GB/T 3058-2019 PDF English
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| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
| GB/T 3058-2019 | English | 165 |
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Determination of arsenic in coal
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| GB/T 3058-2008 | English | 85 |
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Determination of arsenic in coal
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| GB/T 3058-1996 | English | 359 |
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Determination of arsenic in coal
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| GB/T 3058-1982 | English | RFQ |
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Determination of arsenic in coal
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GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 73.040
D 21
Replacing GB/T 3058-2008
Determination of arsenic in coal
(ISO 11723.2016, Solid mineral fuels - Determination of arsenic and selenium
- Eschka's mixture and hydride generation method, NEQ)
Issued on. JUNE 04, 2019
Implemented on. JANUARY 01, 2020
Issued by. State Administration for Market Regulation;
Standardization Administration of PRC.
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative references... 4
3 Arsenic molybdenum blue spectrophotometry... 4
4 Hydride generation-atomic absorption method... 9
5 Precision... 14
6 Test report... 14
Appendix A (Informative) Recovery rate of arsenic measuring device... 15
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard replaces GB/T 3058-2008 "Method for the determination of
arsenic in coal". As compared with GB/T 3058-2008, except for editorial
changes, the main technical changes are as follows.
- In the method summary, CHANGE that "use hydrochloric acid to dissolve
the burnt" into that "use sulfuric acid and hydrochloric acid to dissolve the
burnt" (see 3.1; 3.1 of the 2008 edition);
- MODIFY the requirements for arsenic-free zinc particles (see 3.2.1; 3.2.1
of the 2008 edition);
- ADD the placement position of lead acetate cotton to the diagram of the
arsenic determination device (see Figure 1; Figure 1 of the 2008 edition);
- ADD the calculation method of the recovery rate of the arsenic
determination device by the arsenic molybdenum blue spectrophotometric
method (see Appendix A).
This standard is prepared by using the redrafting method with reference to ISO
11723.2016 "Solid mineral fuels - Determination of arsenic and selenium -
Eschka's mixture and hydride generation method". The degree of consistency
with ISO 11723.2016 is nonequivalent.
This standard was proposed by the China Coal Industry Association.
This standard shall be under the jurisdiction of the National Coal
Standardization Technical Committee (SAC/TC 42).
Drafting organization of this standard. Testing Branch of Coal Science and
Technology Research Institute Co., Ltd.
Drafters of this standard. Chen Huizhu, Fu Kun, Yang Guang, Yang Huayu.
This standard replaces the standard previously issued as follows.
- GB/T 3058-1982, GB/T 3058-1996, GB/T 3058-2008.
Determination of arsenic in coal
1 Scope
This standard specifies the method summary, reagents and materials,
instruments and equipment, samples, test procedures, calculation and
presentation of results, the precision of the method for the determination of
arsenic in coal by arsenic molybdenum blue spectrophotometry and hydride
generation-atomic absorption method. Arsenic molybdenum blue
spectrophotometry is the arbitration method.
This standard applies to lignite, bituminous coal, anthracite.
2 Normative references
The following documents are essential to the application of this document. For
the dated documents, only the versions with the dates indicated are applicable
to this document; for the undated documents, only the latest version (including
all the amendments) is applicable to this standard.
GB/T 483 General rules for analytical and testing methods of coal
GB/T 2304 Chemical reagent - Zinc granular free from arsenic
3 Arsenic molybdenum blue spectrophotometry
3.1 Method summary
The coal sample is mixed with Eschka reagent and burned. The burned material
is dissolved with hydrochloric acid and sulfuric acid. A reducing agent is added
to reduce pentavalent arsenic to trivalent arsenic. Add zinc particles to form and
release arsenic hydride gas. Use iodine solution to absorb and oxidize it to
arsenic acid. Add ammonium molybdate-hydrazine sulfate solution to produce
arsenic molybdenum blue. Then use a spectrophotometer to determine it.
3.2 Reagents and materials
Unless otherwise specified, only use reagents and distilled or deionized water
or equivalent purity water confirmed to be analytically pure in the analysis.
3.2.1 Arsenic-free zinc metal. In accordance with GB/T 2304, screen out zinc
particles with a particle size of not less than 3 mm for use.
3.2.2 Eschka reagent (hereinafter referred to as Aldrin). Commercially available,
or 2 parts by mass of light magnesium oxide and 1 part by mass of anhydrous
sodium carbonate are mixed and ground to a particle size of less than 0.2 mm,
then stored in a closed container.
3.2.3 Hydrochloric acid. The relative density is 1.18.
3.2.4 Hydrochloric acid solution. c(HCl) = 6 mol/L. Mix 1 volume of hydrochloric
acid with 1 volume of water evenly.
3.2.5 Sulfuric acid solution. c(1/2 H2SO4) = 6 mol/L. Measure 167 mL of sulfuric
acid with a relative density of 1.84 and slowly add it to an appropriate amount
of water. Stir it while adding. Then use water to dilute it to 1 L.
3.2.6 Sulfuric acid solution. c (1/2 H2SO4) = 5 mol/L. Measure 139 mL of sulfuric
acid with a relative density of 1.84 and slowly add it to an appropriate amount
of water. Stir it while adding. Then use water to dilute it to 1 L.
3.2.7 Potassium iodide solution. 176.5 g/L. Dissolve 3.0 g of potassium iodide
in 17 mL water and prepare it before use.
3.2.8 Stannous chloride hydrochloric acid solution. 666.7 g/L. Dissolve 8.0 g of
stannous chloride in 12 mL of hydrochloric acid (3.2.3) and prepare it before
use.
3.2.9 Iodine solution. 1.5 g/L. After using a small amount of water to dissolve
9.0 g of potassium iodide and 1.5 g of iodine. Dilute it to 1 L.
3.2.10 Ammonium molybdate solution. 10 g/L. Dissolve 10.0 g of ammonium
molybdate in 1 L sulfuric acid solution (3.2.6).
3.2.11 Hydrazine sulfate solution. 1.2 g/L. Dissolve 1.2 g of hydrazine sulfate in
1 L of water.
3.2.12 Ammonium molybdate-hydrazine sulfate mixed solution. Mix 1 volume
of ammonium molybdate solution (3.2.10) and 1 volume of hydrazine sulfate
solution (3.2.11) evenly. Prepare it before use.
3.2.17 Lead acetate cotton. It is replaced each time of the experiment. The
absorbent cotton is fully soaked in a lead acetate solution which has a mass
concentration of 400 g/L. Take it out and twist it dry. Dry it at 80 °C ~100 °C.
Store it in a desiccator for later use.
3.2.18 Porcelain crucible. The capacity is 30 mL. The enamel on the inner
surface is intact.
3.3 Instrument and equipment
3.5 Test procedure
3.5.1 Drawing of working curve
3.5.1.1 Respectively use the single marking line pipette to take 0.00 mL, 1.00
mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL of arsenic standard working solution
(3.2.16). Place it into the round flask of the arsenic determination device. First
add 10 mL of sulfuric acid solution (3.2.5). Then add 20 mL of hydrochloric acid
solution (3.2.4). Use water to dilute it to 50 mL.
3.5.1.2 Add 2 mL of potassium iodide solution (3.2.7), 1 mL of stannous chloride
solution (3.2.8). Shake it uniformly. Place it at room temperature for 15 min.
3.5.1.3 Use a pipette to add 3 mL of iodine solution (3.2.9), 1 mL of sodium
bicarbonate solution (3.2.13), 6 mL of water to the absorber of the arsenic
determination device. Insert the absorber into the absorber casing which
contains lead acetate cotton (3.2.17).
abscissa and the corresponding absorbance as the ordinate. Proceed it
simultaneously with the analysis of the coal sample.
3.5.2 Sample determination
3.5.2.1 Weigh 2 g of aldrin agent in a porcelain crucible (accurate to 0.01 g).
Then weigh 0.99 g ~ 1.01 g (accurate to 0.0002 g) of coal sample for general
analysis test which has a particle size of less than 0.2 mm. Use a glass rod to
stir it uniformly. Then use 1 g (accurate to 0.01 g) of Aldrin to evenly cover the
mixed coal sample (no black coal particles can be seen). When the ash content
in the coal sample is greater than 40%, or the arsenic content is greater than
50 μg/g or the total sulfur content is greater than 8%, the sample weight is 0.50
g.
3.5.2.5 Determine the absorbance of the sample blank solution and the sample
solution according to the method specified in 3.5.1.6.Check the corresponding
arsenic mass [micrograms (μg)] from the drawn working curve (3.5.1.7).
3.6 Calculation and expression of results
3.6.1 Result calculation
4 Hydride generation-atomic absorption method
4.1 Method summary
The coal sample is mixed with aldrin and burned. The burned material is
dissolved by hydrochloric acid. The pentavalent arsenic is reduced to trivalent
arsenic by potassium iodide.
4.2 Reagents and materials
Unless otherwise specified, only use reagents and distilled or deionized water
or equivalent purity water confirmed to be analytically pure in the analysis.
4.2.1 Aldrin. Same as 3.2.2.
4.2.2 Hydrochloric acid. Same as 3.2.3.
4.2.3 Sodium hydroxide solution. 5 g/L. Weigh 5.0 g of sodium hydroxide and
dissolve it in 1 L of water.
4.2.10 Nitrogen. Purity above 99.9%.
4.2.11 Porcelain crucible. Same as 3.2.18.
4.2.12 Porcelain evaporating dish. The capacity is 100 mL. The enamel on the
inner surface is intact.
4.3 Instrument and equipment
4.3.1 Atomic absorption spectrophotometer. It has the functions of absorption
peak area integration and peak height measurement.
4.3.2 Hydride generator. It can automatically wash and measure liquid, which
has an accuracy of 0.5%.
4.3.3 Light source. Arsenic hollow cathode lamp or arsenic electrodeless
discharge lamp.
4.3.4 Muffle furnace. Same as 3.3.3.
4.3.5 Analytical balance. Same as 3.3.4.
4.3.6 Balance. The division value is 0.01 g.
4.4 Sample
The sample is the same as 3.4.
4.5 Test procedure
4.5.1 Preparation of sample solution
4.5.2 Preparation of blank solution
4.5.4 Hydride generation-atomic absorption determination
4.5.4.1 Instrument preparation
Install the atomizer of the hydride generator on the burner of the atomic
absorption spectrophotometer according to the instrument instructions, so that
the quartz tube is located directly above the burner slit. Adjust the up and down,
front and rear positions and rotation angle of the burner, to make the axis of the
quartz tube coincide with the main optical axis of the atomic absorption
spectrophotometer. Connect the gas path.
4.5.4.2 Selection of working parameters of atomic absorption
spectrophotometer
The parameter selection is as follows.
4.6 Calculation and expression of results
4.6.1 Result calculation
The arsenic content (mass fraction) in the air-dried coal sample is calculated
according to formula (2).
5 Precision
The precision of the determination of arsenic content in coal is specified in Table
1.
6 Test report
The test report shall include at least the following information.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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