SIST ISO 609:1998

SLOVENSKI STANDARD
SIST ISO 609:1998
01-februar-1998
7UGQDIRVLOQDJRULYD'RORþHYDQMHRJOMLNDLQYRGLND0HWRGD]JRUHYDQMDSULYLVRNL
WHPSHUDWXUL
Solid mineral fuels -- Determination of carbon and hydrogen -- High temperature
combustion method
Combustibles minéraux solides -- Dosage du carbone et de l'hydrogène -- Méthode par
combustion à haute température
Ta slovenski standard je istoveten z: ISO 609:1996
ICS:
73.040 Premogi Coals
75.160.10 Trda goriva Solid fuels
SIST ISO 609:1998 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST ISO 609:1998

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SIST ISO 609:1998
I N T E R NAT I O NA L
IS0
STANDARD
609
Second edition
1996-02-1 5
Solid mineral fuels - Determination of
carbon and hydrogen - High temperature
combustion method
Combustibles minéraux solides - Dosage du carbone et de
l'hydrogène - Méthode par combustion à haute température
Reference number
IS0 609:1996(E)

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SIST ISO 609:1998
IS0 609:1996(E)
Foreword
IS0 (the International Organization for Standardization) is a worldwide
federation of national standards bodies (IS0 member bodies). The work
of preparing International Standards is normally carried out through IS0
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. IS0
collaborates closely with the International Electrotechnical Commission
(IEC) on all matters of electrotechnical standardization.
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.
!nternational Standard IS0 609 was prepared by Technical Committee
ISOflC 27, Solid mineral fuels, Subcommittee SC 5, Methods of
analysis.
This second edition cancels and replaces the first edition (IS0 609:1975),
which has been technically revised.
Annex A of this International Standard is for information only.
0 IS0 1996
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
inicrofilm, without permission in writing from the publisher
International Organization for Standardization
Case Postale 56 CH-1 21 1 Genève 20 Switzerland
Printed in Switzerland
II

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Q IS0
SIST ISO 609:1998
IS0 609:1996(E)
Introduction
An alternative method to that specified in this International Standard is
given in IS0 625: 1996, Solid mineral fuels - Determination of carbon and
hydrogen - Liebig method.
...
Ill

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SIST ISO 609:1998

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SIST ISO 609:1998
INTERNATIONAL STANDARD 0 IS0
IS0 609:1996(E)
Solid mineral fuels - Determination of carbon and
hydrogen - High temperature combustion method
IS0 1 O1 5:1992, Brown coals and lignites - Determi-
1 Scope
- Direct volumetric
nation of moisture content
method.
This International Standard specifies a method of de-
termining the total carbon and the total hydrogen in
IS0 1170:1977, Coal and coke - Calculation of
hard coal, brown coal and lignite, and coke, by a high
analyses to different bases.
temperature combustion method.
IS0 1988:1975, Hard coal - Sampling.
The results include the carbon in the carbonates and
the hydrogen combined in the moisture and in the
IS0 2309:1980, Coke -- Sampling.
of constitution of silicates. A determination of
water
at the same time, and an ap-
moisture is carried out
IS0 5068:1983, Brown coals and lignites - Determi-
propriate correction is applied to the hydrogen value
nation of moisture content - Indirect gravimetric
obtained by combustion. A determination of carbon
method.
dioxide may also be made and the total carbon value
corrected for the Dresence of mineral carbonates.
IS0 5069-2:1983, Brown coals and lignites - Prin-
- Part 2: Sample preparation for
ciples of sampling
determination of moisture content and for general
analysis.
2 Normative references
3 Principle
4
The following standards contain provisions which,
A known mass of coal or coke is burnt in a stream of
through reference in this text, constitute provisions
oxygen, at a temperature of 1 350 OC, in a tube
of this International Standard. At the time of publi-
impervious to gases. All the hydrogen is converted to
cation, the editions indicated were valid. All standards
water and all the carbon to carbon dioxide. These
are subject to revision, and parties to agreements
products are absorbed by suitable reagents and de-
based on this International Standard are encouraged
termined gravimetrically. The chlorine and oxides of
to investigate the possibility of applying the most re-
sulfur which are formed are retained by a silver gauze
cent editions of the standards indicated below.
roll at the outlet end of the tube.
Members of IEC and IS0 maintain registers of cur-
rently valid International Standards.
4 Reagents and materials
IS0 331:1983, Coal - Determination of moisture in
WARNING - Care should be exercised when
the analysis sample - Direct gravimetric method.
handling reagents, many of which are toxic and
corrosive.
IS0 687:1974, Coke - Determination of moisture in
the analysis sample.
During the analysis, unless otherwise stated, use only
reagents of recognized analytical grade and only dis-
IS0 925:1980, Solid mineral fuels - Determination
tilled water or water of equivalent purity.
of carbon dioxide content - Gravimetric method.
1

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SIST ISO 609:1998
Q IS0
IS0 609:1996(E)
4.1 Magnesium perchlorate, anhydrous, less than 4.9 Air, compressed.
1,2 mm in size and preferably within the size range
1,2 mm to 0,7 mm.
4.10 Glass wool.
WARNING - Due regard must be taken of local
5 Apparatus
regulations when disposing of exhausted mag-
nesium perchlorate. Regeneration of magnesium
5.1 Analytical balance, capable of weighing to the
perchlorate must not be attempted, owing to the
nearest 0,l mg.
risk of explosion.
5.2 Graduated glassware, conforming to the re-
4.2 Sodium hydroxide on an inert base, preferably
quirements for class A in the International Standards
of a coarse grading, for example 3,O mm to 1,5 mm,
prepared by ISO/TC 48, Laboratory glassware and re-
but not finer than the grading 1,2 mm to 0,7 mm, and
la ted apparat us.
preferably of the self-indicating type.
5.3 Two purification trains, one for absorbing
water vapour and carbon dioxide from the oxygen
4.3 Aluminium oxide (alumina), finely divided, ap-
used for the combustion and the other for similarly
proximately 0,l mm in size.
treating the air used for sweeping out the absorption
train before and after a determination. Assemble each
4.4 Sodium tetraborate, standard volumetric sol-
train using a series of U-tubes or Midvale tubes con-
ution, c(Na2B,0,) = 0,025 mol/l.
taining the following reagents in the order stated, in
the direction of flow:
2 g of sodium tetraborate decahydrate
Dissolve 9,534
in water and dilute to 1 litre. Mix thoroughly.
a) magnesium perchlorate (4.1) for absorbing water;
4.5 Hydrogen peroxide, approximately 30 % (dm).
b) sodium hydroxide on an inert base (4.2) for ab-
sorbing dioxide;
4.6 Pure silver gauze, of mesh approximately
c) magnesium perchlorate for absorbing the water
1 mm, made of wire approximately 0,3 mm in diam-
evolved in the reaction between carbon dioxide
eter.
and sodium hydroxide.
The purification trains shall be large enough to render
4.7 Oxygen, hydrogen-free, preferably prepared
frequent recharging unnecessary, even with continu-
from liquid air and not by electrolysis. Electrolytically
ous use.
prepared oxygen shall be passed over red-hot copper
oxide before use to remove any trace of hydrogen.
NOTE 1 Midvale tubes that have been freshly packed
with absorbent and used in the purification train are thereby
4.8 Mixed indicator solution
conditioned for subsequent use in the absorption train.
5.4 Combustion assembly
4.8.1 Solution A
Dissolve O, 125 g of 2-(4-dimethylaminophenyl-
5.4.1 Heating unit, an electrically heated furnace or
azo)benzoic acid, sodium salt (methyl red) in 100 ml
furnaces, designed to carry a combustion tube (5.4.2)
of water.
and heat it to 1 350 "C over a distance of 125 mm in
the hot zone, and yield a temperature-distribution
profile similar to that shown in figure 1. The heating
4.8.2 Solution B
unit normally requires an auxiliary furnace to ensure
Dissolve 0,083 g of 3,7-bis(dimethylamino)pheno-
that the silver gauze roll (5.9) is maintained at the
thiazine-5-ylium chloride (methylene blue) in 1 O0 ml
correct temperature (approximately 600 "C to
of water. Store in a dark bottle.
800 OC). Suitable furnaces are, for example:
a) molybdenum or tungsten wire wound;
4.8.3 Mixed solution
b) platinum or platinum-rhodium wire wound;
Mix equal volumes of solution A and solution B. Store
in a dark bottle. Discard the mixed solution after
c) heated by silicon carbide rods.
1 week.
2

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SIST ISO 609:1998
INTERNATIONAL STANDARD 0 IS0
IS0 609:1996(E)
Solid mineral fuels - Determination of carbon and
hydrogen - High temperature combustion method
IS0 1 O1 5:1992, Brown coals and lignites - Determi-
1 Scope
- Direct volumetric
nation of moisture content
method.
This International Standard specifies a method of de-
termining the total carbon and the total hydrogen in
IS0 1170:1977, Coal and coke - Calculation of
hard coal, brown coal and lignite, and coke, by a high
analyses to different bases.
temperature combustion method.
IS0 1988:1975, Hard coal - Sampling.
The results include the carbon in the carbonates and
the hydrogen combined in the moisture and in the
IS0 2309:1980, Coke -- Sampling.
of constitution of silicates. A determination of
water
at the same time, and an ap-
moisture is carried out
IS0 5068:1983, Brown coals and lignites - Determi-
propriate correction is applied to the hydrogen value
nation of moisture content - Indirect gravimetric
obtained by combustion. A determination of carbon
method.
dioxide may also be made and the total carbon value
corrected for the Dresence of mineral carbonates.
IS0 5069-2:1983, Brown coals and lignites - Prin-
- Part 2: Sample preparation for
ciples of sampling
determination of moisture content and for general
analysis.
2 Normative references
3 Principle
4
The following standards contain provisions which,
A known mass of coal or coke is burnt in a stream of
through reference in this text, constitute provisions
oxygen, at a temperature of 1 350 OC, in a tube
of this International Standard. At the time of publi-
impervious to gases. All the hydrogen is converted to
cation, the editions indicated were valid. All standards
water and all the carbon to carbon dioxide. These
are subject to revision, and parties to agreements
products are absorbed by suitable reagents and de-
based on this International Standard are encouraged
termined gravimetrically. The chlorine and oxides of
to investigate the possibility of applying the most re-
sulfur which are formed are retained by a silver gauze
cent editions of the standards indicated below.
roll at the outlet end of the tube.
Members of IEC and IS0 maintain registers of cur-
rently valid International Standards.
4 Reagents and materials
IS0 331:1983, Coal - Determination of moisture in
WARNING - Care should be exercised when
the analysis sample - Direct gravimetric method.
handling reagents, many of which are toxic and
corrosive.
IS0 687:1974, Coke - Determination of moisture in
the analysis sample.
During the analysis, unless otherwise stated, use only
reagents of recognized analytical grade and only dis-
IS0 925:1980, Solid mineral fuels - Determination
tilled water or water of equivalent purity.
of carbon dioxide content - Gravimetric method.
1

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S
6IST ISO 609:1998
Q IS0
IS0 609:1996(E)
4.1 Magnesium perchlorate, anhydrous, less than 4.9 Air, compressed.
1,2 mm in size and preferably within the size range
1,2 mm to 0,7 mm.
4.10 Glass wool.
WARNING - Due regard must be taken of local
5 Apparatus
regulations when disposing of exhausted mag-
nesium perchlorate. Regeneration of magnesium
5.1 Analytical balance, capable of weighing to the
perchlorate must not be attempted, owing to the
nearest 0,l mg.
risk of explosion.
5.2 Graduated glassware, conforming to the re-
4.2 Sodium hydroxide on an inert base, preferably
quirements for class A in the International Standards
of a coarse grading, for example 3,O mm to 1,5 mm,
prepared by ISO/TC 48, Laboratory glassware and re-
but not finer than the grading 1,2 mm to 0,7 mm, and
la ted apparat us.
preferably of the self-indicating type.
5.3 Two purification trains, one for absorbing
water vapour and carbon dioxide from the oxygen
4.3 Aluminium oxide (alumina), finely divided, ap-
used for the combustion and the other for similarly
proximately 0,l mm in size.
treating the air used for sweeping out the absorption
train before and after a determination. Assemble each
4.4 Sodium tetraborate, standard volumetric sol-
train using a series of U-tubes or Midvale tubes con-
ution, c(Na2B,0,) = 0,025 mol/l.
taining the following reagents in the order stated, in
the direction of flow:
2 g of sodium tetraborate decahydrate
Dissolve 9,534
in water and dilute to 1 litre. Mix thoroughly.
a) magnesium perchlorate (4.1) for absorbing water;
4.5 Hydrogen peroxide, approximately 30 % (dm).
b) sodium hydroxide on an inert base (4.2) for ab-
sorbing dioxide;
4.6 Pure silver gauze, of mesh approximately
c) magnesium perchlorate for absorbing the water
1 mm, made of wire approximately 0,3 mm in diam-
evolved in the reaction between carbon dioxide
eter.
and sodium hydroxide.
The purification trains shall be large enough to render
4.7 Oxygen, hydrogen-free, preferably prepared
frequent recharging unnecessary, even with continu-
from liquid air and not by electrolysis. Electrolytically
ous use.
prepared oxygen shall be passed over red-hot copper
oxide before use to remove any trace of hydrogen.
NOTE 1 Midvale tubes that have been freshly packed
with absorbent and used in the purification train are thereby
4.8 Mixed indicator solution
conditioned for subsequent use in the absorption train.
5.4 Combustion assembly
4.8.1 Solution A
Dissolve O, 125 g of 2-(4-dimethylaminophenyl-
5.4.1 Heating unit, an electrically heated furnace or
azo)benzoic acid, sodium salt (methyl red) in 100 ml
furnaces, designed to carry a combustion tube (5.4.2)
of water.
and heat it to 1 350 "C over a distance of 125 mm in
the hot zone, and yield a temperature-distribution
profile similar to that shown in figure 1. The heating
4.8.2 Solution B
unit normally requires an auxiliary furnace to ensure
Dissolve 0,083 g of 3,7-bis(dimethylamino)pheno-
that the silver gauze roll (5.9) is maintained at the
thiazine-5-ylium chloride (methylene blue) in 1 O0 ml
correct temperature (approximately 600 "C to
of water. Store in a dark bottle.
800 OC). Suitable furnaces are, for example:
a) molybdenum or tungsten wire wound;
4.8.3 Mixed solution
b) platinum or platinum-rhodium wire wound;
Mix equal volumes of solution A and solution B. Store
in a dark bottle. Discard the mixed solution after
c) heated by silicon carbide rods.
1 week.
2

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SIST ISO 609:1998
Q IS0 IS0 609:1996(E)
O
4-
3-
Key
1 Glass wool 3 Magnesium perchlorate, 1,2 mm to 0,7 mm size
2 Sodium hydroxide (see 4.2)
4
...