GB/T 3286.9-2014 PDF English
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Method for chemical analysis of limestone and dolomite - Part 9: The determination of carbon dioxide content - The caustic asbestos absorption gravimetric method
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| GB/T 3286.9-1998 | English | RFQ |
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Methods for chemical analysis of limestone and dolomite--The determination of carbon dioxide content
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| GB/T 3286.9-1982 | English | RFQ |
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Chemical analysis of limestone and dolomite--The soda asbestos absorption-gravimetric method for determination of carbon dioxide
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PDF Preview: GB/T 3286.9-2014
GB/T 3286.9-2014: PDF in English (GBT 3286.9-2014) GB/T 3286.9-2014
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 73.080
D 52
Replacing GB/T 3286.9-1998
Method for Chemical Analysis of Limestone and Dolomite -
Part 9.The Determination of Carbon Dioxide Content - The
Caustic Asbestos Absorption Gravimetric Method
ISSUED ON. JUNE 9, 2014
IMPLEMENTED ON. JANUARY 1, 2015
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine of the People’s Republic of China;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword... 3
1 Scope... 5
2 Normative References... 5
3 Principle... 5
4 Reagents... 6
5 Instruments and Devices... 6
6 Specimen Preparation... 9
7 Analysis Steps... 10
7.1 Number of Determinations... 10
7.2 Amount of Test Portion... 10
7.3 Inspection of Instruments and Devices... 10
7.4 Calibration of Instruments and Devices... 10
7.5 Determination... 10
8 Calculation and Expression of Analysis Results... 12
8.1 Calculation of Analysis Results... 12
8.2 Determination and Expression of Analysis Results... 12
9 Allowable Differences... 12
10 Test Report... 13
Appendix A (normative) Flow Chart of Specimen Analysis Results Acceptance
Procedures... 14
Appendix B (informative) Determination of Carbon Dioxide Content in Metallurgical
Lime Using Combustion Gas Volumetric Method... 15
Appendix C (informative) Temperature and Pressure Correction Coefficient Table... 22
Method for Chemical Analysis of Limestone and Dolomite -
Part 9.The Determination of Carbon Dioxide Content - The
Caustic Asbestos Absorption Gravimetric Method
WARNING. the personnel using this Part shall have practical experience in formal
laboratory work. This Part does not address all possible safety issues. It is the users’
responsibility to take appropriate safety and health measures and ensure the compliance
with the conditions stipulated in relevant national regulations.
1 Scope
This Part of GB/T 3286 specifies the determination of carbon dioxide content through the
caustic asbestos absorption gravimetric method.
This Part is applicable to the determination of carbon dioxide content in limestone and dolomite,
and also to the determination of carbon dioxide content in metallurgical lime. The determination
range (mass fraction) in limestone and dolomite. carbon dioxide content 30% ~ 50%; the
determination range (mass fraction) in metallurgical lime. carbon dioxide content greater than
0.50%.
2 Normative References
The following documents are indispensable to the application of this document. In terms of
references with a specified date, only versions with a specified date are applicable to this
document. In terms of references without a specified date, the latest version (including all the
modifications) is applicable to this document.
GB/T 2007.2 General Rules for the Sampling and Sample Preparation of Minerals in Bulk -
Manual Method for Sample Preparation
GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods
GB/T 8170 Rules of Rounding off for Numerical Values & Expression and Judgment of
Limiting Values
3 Principle
The test portion is decomposed with phosphoric acid, and dry air with carbon dioxide removed
is used as the carrier gas. The generated carbon dioxide is absorbed by caustic asbestos. In
accordance with the increased mass, calculate the carbon dioxide content.
The moisture generated during the decomposition of the test portion is absorbed by sulfuric
acid and magnesium perchlorate, and the hydrogen sulfide generated from the sulfide is
absorbed and removed by chromium trioxide sulfuric acid solution.
4 Reagents
4.1 Unless it is otherwise stated, only approved analytically pure reagents and above Grade-3
distilled water complying with the stipulations of GB/T 6682 or equivalent water shall be used
in the analysis.
4.2 Soda lime.
4.3 Caustic asbestos, with a particle size of 0.5 mm ~ 1 mm.
4.4 Anhydrous magnesium perchlorate, with a particle size of 0.5 mm ~ 1 mm; dry in a drying
oven at 180 C for 2 hours, quickly transfer to a desiccator, cool and set aside.
NOTE. used magnesium perchlorate can be re-used after drying.
4.5 Anhydrous calcium chloride.
4.6 High-purity calcium carbonate, not lower than 99.99%.
4.7 Dehydrated sulfuric acid. place sulfuric acid (ρ = 1.84 g/mL) in a beaker, heat until it emits
smoke, and maintain for a while, let it slightly cool, then, carefully place in a desiccator, cool
and set aside.
4.8 Phosphoric acid, 1 + 1.
4.9 Chromium trioxide sulfuric acid solution, 10 g/L.
Take 1 g of chromium trioxide in a beaker, add 1 mL of water, add 100 mL of sulfuric acid (ρ
= 1.84 g/mL) to dissolve it, and evenly mix it.
5 Instruments and Devices
The device for measuring carbon dioxide is shown in Figure 1.
5.9 Gas washing bottle (9 in Figure 1), containing chromium trioxide sulfuric acid solution
(4.9).
5.10 Gas washing bottle (10 in Figure 1), containing dehydrated sulfuric acid (4.7), meanwhile,
the speed of bubble generation can be observed.
5.11 U-shaped tube (11 in Figure 1, with side tube and glass piston, 13 mm 100 mm), filled
with anhydrous magnesium perchlorate (4.4).
5.12 Carbon dioxide absorbing U-shaped tube (12 in Figure 1, and the specifications are the
same as the U-shaped tube (5.11)), containing no less than 8 g of caustic asbestos (4.3) and
about 2 g of anhydrous magnesium perchlorate (4.4). The filling method is shown in Figure 2.
NOTE. this carbon dioxide absorbing U-shaped tube can be replaced by an absorption bottle (see
Figure 3 for specifications). The lower part of the bottle is filled with about 40 mm high
caustic asbestos (4.3), and the upper part is filled with 10 mm high anhydrous magnesium
perchlorate (4.4), and a small amount of absorbent cotton is spread in the middle and upper
part.
5.13 Drying tower (13 in Figure 1). the lower part contains anhydrous calcium chloride (4.5),
the upper part contains soda lime (4.2), separated by absorbent cotton in the middle.
5.14 Gas washing bottle (14 in Figure 1), containing water.
5.15 Water flow suction tube (15 in Figure 1), connected to the faucet.
5.16 All parts of the device are connected with rubber hoses of appropriate length as shown in
Figure 1, and each device is fixed with corresponding clamps.
6 Specimen Preparation
6.1 In accordance with GB/T 2007.2, prepare the specimens.
6.2 The specimens shall be processed until the particle size is less than 0.125 mm.
6.3 Before analysis, the limestone and dolomite specimens shall be dried at 105 C ~ 110 C
for 2 hours and placed in a desiccator to cool to room temperature.
6.4 The preparation of metallurgical lime specimens shall be promptly carried out. After
preparation, the specimens shall be immediately sealed in ground bottles or plastic bags and
stored in a desiccator. Before analysis, the specimens shall not be dried.
7 Analysis Steps
7.1 Number of Determinations
For the same specimen (6.3 or 6.4), conduct at least two independent determinations.
7.2 Amount of Test Portion
For limestone and dolomite specimens, weigh-take 0.50 g of test portion, accurate to 0.0001 g.
For metallurgical lime, the test portion shall be quickly weighed. When the carbon dioxide
content is less than 10.0%, weigh-take 2.0 g of test portion. When it is greater than 10.0%,
weigh-take 1.0 g of test portion, accurate to 0.0001 g.
7.3 Inspection of Instruments and Devices
7.3.1 Before the inspection, all spring clips and pistons in the determination system are in an
open state, except C, which is closed.
7.3.2 Open the air extraction water gate and control the water flow speed to stabilize the air
flow rate of the measurement system at around 200 mL/min.
7.3.3 After adjusting the piston, maintain the air flow rate at about 180 mL/min. Close A and
hold for several minutes. At this time, the buttles in the gas washing bottle (5.10) and gas
washing bottle (5.14) shall gradually decrease, until they disappear. Otherwise, it suggests that
there is air leakage in the determination system. If there is air leakage, check it section by
section to identify the leakage location and deal with it, until the entire system is tight and air-
proof.
7.4 Calibration of Instruments and Devices
The calibration of instruments and devices is performed in accordance with 7.5.Weigh-take
0.50 g (accurate to 0.0001 g) of calcium carbonate (4.6) that has been dried at 105 C ~ 110 C
for 2 hours and cooled to room temperature as the test portion. When the determined carbon
dioxide content is within the range of 43.97% 0.35%, it suggests that the determination system
is correct, and that specimen analysis can be performed.
7.5 Determination
7.5.1 Adjust Piston E to control the air flow rate at 170 mL/min ~ 180 mL/min and maintain it
for about 15 min. Close F. After the buttles in the gas washing bottle (5.10) stop, successively
close the pistons of the carbon dioxide absorbing U-shaped tube (5.12) and the U-shaped tube
(5.11) and remove the carbon dioxide absorbing U-shaped tube (5.12). Use clean gauze to
gently wipe it, place it in the balance box for 15 minutes, and weigh it.
NOTE. when the relative humidity of the air is less than 45%, use slightly wet gauze to wipe it, so
as to eliminate the influence of static electricity on the weighing.
7.5.2 Then, connect the carbon dioxide absorbing U-shaped tube (5.12) to the determination
system, and operate in accordance with 7.5.1, until the difference between the two weighings
is not greater than 0.5 mg. Take the last weighed mass as the mass of the U-shaped tube (5.12)
before absorbing carbon dioxide.
7.5.3 Connect the carbon dioxide absorbing U-shaped tube (5.12), close B and D, remove the
sample dissolving conical flask (5.6), transfer the test portion (7.2) to the sample dissolving
conical flask (5.6), and use a small amount of water to rinse the wall of the flask.
7.5.4 Connect the sample dissolving conical flask (5.6) to the determination device and open
the water flow in D and the straight condenser tube (5.7). Add 15 mL of phosphoric acid (4.8)
(for lime specimen, add 30 mL of phosphoric acid to the special-made acid adding tube (5.5)
(TRANSLATOR NOTE. it should be 5.4); slowly open Piston C and add 4 ~ 5 drops of
phosphoric acid (4.8). After the drastic reaction stops, add another 4 ~ 5 drops. Repeat, until the
reaction is completed. Add the remaining acid in the special-made acid adding tube (5.4) to the
sample dissolving conical flask (5.6) (remaining 1 mL ~ 2 mL), add 10 mL of water to the
special-made acid adding tube (5.4), open C, and add water to the sample dissolving conical
flask (5.6), and close C (remaining 1 mL ~ 2 mL of water). Slowly heat the sample dissolving
conical flask (5.6) to boiling and maintain it for 2 minutes, then, turn off the heat source.
7.5.5 Open B, adjust Piston E and maintain the air flow at 170 mL/min ~ 180 mL/min; maintain
ventilation for about 1.5 h.
7.5.6 Close F, wait until the buttles in the gas washing bottle (5.10) stop, successively close the
pistons of the carbon dioxide absorbing U-shaped tube (5.12) and the U-shaped tube (5.11), and
remove the carbon dioxide absorbing U-shaped tube (5.12). Use clean gauze to gently wipe it
(see NOTE in 7.5.1), place it in the balance box for 15 minutes, and weigh it.
7.5.7 Then, connect the carbon dioxide absorbing U-shaped tube (5.12) to the determination
system, open the corresponding piston and spring clip, and re-ventilate for about 20 min. Follow
7.5.6 below, and repeat, until the mass difference between the two weighings is not greater than
0.5 mg. Take the last weighed mass as the mass of the carbon dioxide absorbing U-shaped tube
(5.12).
NOTE 1.all determination processes must be continuously carried out.
NOTE 2.when about 2/3 of the caustic asbestos in the carbon dioxide absorbing U-shaped tube
(5.12) turns white, it shall be replaced by a new U-shaped tube filled with caustic asbestos
in accordance with Figure 2.
7.5.8 After the determination is completed, connect the carbon dioxide absorbing U-shaped tube
(5.12) to the determination system, successively close B, D, G and H, and finally, close the air
extraction water gate to prevent water from flowing back.
Appendix B
(informative)
Determination of Carbon Dioxide Content in Metallurgical Lime Using Combustion Gas
Volumetric Method
B.1 Scope
This Method is applicable to the determination of carbon dioxide in lime that does not contain
organic matter and free carbon. The determination range (mass fraction) is. carbon dioxide
content is greater than 0.50%.
B.2 Principle
The test portion is burned with oxygen in a high-temperature tube furnace, and the carbonate is
decomposed. The generated carbon dioxide and other mixed gases are dried, desulfurized and
collected in a gas measuring tube, and reaches a constant volume. Then, use potassium
hydroxide solution to absorb carbon dioxide in the maxed gases. The difference in gas volume
before and after the absorption is the volume of carbon dioxide, from which, the content of
carbon dioxide is calculated.
B.3 Reagents
B.3.1 Caustic asbestos, with a particle size of 0.5 mm ~ 1 mm.
B.3.2 Anhydrous calcium chloride.
B.3.3 Anhydrous magnesium perchlorate, with a particle size of 0.5 mm ~ 1 mm.
B.3.4 Granular active manganese dioxide (or granular silver vanadate).
B.3.5 Sulfuric acid, ρ = 1.84 g/mL.
B.3.6 Potassium permanganate-potassium hydroxide solution. take 30 g of potassium
hydroxide into 70 mL of saturated potassium permanganate solution.
B.3.7 Potassium hydroxide solution, 400 g/L.
B.3.8 Acidic water. add a few drops of methyl orange solution (0.1 g/100 mL) to 1,000 mL of
sulfuric acid (1 + 1,000). The solution will turn light red and evenly mix it.
B.3.9 Sodium chloride acidic solution, 260 g/L, add a few drops of methyl orange solution (0.1
g/100 mL) and dropwise add sulfuric acid (1 + 1), until it turns light red.
B.4 Instruments and Devices
The device for measuring carbon dioxide is shown in Figure B.1.
B.4.3 Buffer bottle (3 in Figure B.1).
B.4.4 Gas washing bottle (4 in Figure B.1), containing potassium permanganate-potassium
hydroxide solution (B.3.6), and the filling volume accounts for one-third of the height of the
bottle.
B.4.5 Gas washing bottle (5 in Figure B.1), containing sulfuric acid (B.3.1) (TRANSLATOR
NOTE. it should be B.3.5), and the filling volume accounts for one-third of the height of the
bottle.
B.4.6 Drying tower (6 in Figure B.1). the upper layer contains caustic asbestos (B.3.1), the
lower layer contains anhydrous calcium chloride (B.3.2), the middle is separated by glass wool,
and the bottom and top are paved with glass wool.
B.4.7 Oxygen flowing piston (7 in Figure B.1).
B.4.8 Heat-resistant connecting plug (8 in Figure B.1), with side tube, and is connected to the
oxygen flowing piston (B.4.7).
B.4.9 High-temperature tube furnace (9 in Figure B.1), equipped with a thermocouple and
automatic temperature controller (10 in Figure B.1).
B.4.10 Drying tube (11 in Figure B.1), containing anhydrous magnesium perchlorate (B.3.3),
and both ends are paved with glass wool. When the drying capability is reduced, the magnesium
perchlorate shall be replaced in time.
NOTE. the water-absorbing magnesium perchlorate can be re-used after drying in a drying oven at
180 C for 2 hours.
B.4.11 Desulfurization tube (12 in Figure B.1) contains granular active manganese dioxide
(B.3.4), and both ends are paved with glass wool. Granular silver vanadate can be used to
replace granular manganese dioxide.
B.4.12 Caranalyzer (gas volume measuring instrument, 13 in Figure B.1). The caranalyzer shall
be installed at a position 300 mm ~ 500 mm away from the high-temperature tube furnace and
avoid sunlight. The basic components of the caranalyzer are.
a) Condenser tube.
b) Gas measuring tube, containing acidic water (B.3.8) or sodium chloride acidic
solution (B.3.9). The gas measuring tube must be kept clean. If there are water
droplets adhering to the inner wall of the gas measuring tube, the tube must be washed
with chromic acid cleaning solution.
c) Level bottle.
d) Absorber, containing potassium hydroxide solution (B.3.7).
e) Small three-way piston, connecting the condenser tube [B.4.12 a)] and gas measuring
tube [B.4.12 b)]. Or it can respectively connect the condenser tube [B.4.12 a)] or gas
measuring tube [B.4.12 b)] to the atmosphere.
f) Large three-way piston, which allows the air coil to respectively connect to the
condenser tube [B.4.12 a)] or absorber [B.4.12 d)].
B.4.13 Combustion tube (14 in Figure B.1), with a length of 600 mm and an inner diameter of
23 mm. The thick end is connected to the heat-resistant connecting plug (B.4.8), and the tapered
end is connected to the desulfurization tube (B.4.11). During use, firstly, check whether there
is air leakage, then, burn it in sections.
B.4.14 Porcelain boat (15 in Figure B.1), with a length of 88 mm or 97 mm. Before use, burn
it in a tube furnace with oxygen at 1,200 C for 2 min ~ 4 min, or burn it in a high-temperature
furnace at 1,000 C for 1 h. After cooling, store it in an unoiled desiccator containing caustic
asbestos (or soda lime) and anhydrous calcium chloride, and reserve it for later use.
B.4.15 Long hook, made of low-carbon nickel-chromium wire or heat-resistant alloy wire, used
to push and pull out the porcelain boat.
B.4.16 All parts of the device are connected with rubber hoses of appropriate length in
accordance with Figure B.1.
B.5 Specimen Preparation
B.5.1 In accordance with GB/T 2007.2, prepare specimens.
B.5.2 The specimens shall be processed, until the particle size is less than 0.125 mm.
B.5.3 The preparation of metallurgical lime specimens shall be quickly carried out. After
preparation, the specimens shall be immediately sealed in ground bottles or plastic bags and
stored in a desiccator. Before analysis, the specimens shall not be dried.
B.6 Analysis Steps
B.6.1 Number of determinations
For the same specimen (B.5.2 or B.5.3), conduct at least two independent determinations.
B.6.2 Amount of test portion
In accordance with Table B.1, weigh-take test portion, accurate to 0.0001 g. For metallurgical
lime, the test portion shall be quickly weighed.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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