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Method for pretreating soil or sediment sample and method for determining dioxin

A sediment and pretreatment technology, which is applied in the field of pollutant monitoring, can solve the problems of high solvent consumption, inability to automate, and long extraction time, and achieve the effects of high extraction efficiency, convenient operation, and reduced solvent consumption

Inactive Publication Date: 2016-09-28
广州普诺环境检测技术服务有限公司
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Problems solved by technology

[0004] For the extraction method, the most commonly used extraction method is the Soxhlet extraction method. Soxhlet extraction is also known as sand extraction. It uses the principle of solvent reflux and siphon to continuously extract the solid matter by pure solvent. All devices are simple. , easy operation and other advantages, but there are also disadvantages such as long extraction time, high solvent consumption and inability to automate
In addition, as far as the evolutionary method is concerned, the current method used for purification of

Method used

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  • Method for pretreating soil or sediment sample and method for determining dioxin

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Embodiment 1

[0035] The pretreatment of embodiment 1 standard soil sample and the mensuration of dioxin in soil

[0036] The embodiment of the present invention provides a method for pretreatment of soil samples and a method for measuring dioxins, comprising the following steps:

[0037] (1) Sample extraction: Weigh 10g of soil sample (quartz sand matrix + standard solution), use the ultrasonic microwave combined reaction system to extract the soil sample to be tested, and obtain the extract containing dioxin, wherein the ultrasonic microwave combined reaction system The operating parameters of the reaction system are: the ultrasonic power is 300W, the ultrasonic duty cycle is 2s, the microwave power is 300W, the temperature is 100°C, the time is 15min, and the reagent is a mixed solution of 40ml n-hexane and dichloromethane (in the mixed solution, The volume ratio of normal hexane and dichloromethane is 1:1); Add 1.0ng to extract internal standard in sample before extraction, described ex...

Embodiment 2

[0051] In order to further illustrate the beneficial effects of the present invention, respectively collect farmland soil (about 2 kilograms) and sediment (about 2 kilograms) within 5 kilometers around a certain waste incineration plant, first naturally air-dry in a dark and ventilated place, and remove the soil after air-drying. For sundries such as stones and plant roots, grind them with a glass mortar and pass through a 2mm sieve. The obtained soil samples are repeatedly divided into quarters until the amount required for analysis (about 100 grams) is left, and then Pass through 60 mesh sieves (0.25mm) after grinding again, transfer to brown glass bottle at last and seal and keep away from light, obtain soil sample and sediment sample respectively; Then, get respectively 10g described soil sample and sediment sample, according to implementation Example 1 step detects dioxins in the soil sample and sediment sample, and the detection results are shown in Table 3 and Table 4. ...

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Abstract

The invention provides a soil or sediment sample pretreatment method and a dioxin determination method. A soil or sediment sample pretreatment method provided by the present invention comprises the following steps: sample extraction, sample purification, nitrogen blowing concentration. A soil or sediment sample pretreatment method and a dioxin determination method provided by the present invention innovatively combine the method of pretreatment of the soil or sediment sample with an ultrasonic and microwave combined reaction system, and purify The one-stage treatment method is simple and easy to implement, and greatly shortens the sample pretreatment time, reduces solvent consumption and cost, and has a very high promotion and application value.

Description

technical field [0001] The invention relates to the technical field of pollutant monitoring, in particular to a method for pretreatment of soil or sediment samples and a method for measuring dioxins. Background technique [0002] The environmental toxicity of dioxin-like substances has been widely concerned by people all over the world. Since the "International Symposium on Dioxins and Environmental Hormones" held in Beijing in October 1998, Chinese scientists have carried out a series of work to challenge this "drug of the century". Since there are many types of dioxin-like compounds, their content in the environment is very low and their existing matrix is ​​complex, and analytical instruments are required to have a low detection limit, the detection of dioxin-like chemical substances is an important aspect of modern analytical chemistry. difficulty. [0003] Before using the instrument to detect dioxins in the sample, the sample must be pretreated to remove the interfer...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/025G01N2030/062
Inventor 李晓明阮晓玲凌烈李冠霖
Owner 广州普诺环境检测技术服务有限公司
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