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Method for simultaneously determining aniline, nitrobenzene and polycyclic aromatic hydrocarbon in soil

A technology of polycyclic aromatic hydrocarbons and nitrobenzene, which is applied in the field of simultaneous determination of nitrobenzene and aniline and polycyclic aromatic hydrocarbons in soil, can solve the problems of limiting soil pollution detection efficiency, cumbersome operation steps, and unsuitable for popularization and use, and achieve optimal temperature rise Speed, improved analysis efficiency, equivalent detection limit

Inactive Publication Date: 2021-10-26
SHANDONG INST OF GEOPHYSICAL & GEOCHEM EXPLORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aniline, nitrobenzene, and polycyclic aromatic hydrocarbons belong to the semi-volatile organic compounds in the basic items of the "Soil Environmental Quality Construction Land Soil Pollution Risk Control Standard" (GB36600-2018), and are also pollutants with a high detection rate in polluted site surveys. However, the current detection methods for the three types of substances have certain limitations. Aniline substances can be quantitatively analyzed by liquid chromatography-triple quadrupole mass spectrometry, but the operation steps are cumbersome, the extraction efficiency is low, and the instrument cost is high; nitro Benzene and polycyclic aromatic hydrocarbons can be determined by gas chromatography-mass spectrometry, but they need to be treated separately and are not suitable for popularization
At present, there is a lack of a general method for the simultaneous determination of these three types of substances, which limits the detection efficiency of soil pollution.

Method used

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  • Method for simultaneously determining aniline, nitrobenzene and polycyclic aromatic hydrocarbon in soil
  • Method for simultaneously determining aniline, nitrobenzene and polycyclic aromatic hydrocarbon in soil
  • Method for simultaneously determining aniline, nitrobenzene and polycyclic aromatic hydrocarbon in soil

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Embodiment 1

[0054] 1. Sample Preparation

[0055] 1) Sample freeze-dried

[0056] Put the sample on an enamel plate or a stainless steel plate, remove sticks, leaves, stones and other foreign matter, mix it and put it in a vacuum freeze dryer for drying and dehydration for 15-24 hours, after drying, grind it through a sieve with a pore size of 0.25mm, and homogenize Processed into particles of about 250 μm.

[0057] 2) Sample extraction

[0058] Weigh 10.00g sample, put it into the extraction pool, add 200μl ammonia water to adjust the pH to be greater than 10, put it into the accelerated solvent extraction apparatus, select the extraction solvent as acetone:dichloromethane with a volume ratio of 1:1, set the temperature at 100°C, Pressure 105 bar. The extraction was cycled twice, and the extract was collected.

[0059] 3) concentrated

[0060] The extract was placed on a parallel concentrator, and the concentrating conditions were set at a water bath temperature of 30° C. and a conc...

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Abstract

The invention relates to a method for simultaneously determining aniline, nitrobenzene and polycyclic aromatic hydrocarbon in soil, which comprises the following steps: preparing a soil sample, preparing a standard solution, drawing a working curve and determining a sample result, and is characterized by comprising the following steps of: extracting the soil sample on an accelerated solvent extractor; adding 100-500 [mu]l of ammonia water into a sample to adjust the pH value to 10-12, extracting with a solvent of acetone and dichloromethane according to a ratio of 1: 1, concentrating the extract to 1 mL, carrying out phase change, adding an internal standard, filtering with a 0.22 [mu]m filter head, loading on a machine, measuring with a gas chromatography-mass spectrometer, and calculating the content of a to-be-measured substance in the soil. According to the method, the tedious means that aniline, nitrobenzene and polycyclic aromatic hydrocarbon are subjected to pretreatment in three times and are respectively measured in the existing method procedure are simplified, the operation steps are simplified, the experiment cost is reduced, the target object recovery rate is improved, the defects of the current standard are overcome, and the method is easy to popularize and use in actual pollution investigation.

Description

technical field [0001] The invention relates to a method for simultaneously measuring aniline, nitrobenzene and polycyclic aromatic hydrocarbons in soil. Background technique [0002] Soil is the material basis for sustainable economic and social development, and the quality of soil environment is related to the health of the people and the construction of a beautiful China. The country is paying more and more attention to the soil environment. In the battle against soil pollution and soil environment assessment, soil testing has played an irreplaceable role in other disciplines. High-quality testing data provide basic data for scientifically formulating ecological and environmental governance policies, and testing methods The development of is an important way to improve data reliability. [0003] Aniline is easy to volatilize. After entering the water body, due to its very stable molecular structure, it is easy to cause persistent environmental pollution. Aniline is relat...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 高玉花郝杰毕建玲李云龙蒿艳飞孙鹏飞张宁陈璐张佩玉张梦瑶
Owner SHANDONG INST OF GEOPHYSICAL & GEOCHEM EXPLORATION