a Analytical Chemistry Laboratories, Department of Chemistry, La Trobe University, Bundoora, Vic. 3086, Australia
b School of Chemistry, The University of Melbourne, Melbourne, Vic. 3010, Australia
Abstract:
A novel pervaporation-flow injection (PFI) system for the determination of As(III) in aqueous samples at μg l−1 level is described. The analytical procedure involved stopping the acceptor stream and injecting acidified As(III) samples into a 0.3 M HCl stream which was mixed with a 0.14 M sodium borohydride in 0.025 M NaOH stream. The arsine generated was transported in the pervaporation unit across a semi-permeable membrane (1.5 mm thickness) into the static acceptor solution containing 1.0×10−4 M KMnO4 in 0.1 M H2SO4 where it was oxidised. The acceptor stream was restarted after 6.5 min, and the decrease in permanganate absorbance at 528 nm was monitored to determine the initial concentration of As(III) in the samples. The method is characterised by a linear calibration range from 0.25 to 2000 μg l−1, a detection limit of 0.18 μg l−1 and a sampling frequency of 7 h−1. Samples containing As(V) were pre-treated with KI and HCl prior to injection to reduce As(V) to As(III). The effects of common anionic and cationic interferences, and the elimination of some metallic interferences using -cysteine are discussed. The method was applied to the analysis of environmental waters and the results were in good agreement with hydride generation atomic absorption spectrometric data.