of 6 mg or greater. 6.2 Balance, stand-a
36、lone or integrated with the instrument, with a resolution of a least 0,1 % of the test portion to be weighed. 7 Preparation of the test sample The sample shall be the general analysis test sample prepared to a nominal top size of 212 m using ISO 13909-4, ISO 13909-6, ISO 18283 or ISO 5069-2. Sample
37、preparation procedures are described in ISO 13909-4 for coal, ISO 13909-6 for coke and ISO 5069-2 for brown coal and lignites. The moisture content of each test sample and reference material shall be determined in accordance with ISO 11722 for coal, ISO 687 for coke or ISO 5068-2 for brown coals and
38、 lignites. Alternatively, the test sample and reference material shall be dried prior to analysis. 8 Procedure 8.1 Instrument set-up Verify that all instrument operation parameters meet the specifications in the instrument operating manual. Verify the condition and quantity of all chemicals currentl
39、y in use in the instrument to ensure they are satisfactory for the number of samples to be analysed. Prior to any analysis, check for, and if necessary correct, any leaks in the combustion system and carrier gas system. 8.2 Blank analyses Perform blank analyses daily to establish carbon, hydrogen an
40、d nitrogen levels in the combustion and carrier gases. The level of nitrogen in these gases shall not exceed 1 % of the instrument nitrogen response for the lowest mass of calibration material. Repeat blank analyses after changing or renewing gases or other reagents. 8.3 Conditioning and instrument
41、stability check Condition the instrument in accordance with the manufacturers instructions (generally by running at least two test portions of a coal, coke or brown coal or lignite that have a composition typical of the general analysis samples). Select a conditioning sample of similar composition t
42、o a typical sample. Carry out four determinations of the conditioning sample. Discard the first determination. If any maximum difference of three retained repeat determinations for carbon, hydrogen and nitrogen values exceeds 1,2 r, where r is the repeatability limit (see Clause 10) of this Internat
43、ional Standard, instrument stability is suspect. In this case, take corrective action before proceeding with calibration. 8.4 Calibration The instrument shall be calibrated as recommended by the instrument manufacturer, or whenever changes have been made to the equipment and whenever analysis of ver
44、ification samples (see 8.5) indicates an unacceptable difference between the certified and the measured values. BS ISO 29541:2010ISO 29541:2010(E) 4 ISO 2010 All rights reservedSelect amounts of one or more calibration materials (see 5.4) based on the regression to be used and the expected ranges of
45、 carbon, hydrogen and nitrogen in the test samples to be analysed. See Clause A.1 for recommendations about the number of calibration points and Clause A.2 for recommendations concerning calibration masses. NOTE Coal is not used for calibration because coal degrades with time and its composition cha
46、nges. 8.5 Verification of calibration Before analysis of the test samples, verify the acceptability of the calibration by analysing a calibration material (see 5.4) not used for calibration. In Table 2, the limits for the difference between the measured and stoichiometric or certificate values are l
47、isted. Table 2 Calibration acceptance limits Element Acceptance limit Relative percentage (%) Carbon 1,20 Hydrogen 2,10 Nitrogen 1,80 If the verification result does not agree within the limits specified in Table 2, an additional verification run shall be conducted. If the results of the additional
48、verification run do not agree with the measured and stoichiometric or certificate value within the limits, the instrument shall be recalibrated. Clause A.3 gives an example of calibration verification. 8.6 Analysis of test samples As indicated in Clause 7, determine the moisture content of each test
49、 sample concurrently with this analysis. Carry out an analysis of each test sample by weighing out a test portion with a mass normally employed for analysis. All test samples shall be run in duplicate. Verify the calibration at the completion of each test batch, and preferably at least every ten samples, in accordance with 8.5. At the beginning of the appropriate series of test samples, or at the end of the appropriate series of test samples, or both, analyse a reference material as a test
