Abstract:

The objective of this dissertation is to develop on-line sample preparation procedures based on membrane extraction and flow injection (FI) techniques. A novel sample pretreatment technique, which we termed continuous flow liquid membrane extraction(CFLME), was developed for trace-enrichment of polar organic pollutants. The principle and parameters of CFLME were investigated by using sulfonylurea herbicides and bisphenol A as model compounds. At the optimum conditions and with an enrichment time of 120 min and 40 min, metsulfuron methyl and bisphenol A were enriched with an enrichment factor of 1000 and 200, respectively, and the enrichment efficiencies of bisphenol A and the five studied sulfonylurea herbicides were 3.5 ～ 200 fold of that of supported liquid membrane extraction (SLM). Then,an on-line coupled CFLME-HPLC system, with detection limits of 0.05 ～ 0.1 μg/L after 10min of enrichment, was developed for the determination of sulfonylurea herbicides. Futhermore, an on-line coupled CFLME-C18 precolumn-HPLC system was developed for the trace analysis of sulfonylurea herbicides in surface waters at ng/L level. The detection limit of this proposed CFLME-C18 precolumn-HPLC system is 200 fold lower than that of the original C18SPE preconcentration-HPLC detection method. Experiments show that the proposed CFLME technique has the advantages of high selectivity, high enrichment efficiency, low-cost, longterm stability and convenience for coupling on-line with other analytical instruments.On-line sample pretreatment procedures based on FI technique were also studied and approaches for the application of FI technique in routine analysis were proposed. A FI-micropore membrane liquid-liquid system was developed for the routine analysis of anionic surfactants in detergents, and a FI high temperature reaction system was developed for the determination of total inorganic phosphates in detergents and the total reducing sugars in tobacco. To simplify the manifold, aregent-injection-FI technique was proposed for the elimination of matrix background absorption in the determination of chloride in tobacco.

Key words: on-line sample preparation, membrane extraction, flow injection