Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for extracting and purifying octachlorodipropyl ether in soil

A technology of octachlorodipropyl ether and soil purification, which is applied in the direction of measuring devices, instruments, scientific instruments, etc. It can solve the problems of affecting the accuracy of instrument results, unreasonable sulfonation steps, and complex composition of extracts, and achieves easy filling, The effect of short extraction time and short consumption time

Active Publication Date: 2014-09-24
SOUTH CHINA AGRI UNIV
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few literatures on the extraction of octachlorodipropyl ether in soil at home and abroad, and the existing methods have not been separated by column chromatography, which will lead to too many impurities in the sample, which will affect the accuracy of instrument analysis and results.
Some methods use leaching or vibration extraction, the efficiency is low, some extracts have complex compositions, and some sulfonation steps are unreasonable, which will affect the accuracy of the final results

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1 The extraction and determination of octachlorodipropyl ether in vegetable base soil

[0019] 1. Soil sample preparation

[0020] Soil samples of Chinese cabbage, lettuce, and Shanghai green were collected in the vegetable base of South China Agricultural University, the gravel and plant residues in the soil samples were removed, air-dried naturally, then ground, passed through a 18-mesh sieve, and set aside.

[0021] 2. Ultrasonic and centrifugal extraction

[0022] Weigh about 10.00g of soil sample into a conical flask, add 20mL n-hexane-acetone extract (volume ratio about 22:3), ultrasonically extract for 10min, transfer the extract to a 100mL centrifuge tube, centrifuge at 4000r / min for 5min, transfer The supernatant was placed in a round-bottomed flask, and the supernatant was ultrasonically extracted and centrifuged twice, and the supernatant was concentrated to 5 mL in a vacuum rotary evaporator.

[0023] 3. Column chromatography cleanup

[0024] The...

Embodiment 2

[0044] Comparison of octachlorodipropyl ether recovery rate in different methods of embodiment 2

[0045] Set up the following experimental groups:

[0046] The first group: solvent blank, the solvent is n-hexane-acetone mixture (volume ratio 22:3);

[0047] The second group: soil blank, take the soil without octachlorodipropyl ether as a blank control;

[0048] The third group: solvent spike, add octachlorodipropyl ether to n-hexane-acetone mixture, the concentration is 5.0μg / mL;

[0049] The fourth group: soil spiked, adding octachlorodipropyl ether to the soil without octachlorodipropyl ether, the concentration is 10 μg / g;

[0050] Each of the above groups was tested according to steps 2 to 6 in Example 1, and the test results were as follows: the first and second groups did not detect octachlorodipropyl ether, and the recovery rate of the third group of octachlorodipropyl ether was 92.4%. , the recovery rate of the fourth group was 90.4%. .

Embodiment 3

[0051] Example 3 Preparation of the Extraction and Determination of Octachlorodipropyl Ether in Contaminated Soil

[0052] Weigh 5kg of vegetable garden soil, red soil and paddy soil respectively, and then add different amounts of octachlorodipropyl ether to make polluted soil with octachlorodipropyl ether concentration of 10mg / kg, and plant Chinese cabbage. Soil samples were collected during the vegetable harvest period, extracted and detected according to the steps in Example 1, and the results found that the average content of octachlorodipropyl ether in vegetable garden soil, red soil, and paddy soil was 3.76 mg / kg, 3.46 mg / kg, respectively. kg, 1.86mg / kg. After extracting and testing the cabbage hearts harvested on different soils, it was found that octachlorodipropyl ether was found in the cabbage hearts, indicating that the pollutants in the soil had been partially transferred to the crops.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
diameteraaaaaaaaaa
Login to View More

Abstract

The invention discloses a method for extracting and purifying octachlorodipropyl ether in soil, and belongs to the technical field of pesticide residue analysis. The extraction and purification method of the present invention is to add n-hexane-acetone mixed solution to the soil sample, extract and centrifuge, take the supernatant and concentrate, pass the concentrated solution through the chromatographic column, elute with n-hexane, collect the eluate, concentrate, and obtain eight Chlorodipropyl ether extract; the chromatographic column is filled sequentially from top to bottom with 3-4cm of anhydrous sodium sulfate, 9-11cm of silica gel-concentrated sulfuric acid mixture, 3-4cm of anhydrous sodium sulfate, and absorbent cotton. The steps of the extraction method of the invention are simple and easy to operate, and the amount of octachlorodipropyl ether in the extract is closest to the original content in the soil sample, which lays a foundation for the accuracy of subsequent detection.

Description

technical field [0001] The invention belongs to the technical field of pesticide residue analysis, and in particular relates to a method for extracting and purifying octachlorodipropyl ether in soil. Background technique [0002] Octachlorodipropyl ether (S421 for short), chemical name is bis-(2,3,3,3-tetrachloropropyl) ether, molecular formula C 6 h 6 OC l8 . It is light yellow liquid at normal temperature, insoluble in water, soluble in organic solvents such as ethanol, acetone, toluene, etc. Octachlorodipropyl ether is a pesticide synergist, which can activate and synergize a variety of pyrethroid pesticides, and is mostly used in pesticide sprays. Octachlorodipropyl ether is an organochlorine compound whose environmental behavior is similar to that of DDT. Its performance is stable, it stays in the environment for a long time, and it will bioaccumulate in the biological chain, resulting in human and other organisms. Residues are persistent organic pollutants. Accor...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/12
Inventor 吕辉雄蔡全英谭建华田军建曾巧云王慧冼雪晖
Owner SOUTH CHINA AGRI UNIV