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BS 1016-106.4.1:
1993
BS 1016-106.4.1:1993
Date
Comments
BS 1016-106.4.1:1993
Contents
Committees responsible
Foreword
Introduction
1 Scope
2 References
3 Principle
4 Reagents
5 Apparatus
6 Preparation of test sample
7 Procedure
8 Expression of results
9 Precision
10 Test report
Annex A (informative) Derivation of factors used in the
expression of results
Table 1 Test portion for coal
Table A.1 Relative atomic masses
List of references
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Inside front cover
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Inside back cover
BS 1016-106.4.1:1993
Foreword
This Subsection of BS 1016 has been prepared under the direction of the Solid
Mineral Fuels Standards Policy Committee. Part 106 will form a revision of
Part 6 to Part 11 of BS 1016. This Subsection supersedes 8.2 in both
BS 1016-6:1977 and BS 1016-7:1977 which are to be deleted by amendment, from
which the principle changes are as follows.
a) When charging the crucible, some of the 4 g of Eschka mixture is now used
to form a bottom layer in the crucible.
b) A further alternative means, using a Gooch crucible, of filtering the solution
after precipitation of the barium sulfate has been added.
Part 106 is a further Part numbered under a scheme for rationalizing and
restructuring BS 1016. The new series, when complete, will begin with Part 100,
which will include a general introduction. The current Parts are as follows, with
the new Part numbers (which will be given to revisions when they are published)
in parentheses.
Part 1: Total moisture of coal (Part 101);
Part 2: Total moisture of coke (Part 102);
Part 6: Ultimate analysis of coal (Part 106);
Part 7: Ultimate analysis of coke (Part 106);
Part 8: Chlorine in coal and coke (Part 106);
Part 9: Phosphorus in coal and coke (Part 106);
Part 10: Arsenic in coal and coke (Part 106);
Part 11: Forms of sulphur in coal (Part 106);
Part 14: Analysis of coal ash and coke ash (Part 114);
Part 15: Fusibility of coal ash and coke ash (Part 113);
Part 16: Methods of reporting results (Part 100);
Part 17: Size analysis of coal (Part 109);
Part 18: Size analysis of coke (Part 110);
Part 20: Determination of Hardgrove grindability index of hard coal
(Part 112);
Part 21: Determination of moisture-holding capacity of hard coal (Part 103).
The following Parts in the new series have been published.
Part 104: Proximate analysis;
Part 105: Determination of gross calorific value;
Part 107: Caking and swelling properties of coal;
Part 108: Tests special to coke;
Part 111: Determination of abrasion index of coal.
Part 106 will be divided into a number of Sections and Subsections, including the
following.
Section 106.1: Determination of carbon and hydrogen content;
Section 106.2: Determination of nitrogen content;
Section 106.3: Determination of oxygen content;
Section 106.4: Determination of total sulfur content;
Subsection 106.4.1: Eschka method;
Subsection 106.4.2: High temperature combustion method;
Section 106.5: Determination of forms of sulfur;
Section 106.6: Determination of chlorine content;
Subsection 106.6.1: Eschka method;
Subsection 106.6.2: High temperature combustion method;
ii
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BS 1016-106.4.1:1993
Summary of pages
This document comprises a front cover, an inside front cover, pages i to iv,
pages 1 to 6, an inside back cover and a back cover.
This standard has been updated (see copyright date) and may have had
amendments incorporated. This will be indicated in the amendment table on the
inside front cover.
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iii
iv
blank
BS 1016-106.4.1:1993
Introduction
An alternative reference method to that specified in
this Subsection of BS 1016 is given in 8.3 of
BS 1016-6:1977 and 8.3 of BS 1016-7:1977.
Instrumental methods for a more rapid
determination of total sulfur are now available. If
such a method is to be used, it is important to
demonstrate that the method is free from bias, when
compared to this reference method, and will give
levels of repeatability and reproducibility which are
the same as, or better than, those quoted for the
reference method (see clause 9).
1 Scope
This Subsection of BS 1016 specifies a reference
method for determining the total sulfur content of
hard coal and coke by the Eschka method.
2 References
2.1 Normative references
This British Standard incorporates, by reference,
provisions from specific editions of other
publications. These normative references are cited
at the appropriate points in the text and the
publications are listed on the inside back cover.
Subsequent amendments to, or revisions of, any of
these publications apply to this British Standard
only when incorporated in it by updating or revision.
2.2 Informative references
This British Standard refers to other publications
that provide information or guidance. Editions of
these publications current at the time of issue of this
standard are listed on the inside back cover, but
reference should be made to the latest editions.
3 Principle
A test portion is ignited in intimate contact with
Eschka mixture in an oxidizing atmosphere, to
remove combustible matter and to convert the
sulfur to sulfate. This is then extracted with
hydrochloric acid solution and determined
gravimetrically by precipitation with barium
chloride.
4 Reagents
WARNING. Care should be exercised when
handling the reagents, many of which are
toxic and corrosive.
NOTE During the analysis, unless otherwise stated, use only
reagents of recognized analytical grade and only distilled water
or water of equivalent purity.
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5 Apparatus
5.1 Analytical balance, capable of weighing to the
nearest 0.1 mg.
5.2 Graduated glassware, conforming to the
requirements for class A in the appropriate British
Standards.
5.3 Electrically heated muffle furnace, capable of
being maintained at a temperature
of 800 C 25 C. The ventilation through the
muffle furnace shall be such as to give about 5 air
changes per minute.
5.4 Crucible, of platinum, silica or glazed porcelain,
of capacity approximately 25 ml.
5.5 Flat plate, 6 mm thick, of silica (or other suitable
refractory material), which fits easily into the
muffle furnace (5.3).
5.6 Gooch crucible, of glazed porcelain or sintered
glass.
5.7 Air oven, capable of being maintained at a
temperature of 130 C 10 C.
BS 1016-106.4.1:1993
7 Procedure
% (m/m)
<5
5 to 10
> 10
1.0
0.5
0.25
7.5 Extraction
Place a watch-glass on the beaker and then, while
tilting the watch-glass, carefully add enough
hydrochloric acid (4.2) to dissolve the solid
matter (17 ml will normally be required), warming
the contents of the beaker to effect solution. Boil
for 5 min to expel carbon dioxide and filter,
collecting the filtrate in a 400 ml conical beaker.
NOTE A medium-textured, doubly acid-washed filter-paper or
a filter-paper pad is recommended for speed of filtration.
To prepare the filter-paper pad, shake doubly acid-washed
filter-paper clippings, in pieces with areas of
approximately 1 cm2, with water in a bottle until the paper is
thoroughly disintegrated. Place a porcelain filter cone of 25 mm
diameter in a 75 mm funnel, close the stem of the funnel with a
finger and add water until the cone is immersed and the funnel
stem is full. Shake, onto the cone, sufficient paper pulp to form a
pad 5 mm thick, and level it with a fiat-ended glass rod. Allow the
excess water to drain away by removing the finger from the stem
and as drainage ceases, lightly tamp the pad round the edges
with the glass rod. A final wash with water renders the filter
ready for use.
7.3 Ignition
7.3.1 For coal
Place the charged crucible (and any others up to the
limit of the muffle furnace capacity) in the cold
muffle furnace (5.3) and raise the temperature
to 800 C 25 C in about 1 h, maintaining this
temperature for at least a further 1.5 h. Withdrawn
the crucible (or crucibles) and allow to cool.
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BS 1016-106.4.1:1993
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8 Expression of results
The sulfur content, ws, of the sample, expressed as a
percentage by mass, is given by the equation
where
m1
m2
m3
k
2so4
9 Precision
9.1 Repeatability limit
The results of duplicate determinations, carried out
at different times, in the same laboratory, by the
same operator with the same apparatus on
representative portions taken from the same test
sample, should not differ by more than 0.05 %
absolute.
9.2 Reproducibility critical difference
The means of the results of duplicate
determinations, carried out in each of two
laboratories on representative portions taken from
the same sample after the last stage of sample
preparation, should not differ by more than 0.1 %
absolute, at a 95 % confidence level.
BS 1016-106.4.1:1993
10 Test report
The test report shall include the following
particulars:
a) the identification of the sample;
b) the method used, i.e. BS 1016-106.4.1:1993;
c) the date of the test;
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BS 1016-106.4.1:1993
Annex A (informative)
Derivation of factors used in the expression of results
In this annex, relative atomic masses and relative molecular masses are represented by the chemical
formulae in square brackets. The relative atomic masses given in Table A.1 were used in the calculations.
Table A.1 Relative atomic masses
Element
Symbol
Barium
Ba
137.33
Oxygen
15.999
Potassium
39.098
Sulfur
32.06
The mass, expressed in grams, of barium sulfate equivalent to 25 ml of potassium sulfate solution is given
by the formula
where k
2so 4
is the mass concentration, expressed in grams per litre, of the potassium sulfate solution.
Thus, the sulfur content ws of the sample, expressed as a percentage by mass, is given by the equation
where
m1 is the mass, expressed in grams, of the test portion.;
m2 is the mass, expressed in grams, of barium sulfate found in the determination;
m3 is the mass, expressed in grams, of barium sulfate found in the blank test.
Hence
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BS 1016-106.4.1:1993
Informative references
BSI standards publications
BRITISH STANDARDS INSTITUTION, London
ISO 334:1992, Solid mineral fuels Determination of total sulfur Eschka method1).
ISO 1015:1992, Brown coals and lignites Determination of moisture content Direct volumetric
method1).
ISO 5068:1983, Brown coals and lignites Determination of moisture content Indirect gravimetric
method1).
ISO 5069-2:1983, Brown coals and lignites Principles of sampling Part 2: Sample preparation for
determination of moisture content and for general analysis1).
Other references
[1] GREAT BRITAIN. Health and Safety at Work etc. Act 1974. London: HMSO
[2] GREAT BRITAIN. Control of Substances Hazardous to Health Regulations, 1988. London: HMSO
1) Referred
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BS 1016-106.4.1:
1993
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