Chlorine isotope analysis method for organic monomers in chlorinated organic compounds based on nano metal reduction

A technology of chlorinated organic substances and nano-metals, which is applied in the direction of analysis of materials, material separation, and measurement devices, can solve the problems of cumbersome oxidant removal process, unstable test results, and high risk factor, and achieve easy promotion, small risk factor, and transformation high efficiency effect

Inactive Publication Date: 2019-09-17
INST OF HYDROGEOLOGY & ENVIRONMENTAL GEOLOGY CHINESE ACAD OF GEOLOGICAL SCI
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  • Summary
  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0005] The above-mentioned conversion process requires conversion at a high temperature above 600°C, distillation under high temperature conditions, and needs to be carried out under vacuum conditions. The risk factor of the operation is high and it is difficult to master
In the previous work, the application of the hydrogen peroxide system for oxidative dechlorination has achieved good experimental results, but the removal process of a large number of oxidants is relatively cumbersome, and the residual persulfate ions will cause instability in the test results

Method used

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  • Chlorine isotope analysis method for organic monomers in chlorinated organic compounds based on nano metal reduction
  • Chlorine isotope analysis method for organic monomers in chlorinated organic compounds based on nano metal reduction
  • Chlorine isotope analysis method for organic monomers in chlorinated organic compounds based on nano metal reduction

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] The ratio of chlorine isotopes in the trichlorethylene (TCE) produced by three different reagent manufacturers (represented by A, B and C respectively) is measured, and the steps are as follows:

[0043] A. Prepare a 40mL reaction bottle, weigh 1.0g nanometer iron into the reaction bottle in a closed glove box under anaerobic conditions, fully stir and let it stand;

[0044] B. Add 0.01g palladium acetate to the reaction bottle and mix evenly, then quickly add 30mL of prepared trichlorethylene solution (concentration 30mg / L), tighten the reaction bottle and place it on a shaker for 1 hour of shaking reaction;

[0045] Use a gas chromatograph to analyze the residual trichlorethylene in the solution after the reaction to confirm whether the trichlorethylene is completely converted: because the activity of nano-iron or nano-zinc plays a very critical role in whether the reaction can be carried out completely, take step B 10 mL of the reacted sample solution was put into a ...

Embodiment 2

[0054] The ratio of chlorine isotopes in the tetrachlorethylene (PCE) produced by three different reagent manufacturers (represented by A, B, C) is measured, and the steps are as follows:

[0055] A. Prepare a 40mL reaction bottle, weigh 1.0g nanometer iron into the reaction bottle in a closed glove box under anaerobic conditions, fully stir and let it stand;

[0056] B. Add 0.01g of palladium acetate into the reaction bottle and mix evenly, then quickly add 30mL of prepared tetrachlorethylene solution (concentration: 30mg / L), tighten the reaction bottle and place it on a shaker for 1 hour of shaking reaction;

[0057] Adopt the same gas chromatographic method as example 1 to confirm the reaction efficiency of every batch of samples;

[0058] C, the complete solution is filtered through a microporous membrane with a pore size of 0.22 μm;

[0059] D. Separating and purifying the filtered solution by ion chromatography, collecting the distillate of the chloride ion peaking time...

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Abstract

The invention provides a chlorine isotope analysis method for organic monomers in chlorinated organic compounds based on nano metal reduction, and the method comprises the following steps of A, reduction of chlorinated organic compounds; B, extraction and purification of inorganic chloride ions; and C, isotope analysis: determination and calibration of thermal ionization mass spectrometry. The method provided by the invention adopts the nano reduction technology to realize the rapid and efficient conversion of organochlorine to inorganic chlorine. Through the selection of the nano metal and the development of the purification process, the liquid to be tested in the whole process is very clean, so that the test background interference is very small. The whole process has the advantages such as strong operability, small risk factor and easy promotion.

Description

technical field [0001] The invention belongs to the technical field of isotope analysis of organic monomers, in particular to a method for analyzing chlorine isotopes of organic monomers in chlorinated organic matter based on nanometer metal reduction. Background technique [0002] With the continuous deepening of environmental science, earth science, food science and medical research, the new organic monomer isotope technology (CSIA) has become a frontier research hotspot. The use of organic monomer isotope technology (CSIA) can identify and track the source of organic pollution, evaluate the degradation process of organic pollutants and test the effect of control measures, identify the source of major diseases, etc. Trichlorethylene (TCE) and tetrachlorethylene (PCE) are common pollutants in the environment, and the first development of their monomer isotope testing methods has strong practical guiding significance. [0003] Current methods for analyzing isotopes of organ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/90
CPCG01N30/02G01N30/90G01N2030/903
Inventor 桂建业张晶张莉张永涛
Owner INST OF HYDROGEOLOGY & ENVIRONMENTAL GEOLOGY CHINESE ACAD OF GEOLOGICAL SCI
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