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Method for analyzing hexachloroethane in soil or sediment by purge-and-trap gas chromatography- mass spectrometry

A purging and trapping and hexachloroethane technology, which is applied in analysis materials, material separation, measuring devices, etc., can solve the problems of poor precision and accuracy of measurement results, high detection limit of hexachloroethane, and complicated operation steps. and other problems, to achieve the effect of high accuracy, simple, efficient and accurate analysis, and simple and fast pre-processing

Inactive Publication Date: 2019-11-08
上海纺织节能环保中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These pretreatment methods above all use a large amount of organic solvents, and the operation steps are numerous and complicated, and the extraction time is long, which causes loss to the hexachloroethane in the soil, so that the detection limit of the hexachloroethane in the soil and sediment is relatively high, and the measurement The precision and accuracy of the results are poor and cannot meet the needs of the existing technology

Method used

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  • Method for analyzing hexachloroethane in soil or sediment by purge-and-trap gas chromatography- mass spectrometry
  • Method for analyzing hexachloroethane in soil or sediment by purge-and-trap gas chromatography- mass spectrometry
  • Method for analyzing hexachloroethane in soil or sediment by purge-and-trap gas chromatography- mass spectrometry

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Experimental program
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Effect test

Embodiment 1

[0029] When determining the detection limit of the target compound in soil and sediment, quartz sand is usually used instead. Therefore, prepare 7 sampling bottles, weigh 5g of quartz sand respectively, put them into a rotor, add 5mL blank reagent water, 0.025μg six Chloroethane standard substance and 5 μL internal standard / surrogate mixed standard, analyze the content of hexachloroethane in the quartz sand sample according to the optimal conditions, calculate the standard deviation, method detection limit and other parameters, as shown in Table 1.

[0030] Table 1: Detection limit of hexachloroethane (μg / kg)

[0031] Sample serial number 1 2 3 4 5 6 7 standard deviation Method detection limit Hexachloroethane 4.33 4.18 4.07 3.82 4.83 4.10 4.03 0.32 1.0

[0032] The detection limit refers to the lowest concentration or minimum amount of the substance to be detected that can be qualitatively detected from the sample within a given confiden...

Embodiment 2

[0034] Two self-made soil samples and two self-made sediment samples were selected, and the content of hexachloroethane in the above samples was analyzed according to the optimal conditions, and the average value, standard deviation, relative standard deviation and other parameters were calculated respectively, as shown in Table 2.

[0035] Table 2: Determination of HCH in self-made soil samples and self-made sediment samples (μg / kg)

[0036]

[0037]

[0038] It can be seen from Table 2 that the relative standard deviation (ie precision) reflects the degree of agreement between the measured values ​​obtained by repeated analysis of the same sample. Adopt purge-and-trap-gas chromatography to analyze the hexachloroethane in the sample, and the relative standard deviation (being precision) of 7 times of measurement results is in the scope of 2.8-4.8%, illustrates that this method is more stable, and hexachloroethane is measured The reproducibility of the results is high. ...

Embodiment 3

[0040] Select two kinds of self-made soil samples and two kinds of self-made sediment samples, respectively add a certain amount of hexachloroethane, analyze the content of hexachloroethane in the samples according to the optimal conditions, and calculate the recovery rates of the above-mentioned samples respectively, as shown in Table 3 .

[0041] Table 3: Determination of HCH in self-made soil samples and self-made sediment samples (μg / kg)

[0042] Sample serial number Soil sample 1 Soil sample 2 Sediment Sample 1 Sediment Sample 2 1 9.55 25.21 9.58 25.56 2 9.38 23.16 9.48 23.06 average value 9.47 24.19 9.53 24.31 Content before adding standard (μg / kg) 4.78 4.78 4.76 4.76 Determination of spiked amount (μg / kg) 4.69 19.41 4.77 19.55 Theoretical scalaring amount (μg / kg) 5.00 20.00 5.00 20.00 Standard recovery (%) 93.8 97.1 95.4 97.8

[0043] It can be seen from Table 3 that the recovery rate of ...

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Abstract

The invention provides a method for analyzing hexachloroethane in soil or sediment by purge-and-trap gas chromatography- mass spectrometry. The method comprises the following steps of performing purge-and-trap extraction on the hexachloroethane in the soil or sediment to obtain extracted hexachloroethane; and analyzing the extracted hexachloroethane by a gas chromatography-mass spectrometry device. The invention provides simple, high-efficient and accurate method for analyzing the hexachloroethane in the soil or sediment, purge-and-trap can be performed on the hexachloroethane in the soil or sediment, the pre-processing is simple and rapid, the semi-volatile organic compound in the soil or sediment can be effectively purged, no organic solvent is needed for extraction, so that the enrichment efficiency is high, and the method is a high-efficiency pre-processing method. The hyxachloroethane in the coil or sediment is analyzed by the gas chromatography-mass spectrometry device, and the method has the characteristics of low detection limit, high accuracy, rapidness and sensitivity.

Description

technical field [0001] The invention belongs to the technical field of analyzing hexachloroethane in soil and sediment, and in particular relates to a method for analyzing hexachloroethane in soil or sediment by purge and trap gas chromatography. Background technique [0002] Hexachloroethane is the most toxic of chlorinated hydrocarbons. It has toxic effects on the human central nervous system and is a carcinogen. Hexachloroethane has a high boiling point. It is not easy to chemically decompose and biodegrade after being adsorbed in the soil. It is easy to enter the human body through the food chain and endanger human health. Therefore, it is very important to study and analyze the residues of Hexachloroethane in soil. At present, inspectors generally use the detection standard of "HJ834-2017 Determination of Semi-volatile Organic Compounds in Soil and Sediment by Gas Chromatography-Mass Spectrometry" to analyze HCH in soil and sediment. Due to the complexity of the soil m...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 胡丽雅
Owner 上海纺织节能环保中心
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