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Determination method of arsenic valence

A determination method and technology of arsenic valence, which are applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of difficulty in efficient extraction of arsenic, distortion of measurement results, and difficulty in non-destructive extraction, achieving low measurement and equipment maintenance costs, High accuracy and simple operation effect

Active Publication Date: 2015-04-08
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, compared with water and organic samples, the arsenic in fuel incineration ash mainly exists as inorganic trivalent arsenic and pentavalent arsenic. Due to the complex physical and chemical reactions at high temperatures, the arsenic occurrence forms are very complicated and difficult to carry out Non-destructive extraction, specifically as follows: (1) The binding form of arsenic in fuel incineration ash is more stable than that in organic samples, so it is difficult to achieve efficient extraction of arsenic in ash with water, methanol or bionic solvents; (2) ) Some high-valent oxides will be generated during fuel combustion, and trivalent arsenic will be easily oxidized to pentavalent arsenic in the process of arsenic extraction, which will lead to distortion of measurement results; Substances that will affect the separation effect of arsenic in different valence states

Method used

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Embodiment 1

[0029] The assay method of arsenic valence state comprises the following steps:

[0030] (1) Weigh 0.2g of the sample to be tested, configure H 3 PO 4 and ascorbic acid mixed solution as the extract, the H in the extract3 PO 4 The concentration of ascorbic acid is 1.0mol / L, and the concentration of ascorbic acid is 0.2mol / L; The sample to be tested is put into a Teflon digestion tank, and 20mL extract is added to the sample to be tested (solid-liquid ratio is 1:100g / mL), Place it at room temperature for 15 minutes. After the gas generated by the reaction is completely released, seal the digestion tank and put it into a microwave digestion apparatus for digestion (the digestion program is to rise from room temperature to 80°C within 10 minutes, keep warm for 20 minutes, and then naturally Cool to room temperature); filter the digestion solution and collect the filtrate; wash the residue with the extract for more than 3 times, collect the washing solution, mix it with the filt...

Embodiment 2

[0036] H in the extract 3 PO 4 The concentration of ascorbic acid is 1.0mol / L, and the concentration of ascorbic acid is 0.5mol / L, and other experimental conditions are the same with embodiment 1.

Embodiment 3

[0038] H in the extract 3 PO 4 The concentration of ascorbic acid is 0.5mol / L, and the concentration of ascorbic acid is 0.2mol / L, and other experimental conditions are the same as in Example 1.

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Abstract

The invention discloses a determination method of arsenic valence. The method comprises the steps of: (1) adding an extracting solution which is a mixed solution of H3PO4 and ascorbic acid into a sample to be measured, which is coal or household garbage incineration ash, soil or sludge, completely releasing the produced gas, digesting by microwave, filtering a digestion liquid, washing the residue by an extracting solution, collecting the washing liquid, mixing the extracting solution with the filtrate, and making up to volume; (2) separating trivalent and pentavalent arsenic; (3) reducing the separated trivalent and pentavalent arsenic to obtain arsenic hydride gas; and (4) determining the arsenic hydride gas obtained by reduction of arsenic in different valence, so as to obtain the content of trivalent and pentavalent arsenic in the sample to be measured. The method can achieve nondestructive extraction and fast and effective separation of trivalent and pentavalent arsenic, has the advantages of high accuracy of the determination results, simple operation, low cost on determination and equipment maintenance, and is applicable to analysis and determination of arsenic form in solid wastes such as fuel burning ash, soil and sludge.

Description

technical field [0001] The invention belongs to the technical field of arsenic form analysis in fuel combustion products, and more specifically relates to a method for determining the valence state of arsenic. Background technique [0002] The combustion of fuels such as coal, biomass and municipal solid waste is accompanied by the generation of a large amount of incineration ash. The toxic trace element arsenic present in the fuel often transforms into gaseous trivalent arsenic As under high temperature combustion 2 o 3 released into the flue gas in the form of As 2 o 3 Oxidation will generate less volatile pentavalent arsenate, which will be solidified into fly ash or bottom ash to reduce emissions to the atmosphere; at the same time, some As 2 o 3 At low temperatures, it can be captured by fly ash through physical adsorption. Therefore, arsenic mainly exists in the form of trivalent and pentavalent inorganic arsenic in fuel incineration ash. During the treatment an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 姚洪胡红云徐章陈敦奎曹金秀刘欢
Owner HUAZHONG UNIV OF SCI & TECH
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