Solid Phase Extraction Analysis Method for Perfluorooctane Sulfonate in Wastewater

Abstract

The present invention discloses a solid-phase extraction analysis method of perfluorooctane sulfonic acid compounds in wastewater. The solid-phase extraction analysis method comprises: rinsing a solid-phase extraction column sequentially with 0.1% ammonium acetate-containing methanol, pure methanol and ultrapure water, and discarding the solutions after completing the rinsing; using a vacuum solid-phase extraction device to suck a wastewater sample, passing through the solid-phase extraction column, sequentially adding 2 mL of a solution containing acetone, acetonitrile and formic acid according to a ratio of 50:50:1, 3 mL of pure methanol and 3 mL of 0.1% ammonium acetate-containing methanol to carry out elution, and collecting and merging the eluent; blowing the eluent with nitrogen to approach a drying state, adding 1 mL of a solution containing methanol and water according to a ratio of 1:1, and uniformly mixing; and carrying out analysis testing through LC / MS / MS to obtain the result. According to the present invention, the sampling amount of the method is large, such that the samples have the good representativeness and can characterize the performance of the wastewater to the maximum extent; the operation process is simple and efficient, and the reproducibility of the laboratory data is stable; and the standard addition method recovery rate achieves 70%, the detection limit is low and is 0.01 [mu]g / L, the ecological requirements of the environment are met, and the tested compound variety is diverse.

Description

technical field [0001] The invention relates to the field of chemical detection, in particular to an analysis method for perfluorooctane sulfonic acid in waste water. Background technique [0002] Perfluorooctane sulfonates are a class of widely used chemical products. This type of compound has high stability and can withstand strong heat, light and microbial action. It is the most difficult to degrade organic pollutants found in the world. one. Studies have shown that perfluorooctane sulfonic acid compounds are currently one of the most difficult to degrade organic pollutants. After being ingested by organisms through breathing and eating, most of them exist in the blood, and the rest accumulate in the liver tissue and muscles of animals. In tissues. Studies have shown that perfluorooctane sulfonic acid compounds are present in the organs and tissues of birds and fish, surface water, sediment, bottom sewage outlets of wastewater treatment plants, sewer sewage pipes and see...

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Problems solved by technology

[0003] For the analysis of perfluorooctane sulfonate compounds, there are mainly the following difficulties: First, the carbon chain coverage of perfluorooctane sulfonate homologues is wide, usually from C4 to C14, and the polarity of the compounds is quite different, so It brings certain difficulties to sample enrichment and separation; the second is to analyze perfluorooctane sulfonate compounds, the fluorine-containing material of the instrument analysis system is likely to cause background interference and such compounds are easy to adsorb

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