ISO 29541:2010
(Main)Solid mineral fuels — Determination of total carbon, hydrogen and nitrogen content — Instrumental method
Solid mineral fuels — Determination of total carbon, hydrogen and nitrogen content — Instrumental method
ISO 29541:2010 specifies a method for the determination of total carbon, hydrogen and nitrogen in coal and coke by instrumental methods.
Combustibles minéraux solides — Dosage du carbone, de l'hydrogène et de l'azote totaux — Méthode instrumentale
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INTERNATIONAL ISO
STANDARD 29541
First edition
2010-10-01
Solid mineral fuels — Determination of
total carbon, hydrogen and nitrogen
content — Instrumental method
Combustibles minéraux solides — Dosage du carbone, de l'hydrogène
et de l'azote totaux — Méthode instrumentale
Reference number
ISO 29541:2010(E)
©
ISO 2010
---------------------- Page: 1 ----------------------
ISO 29541:2010(E)
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Published in Switzerland
ii © ISO 2010 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 29541:2010(E)
Contents Page
Foreword .iv
Introduction.v
1 Scope.1
2 Normative references.1
3 Terms and definitions .1
4 Principle.2
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 Calibration.3
8.5 Verification of calibration .4
8.6 Analysis of test samples.4
9 Expression of results.4
10 Precision.5
10.1 Repeatability limit.5
10.2 Reproducibility limit .5
11 Test report.6
Annex A (informative) Recommendations for calibration .7
Bibliography.10
© ISO 2010 – All rights reserved iii
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ISO 29541:2010(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 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 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 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
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 subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 29541 was prepared 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.
iv © ISO 2010 – All rights reserved
---------------------- Page: 4 ----------------------
ISO 29541:2010(E)
Introduction
The reliable determination 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.
© ISO 2010 – All rights reserved v
---------------------- Page: 5 ----------------------
INTERNATIONAL STANDARD ISO 29541:2010(E)
Solid 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 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 specifies 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 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 amendments) applies.
ISO 687, Solid mineral fuels — Coke — Determination of moisture in the general analysis test sample
ISO 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 sampling — 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 test 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.
© ISO 2010 – All rights reserved 1
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ISO 29541:2010(E)
4 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 (CO , H O,
2 2
N /NO ) occurs during combustion of the sample at an elevated temperature in an atmosphere of oxygen.
2 x
Combustion products which would interfere with the subsequent gas analysis are removed. Oxides of nitrogen
(NO ) produced during the combustion are reduced to N before detection. The carbon dioxide, water vapour
x 2
and elemental nitrogen in the gas stream are then 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 instrument 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 Nitrogen
EDTA
C H N O
41,1 5,5 9,6
10 16 2 8
(ethylene diamine tetra-acetic acid)
C H NO
Phenylalanine 65,4 6,7 8,5
9 11 2
C H NO
Acetanilide 71,1 6,7 10,4
8 9
BBOT (CAS-No 7128-64-5)
C H N O S
72,5 6,1 6,5
26 26 2 2
2,5-bis (5′-tert-butyl-2-benzoxazolyl) thiophene
If these materials are accompanied by a traceable certificate of analysis 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 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 those 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 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 change during
storage, coals shall not be used for calibration.
2 © ISO 2010 – All rights reserved
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ISO 29541:2010(E)
6 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-alone 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 µm using
ISO 13909-4, ISO 13909-6, ISO 18283 or ISO 5069-2. Sample 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 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 currently 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 and 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 stability check
Condition the instrument in accordance with the manufacturer's 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
sample
...
DRAFT INTERNATIONAL STANDARD ISO/DIS 29541
ISO/TC 27/SC 5 Secretariat: SA
Voting begins on: Voting terminates on:
2009-04-10 2009-09-10
INTERNATIONAL ORGANIZATION FOR STANDARDIZATION • МЕЖДУНАРОДНАЯ ОРГАНИЗАЦИЯ ПО СТАНДАРТИЗАЦИИ • ORGANISATION INTERNATIONALE DE NORMALISATION
Solid mineral fuels — Determination of total carbon, hydrogen
and nitrogen content — Instrumental method
Combustibles minéraux solides — Dosage du carbone, de l'hydrogène et de l'azote totaux — Méthode
instrumentale
ICS 73.040; 75.160.10
In accordance with the provisions of Council Resolution 15/1993 this document is circulated in
the English language only.
Conformément aux dispositions de la Résolution du Conseil 15/1993, ce document est distribué
en version anglaise seulement.
To expedite distribution, this document is circulated as received from the committee secretariat.
ISO Central Secretariat work of editing and text composition will be undertaken at publication
stage.
Pour accélérer la distribution, le présent document est distribué tel qu'il est parvenu du
secrétariat du comité. Le travail de rédaction et de composition de texte sera effectué au
Secrétariat central de l'ISO au stade de publication.
THIS DOCUMENT IS A DRAFT CIRCULATED FOR COMMENT AND APPROVAL. IT IS THEREFORE SUBJECT TO CHANGE AND MAY NOT BE
REFERRED TO AS AN INTERNATIONAL STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS BEING ACCEPTABLE FOR INDUSTRIAL, TECHNOLOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
INTERNATIONAL STANDARDS MAY ON OCCASION HAVE TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN NATIONAL REGULATIONS.
RECIPIENTS OF THIS DRAFT ARE INVITED TO SUBMIT, WITH THEIR COMMENTS, NOTIFICATION OF ANY RELEVANT PATENT RIGHTS OF WHICH
THEY ARE AWARE AND TO PROVIDE SUPPORTING DOCUMENTATION.
©
International Organization for Standardization, 2009
---------------------- Page: 1 ----------------------
ISO/DIS 29541
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's 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 editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the
unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
Copyright notice
This ISO document is a Draft International Standard and is copyright-protected by ISO. Except as permitted
under the applicable laws of the user's country, neither this ISO draft nor any extract from it may be
reproduced, stored in a retrieval system or transmitted in any form or by any means, electronic, photocopying,
recording or otherwise, without prior written permission being secured.
Requests for permission to reproduce should be addressed to either ISO at the address below or ISO's
member body in the country of the requester.
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Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
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Web www.iso.org
Reproduction may be subject to royalty payments or a licensing agreement.
Violators may be prosecuted.
©
ii ISO 2009 – All rights reserved
---------------------- Page: 2 ----------------------
ISO/DIS 29541
Contents Page
Foreword .iv
Introduction.v
1 Scope.1
2 Normative references.1
3 Terms and definitions .1
4 Principle.1
5 Reagents .2
5.1 General .2
5.2 Carrier gas.2
5.3 Oxygen.2
5.4 Additional reagents.2
5.5 Calibration materials.2
5.6 Certified reference materials.3
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 .4
8.4 Calibration.4
8.5 Verification of calibration .4
8.6 Analysis of test samples.4
9 Expression of results.5
10 Precision.6
10.1 Repeatability limit.6
10.2 Reproducibility critical difference .6
11 Test report.6
Annex A Recommendations for calibration (Normative) .7
A.1 Recommended number of calibration points.7
A.2 Recommended calibration masses .7
A.3 Calibration verification.8
A.4 Acceptance of results for certified reference material coal (s) .9
Annex B Test sample and test results (Informative) .11
B.1 Optimum test sample mass for the determination of total carbon .11
B.2 Checking test results and determining the final quoted result .12
B.2.1 Checking the acceptability of results obtained under repeatability conditions.12
B.2.2 Checking the acceptability of results obtained under reproducibility conditions .12
© ISO 2008 – All rights reserved iii
DRAFT 2009
---------------------- Page: 3 ----------------------
ISO/DIS 29541
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 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 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.
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. 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
International 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 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 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 prepared by Technical Committee ISO/TC 27, Solid Mineral Fuels, Subcommittee SC 5,
Methods of analysis.
This second/third/. edition cancels and replaces the first/second/. edition (), [Clause (s) / subClause (s) /
table(s) / figure(s) / annex(es)] of which [has / have] been technically revised.
iv © ISO 2008 – All rights reserved
DRAFT 2009
---------------------- Page: 4 ----------------------
ISO/DIS 29541
Introduction
The reliable determination 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.
© ISO 2008 – All rights reserved v
DRAFT 2009
---------------------- Page: 5 ----------------------
DRAFT INTERNATIONAL STANDARD ISO/DIS 29541
Solid mineral fuels — Determination of total carbon, hydrogen
and nitrogen content — Instrumental method
1 Scope
This Standard specifies a method for the determination of total carbon, hydrogen and nitrogen in coal and
coke by instrumental methods.
NOTE: This standard has been validated in accordance with the principles of ISO 5725 for coal only.
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 amendments) applies.
ISO 687, Coke—Determination of moisture in the analysis sample
ISO 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—Indirect gravimetric method,
Part 2: Moisture of analysis sample
ISO 5069-2, Brown coals and lignites—Principles of sampling—Part 2: Sample preparation for determination
of moisture content and for general analysis
ISO 5725-6, Accuracy (trueness and precision) of measurement methods and results Part 6: Use in practice
of accuracy values
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 test 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 purpose of this Standard, the definitions given in ISO 1213-2 apply.
4 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 (CO , H O,
2 2
© ISO 2008 – All rights reserved 1
DRAFT 2009
---------------------- Page: 6 ----------------------
ISO/DIS 29541
N /NO ) occurs during combustion of the sample at an elevated temperature in an atmosphere of oxygen.
2 x
Combustion products which would interfere with the subsequent gas analysis are removed. Oxides of nitrogen
(NO ) produced during the combustion are reduced to N before detection. The carbon dioxide, water vapour
x 2
and elemental nitrogen in the gas stream are then determined quantitatively by appropriate instrumental gas-
analysis procedures.
5 Reagents
5.1 General
Unless otherwise specified, all reagents shall be analytical reagent grade.
5.2 Carrier gas
Helium or other suitable gas as specified by the instrument.
5.3 Oxygen
As specified by the instrument.
5.4 Additional reagents
Of types and qualities specified by the instrument.
5.5 Calibration materials
Table 1. Examples of suitable calibration materials and their stoichiometric contents of C, H and N
Mass fraction in percent
Name Formula
Carbon Hydrogen Nitrogen
EDTA
C H N O 41,1 5,5 9,6
10 16 2 8
(ethylene diamine tetra-acetic acid)
Phenylalanine C H NO 65,4 6,7 8,5
9 11 2
Acetanilide C HNO 71,1 6,7 10,4
8 9
BBOT (CAS-No 7128-64-5)
C H N OS 72,5 6,1 6,5
26 26 2 2
2.5-bis (5′-tert-butyl-2-benzoxazolyl) thiophene)
If these materials are accompanied by a traceable certificate of analysis 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 the compounds in a dry state.
NOTE: Table 1 includes those pure substances that were included in the interlaboratory study (ILS) employed to
determine the calibration requirements and precision of this standard. This ILS indicated benzoic acid is not suitable for
calibration. Pure substances other than those listed in Table 1 can be used for calibration provided the substances meet
the purity and calibration requirements of this standard.
2 © ISO 2008 – All rights reserved
DRAFT 2009
---------------------- Page: 7 ----------------------
ISO/DIS 29541
5.6 Certified reference materials
Certified reference material (CRM) coal(s) with a certified composition and uncertainty for carbon, hydrogen
and nitrogen may be used as a check to monitor changes in instrument response that 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 change during storage, coals shall not be used for calibration.
6 Apparatus
Analytical instrument
An instrument capable of analysing a test portion of 6 mg or greater. It includes a furnace capable of
maintaining a temperature in the range to ensure quantitative recovery of carbon, hydrogen and nitrogen as
their corresponding gases (CO , H O, N /NO ). The combustion gases or a representative aliquot shall be
2 2 2 X
treated to remove or convert any components that can interfere with the measurement of carbon dioxide,
water vapour or nitrogen (produced by the reduction of NO prior to measurement). The detection system shall
x
include provisions for evaluation of the response in a manner that correlates accurately with the carbon
dioxide, water vapour and nitrogen present in the treated combustion gases.
NOTE Coal contains constituents that can affect the performance of chemicals used to ensure the consistent and
uniform conversion and recovery of carbon, hydrogen and nitrogen.
Balance
A stand-alone balance or a balance integrated with the instrument, with a resolution of a least 0,1% relative of
the test portion to be weighed.
7 Preparation of the test sample
The sample shall be the general analysis sample prepared to a nominal top size of 212 μm using ISO 13909-6,
ISO 18283 or ISO 5069-2. Sample 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 lignites. Alternatively the test sample
and reference material shall be dried prior to analysis.
8 Procedure
8.1 Instrument set-up
Verify all instrument operation parameters meet the specifications in the instrument operating manual. Verify
the condition and quantity of all chemicals currently in use in the instrument to ensure they are satisfactory for
the number of samples to be analysed. Instruments that employ gas to open and close valves shall use extra
dry gas for this purpose. 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 to establish carbon, hydrogen and nitrogen levels in the combustion and carrier gases.
The level of nitrogen in these gases shall not exceed 1% of the instrument nitrog
...
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