Low-temperature conversion and determination method of chlorine isotopes in chloro herbicide

A chlorine isotope and low-temperature conversion technology, which is applied in the fields of food, geology, medicine, and environmental protection. It can solve the problems of isotope analysis difficulties and no literature reports on chlorine isotope determination methods in chlorinated herbicides. It achieves low test background and is easy to use. Promotion, precision and high effect

Inactive Publication Date: 2014-08-13
INST OF HYDROGEOLOGY & ENVIRONMENTAL GEOLOGY CHINESE ACAD OF GEOLOGICAL SCI
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Problems solved by technology

[0003] Current methods for analyzing isotopes of organic monomers include gas chromatography quadrupole mass spectrometry (GC/qMS), gas chromatography-isotope ratio mass spectrometry (GC/IRMS), thermal ionization mass spectrometry (TIMS), etc. It has special pro

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  • Low-temperature conversion and determination method of chlorine isotopes in chloro herbicide

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Embodiment 1

[0028] To determine the ratio of chlorine isotopes in "2,4-D", the steps are as follows:

[0029] A. Prepare a 10mL derivative bottle, add 2mL of pure water, acidify with dilute sulfuric acid to pH ≤ 2, take 10uL of 2,4-drops and inject it under the liquid surface, irradiate with 250W ultraviolet light for 3 hours, and set aside;

[0030] B. Add 0.1uL of ferrous sulfate powder into the reaction vessel, add 5mL of 1% hydrogen peroxide, quickly cover the derivative bottle cap, and shake well;

[0031] C. Place the reaction vessel in an ultrasonic instrument for ultrasonic reaction at a temperature range of 90 degrees for 6 hours, and the power of the ultrasonic instrument is 750 watts; then place the reaction vessel under strong ultraviolet light for photocatalytic reaction for 3 hours; ultrasonic and ultraviolet combined treatment Can make the material conversion rate close to 100%;

[0032] D, adopt 2mL methanol and 2mL pure water to activate C18 solid-phase extraction column...

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Abstract

The invention discloses a low-temperature conversion and determination method of chlorine isotopes in chloro herbicide. The method comprises the following steps: A, dechlorinating the chloro herbicide at low temperature; A-1, feeding pure water into a closed reaction vessel, and injecting the chloro herbicide to be below the liquid surface, and radiating the liquid by utilizing high-energy ultraviolet light; A-2, adding ferrous sulfate powder and hydrogen peroxide; A-3, placing the reaction vessel in an ultrasonic instrument to have ultrasonic reaction for 5h to 10h in the temperature range of 80 to 100 DEG C; A-4, placing the reaction vessel in the strong ultraviolet light to be radiated for 3h; B, extracting and purifying inorganic chlorine; C, ion exchanging preparation and thermo ionization mass spectrum determination and correction: C-1, coating the graphite of a thermo ionization mass spectrum instrument with the high-purity cesium chloride solution obtained in the previous step, carrying out the thermo ionization mass spectrum testing, simultaneously receiving the intensity of ion peaks with m/e of 301 and 303 by utilizing a faraday cup, and obtaining a final theta 37Cl' value through calculation. By adopting the method, the chloro herbicide can be high-efficiently converted and purified under low-temperature condition, and finally a constant value of the isotope of organic monomer chlorine can be conveniently realized.

Description

technical field [0001] The invention relates to a method for testing, comparing and correcting chlorine isotopes in chlorinated herbicides, which belongs to the category of organic monomer isotope analysis technology (CSIA), and can be applied to the fields of environmental protection, geology, food, medicine and the like. 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. Chlorinated herbicides (such as 2,4-D) are common pollutants in the environment, and it is of great practical significance to develop a test method for its monomer isotope first. [0003] ...

Claims

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Application Information

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IPC IPC(8): G01N27/62G01N1/28G01N27/626
Inventor 桂建业张莉张永涛李晓亚张辰凌
Owner INST OF HYDROGEOLOGY & ENVIRONMENTAL GEOLOGY CHINESE ACAD OF GEOLOGICAL SCI
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