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Method for catching and detecting static headspace gas chromatography electrons of eleven chlorobenzene compounds in water

A technology of electron capture detection and headspace gas chromatography, which is applied to measurement devices, instruments, scientific instruments, etc. Determination of chlorobenzene, 1,2-dichlorobenzene, 1,3-dichlorobenzene, 1,4-dichlorobenzene, 1,2,4-trichlorobenzene by headspace gas chromatography electron capture detection method reported by chlorobenzene and Han Changmian et al. Chlorine and other problems, to achieve the effect of accurate results, high degree of automation and simple operation

Inactive Publication Date: 2014-04-16
MARINE FISHERIES RES INST OF ZHEJIANG
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, after reviewing the current domestic and foreign literature, except for the headspace gas chromatography hydrogen flame ionization detection method reported by Che Xuan for the determination of chlorobenzene, 1,2-dichlorobenzene, 1,4-dichlorobenzene, 1,2,4- Headspace gas chromatography electron capture detection method reported by trichlorobenzene and Han Changmian et al. for the determination of chlorobenzene, 1,2-dichlorobenzene, 1,3-dichlorobenzene, There are a few literatures such as trichlorobenzene, but there is no report on the combination of static headspace technology and gas chromatography electron capture detection method for the detection of 11 chlorobenzene compounds

Method used

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  • Method for catching and detecting static headspace gas chromatography electrons of eleven chlorobenzene compounds in water
  • Method for catching and detecting static headspace gas chromatography electrons of eleven chlorobenzene compounds in water
  • Method for catching and detecting static headspace gas chromatography electrons of eleven chlorobenzene compounds in water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: Determination of 11 kinds of chlorobenzene compounds in Wahaha purified water

[0033] (1) Sampling: Measure 10.00 mL of Wahaha purified water or 10.00 mL of spiked Wahaha purified water containing a certain amount of chlorobenzene compounds (see Table 2 for the content of chlorobenzene compounds) in a 20 mL headspace bottle, and make The gas-liquid volume ratio in the headspace bottle is 1:1, add 2.00 g of sodium chloride, and immediately use the headspace bottle mouth sealer to cover the bottle mouth of the headspace bottle with an aluminum cap with a silicone pad coated with a polytetrafluoroethylene film inside. Seal it; vortex with a vortex shaker to dissolve sodium chloride so that the concentration of added sodium chloride is 20% (v / w), and place the sample on a 32-position headspace sampler.

[0034] (2) Setup and operation of the static headspace sampling program: the static headspace sampling conditions were an equilibrium temperature of 70°C, an eq...

Embodiment 2

[0038] Embodiment 2: the mensuration of 11 kinds of chlorobenzene compounds in laboratory tap water

[0039] (1) Sampling: Measure 10.00 mL of laboratory tap water or 10.00 mL of spiked laboratory tap water containing a certain amount of chlorobenzene compounds (see Table 2 for the content of chlorobenzene compounds) in a 20 mL headspace bottle, and make The gas-liquid volume ratio in the headspace bottle is 1:1, add 2.00 g of sodium chloride, and immediately use the headspace bottle mouth sealer to cover the bottle mouth of the headspace bottle with an aluminum cap with a silicone pad coated with a polytetrafluoroethylene film inside. Seal it; vortex with a vortex shaker to dissolve sodium chloride so that the concentration of added sodium chloride is 20% (v / w), and place the sample on a 32-position headspace sampler.

[0040] (2) Setup and operation of the static headspace sampling program: the static headspace sampling conditions were an equilibrium temperature of 70°C, an ...

Embodiment 3

[0044] Embodiment 3: Determination of 11 kinds of chlorobenzene compounds in seawater of Zhoushan sea area

[0045] (1) Sampling: Measure 10.00 mL of seawater from Zhoushan sea area or 10.00 mL of spiked seawater from Zhoushan sea area containing a certain amount of chlorobenzene compounds (see Table 2 for the content of chlorobenzene compounds) in a 20 mL headspace bottle. The gas-liquid volume ratio in the headspace bottle is 1:1, add 2.00 g of sodium chloride, and immediately use the headspace bottle mouth sealer to cover the bottle mouth of the headspace bottle with an aluminum cap with a silicone pad coated with a polytetrafluoroethylene film inside. Seal it; vortex with a vortex shaker to dissolve sodium chloride so that the concentration of added sodium chloride is 20% (v / w), and place the sample on a 32-position headspace sampler.

[0046] (2) Setup and operation of the static headspace sampling program: the static headspace sampling conditions were an equilibrium temp...

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Abstract

The invention discloses a method for catching and detecting static headspace gas chromatography electrons of eleven chlorobenzene compounds in water, which belongs to the field of a water pollution detection technology. Eleven chlorobenzene compounds are as follows: 1, 4-dichlorobenzene, 1, 3-dichlorobenzene, 1, 2-dichlorobenzene, 1, 3, 5-trichlorobenzene, 1, 2, 4-trichlorobenzene, 1, 2, 3-trichlorobenzene, 1, 2, 3, 4, 5-tetrachlorobenzene, 1, 2, 4, 5-tetrachlorobenzene, pentachlorobenzene and hexachlorobenzene. According to the method, a water sample containing 20% of sodium chloride is added into a 20mL of headspace bottle, an aluminium cover containing PTFE (polytetrafluoroethylene) is utilized to seal instantly, and 800 [mu] L of gas in a top space of the headspace bottle is taken to detect in a gaschromatograph after the headspace bottle added with the water sample is balanced with the vibrating speed of 500rpm for 30 min at 70 DEG C. A detection limit of the eleven chlorobenzene compounds is 0.0002-0.04 [mu] g / L, and the recovery rate is 83-116%. The method provided by the invention is environmentally friendly, free of organic solvent, simple to operate, wide in linear range, good in repeatability, high in recovery rate and is capable of quickly detecting the concentration of the chlorobenzene compounds in water.

Description

technical field [0001] The invention relates to 1,4-dichlorobenzene, 1,3-dichlorobenzene, 1,2-dichlorobenzene, 1,3,5-trichlorobenzene, 1,2,4-trichlorobenzene in water , 1,2,3-Trichlorobenzene, 1,2,3,5-Tetrachlorobenzene, 1,2,4,5-Tetrachlorobenzene, 1,2,3,4-Tetrachlorobenzene, Pentachlorobenzene 1. The static headspace gas chromatography electron capture detection method of 11 kinds of chlorobenzene compounds of hexachlorobenzene belongs to the technical field of water pollution detection. 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. They have been...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 胡红美郭远明孙秀梅钟志金衍健丁跃平鲍静姣尤炬炬
Owner MARINE FISHERIES RES INST OF ZHEJIANG
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