BS ISO 5071-1:2013

BSI Standards Publication

Brown coals and lignites —

Determination of the volatile
matter in the analysis sample
Part 1: Two-furnace method
 BS ISO 5071-1:2013

INTERNATIONAL ISO
STANDARD 5071-1

Second edition
2013-05-01

Brown coals and lignites —

Determination of the volatile matter
in the analysis sample —
Part 1:
Two-furnace method
Charbons bruns et lignites — Détermination des matières volatiles
dans l’échantillon pour analyse —
Partie 1: Méthode avec utilisation de deux fours

Reference number
ISO 5071-1:2013(E)

© ISO 2013
BS ISO 5071-1:2013
ISO 5071-1:2013(E)


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 BS ISO 5071-1:2013
ISO 5071-1:2013(E)


Contents Page

Foreword......................................................................................................................................................................................................................................... iv
Introduction...................................................................................................................................................................................................................................v
1 Scope.................................................................................................................................................................................................................................. 1
2 Normative references....................................................................................................................................................................................... 1
3 Terms and definitions...................................................................................................................................................................................... 1
4 Principle......................................................................................................................................................................................................................... 1
5 Reagents......................................................................................................................................................................................................................... 1
6 Apparatus...................................................................................................................................................................................................................... 2
7 Sample.............................................................................................................................................................................................................................. 6
8 Procedure..................................................................................................................................................................................................................... 6
8.1 Preliminary procedure...................................................................................................................................................................... 6
8.2 Predetermination procedure....................................................................................................................................................... 6
8.3 Method using oven-dried coal.................................................................................................................................................... 6
8.4 Method using air-dried coal......................................................................................................................................................... 6
9 Calculation of results........................................................................................................................................................................................ 6
9.1 For oven-dried coal.............................................................................................................................................................................. 7
9.2 For air-dried coal................................................................................................................................................................................... 7
10 Precision of the method................................................................................................................................................................................. 7
10.1 Repeatability limit................................................................................................................................................................................. 7
10.2 Reproducibility limit........................................................................................................................................................................... 7
11 Test report.................................................................................................................................................................................................................... 8

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BS ISO 5071-1:2013
ISO 5071-1:2013(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 5071-1 was prepared by Technical Committee ISO/TC 27, Solid mineral fuels, Subcommittee SC 5,
Methods of analysis.
This second edition cancels and replaces the first edition (ISO 5071-1:1997), of which this constitutes a
minor revision.
ISO 5071 consists of the following parts, under the general title Brown coals and lignites — Determination
of volatile matter in the analysis sample:
Part 1: Two-furnace method

iv  © ISO 2013 – All rights reserved

 BS ISO 5071-1:2013
ISO 5071-1:2013(E)


Introduction
The volatile matter is determined as the loss in mass, corrected for moisture, when an analysis sample
of brown coal or lignite is heated out of contact with air under specified conditions. The test is empirical
and, in order to obtain reproducible results, it is essential that the rate of heating, the final temperature
and the overall duration of the test be carefully controlled. Due to the nature of brown coals and lignites,
initial heating of the sample at 400 °C is necessary to minimize the possibility of ejection of sample from
the test crucible.
Mineral matter associated with the sample may also lose mass under the conditions of the test, the
magnitude of the loss being dependent on both the nature and the quantity of the minerals present.

© ISO 2013 – All rights reserved  v

BS ISO 5071-1:2013
 BS ISO 5071-1:2013
INTERNATIONAL STANDARD ISO 5071-1:2013(E)

Brown coals and lignites — Determination of the volatile

matter in the analysis sample —
Part 1:
Two-furnace method

1 Scope
This part of ISO 5071 specifies a method of determining the volatile matter of 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 edition of the referenced
document (including any amendments) applies.
ISO 1170, Coal and coke — Calculation of analyses to different bases
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

3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 1213-2 apply.

4 Principle
The coal is heated out of contact with air for 7 min at 400 °C, then immediately transferred to another
furnace and heated at 900 °C for a further 7 min. The percentage of volatile matter is calculated from the
loss in mass of the oven-dried sample or from the loss in mass of the analysis sample corrected for moisture.

5 Reagents

5.1 Desiccants, fresh or freshly regenerated and preferably self-indicating. Suitable desiccants are
magnesium perchlorate, silica gel, activated alumina and anhydrous calcium sulfate.

WARNING — Magnesium perchlorate is a strong oxidizing agent. Do not attempt to regenerate

the absorbent. Do not permit contact with organic materials or reducing agent.

5.2 Nitrogen, dry, with a maximum oxygen content of 30 μl per litre.

© ISO 2013 – All rights reserved  1

BS ISO 5071-1:2013
ISO 5071-1:2013(E)


6 Apparatus

6.1 Furnace (Figure 1), heated by electricity. Two such furnaces are required. One furnace shall have a
zone of 160 mm × 100 mm maintained at a uniform temperature of 400 °C ± 10 °C. The second shall have
a zone of 160 mm × 100 mm maintained at a uniform temperature of 900 °C ± 5 °C. The furnaces may be
the stop-ended type or fitted at the back with a flue approximately 25 mm in diameter by 150 mm long.

The heat capacity of the 900 °C and/or 400 °C furnace shall be such that, with an initial temperature of
900 °C and/or 400 °C, a temperature of 900 °C ± 10 °C and/or 400 °C ± 10 °C is regained within 4 min
after insertion of a cold stand and its crucibles. The temperature shall be measured with a thermocouple
as described in 6.3. The furnace can be designed specifically either for multiple determinations using
a number of crucibles in one stand or for receiving one crucible and its stand. A position for the
crucible stand shall be chosen within the zone of uniform temperature and this position used for all
determinations.

6.2 Oven, capable of being controlled at a temperature within the range 105  °C to 110  °C and with
provision for passing a current of dry, oxygen-free nitrogen through it at a rate sufficient to change the
atmosphere 15 times per hour. The size of the chamber is suitable for containing the crucible (6.4).

6.3 Thermocouple, unsheathed, of wire not thicker than 1  mm, used to check the temperature
characteristics of the furnace. The thermo-junction shall be inserted midway between the base of the
crucible in its stand and the floor of the furnace. 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 with its thermo-junction as close as possible to the centre of the zone
of uniform temperature; in this case, its temperature readings shall be correlated at frequent intervals
with those of the unsheathed thermocouple, which is then inserted only when necessary.
NOTE The temperature/electromotive force relationship of a thermo-junction maintained at elevated
temperatures gradually changes with time.

6.4 Crucible and lid, a cylindrical crucible with a well fitting lid, both made of fused silica. The crucible
and lid shall weigh between 10 g and 14 g and have dimensions approximating those shown in Figure 2.
The fit of the lid on the crucible is critical to the determination and a lid shall be selected to match the
crucible so that the horizontal clearance between them is not 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. Crucibles of other refractory materials, or of platinum, can be used, provided that
they give results which agree with the recommended silica crucible, within the stated precision of the
method (Clause 10).

6.5 Stand, on which the crucible is placed in the muffle furnace, so that the appropriate specified rate
of heating can be achieved. For example, it may consist of the following:

a) for a single determination, a ring of heat-resistant steel wire as shown in Figure 3 a), 27  mm in
diameter and 1,5 mm thick, resting on the inner projection of its legs,
or
b) for multiple determinations, 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.

6.6 Balance, sensitive to 0,1 mg.

6.7 Desiccator.

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 BS ISO 5071-1:2013
ISO 5071-1:2013(E)


Dimensions in millimetres

Key
1 heating system
2 flue
3 thermocouple
a Chamber width is 200 mm.

Figure 1 — Example of a suitable furnace

© ISO 2013 – All rights reserved  3

BS ISO 5071-1:2013
ISO 5071-1:2013(E)


Dimensions in millimetres

Figure 2 — Silica crucible and lid

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 BS ISO 5071-1:2013
ISO 5071-1:2013(E)


Dimensions in millimetres

a) Suitable for a single determination

b) Suitable for multiple determinations

Key
1 three legs spaced 120° apart 3 handle
2 ring 4 ceramic plates

Figure 3 — Crucible stands

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BS ISO 5071-1:2013
ISO 5071-1:2013(E)


7 Sample
Prepare the sample for the determination of volatile matter in the analysis sample in accordance
with ISO 5069-2.

8 Procedure

8.1 Preliminary procedure

Adjust the temperature of the zone in the furnaces (6.1), loaded with a stand and empty crucibles where
appropriate, to 400 °C ± 10 °C and 900 °C ± 5 °C respectively, as indicated by the correctly unsheathed
thermocouple (6.3). Remove the stand and crucibles and close the doors of the furnace. Heat, in a furnace
(6.1) at 900 °C for 7 min, either one crucible and lid (6.4) or the requisite number of crucibles and lids to
fill the multiple stand. Remove the crucible(s) from the furnace and cool them, first on a metal slab and
finally in a desiccator (6.7) located next to the balance. As soon as they are cool, weigh each empty crucible
and lid. Record the mass(es) of the preconditioned crucibles and lids to the nearest 0,1 mg (8.4, Note 1).

8.2 Predetermination procedure

Before commencing the determination, mix the analysis sample for at least 1 min, preferably by
mechanical means. Accurately weigh 1,00 g to 1,01 g of sample (Clause 7) to the nearest 0,1 mg into each
preconditioned crucible. Replace the lid and tap the crucible on a clean hard surface until the sample
forms a layer of even thickness on the bottom of the crucible. Proceed in accordance with either 8.3 or
8.4 depending on whether or not the coal has been oven-dried or air-dried.

8.3 Method using oven-dried coal

Place the charged crucible(s), with lid(s) removed, in the oven (6.2) at 105 °C to 110 °C. Dry the sample(s)
to constant mass in accordance with the procedure for moisture determination specified in ISO 5068-2.
Record the mass(es) of the oven-dried crucible(s), lid(s) and sample(s) to the nearest 0,1 mg.
Place the crucible(s) fitted with lid(s) containing the oven-dried sample(s) in a suitable stand (8.4, Note 2)
and transfer to the furnace set at 400 °C for 7 min. Immediately transfer to the furnace set at 900 °C for
a further 7 min.
Remove the crucible(s) and cool and weigh them in the same manner as for empty crucible(s) (see 8.1). If
ash deposits are visible on the stand or crucible(s) then discard the test and repeat (8.4, Note 3).

8.4 Method using air-dried coal

Place the charged crucible(s) with the lid(s) in a suitable cool stand (Note 2) and transfer to the muffle
furnace set at 400 °C for 7 min. Immediately transfer to the furnace set at 900 °C for a further 7 min.
Remove the crucible(s) and cool and weigh them in the same manner as for the empty crucible(s) (see 8.1).
NOTE 1 Precisely similar treatment of the crucible(s) and lid(s) before and after the determination minimizes
the effect of any film of water absorbed on its surface, while the rapid cooling reduces absorption of moisture by
the coal residue.

NOTE 2 If multiple determinations are being made, fill any vacant places in the stand with empty crucibles.

NOTE 3 Certain brown coals and lignites may consistently produce ash deposits either on the crucible lid or
the sample tray when tested using the two-furnace procedure. In such a case, it is recommended to press the air-
dried sample into small pellets, then determine the volatile matter.

9 Calculation of results
Calculate the percentage by mass of volatile matter on a dry basis, Vd, according to the formulas in 9.1 and 9.2.

6  © ISO 2013 – All rights reserved

 BS ISO 5071-1:2013
ISO 5071-1:2013(E)


9.1 For oven-dried coal

(m2 − m3 )
Vd = 100 ×
m2 − m1
where
m1 is the mass, in grams, of the empty crucible and lid (8.1);

m2 is the mass, in grams,of crucible, lid and oven-dried sample (8.3};

m3 is the mass, in grams, of crucible, lid and sample after heating in the furnace (8.3).

9.2 For air-dried coal

100(m2 − m3 )
Vad = − M ad
m2 − m1

100
Vd = × Vad
100 − M ad
where
m1 is the mass, in grams, of the empty crucible and lid (8.1);

m2 is the mass, in grams, of crucible, lid and air-dried sample (8.2);

m3 is the mass, in grams, of crucible, lid and sample after heating (8.4);

Mad is the moisture content, expressed as a percentage by mass, in the air-dried sample, deter-
mined according to ISO 5068-2;

Vad is the volatile matter on an air-dried basis, expressed as a percentage by mass.

The results (the mean of duplicate determinations) shall be reported to the nearest 0,1 %.
Calculate the results to other bases in accordance with ISO 1170.

10 Precision of the method

10.1 Repeatability limit

The results of duplicate determinations, carried out in the same laboratory by the same operator using
the same apparatus on the same sample within short intervals of time, shall not differ by more than the
value given in Table 1.

10.2 Reproducibility limit

The means of the results of duplicate determinations, carried out in each of two laboratories on
representative test portions taken from the same sample, shall not differ by more than the value given
in Table 1.

Table 1 — Precision of the method

Repeatability Reproducibility
1,0 % absolute 3,0 % absolute

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BS ISO 5071-1:2013
ISO 5071-1:2013(E)


11 Test report
The test report shall include the following information:
a) a reference to this International Standard, including year of publication;
b) the identification of the sample tested;
c) the result of the determination, together with the analysis basis;
d) any unusual features noted during the determination.

8  © ISO 2013 – All rights reserved

BS ISO 5071-1:2013
BS ISO 5071-1:2013
ISO 5071-1:2013(E)


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