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A method for simultaneous extraction, purification and detection of chlorinated polycyclic aromatic hydrocarbons in soil

A chlorinated polycyclic aromatic hydrocarbon and synchronous extraction technology, which is applied to measurement devices, instruments, scientific instruments, etc., can solve the problems of poor detection effect, complicated pretreatment of chlorinated polycyclic aromatic hydrocarbons, etc., and achieves short time consumption and wide detection range. Comprehensive, highly automated effects

Active Publication Date: 2016-11-30
NANJING UNIV +1
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  • Description
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  • Application Information

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Problems solved by technology

[0005] Aiming at the problems of complex pretreatment and poor detection effect of chlorinated polycyclic aromatic hydrocarbons in the complex environment existing in the prior art, the present invention provides a method for synchronously extracting, purifying and detecting chlorinated polycyclic aromatic hydrocarbons in soil

Method used

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  • A method for simultaneous extraction, purification and detection of chlorinated polycyclic aromatic hydrocarbons in soil
  • A method for simultaneous extraction, purification and detection of chlorinated polycyclic aromatic hydrocarbons in soil
  • A method for simultaneous extraction, purification and detection of chlorinated polycyclic aromatic hydrocarbons in soil

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Experimental program
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Effect test

Embodiment 1

[0032] Qualitative and quantitative detection of chlorinated polycyclic aromatic hydrocarbons in soil samples was carried out by gas chromatography-mass spectrometry GC-MS. According to the retention time and selected characteristic ions (Table 1), the spectra of the standard compounds ( figure 2 ) comparison, it can be judged whether the compound is contained in the soil sample; according to the target peak area, the concentration of polycyclic aromatic hydrocarbons in the soil sample is calculated by using the external standard method.

[0033] Instruments and reagents:

[0034] Gas chromatograph: American ThermoFisher Company; Chromatographic column: AglientDB-5MS chromatographic column (30m×0.25mm×0.25μm); Carrier gas: helium (purity 99.999%).

[0035] Mass spectrometer: American Thermo Fisher Company.

[0036] Standard stock solution of chlorinated polycyclic aromatic hydrocarbons: prepare standard mixed stock solutions of 6 kinds of chlorinated polycyclic aromatic hydr...

Embodiment 2

[0055] Sampling analysis and detection of chlorinated polycyclic aromatic hydrocarbons in soil in a chemical industrial park.

[0056] Step (a), sample collection and processing: brush off branches, leaves and gravel on the ground surface during sampling. Collect the surface soil of 3-20cm, select the soil at 17 points, wrap the collected soil with tin foil, pre-freeze in the refrigerator at -20°C, freeze-dry with a freeze dryer, grind with a mortar, and pass through 200 mesh metal Sieve and store at -20°C until analysis.

[0057] Steps (b)-(e): Take 5g of the soil sample at each point, according to the blank addition recovery experiment of chlorinated polycyclic aromatic hydrocarbons in the standard soil sample in Example 1, steps (b)-(e) for 17 The soil at each point is treated, and the treated sample solution is subjected to qualitative and quantitative detection by GC-MS. The test results see image 3 .

[0058] Effective extraction and detection of chlorinated polycyc...

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Abstract

The invention discloses a method for synchronously extracting and purifying various chlorinated polycyclic aromatic hydrocarbons in soil, which belongs to the field of detection of the chlorinated polycyclic aromatic hydrocarbons. The method comprises the following steps: firstly removing moisture in a soil sample by virtue of a freezing dryer, grinding the soil sample, and filtering the ground soil sample by virtue of a 200-mesh sieve for later use; and extracting a target matter in the soil sample by utilizing an acceleration solvent extractor, purifying the target matter in a gel permeation chromatography, finally concentrating the target matter and sizing the target matter. According to the method, a preprocessing method of the chlorinated polycyclic aromatic hydrocarbons in the soil is established, less solvent is used in the entire process, the automation degree is high, less time is used, the safety is high, fewer steps are used, and various chlorinated polycyclic aromatic hydrocarbons in the soil can be accurately, qualitatively and quantitatively determined. The chlorinated polycyclic aromatic hydrocarbons in the soil are quantitatively detected by utilizing the gas phase chromatography-mass spectrometry, the detection limit is low (when S / N is equal to 3, the detection limit is 2.6 to 25pg / g), the precision is high (RSD=6.30 to 12.0 percent), the blank mark recovery rate is 64.1 to 109.2 percent, the synchronous analysis and detection of various trace chlorinated polycyclic aromatic hydrocarbons in the complicated environment medium such as the soil can be realized, sensitivity and accuracy can be realized, and the weaknesses of the prior art can be overcome.

Description

technical field [0001] The invention relates to the field of detection of chlorinated polycyclic aromatic hydrocarbons, in particular to a method for synchronously extracting, purifying and detecting chlorinated polycyclic aromatic hydrocarbons in soil. Background technique [0002] Chlorinated polycyclic aromatic hydrocarbons (Cl-PAHs) are polycyclic aromatic hydrocarbons (polycyclic aromatic hydrocarbons, PAHs), aromatic hydrocarbon compounds in which one or more hydrogen atoms on the two rings are replaced by chlorine atoms, from From the structural point of view, it can be called a hybrid of dioxin and polycyclic aromatic hydrocarbons. The formation mechanism is similar to that of dioxin and PAHs, and it is a by-product of human unconscious production. Currently, Cl-PAHs in the environment are mainly by-products of automobile exhaust emissions, organic matter incineration and other industrial activities. Studies have shown that some Cl-PAHs have carcinogenic and mutagen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/14
Inventor 孙成原文婷胡冠久张涛陈素兰高占啓
Owner NANJING UNIV
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