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GB/T 476-2008 English PDF (GBT476-2008)
GB/T 476-2008 English PDF (GBT476-2008)
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GB/T 476-2008: Determination of carbon and hydrogen in coal
GB/T 476-2008
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 73.040
D 21
Replacing GB/T 476-2001, GB/T 15460-2003, GB/T 18856.11-2002
Determination of carbon and hydrogen in coal
(ISO 625:1996, Solid mineral fuels - Determination of carbon and hydrogen -
Liebig method, MOD)
ISSUED ON: JULY 29, 2008
IMPLEMENTED ON: MAY 01, 2009
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of PRC;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative references ... 5
3 Three-stage furnace method and two-stage furnace method ... 5
4 Coulometric-gravimetric method ... 16
5 Method precision ... 24
6 Test report ... 25
Appendix A (Informative) Comparison of clause numbers between this standard
and ISO 625:1996 ... 26
Appendix B (Informative) The technical differences between the chapter
numbers of this standard and ISO 625:1996 and their reasons ... 27
Determination of carbon and hydrogen in coal
1 Scope
This standard specifies the method principles, reagents and materials, devices,
test procedures, result calculation, precision, etc., of the three-stage furnace
method, two-stage furnace method, electricity consumption method, for the
determination of the hydrogen in the coal and coal-water slurry dried coal
sample, AND the weight method for the determination of carbon, in the carbon
and hydrogen analysis of coal and coal-water slurry.
This standard applies to lignite, bituminous coal, anthracite, coal-water slurry.
2 Normative references
The provisions in following documents become the provisions of this Standard
through reference in this Standard. For the dated references, the subsequent
amendments (excluding corrections) or revisions do not apply to this Standard;
however, parties who reach an agreement based on this Standard are
encouraged to study if the latest versions of these documents are applicable.
For undated references, the latest edition of the referenced document applies.
GB/T 212 Proximate analysis of coal (GB/T 212-2008, ISO 11722:1999, ISO
1171:1997, ISO 562:1998, NEQ)
GB/T 218 Determination of carbon dioxide content in the mineral carbonates
associated with coal (GB/T 218-1996, eqv ISO 925:1980)
GB/T 18856.1 Test methods for quality of coal water mixture - Part 1:
Sampling for coal water mixture
3 Three-stage furnace method and two-stage furnace
method
3.1 Method principle
A certain amount of coal sample OR coal-water slurry dried coal sample is
burned in an oxygen flow; the generated water and carbon dioxide are
absorbed by a water absorbent and a carbon dioxide absorbent, respectively;
the mass fraction of carbon and hydrogen, in the coal, is calculated from the
increase of the absorbent. The interference of sulfur and chlorine, in coal
samples, on carbon determination, is eliminated by lead chromate and silver
wire coils, in the three-stage furnace; it is eliminated by the pyrolysis product of
silver permanganate, in the two-stage furnace. The interference of nitrogen on
carbon determination, is eliminated by granular manganese dioxide.
3.2 Reagents and materials
3.2.1 Anhydrous magnesium perchlorate: Analytically pure, which has a particle
size of 1 mm ~ 3 mm. OR anhydrous calcium chloride: Analytically pure, which
has a particle size of 2 mm ~ 5 mm.
3.2.2 Granular manganese dioxide: Chemically pure, which is commercially
available or prepared from manganese sulfate and potassium permanganate.
Preparation method: Weigh 25 g of manganese sulfate. Dissolve it in 500 mL
of distilled water. Weigh another 16.4 g of potassium permanganate. Dissolve
in 300 mL of distilled water. The two solutions are heated to 50 °C ~ 60 °C,
respectively. Slowly pour the potassium permanganate solution, into the
manganese sulfate solution, with constant stirring. Vigorously stir it. Then add
10 mL of (1 + 1) sulfuric acid. Heat the solution to 70 °C ~ 80 °C. Continue to
stir for another 5 min. Stop heating. Let it stand for 2 h ~ 3 h. Use hot distilled
water, to pour-wash it to neutrality. Move the precipitate into a funnel for
filtration, to remove moisture. Then place it in a drying oven, for drying, at about
150 °C, for 2 h ~ 3 h, to obtain brown, loose manganese dioxide. Carefully crush
and sieve it, to obtain a particle size of 0.5 mm ~ 2 mm, for later use.
3.2.3 Copper wire coil: The wire diameter is about 0.5 mm. Copper wire mesh:
0.15 mm (100 mesh).
3.2.4 Copper oxide: Chemically pure, linear (about 5 mm in length).
3.2.5 Lead chromate: Analytically pure, which is prepared to a particle size of 1
mm ~ 4 mm.
Preparation method: Use distilled water, to mix commercially available lead
chromate into a paste. Extrude to shape it. Put it in a muffle furnace. Burn it at
850 °C, for 2 h. Take it out. Cool it, for later use.
3.2.6 Silver wire coil: The wire diameter is about 0.25 mm.
3.2.7 Oxygen: 99.9%, without hydrogen. Oxygen cylinders need to be equipped
with a pressure gauge, which has a pressure reducing valve with adjustable
flow (medical oxygen inhalers can be used).
3.2.8 Tungsten trioxide: Analytically pure.
3.2.9 Soda asbestos: Chemically pure, which has a particle size of 1 mm ~ 2
Figure 1 -- Schematic diagram of the carbon and hydrogen analyzers by
three-segment furnaces and two-stage furnaces
3.3.1.1 Purification system, including the following components:
a) Gas drying tower: Capacity 500 mL, 2 units, the upper part (about 2/3) of
one unit (A) is filled with anhydrous calcium chloride (or anhydrous
magnesium perchlorate), the lower part (about 1/3) is filled with alkali
asbestos (or soda lime); another one unit (B) is filled with anhydrous
calcium chloride (or anhydrous magnesium perchlorate);
b) Flowmeter: Measuring range (0 ~ 150) mL/min.
3.3.1.2 Combustion device: It consists of a three-stage (or two-stage) pipe
furnace and its temperature control system, mainly including the following
components:
a) Electric furnace: three-stage furnace or two-stage furnace (double-pipe
furnace or single-pipe furnace); the diameter of the furnace is about 35
mm.
Three-stage furnace: The first stage is about 230 mm long, which can be
heated to (850 ± 10) °C, AND can move in the horizontal direction; the
second stage is 330 mm ~ 350 mm long, which can be heated to (800 ±
10) °C; the third stage is 130 mm ~ 150 mm long, which can be heated to
(600 ± 10) °C.
Two-stage furnace: The first stage is about 230 mm long, which can be
heated to (850 ± 10) °C, AND can move in the horizontal direction; the
second stage is 130 mm ~ 150 mm long, which can be heated to (500 ±
10) °C.
Each stage of the furnace is equipped with thermocouples, temperature
measurement, temperature control devices.
b) Combustion pipe: It is made of bisque, quartz, corundum or stainless steel,
which is about 1100 mm ~ 1200 mm in length (about 800 mm in length
when using a two-stage furnace), has an inner diameter of 20 mm ~ 22
mm, AND a wall thickness of about 2 mm.
c) Burning boat: It is made of bisque or quartz, at about 80 mm long.
d) Rubber stopper or rubber cap (preferably with heat-resistant silicone
rubber) or copper joint.
e) Nickel-chromium wire hook: It is about 2 mm in diameter AND about 700
mm in length; one end is bent into a hook.
Connect the containers of the absorption system, which is prepared in
accordance with the requirements of 4.3.5, in the order as shown in ...
Get QUOTATION in 1-minute: Click GB/T 476-2008
Historical versions: GB/T 476-2008
Preview True-PDF (Reload/Scroll if blank)
GB/T 476-2008: Determination of carbon and hydrogen in coal
GB/T 476-2008
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 73.040
D 21
Replacing GB/T 476-2001, GB/T 15460-2003, GB/T 18856.11-2002
Determination of carbon and hydrogen in coal
(ISO 625:1996, Solid mineral fuels - Determination of carbon and hydrogen -
Liebig method, MOD)
ISSUED ON: JULY 29, 2008
IMPLEMENTED ON: MAY 01, 2009
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of PRC;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative references ... 5
3 Three-stage furnace method and two-stage furnace method ... 5
4 Coulometric-gravimetric method ... 16
5 Method precision ... 24
6 Test report ... 25
Appendix A (Informative) Comparison of clause numbers between this standard
and ISO 625:1996 ... 26
Appendix B (Informative) The technical differences between the chapter
numbers of this standard and ISO 625:1996 and their reasons ... 27
Determination of carbon and hydrogen in coal
1 Scope
This standard specifies the method principles, reagents and materials, devices,
test procedures, result calculation, precision, etc., of the three-stage furnace
method, two-stage furnace method, electricity consumption method, for the
determination of the hydrogen in the coal and coal-water slurry dried coal
sample, AND the weight method for the determination of carbon, in the carbon
and hydrogen analysis of coal and coal-water slurry.
This standard applies to lignite, bituminous coal, anthracite, coal-water slurry.
2 Normative references
The provisions in following documents become the provisions of this Standard
through reference in this Standard. For the dated references, the subsequent
amendments (excluding corrections) or revisions do not apply to this Standard;
however, parties who reach an agreement based on this Standard are
encouraged to study if the latest versions of these documents are applicable.
For undated references, the latest edition of the referenced document applies.
GB/T 212 Proximate analysis of coal (GB/T 212-2008, ISO 11722:1999, ISO
1171:1997, ISO 562:1998, NEQ)
GB/T 218 Determination of carbon dioxide content in the mineral carbonates
associated with coal (GB/T 218-1996, eqv ISO 925:1980)
GB/T 18856.1 Test methods for quality of coal water mixture - Part 1:
Sampling for coal water mixture
3 Three-stage furnace method and two-stage furnace
method
3.1 Method principle
A certain amount of coal sample OR coal-water slurry dried coal sample is
burned in an oxygen flow; the generated water and carbon dioxide are
absorbed by a water absorbent and a carbon dioxide absorbent, respectively;
the mass fraction of carbon and hydrogen, in the coal, is calculated from the
increase of the absorbent. The interference of sulfur and chlorine, in coal
samples, on carbon determination, is eliminated by lead chromate and silver
wire coils, in the three-stage furnace; it is eliminated by the pyrolysis product of
silver permanganate, in the two-stage furnace. The interference of nitrogen on
carbon determination, is eliminated by granular manganese dioxide.
3.2 Reagents and materials
3.2.1 Anhydrous magnesium perchlorate: Analytically pure, which has a particle
size of 1 mm ~ 3 mm. OR anhydrous calcium chloride: Analytically pure, which
has a particle size of 2 mm ~ 5 mm.
3.2.2 Granular manganese dioxide: Chemically pure, which is commercially
available or prepared from manganese sulfate and potassium permanganate.
Preparation method: Weigh 25 g of manganese sulfate. Dissolve it in 500 mL
of distilled water. Weigh another 16.4 g of potassium permanganate. Dissolve
in 300 mL of distilled water. The two solutions are heated to 50 °C ~ 60 °C,
respectively. Slowly pour the potassium permanganate solution, into the
manganese sulfate solution, with constant stirring. Vigorously stir it. Then add
10 mL of (1 + 1) sulfuric acid. Heat the solution to 70 °C ~ 80 °C. Continue to
stir for another 5 min. Stop heating. Let it stand for 2 h ~ 3 h. Use hot distilled
water, to pour-wash it to neutrality. Move the precipitate into a funnel for
filtration, to remove moisture. Then place it in a drying oven, for drying, at about
150 °C, for 2 h ~ 3 h, to obtain brown, loose manganese dioxide. Carefully crush
and sieve it, to obtain a particle size of 0.5 mm ~ 2 mm, for later use.
3.2.3 Copper wire coil: The wire diameter is about 0.5 mm. Copper wire mesh:
0.15 mm (100 mesh).
3.2.4 Copper oxide: Chemically pure, linear (about 5 mm in length).
3.2.5 Lead chromate: Analytically pure, which is prepared to a particle size of 1
mm ~ 4 mm.
Preparation method: Use distilled water, to mix commercially available lead
chromate into a paste. Extrude to shape it. Put it in a muffle furnace. Burn it at
850 °C, for 2 h. Take it out. Cool it, for later use.
3.2.6 Silver wire coil: The wire diameter is about 0.25 mm.
3.2.7 Oxygen: 99.9%, without hydrogen. Oxygen cylinders need to be equipped
with a pressure gauge, which has a pressure reducing valve with adjustable
flow (medical oxygen inhalers can be used).
3.2.8 Tungsten trioxide: Analytically pure.
3.2.9 Soda asbestos: Chemically pure, which has a particle size of 1 mm ~ 2
Figure 1 -- Schematic diagram of the carbon and hydrogen analyzers by
three-segment furnaces and two-stage furnaces
3.3.1.1 Purification system, including the following components:
a) Gas drying tower: Capacity 500 mL, 2 units, the upper part (about 2/3) of
one unit (A) is filled with anhydrous calcium chloride (or anhydrous
magnesium perchlorate), the lower part (about 1/3) is filled with alkali
asbestos (or soda lime); another one unit (B) is filled with anhydrous
calcium chloride (or anhydrous magnesium perchlorate);
b) Flowmeter: Measuring range (0 ~ 150) mL/min.
3.3.1.2 Combustion device: It consists of a three-stage (or two-stage) pipe
furnace and its temperature control system, mainly including the following
components:
a) Electric furnace: three-stage furnace or two-stage furnace (double-pipe
furnace or single-pipe furnace); the diameter of the furnace is about 35
mm.
Three-stage furnace: The first stage is about 230 mm long, which can be
heated to (850 ± 10) °C, AND can move in the horizontal direction; the
second stage is 330 mm ~ 350 mm long, which can be heated to (800 ±
10) °C; the third stage is 130 mm ~ 150 mm long, which can be heated to
(600 ± 10) °C.
Two-stage furnace: The first stage is about 230 mm long, which can be
heated to (850 ± 10) °C, AND can move in the horizontal direction; the
second stage is 130 mm ~ 150 mm long, which can be heated to (500 ±
10) °C.
Each stage of the furnace is equipped with thermocouples, temperature
measurement, temperature control devices.
b) Combustion pipe: It is made of bisque, quartz, corundum or stainless steel,
which is about 1100 mm ~ 1200 mm in length (about 800 mm in length
when using a two-stage furnace), has an inner diameter of 20 mm ~ 22
mm, AND a wall thickness of about 2 mm.
c) Burning boat: It is made of bisque or quartz, at about 80 mm long.
d) Rubber stopper or rubber cap (preferably with heat-resistant silicone
rubber) or copper joint.
e) Nickel-chromium wire hook: It is about 2 mm in diameter AND about 700
mm in length; one end is bent into a hook.
Connect the containers of the absorption system, which is prepared in
accordance with the requirements of 4.3.5, in the order as shown in ...
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