Method for determining aniline in soil and sediment

Abstract

The invention relates to a method for determining aniline in soil and sediment. The method comprises the following steps: 1, pretreating: weighing 2 g of soil or sediment to be determined, putting thesoil or sediment into a headspace bottle, adding sodium chloride with the mass of more than 4 g, adding a pure water solution with the pH value of more than 11, adding an internal standard substance1,2-dichlorobenzene-d4, tightening a bottle cap, and putting the bottle into a sample introduction disc for determination; 2, carrying out solid-phase micro-extraction: uniformly mixing before extraction, and extracting by using a solid-phase micro-extraction fiber head; and 3, determining by using a gas chromatography-mass spectrometer. A solid-phase microextraction process is adopted, so that asoil or sediment sample does not need to be pretreated, and manpower, time, reagents and the like are saved; the solid-phase microextraction process is adopted, the detection limit can be lower without a concentration step, the split ratio is set to be 20, and a larger split ratio can be set if the soil with higher concentration is measured; and gas chromatography-mass spectrometry determination is adopted, and simultaneous determination of selective ion scanning and full scanning is adopted, so qualitative and quantitative determination of aniline is more accurate.

Description

technical field [0001] The invention relates to the technical field of soil and sediment detection, in particular to a method for determining aniline in soil and sediment. Background technique [0002] Aniline is an organic chemical raw material and chemical product with a wide range of uses. There are more than 300 kinds of chemical products and intermediates. It is widely used in printing and dyeing, dye manufacturing, vulcanized rubber, photographic developer, solvent, resin production, pharmaceuticals and other industries. When the aniline entering the soil system and sediment accumulates beyond the original self-purification capacity of the soil system or river, it will cause structural changes in the soil system and natural dysfunction of the river. Since aniline is an oily liquid at normal temperature, the soil and sediments have a good absorption effect on it. The aniline mixed into the soil and sediments is difficult to decompose in a short time, which will cause lo...

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Problems solved by technology

[0003] At present, aniline in soil and sediment should be detected and analyzed according to "Determination of Semi-volatile Organic Compounds in Soil and Sediment by Gas Chromatography-Mass Spectrometry" (HJ834), but there is no parameter "aniline" in the standard method of HJ834, soil The method for detecting aniline in sediments and sediments is mainly to detect by accelerated solvent extraction gas method. The recovery rate of this method is low, and the recovery rate of accelerated solvent extraction is only 30%-50%. The operation is cumbersome, the extraction time is long, and the organic solvent Large dosage, low detection sensitivity

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