GB/T 16659-2024 PDF English
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| GB/T 16659-2024 | English | 340 |
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Determination of mercury of coal
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| GB/T 16659-2008 | English | 70 |
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Determination of mercury in coal
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| GB/T 16659-1996 | English | 279 |
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Determination of mercury in coal
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GB/T 16659-2024: Determination of mercury of coal---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT16659-2024
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 73.040
CCS D 21
Replacing GB/T 16659-2008
Determination of Mercury of Coal
(ISO 15237.2016, Solid Mineral Fuels – Determination of Total Mercury
Content of Coal)
Issued on. APRIL 25, 2024
Implemented on. NOVEMBER 1, 2024
Issued by. State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative References... 4
3 Terms and Definitions... 4
4 Reagents and Materials... 4
5 Apparatus... 6
6 Test Conditions... 7
7 Samples... 7
8 Cold Atomic Absorption Spectrophotometry... 8
9 Atomic Fluorescence Spectrometry... 10
10 Mercury Detector Method... 12
11 Solid Sampling Direct Mercury Detector Method... 12
12 Precision... 14
13 Test Report... 15
Appendix A (Informative) Instrument Reference Working Conditions... 16
1 Scope
This Document specifies the reagents and materials, instruments and equipment, test conditions,
samples, test procedures, test data processing, precision and test reports for the determination
of mercury in coal by cold atomic absorption spectrophotometry, atomic fluorescence
spectrometry, mercury detector method and solid sampling direct mercury detector method.
This Document is applicable to the determination of mercury content in lignite, bituminous coal,
anthracite and coal gangue.
2 Normative References
The provisions in following documents become the essential provisions of this Document
through reference in 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 Document.
GB/T 213 Determination of calorific value of coal
GB/T 474 Preparation of coal sample
GB/T 483 General rules for analytical and testing methods of coal
GB/T 6682 Water for analytical laboratory use - Specification and test methods
GB/T 19494.2 Mechanical sampling of coal - Part 2.Method for sample preparaion
3 Terms and Definitions
For the purposes of this Document, there are no terms and definitions apply.
4 Reagents and Materials
Unless otherwise specified, only reagents confirmed as analytically pure are used in the analysis;
and the used water is Class-II water or water of equivalent purity as specified in GB/T 6682.
4.1 Oxygen. in accordance with GB/T 213.
4.2 Argon. purity above 99.99%.
4.3 Nitric acid. guarantee reagent, ρ=1.42g/mL.
4.4 Sulfuric acid. guarantee reagent, ρ=1.84g/mL.
4.5 Hydrochloric acid. guarantee reagent, ρ=1.19g/mL.
4.6 Vanadium pentoxide.
4.7 Hydrogen peroxide. 30% (mass fraction).
4.8 Anhydrous ethanol.
4.9 Nitric acid solution. volume ratio is (1+9).
4.10 Nitric acid solution. volume ratio is (5+95).
4.13 Fixed solution. 0.5g/L.
Pipette 10.00mL of potassium dichromate solution (4.12) into a 1L volumetric flask; add
appropriate amount of water; then add 50mL of nitric acid (4.3); dilute to scale with water; and
make constant volume.
4.14 Potassium permanganate solution. 50g/L.
Weigh 5.0g of potassium permanganate and dissolve in 100mL of water; and store in a brown
reagent bottle.
4.15 Hydroxylamine hydrochloride solution. 15g/L.
Weigh 1.5g of hydroxylamine hydrochloride and dissolve in 100mL of water.
4.16 Potassium hydroxide solution. 5.0g/L.
Weigh 5.0g of potassium hydroxide and dissolve it in 1L of water.
4.17 Potassium borohydride solution or sodium borohydride solution. 5.0g/L.
Weigh 5.0g of potassium borohydride (guarantee reagent) or sodium borohydride (guarantee
reagent) and dissolve it in 1L of potassium hydroxide solution (4.16); prepare it before use.
5 Apparatus
5.1 Analytical balance. graduation value 0.1mg.
5.2 Atomic absorption spectrophotometer. equipped with a mercury hollow cathode lamp with
a wavelength of 253.7nm.
5.3 Atomic fluorescence spectrometer. equipped with a mercury hollow cathode lamp with a
wavelength of 253.7nm.
5.4 Mercury detector. cold atomic absorption mercury detector or cold atomic fluorescence
mercury detector.
5.5 Solid sampling direct mercury detector.
5.6 Electric heating plate. controllable in the range of 50℃~200℃.
5.7 Microwave digestion system. including microwave digestion instrument, digestion tank, etc.
5.8 Mercury vapor generation bottle. a conical bottle with a scale of 50mL and a tightly fitting
plug, with inlet and outlet pipes on the plug and the end of the inlet pipe 5mm~10mm away
from the bottom of the bottle.
6 Test Conditions
6.1 The test shall be carried out in a room with a temperature above 10°C.
6.2 All glassware used in the test must be soaked in nitric acid solution (4.10) for at least 24 h
before use, and then washed by water for later use.
7 Samples
7.1 Specimens
The coal samples for the general analysis test shall be prepared according to GB/T 474 or GB/T 19494.2.
7.2 Preparation of sample solution
7.2.1 Wet digestion
Weigh about 0.1g (accurate to 0.0002g) of the coal sample for general analysis test into a
mercury vapor generator bottle. Add 50mg of vanadium pentoxide (4.6) and a few drops of
anhydrous ethanol (4.8) to moisten the specimen; then add 10mL of nitric acid (4.3);
immediately cover the mercury vapor generator bottle with a porcelain cover; leave it overnight.
Add 4mL of sulfuric acid (4.4) and place it on a electric hot plate; first heat at (120±10) ℃ for
about 1.5h; then gradually increase the temperature to (160±10) ℃; and continue heating until
sulfur trioxide smoke just emerges.
7.2.2 Oxygen bomb combustion
According to the provisions of GB/T 213, weigh about 0.99g~1.01g (accurate to 0.0002g) of
coal sample for general analytical test in a dry combustion dish and ignite it for combustion.
After the combustion is completed, wait for the oxygen bomb to cool down, and then slowly
and evenly release the gas. The entire release process lasts for no less than 2 min.
7.2.3 Microwave digestion
Weigh about 0.1g (accurate to 0.0002g) of the coal sample for general analysis test into a
digestion tank; add 6mL of nitric acid (4.3); stand for 30min. Add 1mL of hydrogen peroxide
(4.7); and after the reaction is moderated; tighten the tank cover and place it in a microwave
digestion instrument. Digestion is performed according to the digestion procedure in Table A.1
in Appendix A (it can also be determined according to the conditions of the microwave digestion
instrument used in the laboratory).
8 Cold Atomic Absorption Spectrophotometry
8.1 Method summary
Treat the specimen into a solution to convert mercury into divalent mercuric ions. Under acidic
conditions, use stannous chloride as a reducing agent to reduce the mercury ions into mercury
atomic vapor; and measure it with an atomic absorption spectrophotometer.
8.2 Test procedures
8.2.1 Drawing of working curve
8.2.1.1 Drawing the working curve of wet digestion method
8.2.1.1.1 Accurately pipette 0.00mL, 0.25mL, 0.50mL, 1.00mL, and 1.50mL of mercury
standard working solution (4.20) to five mercury vapor generating bottles respectively; titrate
potassium dichromate solution (4.12) until the solution turns yellow; add 2mL of anhydrous
ethanol (4.8), and adjust to 30mL with water.
8.2.1.2 Drawing the working curve of oxygen bomb combustion method
8.2.1.2.1 Accurately pipette 0.00mL, 1.00mL, 2.00mL, 5.00mL, and 10.00mL of mercury
standard working solution (4.20) to five 50mL volumetric flasks respectively. Add 5mL of nitric
acid solution (4.9) and 0.5mL of potassium permanganate solution (4.14); shake well. And
slowly titrate hydroxylamine hydrochloride solution (4.15) while shaking the volumetric flask
until the color of potassium permanganate just fades; dilute to the scale with water; and make
constant volume.
8.2.1.2.2 Transfer the standard solution to the mercury vapor generating bottle; and perform the
rest of the operation as in 8.2.1.1.2.
8.2.1.3 Drawing the working curve of microwave digestion method
8.2.2 Determination of sample
Transfer the specimen solution (7.2.1 or 7.2.3) or accurately pipette 50mL of the specimen
solution (7.2.2) into the mercury vapor generating bottle; add 1mL of stannous chloride solution
(4.11) and immediately cover the bottle with the stopper; and shake well. After standing for a
while, connect the mercury vapor generating bottle to the atomic absorption spectrophotometer
for determination and record the maximum absorbance; and obtain the mercury content in the
specimen solution from the working curve.
8.2.3 Blank test
For each batch of coal samples, prepare two blank solutions (without adding coal samples)
according to 7.2; and determine the mercury content in the blank solutions according to 8.2.2;
and take the average value as the blank value.
8.3 Test data processing
8.3.1 Calculation of result
8.3.2 Expression of result
The result is the arithmetic mean of repeated measurements, rounded off to three digits after
the decimal point according to GB/T 483.
9 Atomic Fluorescence Spectrometry
9.1 Method summary
The sample is treated into a solution. In an acidic medium, potassium borohydride is used as a
reducing agent to reduce the mercury in the test solution to mercury vapor. Argon is used as a
carrier gas to introduce it into the atomizer and measured by atomic fluorescence spectrometer.
9.2 Test procedures
9.2.1 Drawing of working curve
Except for not adding stannous chloride reducing agent, prepare the standard series solution in
five 50mL volumetric flasks according to the requirements of 8.2.1 and dilute with water to the
scale. Introduce nitric acid solution (4.10), potassium borohydride solution (4.17) and standard
series solution into the electric quartz furnace atomizer; measure the fluorescence intensity of
mercury in the standard solution.
9.2.2 Determination of sample
Adjust the instrument to the best working state according to the instrument manual. The
reference measurement conditions are shown in Table A.2.Introduce the specimen solution
(7.2), nitric acid solution (4.10) and potassium borohydride solution (4.17) into the electric
quartz furnace atomizer; measure the fluorescence intensity of mercury in the sample solution;
and obtain the mass concentration (μg/L) of mercury in the specimen solution from the working curve.
9.2.3 Blank test
For each batch of coal samples, prepare 2 blank solutions (without adding coal samples)
according to 7.2; and determine the mass concentration (μg/L) of mercury in the blank solutions
according to 9.2.2; and take the average value as the blank value.
9.3 Test data processing
9.3.1 Calculation of result
The content of mercury in the coal sample for the general analysis test is calculated according
to Formula (3).
9.3.2 Expression of result
The same as 8.3.2.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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