GB/T 16415-2008 PDF English
US$145.00 · In stock · Download in 9 secondsGB/T 16415-2008: Determination of selenium in coal -- Hydride generation-atomic absorption method Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedureStatus: Valid GB/T 16415: Evolution and historical versions
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
| GB/T 16415-2008 | English | 145 |
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Determination of selenium in coal -- Hydride generation-atomic absorption method
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| GB/T 16415-1996 | English | 199 |
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Determination of selenium in coal--Hydride generation-atomic absorption method
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GB/T 16415-2008: Determination of selenium in coal -- Hydride generation-atomic absorption method---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/GBT16415-2008
GB
NATIONAL STANDARD OF THE
PEOPLE'S REPUBLIC OF CHINA
ICS 73.040
D 21
Replacing GB/T 16415-1996
Determination of selenium in coal - Hydride generation-
atomic absorption method
(ISO 11723.2004, Solid mineral fuels - Determination of arsenic and selenium -
Eschka's mixture and hydride generation method, MOD)
Issued on: JULY 29, 2008
Implemented on: MAY 1, 2009
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine of PRC;
Standardization Administration of PRC.
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative references... 4
3 Method summary... 4
4 Reagents and materials... 4
5 Instruments and equipment... 5
6 Analysis steps... 6
7 Result calculation... 8
8 Method precision... 8
9 Test report... 8
Appendix A (Informative) Comparison list of clause numbers of this standard and ISO
11723.2004... 10
Appendix B (Informative) Technical differences between this standard and ISO
11723.2004 and their reasons... 11
Determination of selenium in coal - Hydride generation-
atomic absorption method
1 Scope
This standard specifies the reagents and materials, instruments and equipment,
analytical procedures, result calculation, method precision and test report for the
determination of selenium in coal.
This standard applies to lignite, bituminous coal and anthracite.
2 Normative references
The clauses in the following documents become clauses of this standard through
reference in this standard. For dated referenced documents, all subsequent amendments
(excluding errata) or revisions are not applicable to this standard. However, parties who
reach an agreement based on this standard are encouraged to investigate whether the
latest versions of these documents are applicable. For undated referenced documents,
the latest versions apply to this standard.
GB/T 483 General rules for analytical and testing methods of coal (GB/T 483-2007,
ISO 1213-2.1992, Solid mineral fuels - Vocabulary - Part 2.Terms relating to
sampling, testing and analysis, NEQ)
GB/T 6682 Water for analytical laboratory use - Specification and test methods
(GB/T 6682-2008, ISO 3696.1987, Water for analytical use - Specification and test
methods, MOD)
3 Method summary
The coal sample is mixed with Aldrin, burned at 800 °C, dissolved with hydrochloric
acid, and heated to reduce hexavalent selenium to tetravalent selenium. Then, sodium
borohydride is used to reduce tetravalent selenium to selenium hydride. The mixture is
introduced into a quartz tube atomizer using nitrogen as a carrier gas and determined
by atomic absorption method.
4 Reagents and materials
The water used in this standard shall comply with the requirements for Grade 3 water
in GB/T 6682.
4.1 Aldrin. Take 2 parts by mass of light calcined magnesium oxide and 1 part by mass
of anhydrous sodium carbonate, grind to a particle size of less than 0.2 mm, mix well,
and store in a sealed container.
4.2 Hydrochloric acid. with a relative density of 1.18.
4.3 Sodium borohydride solution. 18 g/L. Weigh 1.8 g of sodium borohydride and
dissolve it in 100 mL of 5 g/L sodium hydroxide solution. Prepare the solution before
use.
4.4 Selenium standard stock solution. 1 mg/mL. Weigh 0.1000 g of high-purity
selenium into a 100 mL beaker, add 5 mL of nitric acid, heat at low temperature until
dissolved, continue heating to drive out nitrogen oxides, cool, transfer to a 100 mL
volumetric flask, dilute to the mark with water, and shake well.
Commercially available certified reference materials can also be used as selenium
standard stock solutions.
4.5 Selenium standard intermediate solution. 10 μg/mL. Pipette 1 mL of the selenium
standard stock solution (4.4) into a 100 mL volumetric flask, dilute to the mark with the
blank solution (6.2.2), and shake well.
4.6 Selenium standard working solution. 0.2 μg/mL. Pipette 1 mL of the selenium
standard intermediate solution (4.5) into a 50 mL volumetric flask, dilute to the mark
with the blank solution (6.2.2), and shake well.
4.7 Nitrogen. The purity is above 99.9%.
4.8 Acetylene. High-purity acetylene.
5 Instruments and equipment
5.1 Analytical balance. The sensitivity is 0.1 mg.
5.2 Porcelain crucible. 30 mL. The inner surface of the enamel shall be intact.
5.3 Muffle furnace. The temperature can be controlled at 800 °C±20 °C; the ventilation
is good.
5.4 Atomic absorption spectrophotometer. with absorption peak area integration and
peak height measurement functions.
5.5 Light source. Selenium hollow cathode lamp or selenium electrodeless discharge
lamp.
5.6 Automatic hydride generator. It is capable of automatic washing, liquid metering
and liquid addition, with an accuracy of 0.5%.
5.7 Electric heating plate. It can maintain the temperature at 60 °C~90 °C.
6 Analysis steps
6.1 Preparation of sample solution
6.1.1 Accurately weigh 1 g of air-dried coal sample with a particle size of less than 0.2
mm (accurate to 0.0002 g) (when Ad of the coal sample is greater than 40.00% or St,d is
greater than 8.00%, or Sed is greater than 15 μg/g, weigh 0.5 g of coal sample), place it
in a porcelain crucible pre-filled with 1.5 g of Aldrin, mix the coal sample and aldrin
evenly, and then evenly cover it with about 1.5 g of Aldrin.
6.1.2 Place the crucible in a cold muffle furnace, slowly raise the temperature to 500 °C
and heat at this temperature for 1 hour. Then raise the temperature to 800 °C and heat
at this temperature for another 3 hours. Remove the crucible and cool to room
temperature.
6.1.3 Crush the calcined sample and transfer it to a 150 mL beaker containing 20~30
mL of hot water. Add 5 mL of hydrochloric acid to the crucible to dissolve the remaining
residue, then pour it into the beaker. Wash the crucible with 15 mL of hydrochloric acid
three times (5 mL each time), and transfer the wash solution to the beaker. Stir the
solution. After cooling, transfer the entire solution to a 100 mL volumetric flask, dilute
to the mark with water, and shake well.
NOTE. Some samples may contain solid residue, but it will not affect the test results.
6.2 Preparation of blank solution
6.2.1 Weigh 15 g of aldrin into a 100 mL evaporating dish. Place the dish in a cold
muffle furnace, slowly raise the temperature to 500 °C, and heat at this temperature for
1 hour. Then raise the temperature to 800 °C and continue heating for 3 hours. Remove
the evaporating dish and cool to room temperature.
6.2.2 Transfer the ignited aldrin to a beaker containing 100~150 mL of hot water.
Dissolve the residue in the dish with 25 mL of hydrochloric acid, transfer it to the beaker,
and rinse the residue into the beaker with water. Rinse the evaporating dish with 75 mL
of hydrochloric acid three times (25 mL each time) and transfer the solution to the
beaker. Stir until the aldrin is completely dissolved. Cool to room temperature, transfer
to a 500 mL volumetric flask, dilute to the mark with water, and shake well. Transfer it
to a plastic bottle for storage.
6.3 Preparation of standard solutions
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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