Method for simultaneously determining arsenic and mercury in textiles while achieving microwave digestion

A microwave digestion and textile technology, applied in the field of heavy metal detection, can solve the problems of strong interference in the detection of arsenic and mercury, and the inability to detect arsenic and mercury at the same time.

Active Publication Date: 2020-04-10
SUZHOU FIBER EXAMINATION INST
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the defect in the prior art that due to the complex composition of textiles (natural fibers and synthetic fibers), the detection of arsenic and mercury has strong interference, and the simultaneous detection of arsenic and mercury cannot be satisfied, and a microwave digestion method is proposed. Method for Determination of Arsenic and Mercury in Textiles

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  • Method for simultaneously determining arsenic and mercury in textiles while achieving microwave digestion
  • Method for simultaneously determining arsenic and mercury in textiles while achieving microwave digestion
  • Method for simultaneously determining arsenic and mercury in textiles while achieving microwave digestion

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Embodiment 1

[0052] The selection of embodiment 1 solvent concentration

[0053] Simultaneous determination of arsenic and mercury in textiles requires that arsenic and mercury can coexist in the same solvent without interfering with each other. The present invention uses a mixed solution of nitric acid and sodium chloride with a certain concentration as the solvent for the coexistence of arsenic and mercury. According to the making method of the standard curve that arsenic and mercury mixed standard solution gained, adopt single factor variable analysis, take the volume concentration of the concentrated nitric acid in the standard solution and the mass concentration of sodium chloride as variable; According to table 1 respectively, different concentration The concentrations of sodium chloride and nitric acid were prepared with arsenic concentration: 0ng / mL, 2ng / mL, 4ng / mL, 8ng / mL; mercury concentration: 0ng / mL, 0.2ng / mL, 0.4ng / mL, 0.8ng / mL.

[0054] The fluorescence intensities of various...

Embodiment 2

[0061] Embodiment 2 thiourea, ascorbic acid system

[0062] Pentavalent arsenic cannot react with potassium borohydride to form AsH 3 , Ascorbic acid can convert 5-valent arsenic to 3-valent arsenic, and potassium borohydride can generate AsH 3 , thiourea has a stabilizing effect on ascorbic acid, ensuring the stability of arsenic during reduction, and thiourea interacts with ascorbic acid. This experiment adopts an orthogonal experiment with 3 factors and 4 levels, and considers the interaction between ascorbic acid and thiourea. In the case of different factors, the linear relationship between arsenic and mercury is analyzed, and the correlation coefficient of the linear relationship between arsenic and mercury is used as the evaluation result. Among them, the degree of freedom of factor A is 2, the degree of freedom of factor B is 2, the degree of freedom of factor C is 2, the degree of freedom of interaction between A and B is 4, and the total degree of freedom is 10, so ...

Embodiment 3

[0073] The optimization of embodiment 3 atomic fluorescence spectrometry conditions

[0074] 1. Experimental program design

[0075] Potassium borohydride reacts with acid to produce hydrogen gas and arsenic to form hydride, and arsenic atoms are produced at high temperature; mercury directly reacts with potassium borohydride to produce mercury atoms, and then arsenic and mercury atoms produce fluorescence under the hollow cathode lamp. , Mercury detection is critical. According to experimental analysis, sulfuric acid is used as a carrier to easily precipitate arsenic, and the decomposition product of nitric acid is easy to produce quenching. Hydrochloric acid has the best effect, so the present invention selects hydrochloric acid as a carrier. Hydrochloric acid reacts with potassium borohydride to generate hydrogen, and forms a hydride with trivalent arsenic , if the concentration is too low, the fluorescence intensity of arsenic and mercury will be weakened. High-concentrat...

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Abstract

The invention belongs to the technical field of heavy metal detection, and particularly relates to a method for simultaneously determining arsenic and mercury in textiles while achieving microwave digestion. The method is used for digesting textiles containing arsenic and mercury targets by adopting microwave heating, and then detecting fluorescence intensity of a digestion solution by adopting adouble-channel atomic fluorescence spectrophotometer; and the method adopts an aqueous solution of a nitric acid and a sodium chloride as a solvent to serve as an arsenic and mercury coexisting solvent, and finds that the sodium chloride with certain concentration has an enhancing effect on the fluorescence intensity of arsenic. According to the method, the total content of arsenic and mercury inthe textiles (natural fibers and synthetic fibers) can be simultaneously tested, the result has no significant difference compared with independent tests, various heavy metal ions have no obvious interference on detection of arsenic and mercury, the deviation of intraday precision, daytime precision, reproducibility and repeatability is smaller than 5%, and the method is guaranteed to have generalizability.

Description

technical field [0001] The invention belongs to the technical field of heavy metal detection, and more specifically relates to a method for simultaneously determining arsenic and mercury in textiles by microwave digestion. Background technique [0002] The sources of arsenic and mercury pollution in textiles mainly come from the following three sources: ① Exist in various ores and biospheres; ② Industrial activities produce a large amount of waste gas, waste residue, and waste liquid; in the dose. Arsenic, mercury and their compounds from the above sources enter the atmosphere, soil, and water bodies, and enter plants (such as: cotton, flax, silkworm chrysalis, etc.), animals (such as: sheep, etc.) through mutual migration, absorption, and enrichment in various environments. , cattle, poultry, etc.), the textiles, clothing, leather, toys, etc. made from the above animals and plants as raw materials contain arsenic and mercury. For natural fibers, such as cotton, linen, sil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/44G01N21/64
CPCG01N1/44G01N21/6404G01N2021/6406
Inventor 薛正元丁力进孙峰陈明芳郭建峰孙晨晓顾伟褚静
Owner SUZHOU FIBER EXAMINATION INST
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