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GB/T 39538-2020: (Determination of arsenic, selenium and mercury in coal-hydride generation-atomic fluorescence spectrometry)
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| GB/T 39538-2020 | English | 189 |
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(Determination of arsenic, selenium and mercury in coal-hydride generation-atomic fluorescence spectrometry)
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GB/T 39538-2020
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Basic data | Standard ID | GB/T 39538-2020 (GB/T39538-2020) | | Description (Translated English) | (Determination of arsenic, selenium and mercury in coal-hydride generation-atomic fluorescence spectrometry) | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | D21 | | Word Count Estimation | 10,190 | | Date of Issue | 2020-11-19 | | Date of Implementation | 2021-06-01 | | Regulation (derived from) | National Standard Announcement No. 26 of 2020 | | Issuing agency(ies) | State Administration for Market Regulation, China National Standardization Administration | GB/T 39538-2020: (Determination of arsenic, selenium and mercury in coal-hydride generation-atomic fluorescence spectrometry)
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(Determination of arsenic, selenium and mercury in coal-hydride generation-atomic fluorescence spectrometry)
ICS 73.040
D21
National Standards of People's Republic of China
Determination of arsenic, selenium and mercury in coal
Hydride generation-atomic fluorescence spectrometry
2020-11-19 released
2021-06-01 implementation
State Administration for Market Regulation
Issued by the National Standardization Management Committee
Table of contents
Foreword Ⅰ
1 Scope 1
2 Normative references 1
3 Determination of arsenic and selenium 1
3.1 Method summary 1
3.2 Reagents and materials 1
3.3 Equipment 2
3.4 Sample 2
3.5 Test Step 2
3.6 Calculation and expression of results 3
3.7 Precision 4
4 Determination of mercury 4
4.1 Method summary 4
4.2 Reagents and materials 4
4.3 Apparatus 5
4.4 Sample 5
4.5 Test Step 5
4.6 Calculation and expression of results 6
4.7 Precision 7
5 Test report 7
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard was proposed by the China Coal Industry Association.
This standard is under the jurisdiction of the National Coal Standardization Technical Committee (SAC/TC42).
Drafting organization of this standard. Testing Branch of Coal Science and Technology Research Institute Co., Ltd.
The main drafters of this standard. Fu Kun, Chen Huizhu, Gong Wanli, He Chengyou.
Determination of arsenic, selenium and mercury in coal
Hydride generation-atomic fluorescence spectrometry
1 Scope
This standard specifies the method summary, reagents and materials, instruments and equipment for the determination of arsenic, selenium and mercury in coal by hydride generation-atomic fluorescence spectrometry.
Samples, test procedures, calculation and presentation of results, method precision and test reports.
This standard applies to lignite, bituminous coal and anthracite.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article
Pieces. For undated references, the latest version (including all amendments) applies to this document.
GB/T 213 Method for measuring calorific value of coal
GB/T 483 General rules for coal analysis and test methods
GB/T 21191 Atomic Fluorescence Spectrometer
3 Determination of arsenic and selenium
3.1 Method summary
The coal sample is mixed with Eschka reagent and burned, and the burned substance is dissolved with hydrochloric acid. When arsenic is measured, thiourea-ascorbic acid is used to reduce pentavalent arsenic to three.
When determining selenium, use hydrochloric acid heating to reduce hexavalent selenium to tetravalent selenium, then use sodium borohydride as a reducing agent, and argon as a carrier gas to reduce the result
The obtained gaseous hydride is introduced into an atomizer and measured by an atomic fluorescence spectrometer.
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 Ashika reagent (hereinafter referred to as Aldrin). commercially available, or mix 2 parts by mass of light magnesium oxide and 1 part by mass of anhydrous sodium carbonate
After grinding to a particle size of less than 0.2mm, store it in a closed container.
3.2.2 Argon gas. purity above 99.99%.
3.2.3 Hydrochloric acid. the relative density is 1.18.
3.2.4 Hydrochloric acid solution. 50mL/L, add 50mL of hydrochloric acid (3.2.3) to an appropriate amount of water, and then dilute to 1L with water.
3.2.5 Sulfuric acid solution. c(1/2H2SO4)=6mol/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 while adding, then dilute to 1L with water.
3.2.6 Sodium hydroxide solution. 5g/L. Weigh 5.0g of sodium hydroxide and dissolve in 1L of water.
3.2.7 Sodium hydroxide solution. c(NaOH)=6mol/L. Weigh 48.0g of sodium hydroxide dissolved in a small amount of water and dilute to.200mL.
3.2.8 Sodium borohydride solution. 10g/L. Weigh 10.0g of sodium borohydride and dissolve it in 1L of sodium hydroxide solution (3.2.6) and prepare it before use.
3.2.9 Thiourea-ascorbic acid solution. 50g/L. Weigh 5.0 g of thiourea and 5.0 g of ascorbic acid, dissolve them in 100 mL of water, and prepare them before use.
3.2.10 Arsenic standard stock solution. 100μg/mL. Accurately weigh the premium grade pure arsenic trioxide that has been dried at 105℃~110℃ for about 2h
0.1320g dissolved in 2mL sodium hydroxide solution (3.2.7), add about 50mL water, after it is completely dissolved, add 2.5mL sulfuric acid solution
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