Method for detecting phenylamine compounds in environmental water samples by using synchronous derivation ultrasonic emulsification micro-extraction gas chromatography

Abstract

The invention discloses a method for detecting phenylamine compounds in environmental water samples by using a synchronous derivation ultrasonic emulsification micro-extraction gas chromatography. The method for detecting the phenylamine compounds in the environmental water samples by using the synchronous derivation ultrasonic emulsification micro-extraction gas chromatography comprises the following steps: (1) injecting liquid samples into a sharp-bottom glass centrifugal tube, quickly injecting n-butyl chloroformate which is used as a derivating agent / an extraction phase into the liquid samples by using a micro-syringe, subsequently putting into a high-power numerical control ultrasonic wave washing machine; (2) carrying out the ultrasonic treatment for 7 minutes under the conditions that the frequency is 40kHz, the power is 50W and the temperature is 2 DEG C, preparing the liquid samples in the glass centrifugal tube into an emulsion, centrifuging and fully separating phases of the emulsion in a test tube; (3) sucking a deposition phase at the bottom of the test tube by using a gas chromatography syringe and injecting the deposition phase into a gas chromatograph for analyzing; and (4) analyzing and detecting the phenylamine compounds by using the gas chromatograph. Compared with a conventional detection method, for the method disclosed by the invention, not only the analysis time is shortened, but also organic solvents with toxic action on a human body are reduced.

Description

technical field [0001] The invention relates to the field of detection of pollutants in environmental water bodies, in particular to a method for determining aniline compounds in environmental water samples by synchronous derivation ultrasonic emulsification micro-extraction gas chromatography. Background technique [0002] In the production process of dyes, spices, synthetic resins, pesticides and pharmaceuticals, aniline compounds are widely used as synthetic intermediates, and they are easily discharged into rivers, lakes and soil along with industrial wastes, becoming harmful to the ecological environment. Organic pollutants that cause great harm, some aromatic amines are highly toxic to humans and have been identified as carcinogens. Aniline compounds are more polar than their precursor substances, so they are more water-soluble, which leads to their greatly enhanced migration ability in the water environment, and their existence in small doses may cause serious damage ...

AI Technical Summary

Problems solved by technology

Among the traditional pretreatment methods for aniline compound samples, the cost of solid phase extraction (SPE) is relatively high and the steps are cumbersome. Although the improved solid phase microextraction (SPME) is easier to operate, it is Quartz fiber is brittle and has a limited service life, so this method is more expensive. In addition, the residue of analytes on the extraction head is also a very important problem; liquid phase extraction (LLE), based on the analyte in the liquid sample and insoluble The transfer between water extractants is a widely used sample pretreatment method, but it has the disadvantages of cumbersome operation, long extraction time and large amount of organic solvent. Its improved liquid phase microextraction (LPME) realizes a one-step Extraction, only a small volume of organic solvent is required to extract the analyte compound in the liquid sample, and the enrichment factor is high. Recently, for this method, a suspended droplet microextraction method (SDME) has been developed. Hollow fiber membrane microextraction New methods such as HF‐LPME and headspace liquid phase microextraction (HS‐LPME)

However, in the actual operation of the SDME method, the stability of the suspended droplets is difficult to guarantee, and the HF-LPME method also has the problem of long pretreatment time.

In response to these problems, Assadi et al. (2006) proposed a new liquid-phase microextraction technique - dispersed liquid-phase microextraction (DLLME). This method has attracted widespread attention because of its simple and fast operation and high enrichment factor. However, during the operation of the DLLME method, a considerable amount of organic solvents still needs to be used, which is harmful to the operator.

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