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Soil analysis method with coupling of solid-liquid extraction and solid phase microextraction

An analysis method and extraction technology, which are applied in the analysis field of solid-liquid extraction coupled with solid-phase microextraction, can solve the problems of high detection limit, inability to analyze semi-volatile organic compounds, time-consuming and labor-intensive analysis process, etc., so as to reduce costs and workload. Effect

Inactive Publication Date: 2015-12-16
迪天环境技术南京股份有限公司
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Problems solved by technology

[0005] The technical problem to be solved by the present invention is: the detection limit of the existing semi-volatile organic compounds in the soil is generally high, and the semi-volatile organic compounds in the soil cannot be analyzed under natural conditions; or the analysis process is very time-consuming and laborious

Method used

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Embodiment

[0014] Example: 1) Weigh 20g of sample (sample configuration method is attached), wrap it with filter paper and put it into a device such as Soxhlet extraction or accelerated solvent extraction.

[0015] 2) Extraction solvent Use acetone and dichloromethane (pesticide residue analysis grade, should be degassed before use, each 150mL) to extract the soil sample to obtain 300mL of extract.

[0016] 3) Take 5ml from the extract and put it into a volumetric flask, add 100ul internal standard intermediate use solution (internal standard stock solution 2mg / mL, phenanthrene-d10, naphthalene-d12, pyrene-d12, 1,4- Dichlorobenzene-d4) and substitutes (nitrobenzene-d5, 2-fluorobiphenyl, phenol-d5, terphenyl-d14), so that both the internal standard and the substitutes have a concentration of 10ug / ml.

[0017] 4) Use a solid-phase microextraction device to perform secondary extraction, purification, and concentration on the 5 mL extract solution added with internal standards and substitute...

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Abstract

The invention discloses a soil analysis method with coupling of solid-liquid extraction and solid phase microextraction. The method mainly comprises the following steps: weighing a certain quantity of soil sample, packaging with filter paper and then putting into an extracting device; extracting the soil sample with an extracting solvent to obtain an extracting solution; quantitatively adding the extracting solution obtained in the last step to a volumetric flask, adding an internal standard intermediate working solution and a substitution with certain concentration to the volumetric flask to obtain mixed liquor 1; carrying out secondary extracting, purifying and concentrating on the mixed liquor 1 by using a solid phase microextraction device to obtain mixed liquor 2; analyzing the mixed liquor 2 by using the solid phase microextraction device and a gas chromatography-mass spectrometer; repeatedly measuring a parallel sample and a gradient labeling sample and computing the detection limit and the accuracy. According to the invention, solid-liquid extraction is coupled with solid phase microextraction for the first time, so that the method is suitable for analyzing trace semi-volatile organic compounds in the soil, and is low in cost, small in work load and low in detection limit.

Description

technical field [0001] The invention relates to an extraction method applied to the analysis of trace organic matter, in particular to an analysis method of solid-liquid extraction coupled with solid-phase microextraction for analyzing semi-volatile organic matter in soil. Background technique [0002] Semi-volatile organic compounds are a large class of organic compounds that are slower to volatilize than volatile organic compounds. They are easier to migrate and transform in soil, air, biological and other media, exist in the soil for a long time, and endanger human health through bioaccumulation; their environment The destination is usually soil and sediment. The commonality of this type of organic matter is that it is fat-soluble and easily soluble in organic solvents, but there are also highly polar ones that are slightly soluble in water (such as aniline, esters, aldehydes and ketones, etc.). Due to the large molecular weight and high boiling point of semi-volatile org...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
Inventor 秦丰林张燕
Owner 迪天环境技术南京股份有限公司
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