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Detection method of gas chromatography-electron capture detector of halogenated benzoquinone

A halogenated benzoquinone and electron capture technology, which is applied in the direction of instruments, measuring devices, scientific instruments, etc., can solve the problems of inability to detect, high test cost, lack of testing instruments in the laboratory, etc., achieve low detection limit, convenient operation, The effect of high sensitivity

Inactive Publication Date: 2018-09-28
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has some limitations, the test cost is relatively high, and more expensive liquid chromatography / mass spectrometers are required
Laboratories in many parts of our country (especially remote areas with backward economy and technology) cannot perform testing due to lack of corresponding testing instruments

Method used

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  • Detection method of gas chromatography-electron capture detector of halogenated benzoquinone
  • Detection method of gas chromatography-electron capture detector of halogenated benzoquinone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The gas chromatography-electron capture detector detection method of halogenated benzoquinone comprises the steps:

[0021] 1) Use methyl tert-butyl ether as solvent to prepare standard substance 2,6-dichloro-1,4-benzene with gradient concentration ranging from 2, 5, 10, 15, 20, 30 μg / L in the sampling bottle The quinone solution is a series of standard solutions, which are respectively placed in the sampling tray of the gas chromatograph, and the methyl tert-butyl ether in the blank sampling bottle and the sample in the sampling bottle are extracted by the method of automatic sampling, and detected by electron capture. The detector is used to detect and record the spectrum; determine the peak time of the standard; draw the standard curve between the peak area and the concentration according to the gas chromatograms obtained by the standard solutions of different concentrations, and obtain the linear relationship between the peak area and the concentration, see figure 1...

Embodiment 2

[0031] The gas chromatography-electron capture detector detection method of halogenated benzoquinone is characterized in that comprising the steps:

[0032] 1) with embodiment 1 step 1);

[0033] 2) The tap water sample to be tested in a city in northern China was filtered through a 0.45 μm filter membrane and poured into a brown reagent bottle, and the pH was adjusted to 3.3 with formic acid;

[0034] 3) Put 200mL of the water sample obtained in step 2) into a brown reagent bottle, add 30g of sodium sulfate that has been dried in a constant temperature drying oven, shake to dissolve, add 20mL of methyl tert-butyl ether as an extract and shake on a shaker Extract for 5 minutes, stand still to separate the layers, take the upper layer and blow it to 0.5mL with nitrogen flow at room temperature, then dilute it to 1mL with methyl tert-butyl ether, and transfer it to a gas-phase sampling bottle;

[0035] 4) Put the gas-phase sampling bottle obtained in step 3) into the sample tra...

Embodiment 3

[0040] The gas chromatography-electron capture detector detection method of halogenated benzoquinone is characterized in that comprising the steps:

[0041] 1) with embodiment 1 step 1);

[0042] 2) Filter the sterilized effluent from a sewage treatment plant in a city in northern China through a 0.45 μm filter membrane and pour it into a brown reagent bottle, and adjust the pH to 3.1 with formic acid;

[0043] 3) Put 200mL of the water sample obtained in step 2) into a brown reagent bottle, add 50g of sodium sulfate that has been dried in a constant temperature drying oven, shake to dissolve, add 30mL of methyl tert-butyl ether as an extract and shake on a shaker Extract for 10 min, stand still to separate the layers, take the upper layer and blow it to 0.5 mL with nitrogen flow at room temperature, then dilute to 1 mL with methyl tert-butyl ether, and transfer it to a gas-phase sampling bottle;

[0044] 4) the gas-phase sampling bottle obtained by step (3) is put into the s...

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Abstract

The invention discloses a detection method of a gas chromatography-electron capture detector of halogenated benzoquinone. The detection method comprises the following steps that (1) a standard halogenated benzoquinone solution is prepared as a series standard solution, the gas chromatography-electron capture detector detects the series standard solution, and a standard curve between peak area andconcentration is drawn; (2) a to-be-detected water sample is filtered, and a pH value is adjusted; (3) the filtered to-be-detected water sample is placed in a brown reagent bottle, dried sodium sulfate is added and dissolved, an extraction liquid is added, standing is carried out so as to generate delamination, the upper layer liquid nitrogen airflow is taken and blown, then methyl tertiary butylether is used for performing constant volume, and the upper layer liquid nitrogen airflow is transferred to a gas phase sample inlet bottle; (4) the obtained gas phase sample inlet bottle in step (3)is detected by the gas chromatography-electron capture detector, and an atlas is recorded; (5) in the to-be-detected sample, a chromatographic peak is found out according to the peak outlet time, thechromatographic peak is integrated to obtain the peak area, and according to the obtained standard curve in step (1) and corresponding recovery rate, the content of halogenated benzoquinone in the to-be-detected sample is obtained. The detection method of the gas chromatography-electron capture detector of the halogenated benzoquinone has the advantages that the cost is lower, the operation is simple, the sensitivity is high, and the measuring is simultaneous.

Description

technical field [0001] The invention belongs to the technical field of detecting trace pollutants in water, and in particular relates to a gas chromatography-electron capture detector detection method for halogenated benzoquinones. Background technique [0002] With the improvement of detection technology, aromatic disinfection by-products (Disinfection By-products, DBPs) with more complex structures were discovered and attracted people's attention. Halogenated benzoquinones are a new type of aromatic DBPs that are currently being concerned, and are detected in drinking water and swimming pools. 2,6-dichloro-1,4-benzoquinone and 2,6-dibromo-p-benzoquinone in halogenated benzoquinones are widely present in disinfected drinking water, and are more common than conventional carbon-containing disinfection by-products (trihalogenated Methane, haloacetic acid) have stronger cytotoxicity and genotoxicity. However, the concentration of 2,6-dichloro-1,4-benzoquinone and 2,6-dibromo-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/70
CPCG01N30/02G01N30/06G01N30/70G01N2030/062
Inventor 翟洪艳于珊珊闫雨薇顾昕
Owner TIANJIN UNIV
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