Method for simultaneously extracting and purifying plurality of types of chlorinated polycyclic aromatic hydrocarbons in soil

A technology for chlorinated polycyclic aromatic hydrocarbons and soil purification, applied in measuring devices, instruments, scientific instruments, etc., can solve problems such as large consumption of organic solvents, poor detection effect, complicated pretreatment of chlorinated polycyclic aromatic hydrocarbons, etc., and achieve simultaneous extraction Effect

Inactive Publication Date: 2016-08-17
HENAN UNIV OF URBAN CONSTR
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0004] In view of the existing difficulties in the detection of various chlorinated polycyclic aromatic hydrocarbons in soil, the present invention provides a method for synchronously extracting and purifying various chlorinated polycyclic aromatic hydrocarbons in soil, and optimizes the pretreatment conditions of each extraction and purification, thereby overcoming Problems of complex pre-treatment of chlorinated polycyclic aromatic hydrocarbons in complex environments, large consumption of organic solvents, and poor detection results

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1: the detection of standard sample:

[0027] Step 1: Preparation of standard samples: Take 100 μl of 1000 μg / ml mixed stock solution and dilute it to 10 ml with n-hexane to prepare 10 μg / ml standard solution for future use. Take 1ml, 800μl, 500μl, 200μl, 100μl, 50μl, 20μl, 10μl, 5μl, 1μl of the 10μg / ml standard solution and dilute it to 10ml with n-hexane, and the prepared concentrations are 1000ng / ml, 800ng / ml, 500ng / ml respectively. ml, 200ng / ml, 100ng / ml, 50ng / ml, 10ng / ml, 5ng / ml, 1ng / ml mixed solution.

[0028] Step 2: Perform GC-MS detection on the mixed standard solution of each concentration above, set the chromatographic conditions as follows: flow rate 1 mL / min; inlet temperature 250°C, injection volume 1 μL, pulse splitless injection; chromatographic column initial The temperature was 80°C, kept for 1 min, then raised to 200°C at 25°C / min, kept for 0 min; then raised to 213°C at a rate of 1°C / min, and kept for 1 min. Transfer line temperature 280...

Embodiment 2

[0030] Example 2 Blank spike recovery experiment of chlorinated polycyclic aromatic hydrocarbons in standard soil samples:

[0031] Step 1: Take 13 parts of 5g freeze-dried and sieved soil samples, add 100 μl, 1 μg / ml chlorinated polycyclic aromatic hydrocarbon mixed solution to 6 parts, add 1 mL, 1 μg / ml chlorinated polycyclic aromatic hydrocarbons to the other 6 parts Aromatics mixed solution, the last one without solution, as a blank control.

[0032] Step 2: Put 13 samples into the ASE extraction cell, under the conditions of 1500 psi pressure, extraction solvent ultrapure water: acetone (3:1, v / v), 150°C extraction temperature, static extraction for 5 min, cycle The number of times is 3 times, and the extraction cell is flushed with 90% of the solvent of the extraction cell volume, and finally purged with nitrogen for 110 s. After the extraction, the extract was collected, diluted 5 times, and then purified and enriched by SPE in the next step.

[0033] Step 3: SPE enrich...

Embodiment 3

[0037] Example 3 Sampling analysis and detection of chlorinated polycyclic aromatic hydrocarbons in soil in a certain chemical industry park:

[0038] Step 1, sample collection and processing: brush off the branches, leaves and gravel on the surface layer when sampling. Collect about 3-20 cm topsoil, wrap it in tin foil paper, transport it back to the laboratory, pre-freeze it in a refrigerator at -20°C, freeze-dry it with a freeze dryer, grind it with a mortar, pass it through a 200-mesh metal sieve, and store it at -20°C. Stored at °C until analysis.

[0039] Step 2: Take 5g of soil samples at each point, and perform pretreatment on the samples according to the sample pretreatment method in Step 2 to Step 4 in Example 2.

[0040] Step 3: The processed sample solution is subjected to qualitative and quantitative detection by GC-MS according to Step 5 in Example 2.

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Abstract

The invention relates to a method for simultaneously extracting and purifying a plurality of types of chlorinated polycyclic aromatic hydrocarbons in soil. The method comprises the following steps of: pre-treating a soil sample, namely putting a pre-frozen soil sample into a freezing dryer, and freeze-drying to remove moisture; grinding the freeze-dried soil sample and sieving with a 200-mesh sieve to prepare soil for later use; accelerating solvent extraction; extracting a target matter by utilizing a water solution under high temperature and high pressure to obtain an extracting solution; after diluting the extracting solution for 5 times, carrying out concentration and purification by adopting an Oasis HLB solid-phase extraction column; carrying out rotary evaporation and nitrogen blowing concentration on the concentrated and purified extracting solution; after replacing a solvent, making the volume constant; then transferring the extracting solution into a small bottle for detecting; and detecting the sample in the small bottle by utilizing a gas chromatographic-mass spectrometry. By combining a plurality of types of technologies including subcritical water solution-solvent extraction acceleration, solid-phase extraction, concentration and purification, and gas chromatographic-mass spectrometry detection and the like, simultaneous extraction, purification and determination of eight types of the chlorinated polycyclic aromatic hydrocarbons in the soil can be realized.

Description

technical field [0001] The invention relates to the popularization and application of a method for synchronously extracting and purifying chlorinated polycyclic aromatic hydrocarbons in soil, in particular to a method for synchronously extracting and purifying various chlorinated polycyclic aromatic hydrocarbons in soil. Background technique [0002] Chlorinated polycyclic aromatic hydrocarbons (Cl-PAHs) are aromatic hydrocarbon compounds in which one or more hydrogen atoms of polycyclic aromatic hydrocarbons (PAHs, ≥3 rings) are replaced by chlorine atoms. It can be regarded as a hybrid of dioxins and PAHs. Cl-PAHs can be generated from vehicle exhaust emissions, solid waste incineration, fossil fuel combustion, extensive dismantling of electronic waste, and other chlorine-containing chemical industrial processes. Cl-PAHs are very stable and persistent in the environment. Toxicological studies have shown that Cl-PAHs have carcinogenic, teratogenic, and mutagenic toxicity ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/025G01N2030/062G01N2030/126
Inventor 吴俊峰王现丽杜敬方冰郭一飞张岩康海彦谭水成袁英贤刘彪朱新锋牛云峰宋丰明朱慧杰何亚丽尹玉先武晓刚
Owner HENAN UNIV OF URBAN CONSTR
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