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ls 15441 :2004
ISO 625:1996
Indian Standard
SOLID MINERAL FUELS DETERMINATION OF
CARBON AND HYDROGEN LIEBIG METHOD
..
Ics 73.040
@ BIS 2004
BUREAU
MANAK
OF
BHAVAN,
IN DIANSTAN
9 BAHADUR
NEW DELHI
March 2004
m-
II
SHAH
DAR
ZAFAR
DS
MARG
110002
Price Group 7
1-
PCD 7
NATIONAL FOREWORD
This Indian Standard which is identical with ISO 625:1996 Solid mineral fuels Determination of carbon
and hydrozen Liebig method issued by the International Organization for Standardization
(ISO) was
adopted by the Bureau of Indian Standards on the recommendations
of the Solid Mineral Fuels Sectional
Committee and approval of the Petroleum, Coal and Related Products Division Council.
The text of ISO Standard has been proposed to be approved as suitable for publication as an Indian Standard
without deviations. Certain conventions are, however, not identical to those used in Indian Standards. Attention
is particularly drawn to the following:
a)
b)
Comma (,) has been used as a decimal marker, while in Indian Standards,
use a point (.) as the decimal marker.
Technical Corrigendum
In this adopted standard reference appears to certain International Standards for which Indian Standards
also exist. The corresponding Indian Standards which are to be substituted in their places are listed below
along with their degree of equivalence for the editions indicated. However, that International Standard
cross-referred in this adopted ISO Standard which has subsequently been revised, position in respect of
latest ISO Standard has been given:
International
Standard
Corresponding
Indian Standard
Degree of
Equivalence
Direct
analysis
gravimetric method
Technically
not equivalent
do
Determination
of
carbon
content
carbonate
Gravimetric method
do
Determinaand
tion of moisture
content
Direct volumetric method
to different
bases
analyses
Nil
Identical
(Continued
on third cover)
IS
ISO
15441
:2004
625:1996
Indian Standard
SOLID MINERAL FUELS DETERMINATION OF
CARBON AND HYDROGEN LIEBIG METHOD
Scope
This International Standard specifies a method of determining the total carbon and the total hydrogen in
hard coal, brown coal and lignite, and coke, by the
Liebig method.
The results include the carbon in the carbonates and
the hydrogen combined in the moisture and in the
water of constitution
of silicates. A determination
of
moisture is carried out at the same time, and an appropriate correction is applied to the hydrogen value
obtained by combustion.
A determination
of carbon
dioxide may also be made and the total carbon value
corrected for the presence of mineral carbonates.
Normative references
ISO 1170:1977,
Coal and coke Calculation
analyses to different bases.
ISO 1988:1975,
ISO 2309:1980,
Coke Sampling.
ISO 331:1983,
of moisture in
of
ISO 5068:1983, Brown coals and /ignites Determination of moisture content Indirect gravimetric
method.
Brown coals and /ignites Principles of sampling Part 2: Sample preparation for
determination of moisture content and for general
analysis.
LSO 5069-2:1983,
The following
standards contain provisions which,
through reference in this text, constitute
provisions
of this International
Standard. At the time of publication, the editions indicated were valid. All standards
are subject to revision, and parties to agreements
based on this International Standard are encouraged
to investigate the possibility of applying the most recent editions
of the standards
indicated
below.
Members of IEC and ISO maintain registers of currently valid International Standards.
ISO 1015:1992, Brown coals and /ignites Determination of moisture content Direct volumetric
method.
Principle
IS
ISO
15441
:2004
625:1996
dioxide,
granular,
1,2 mm
a)
magnesium
b)
c)
magnesium
perchlorate
evolved in the reaction
and sodium hydroxide.
5.3
Combustion assembly
a)
b)
c)
1 mm
5.3.2
Combustion tube, of fused silica or suitable
hard glass. The diameter of the tube shall be 12 mm
to 15 mm. A suitable length is 1,25 m.
5.3.3
Combustion boat, of platinum,
fused silica, approximately 70 mm long.
porcelain
or
a)
4.9
water;
Dissolve manganese
sulfate in water and boil the
solution. Make the solution alkaline with ammonium
hydroxide and add solid ammonium
persulfate,
in
small portions, to the boiling solution until precipitation is complete. Filter through a hardened fast-filter
paper, wash with water by recantation,
then with dilute sulfuric acid and finally with water until acid-free.
Transfer the moist precipitate to a morlar and place in
an oven until most of the water has evaporated, but
the powder is still damp. Press the mass into a cake
with a pestle, using firm pressure. Complete the drying, break up the cake cautiously and sieve to separate the 1,2 mm to 0,7 mm size.
approximately
perchlorate
to
to the
Apparatus
Glass wool.
..
.-,
.*
IS
ISO
b)
granular manganese
oxides of nitrogen;
dioxide
c)
magnesium
perchlorate for absorbing
evolved from the manganese dioxide;
15441
:2004
625:1996
manganese
dioxide, which is contained
in a guard
tube (figure 2), providing a long contact time with
minimum mass.
the water
d)
e)
magnesium
perchlorate for absorbing the water
pro~uced in the reaction between carbon dioxide
and sodium hydroxide.
Dimensions in millimetres
Indicator spot ..
0 ext. 5,5 to 6
Hollow stopper
n
-.
0
+
n
v
--
25
0) ext. 33 to 34
~,,tod
&
<
.
.*.,....
IS
ISO
15441
:2004
625:1996
\
b
ml
:1
--
m
.
0
4
.
Mangan
Figure
2 Guadtube
..
.,
Dimensions in millimetres
Is
15441
:2004
ISO 625:1996
Key
perchlorate,
Magnesium
Glass wool
Manganese
Inlet
dioxide
NOTE In this illustration the optional second carbon dioxide absorber, E, is shown
Figure
Stoppered
U-tubes
may be used,
if preferred,
3 Absorption train
in place
di-
oxide.
f
If water is condensed in the first absorber, some nitrogen dioxide may dissolve in it and be considered
as water. Because of the conversion
factor from
water to hydrogen, the error in the hydrogen determination thus caused is small, in the order of 0,05 %0
of hydrogen. This can only be avoided by heating the
absorption tube to a temperature
that is sufficiently
high to prevent condensation of water.
NOTE 1
Oxides of nitrogen formed in the combustion
would, in the absence of precautions, be absorbed by the
sodium hydroxide and measured as carbon dioxide. The error in the carbon determination thus caused, in the order of
0,2 % of carbon, is substantially avoided by the use of a
guard tube (see figure 2) in which the gases pass through
an annular space to allow oxidation of nitrogen monoxide to
stopper
5.6 Heat-resistant
(acrylonitrile
or
chloroprene) for connecting the absorption train to the
combustion tube.
5.7
IS
15441
ISO
:2004
625:1996
6.1
Preparation
of the combustion
tube
For a combustion
tube 1,25 mm long and 12 mm to
15 mm in diameter, the following arrangement of the
spacing is suitable:
is shown
stopper
(5.6).
in figure 4.
NOTE 2
The copper gauze spiral and rolls are oxidized
during the preliminary heating in a current of oxygen.
6.2
Condtiioningthe combustiontube
by a copper
boat (5.3.3);
50 mm space to prevent the front of the boat being heated too soon;
occupied
by a plug
(4.6);
roll of the
copper
gauze;
fibre
to
prevent
6.3
Condtiioningthe absorptiontrain
n
-.
a
c
z
InLet
Stopper
11
80
Copper
gauze
spiral
Space
Space
50
rl~
Coppergauze roll \
Sample
boat
70
Final position
300
1
I
Furnace 1
Initial pasition
,-------+}
1
t
Copperoxide
450
II
Furnace 2
.---L.
;:::::~
..
100
:~:ergauz~s
100
Furnace 3
-.
3
IS
15441
ISO
:2004
625:1996
Prepare the test sample for general analysis in accordance with ISO 1988, ISO 2309 or ISO 5069-2, as
appropriate.
Ensure that the moisture content of the
sample is in equilibrium
with the laboratory atmosphere, exposing it, if necessaty, in a thin layer for the
minimum time to achieve equilibrium.
Before commencing
mix the test sample
mechanical means.
Carefully inspect the ash in the boat for unburnt carbon; if present, this invalidates the determination,
which shall then be repeated.
Particular care must be taken during the combustion
of brown coals and Iignites, since heating too rapidly
could result in incomplete combustion.
the determination,
thoroughly
for at least 1 rein, preferably by
NOTES
4 Two hours are usually sufficient to complete the combustion of coal samples and 1 h may be sufficient for most
coke samples.
After weighing the test portion (see clause 8), determine the moisture content using a further portion of
the test sample by the method described in ISO 331,
ISO 687, ISO 1015 or ISO 5068, as appropriate.
A
further portion should be set aside if the determination of carbon dioxide (ISO 925) is required.
Procedure
When
raise
starting
the
the
first
temperatures
determination
of
the
of each
furnaces
(5.3.1)
Blank test
day,
to
Expression of results
10
10.1
Total carboncontent
The total carbon content, Wc, of the sample as anaIysed, expressed as a percentage by mass, is given
by the equation
Wc = 27,29
X :1%
where
After combustion
is complete,
switch off furnace
No. 1, allow the exit end of the combustion tube to
cool and disconnect the absorption train. Wipe ab-
ml
a..
-.
IS
ISO
10.2
0,2729
625:1996
as a percentage
by
WH,=WH0,1119M
where M is the moisture content, expressed
percentage by mass, in the sample as analysed.
10.5
Total hydrogen
content
:2004
as a
Wq
where WC02 is the carbon dioxide content of the mineral carbonates in the sample as analysed (determined
according
to ISO 925), expressed
as a
percentage by mass.
10.3
15441
Additional
information
d;lms
11
Precision
where
11.1 Repeatabili~limit
ml
m4
11.2 Reproducibility
10.4
Total hydrogen
present as moisture
The total hydrogen
content,
less that present as
moisture, WH, (organic hydrogen plus that present in
the water of constitution of the mineral matter), of the
critical difference
Table 1
Element
Reproducibilitycritical difference
Carbon
0,25 % absolute
0,5 % absolute
Hydrogen
0,12 Yo absolute
IS
15441
:2004
ISO
625:1996
12
Test report
the method
Standard;
used by reference
b)
the identification
d)
e)
any operation
not included in this
Standard, or regarded as optional;
f)
information:
to this International
10
.,
*,&
..-
International
IS
15441
:2004
1S() 625:1996
Annex A
(informative)
General
Symbol
Hence
27,29
Wc =
Table A.1
Element
X (~
Relativeatomicmass
A.3
Carbon
12,011
Hydrogen
1,008
Oxygen
15,999
WH=
[H20]
A.2
Wc=
~)
ml
[c]x(~-mJx
loo
[co~] x m,
WH, in the
test
x 100
x ml
where
ml
m4
where
Hence
ml
11,19x
(m4nkJ
ml
11
.... .
IS
ISO
15441
:2004
625:1996
CORRIGENDUM
Technical Corrigendum 1 to International Standard ISO 625:1996 was prepared by Technical Committee
Solid mineral fue/s, Subcommittee
SC 5, Methods of arra/ysis.
to 1,25 m in line 2.
to 1,25 m in line 1.
Page 8, clause 8
Delete (see note 5) in lines 14 and 15 of the second paragraph.
Transfer the last paragraph before the notes to the second paragraph, before the final sentence.
Change (see note 7) to (see note 5) in the last line of the third paragraph.
...-.
lSO/TC 27,
IS
ISO
15441
Change B and C to D and E in the fourth and sixth lines after the equation.
Page 10, subclause 10.4
Page 11, clause A.3
Change formula to equation
Page 5 figure 3
Replace figure 3 by the following:
f
iii
-43
3
Key
Manganese
Inlet
Glass wool
dioxide
NOTE In this illustration the optional second carbon dioxide absorber, E, is shown,
:2004
625:1996
(Continued
International
ISO
1988
Standard
: 1975
Hard
Corresponding
Indian Standard
coal
Sampling
for sampling
1) :1964
of coal
Methods
and coke:
Sampling
of coal, Section
sampling
(revised )
Degree of
Equivalence
Part 1
1 Manual
ISO
1988
cover
2309
Coke
1980
Iignites
moisture
gravimetric
and
moisture
general
Sampling
of coke
and
Methods
coke:
of
Part 2
whereas
mechanical
covered
under ISO 13909 (Parts 1-8)
IS 436
(Part l/See 1) and
IS 436
(Part 2) are being
revised to align with corresponding ISO Standards
have
been
Nil
Indirect
method
:1983
Iignites
preparation
coals
of coal
and
Determination
content
ISO 5069-2
sampling
Brown
2309
sampling.
These
ISO
Standards
are
being
revised
to
cover
manual
sampling
ISO
ISO
mechanical
manual
sampling
Sampling
and
both
Part
Brown
Principles
2 :
coals
of
Sample
for determination
of
and
for
content
analysis
Nil
The Technical Committee responsible for the preparation of this standard will review the provisions of ISO
331, ISO 687, ISO 925, 1S0 1015, ISO 1170, ISO 1988, ISO 2309, ISO 5068 and ISO 5069-2 and will
decide whether they are acceptable for use in conjunction with this standard.
In reporting the results of a test or analysis, made in accordance with this standard, if the final value,
observed or calculated, is to be rounded off, it shall be done in accordance with IS 2 : 1960 Rules for
rounding off numerical values (revised).
..
,.,-.
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tions. Enquiries elating to copyright be addressed to the Director (Publications),
BIS.
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