Preparation and application method of solid phase extractant capable of simultaneously accumulating multiple heavy metal ions

Abstract

The invention relates to a preparation and application method of a solid phase extractant capable of simultaneously accumulating multiple heavy metal ions. Firstly, 2.5g of carboxylation carbon nano tube and 30 mL of anhydrous thionyl chloride react for 1-2 days at the temperature of 60-90 DEG C; pump filtration is carried out; after being cleaned, filter residue is dried in vacuum for the whole night to obtain an acylation carbon nano tube; the acylation carbon nano tube is dispersed in a solution composed of 1g of thiosemicarbazide and 100 mL of anhydrous N, N-dimethyl formamide; the mixture reacts under the protection of nitrogen with the temperature of 100 DEG C for 48 hours; pump filtration is carried out; after being cleaned, the filter residue is dried in vacuum for 1-2 days to obtain the solid phase extractant capable of simultaneously accumulating multiple heavy metal ions. The solid phase extractant serves as a column filler to dynamically accumulate 0.5-1 L of water samplesto be detected, wherein the heavy metal ion content of the water samples is 1-5 mu g / L; and the solid phase extractant in which the heavy metal ions are accumulated is eluted and desorbed by utilizing dilute nitric acid, wherein the recovery rate is above 95%, and the desorbed solid phase extractant is repeatedly recycled for 2-3 times. The invention has high efficiency, is simple and can simultaneously accumulate various heavy metal ions, i.e. Cu (II), Ni (II), Zn (II), Cd (II) and Pb (II).

Description

technical field [0001] The invention relates to the preparation and application method of a solid-phase extraction agent capable of enriching various heavy metal ions at the same time, in particular to a functionalized carbon nanometer for solid-phase extraction of various trace heavy metal ions in environmental water and liquid samples. The preparation method of the pipe; further relates to the use method of extracting various heavy metal ions with the solid phase extractant. The invention belongs to the technical field of separation, analysis and detection. Background technique [0002] With the rapid development of industry and agriculture, a large number of pollutants enter the environment, causing serious deterioration of environmental quality, among which heavy metal pollution is one of the most serious pollution. Unlike other pollutants, heavy metal pollution has the characteristics of concealment, irreversibility and long-term nature. It is easy to accumulate in th...

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Problems solved by technology

In recent years, the study of properly functionalizing carbon nanotubes and utilizing the coordination of active groups to enrich metal ions has also attracted widespread attention (Y.Liu, Y.Li, X.P.Yan, Adv.Funct.Mater .2008, 18, 1536-1543.), but due to the coordination selectivity of the ligand, this kind of material only has good selectivity for a certain metal, which cannot meet the requirements of extracting more than one metal at the same time in order to improve the extraction efficiency. metal requirements

Although carboxylated carbon nanotubes can simultaneously enrich and adsorb various heavy metal ions, and can realize the simultaneous enrichment and extraction of various heavy metal ions, the limitation of the characteristics of carboxyl coordination often limits its adsorption capacity and the capacity of adsorbed ions. Species (A.Staffej, K.Pyrzynska, Microchem.J., 2008, 89, 29-33)