A hybrid sequential injection–stopped flow injection system was developed for the speciation of arsenic based on the quenching of mercaptoacetic acid capped cadmium sulfide quantum dots (CdS–MAA QDs) fluorescence intensity. The analytical procedure involves the generation of arsine from As(III) by sodium borohydride in acetate buffer medium pH 6.0. The generated arsine (donor stream) diffuses across the PTFE membrane of the gas–diffusion unit into an acceptor stream and then interacts with CdS–MAA QDs. Total arsenic was determined after pre-reduction of As(V) to As(III) with 1% (m/v) mercaptoacetic acid. Concentration of As(V) in the sample solutions can be deduced from the difference of total arsenic and As(III). Optimization of the experimental conditions and instrumental parameters were investigated. Under optimal conditions, limits of detection were 20μgL−1 for As(III) and 40μgL−1 for As(V). Recoveries in the range 84–103% were obtained from sediment sample.
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