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Method for determining hexachloro-cyclohexane soprocide and dichlorodiphenyl trichloroethane through ultrasonic extraction-gas chromatography

A gas chromatographic and hexachloropyridine technology, which is applied to the detection field of hexachloropyridine and DDT in soil, can solve the problems of not being suitable for mass processing of soil samples, time-consuming, etc., shortening the pretreatment time, and improving the recovery of standard additions. rate effect

Pending Publication Date: 2018-11-20
内蒙古恒胜测试科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the national standard method is classic and accurate, the pre-treatment soil needs to be soaked, and the Soxhlet extraction takes 16 hours. In addition to other pre-treatments, it takes about 24 hours to test on the machine, which is too time-consuming and not suitable for large-scale processing of soil samples.

Method used

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  • Method for determining hexachloro-cyclohexane soprocide and dichlorodiphenyl trichloroethane through ultrasonic extraction-gas chromatography
  • Method for determining hexachloro-cyclohexane soprocide and dichlorodiphenyl trichloroethane through ultrasonic extraction-gas chromatography

Examples

Experimental program
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Effect test

Embodiment 1

[0029] (1) Sample pretreatment:

[0030] In the soil pretreatment room, pour the soil on the enamel tray, crush it with a hammer and rod, pick out the impurities and divide the crushed sample by quarter method, and pass it through a 60-mesh nylon sieve to make a soil sample. Weigh 10g of soil sample into a beaker, add 2mL of distilled water, mix well, and add 20μL of mixed standard solution (α-66, β-66, γ-66, δ-66 in mixed standard solution 6. The concentration of p.p'-DDE and p.p'-DDD are both 4μg / mL, and the concentration of o.p'-DDT and p.p'-DDT are both 32μg / mL) as a standard addition, the number of sets Add 100 mL of a mixture of acetone and n-hexane (volume ratio is 1:1), seal the beaker containing the mixture of acetone and n-hexane and soil with a sealing film to prevent volatilization, and put it in an ultrasonic machine for extraction for 20 minutes. After extraction, the sample and the extract are separated with an all-glass sand core filter device. The extract is add...

Embodiment 2

[0037] The ultrasonic extraction time is 10 minutes, and the rest of the operation steps are the same as in Example 1.

Embodiment 3

[0039] The ultrasonic extraction time is 30 minutes, and the rest of the operation steps are the same as in Example 1.

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Abstract

The invention discloses a method for determining hexachloro-cyclohexane soprocide and dichlorodiphenyl trichloroethane through ultrasonic extraction-gas chromatography. The method comprises the following steps: weighing a prepared soil sample to be added into a beaker, adding a mixed solution of acetone and normal hexane, extracting in an ultrasonic machine, adding the extracting solution into a separating funnel after filtration, and flushing the beaker, the soil sample and the filtering device; merging the flushing fluid and adding into the separating funnel, adding a sodium sulfate solution, standing after oscillating, removing the aqueous solution of acetone, and remaining the normal hexane extracting solution; purifying and concentrating the normal hexane extracting solution so as toobtain a to-be-detected solution of the sample; detecting the concentration of the hexachloro-cyclohexane soprocide and dichlorodiphenyl trichloroethane in the obtained to-be-detected solution of thesample by using a gas chromatograph. According to the method, the hexachloro-cyclohexane soprocide and dichlorodiphenyl trichloroethane in the soil sample can be extracted by the ultrasonic extractionmethod, the pretreatment time is greatly shortened, and the method is applicable to rapid and accurate treatment of large-scale soil samples.

Description

Technical field [0001] The invention relates to the technical field of pesticide analysis, in particular to a detection method of BHC and DDT in soil. Background technique [0002] Organochlorine pesticides are the first-generation pesticides and a class of synthetic environmental hormones that pose a serious threat to the environment. Among them, BHC and DDT are the earliest and most widely used pesticides, and they are the most serious environmental pollution. Although BHC and DDT have been banned, they are still widely present in the environment because of their stable nature, high residues in soil, water, organisms, and atmosphere, and they are difficult to degrade. According to existing data records, the main isomer of BHC α-HCH has a hydrogenolysis half-life of 26 years and a hydrolysis half-life of 64 years, but it is the most unstable and degradation rate of all BHC isomers. The fastest one. In addition, it will take 30 years for DDT to degrade 95% in the natural enviro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/54
CPCG01N30/02G01N30/06G01N30/14G01N30/54G01N2030/025G01N2030/062
Inventor 景慧马玉平
Owner 内蒙古恒胜测试科技有限公司
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