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Solid phase membrane extraction-gas chromatography detection method for chlorobenzene compounds in water body

A technology of gas chromatography and detection method, which is applied in the field of solid-phase membrane extraction gas chromatography detection of chlorobenzene compounds in water, and achieves the effects of simple operation, satisfactory recovery rate and reproducibility, and high sensitivity

Inactive Publication Date: 2013-11-20
MARINE FISHERIES RES INST OF ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, according to the current domestic and foreign literature, there is no report on the combination of solid-phase membrane extraction technology and gas chromatography electron capture detection method for the detection of 11 chlorobenzene compounds in water.

Method used

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  • Solid phase membrane extraction-gas chromatography detection method for chlorobenzene compounds in water body
  • Solid phase membrane extraction-gas chromatography detection method for chlorobenzene compounds in water body
  • Solid phase membrane extraction-gas chromatography detection method for chlorobenzene compounds in water body

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Step (1). Sampling and sample preparation:

[0052] The collected water samples were filtered through a polyvinylidene fluoride microporous membrane with a pore size of 0.45 μm, stored in a brown glass bottle, and the pH value of the water samples was adjusted to 2.5 to obtain a pretreated water sample.

[0053] Step (2). Solid phase membrane extraction:

[0054] 2-1. The solid-phase extraction membrane needs to be activated before use. The specific activation operation is as follows: the solid-phase extraction membrane is first rinsed with 20mL of ethyl acetate and 10mL of acetone, and then activated with 20mL of methanol and 20mL of double-distilled water to obtain Activated solid-phase extraction membrane; during the activation of the solid-phase extraction membrane, the solid-phase extraction membrane should not be exposed to air.

[0055] 2-2. During extraction, take 500mL of pretreated water sample and pass it through the activated solid-phase extraction membrane...

Embodiment 2

[0084] Embodiment 2. Determination of 11 kinds of chlorobenzene compounds in Wahaha purified water

[0085] (1) Sampling and sample preparation: Wahaha purified water is passed through a 0.45 μm polyvinylidene fluoride microporous filter membrane

[0086] After filtering, store in a 500mL brown glass bottle and adjust its pH to 2.5.

[0087] Add standard Wahaha purified water: add dichlorobenzene 0.8mg / L, trichlorobenzene 0.088mg / L, tetrachlorobenzene 0.02mg / L, pentachlorobenzene and hexachlorobenzene to 500mL processed Wahaha purified water 0.01mg / L chlorobenzene compound standard mixed solution 12.5μL, the obtained concentration is 0.02μg / L of dichlorobenzene, 0.0022μg / L of trichlorobenzene, 0.0005μg / L of tetrachlorobenzene, pentachlorobenzene and hexachlorobenzene Wahaha purified water spiked at 0.00025 μg / L.

[0088] (2) Solid-phase membrane extraction: before use, the solid-phase extraction membrane was rinsed with 20mL ethyl acetate and 10mL acetone, and then activated...

Embodiment 3

[0094] Embodiment 3. The mensuration of 11 kinds of chlorobenzene compounds in laboratory tap water

[0095] (1) Sampling and sample preparation: After the tap water in the laboratory is filtered through a 0.45 μm polyvinylidene fluoride microporous membrane, it is stored in a 500 mL brown glass bottle, and its pH value is adjusted to 2.5.

[0096] Add standard laboratory tap water: add dichlorobenzene 0.8mg / L, trichlorobenzene 0.088mg / L, tetrachlorobenzene 0.02mg / L, pentachlorobenzene and hexachlorobenzene to 500mL treated laboratory tap water 0.01mg / L chlorobenzene compound standard mixed solution 62.5μL, the obtained concentration is 0.1μg / L of dichlorobenzene, 0.011μg / L of trichlorobenzene, 0.0025μg / L of tetrachlorobenzene, pentachlorobenzene and hexachlorobenzene Benzene is 0.00125μg / L spiked laboratory tap water.

[0097] (2) Solid-phase membrane extraction: before use, the solid-phase extraction membrane was rinsed with 20mL ethyl acetate and 10mL acetone, and then act...

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Abstract

The present invention relates to a solid phase membrane extraction-gas chromatography detection method for chlorobenzene compounds in water body. The method comprises the steps of gathering 500 mL of a water sample with a pH value of 2.5 by flowing through a C18 solid phase extraction membrane at a flow rate of 5-50 mL / min; then eluting with 5 mL of acetone and 3*5 mL of dichloromethane; drying an elution by rotary evaporation; dissolving by n-hexane; diluting to 1 mL; introducing 1 [mu]L of the product into a gas chromatography-electron capture detector for the detection. A detection limit of eleven chlorobenzene compounds ranges from 0.05 ng / L to 4 ng / L; recovery rate ranges from 91% to 115%; and relative standard deviation (n=5) is 3.6-7.6%. The detection method is simple and sensitive, has wide linearity range, good repeatability and high recovery rate, and can rapidly determine concentrations of the chlorobenzene compounds in the water body.

Description

technical field [0001] The invention belongs to the technical field of water pollution detection and relates to 1,4-dichlorobenzene, 1,3-dichlorobenzene, 1,2-dichlorobenzene, 1,3,5-trichlorobenzene, 1, 2,4-Trichlorobenzene, 1,2,3-Trichlorobenzene, 1,2,3,5-Tetrachlorobenzene, 1,2,4,5-Tetrachlorobenzene, 1,2,3,4- Solid-phase membrane extraction-gas chromatography electron capture detection method for 11 kinds of chlorobenzene compounds including tetrachlorobenzene, pentachlorobenzene and hexachlorobenzene. Background technique [0002] In recent decades, chlorobenzene compounds have been widely used in the chemical synthesis of pesticides, medicines, dyes, plastics, and other chemical products, which are widely distributed in the aquatic environment due to uncontrolled wastewater release and industrial atmospheric emissions. Chlorobenzene compounds are lipophilic compounds with stable chemical properties and are not easy to degrade. Long-term inhalation may cause liver cancer...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 胡红美郭远明李铁军尤炬炬钟志孙秀梅
Owner MARINE FISHERIES RES INST OF ZHEJIANG
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