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Method of determining content of arsenic element in coal-containing sample

A method for measuring arsenic, which is applied in the field of coal chemical industry, can solve the problems of poor accuracy and precision of measurement results, and achieve the effects of low detection limit, improved accuracy and precision, and fast test speed

Inactive Publication Date: 2015-12-09
CHNA ENERGY INVESTMENT CORP LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The main purpose of the present invention is to provide a method for determining the content of arsenic in coal-containing samples, so as to solve the problem that the accuracy and precision of the measurement results are poor when the existing determination methods are used to measure the content of arsenic in coal-containing samples

Method used

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  • Method of determining content of arsenic element in coal-containing sample
  • Method of determining content of arsenic element in coal-containing sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1 to 3

[0054] Use instrument and device among the embodiment 1 to 3:

[0055] XGY-1011A model atomic fluorescence spectrometer, arsenic single-element high-intensity hollow cathode lamp, argon gas (purity ≥ 99.99%), and the parameters of the atomic fluorescence spectrometer are shown in Table 1.

[0056] Table 1

[0057] the element

Embodiment 1

[0073] Weigh 2.00 g of the first Aldrin reagent in the crucible, and mix the above-mentioned first Erdrin reagent with 1.00 ± 0.0001 g of a coal-containing sample with a particle size of less than 0.2 mm to obtain a mixture, and then use 1.00 g of the second Aldrin Spread over the above mixture.

[0074] Put the crucible into the muffle furnace, heat it from room temperature to (800±10)°C within 2 hours, and keep it at this temperature for 2-3 hours, take out the crucible, cool it to room temperature, and get the burnt product.

[0075] Transfer the burning material to a 50mL polytetrafluoroethylene beaker, rinse the crucible with 18.3% hydrochloric acid solution for 2 to 3 times, carefully transfer the washing liquid in the crucible to the polytetrafluoroethylene beaker, and then add 15mL mass fraction The hydrochloric acid solution with a fraction of 18.3% is heated and dissolved on a low-temperature electric hot plate, then removed and cooled, and water is added to the abov...

Embodiment 2

[0080] In a 25mL polyethylene test tube, mix 0.4500g of the coal-containing sample with 10mL (1+1) aqua regia, place the above polyethylene test tube in a boiling water bath for 1 hour, shake it once during the period, take it out and cool it to obtain a digestion solution . To the above digestion solution, add 1mL10g / LKMnO 4 solution, shake it up and place it for 30 minutes to obtain the first system to be reacted;

[0081] Then add 14mL of 10g / L oxalic acid solution to the first system to be reacted to make the volume of the first system to be reacted is 25mL, shake well, and place to obtain a clear solution.

[0082] Mix 5.0mL of clear solution, 2.5mL of 1g / L ferric chloride solution and 1mL of 5%wt thiourea-5%wt ascorbic acid solution to obtain the solution to be tested, shake well, and stand for 30min.

[0083] In a hydride generator, reduce 2.0mL of the above-mentioned solution to be tested with 20.00mL of 7g / L potassium borohydride to obtain arsine; according to the p...

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Abstract

The invention provides a method of determining the content of an arsenic element in a coal-containing sample. The method comprises the following steps: S1, preparing a solution to be detected for the coal-containing sample, wherein the solution to be detected contains the arsenic element; S2, determining the arsenic element in the solution to be detected by using hydride generation-atomic fluorescence spectrometry to obtain a detection value of arsenic atomic fluorescence intensity; S3, comparing the detection value with a calibration curve of the arsenic element to obtain the content of the arsenic element in the solution to be detected so as to further obtain the content of the arsenic element in the coal-containing sample, wherein in the hydride generation-atomic fluorescence spectrometry, working parameters of an atomic fluorescence spectrometer are as follows: the lamp current is 60 to 65mA; the negative high voltage is 280 to 290V; the height of an atomizer is 7.0 to 7.1mm; the temperature of the atomizer is 200 to 220 DEG C, and the carrier gas flow is 800 to 815mL.min<-1>. Test parameters and the addition amount of a reagent are adjusted, thereby improving the accuracy and the precision of the method.

Description

technical field [0001] The invention relates to the field of coal chemical industry, in particular to a method for determining the content of arsenic in a coal-containing sample. Background technique [0002] There are many methods for determining the content of arsenic in coal-containing samples. The advantages and disadvantages of each method are as follows: [0003] 1) Arsenic-molybdenum blue photometry is a widely used method with high accuracy and precision. This method is used in the national standard method of our country. However, the operation steps are many, the cycle is long, and the reagents used are many. The quality of each reagent and the correctness of the solution preparation will have an impact on the measurement results. [0004] 2) Atomic absorption spectrometry [0005] ①Cyanide generation-atomic absorption spectrometry: the combination of arsine generation and atomic absorption spectrometry reduces the interference of the matrix, and realizes the anal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64
Inventor 曲国兴杨少林孙伟
Owner CHNA ENERGY INVESTMENT CORP LTD
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