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A kind of pretreatment method of soil sample and its determination method of dioxin in soil

A soil sample and pretreatment technology, applied in measuring devices, instruments, scientific instruments, etc., can solve problems such as difficulties in research and evaluation of dioxin pollution, high technical requirements for testing personnel, low dioxin content, etc. Processing time, improved detection accuracy, and good selectivity

Active Publication Date: 2020-08-18
安徽众诚环境检测有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] The content of dioxin in nature is extremely low, far below the detection limit and quantification limit of modern analytical instruments, and its molecular structure has strong adsorption and burial properties, and it is easy to enter other substances, such as the internal deep structure of soil Long-term accumulation has brought double difficulties to the research and evaluation of dioxin pollution
However, due to the harsh extraction conditions and high technical requirements for inspectors, there are also disadvantages of high extraction costs

Method used

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  • A kind of pretreatment method of soil sample and its determination method of dioxin in soil
  • A kind of pretreatment method of soil sample and its determination method of dioxin in soil

Examples

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Effect test

Embodiment 1

[0031] A kind of determination method of dioxin in soil, the pretreatment process of soil sample comprises the following steps:

[0032] S1. Air-dry the soil sample, grind and sieve it, add solvent, vortex, heat to 35°C for ultrasonic extraction, let it stand, and centrifugally filter the filtrate, blow it with nitrogen until it is nearly dry to obtain the pre-extraction solution;

[0033] S2. Disperse the magnetic nanomaterials in an organic solvent, leave it still after ultrasonication, pour off the organic solvent, add the pre-extracted solution obtained in S1, add distilled water to dilute, add hydrochloric acid solution to adjust the pH to 3.0, oscillate, and pour off the upper layer after centrifugation , eluting with a washing solvent, collecting the eluate to obtain an extract;

[0034] S3, purifying the extract with a silica gel column, blowing nitrogen to concentrate, and obtaining a purification sample to be tested containing dioxin;

[0035] After pretreatment of ...

Embodiment 2

[0037] A kind of determination method of dioxin in soil, the pretreatment process of soil sample comprises the following steps:

[0038] S1. Air-dry the soil sample, grind and sieve it, add a solvent, vortex, heat to 45°C for ultrasonic extraction, let it stand, and centrifugally filter the filtrate and blow it with nitrogen until it is nearly dry to obtain a pre-extraction solution;

[0039] S2. Disperse the magnetic nanomaterials in an organic solvent, leave it still after ultrasonication, pour off the organic solvent, add the pre-extracted solution obtained in S1, add distilled water to dilute, add hydrochloric acid solution to adjust the pH to 4.0, oscillate, and pour off the upper layer after centrifugation , eluting with a washing solvent, collecting the eluate to obtain an extract;

[0040] S3, purifying the extract with a silica gel column, blowing nitrogen to concentrate, and obtaining a purification sample to be tested containing dioxin;

[0041] Wherein, in S1, the...

Embodiment 3

[0045] A kind of determination method of dioxin in soil, the pretreatment process of soil sample comprises the following steps:

[0046] S1. Air-dried the soil sample, crushed and sieved, added solvent, vortexed, heated to 40°C for ultrasonic extraction, left to stand, centrifugally filtered, and the filtrate was blown with nitrogen to nearly dry to obtain the pre-extraction solution;

[0047] S2. Disperse the magnetic nanomaterials in an organic solvent, leave it still after ultrasonication, pour off the organic solvent, add the pre-extracted solution obtained in S1, add distilled water to dilute, add hydrochloric acid solution to adjust the pH to 3.5, oscillate, and pour off the upper layer after centrifugation , eluting with a washing solvent, collecting the eluate to obtain an extract;

[0048] S3, purifying the extract with a silica gel column, blowing nitrogen to concentrate, and obtaining a purification sample to be tested containing dioxin;

[0049] Among them, in S1,...

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Abstract

The invention discloses a soil sample pretreatment method, which includes the following steps: (S1) after being air-dried, a soil sample is ground, screened, added into a solvent vortex, heated to 35 DEG C to 45 DEG C, ultrasonically extracted, kept still and centrifugally filtered, filtrate is extracted, and after the filtrate is blown by nitrogen to be almost dry, a pre-extracted solution is obtained; (S2) a magnetic nanomaterial is dispersed into organic solvent, and is kept still after being ultrasonically treated, the organic solvent is poured out, the pre-extracted solution obtained in S1 is added, distilled water is added for dilution, hydrochloric acid solution is added to regulate pH to 3.0 to 4.0, oscillation is carried out, supernate is poured out after centrifuging, cleaning solvent is used for elution, eluent is collected, and thereby an extracted solution is obtained; (S3) the extracted solution is purified by a silica gel column, nitrogen is blown for concentration, and thereby a to-be-tested purified sample containing dioxin is obtained. The invention further proposes a determination method for dioxin in soil. The invention adopts ultrasonic extraction and magnetic nanomaterial-silica gel column joint purification, consequently, the time of pretreating a soil sample is saved, and the efficiency of detecting dioxin content in soil is increased.

Description

technical field [0001] The present invention relates to the technical field of pretreatment methods for the determination of dioxins in soil, in particular to a pretreatment method for soil samples and a method for the determination of dioxins in soil. Background technique [0002] The content of dioxin in nature is extremely low, far below the detection limit and quantification limit of modern analytical instruments, and its molecular structure has strong adsorption and burial properties, and it is easy to enter other substances, such as the internal deep structure of soil Long-term accumulation has brought double difficulties to the research and evaluation of dioxin pollution. Therefore, whether the dioxins hidden in the carrier can be completely extracted is one of the key technologies urgently needed to be solved for the detection of dioxins in the soil. [0003] The commonly used dioxin extraction method is Soxhlet extraction, which has the advantages of high extractio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/14G01N30/02G01N30/72
CPCG01N30/02G01N30/06G01N30/14G01N30/72
Inventor 吕光辉孙小妹
Owner 安徽众诚环境检测有限公司
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