Selective extraction of iron oxide associated arsenic species from sediments for speciation with coupled HPLC-HG-AAS

Abstract

A procedure for the extraction of arsenic species from estuarine iron oxide rich sediments was developed based on the use of hydroxylammonium hydrochloride solution as leaching agent. Different variables such as extractant volume, concentration and time of extraction were used. Optimum conditions were obtained by using 40 ml of 0.4 M hydroxylammonium hydrochloride for 8 h at 95 °C with occasional shaking. Speciation of arsenic was performed with coupled HPLC-HG-AAS, using a strong anion-exchange column for the separation of arsenite, dimethylarsinic acid, monomethylarsonic acid and arsenate. The influence of the concentration of the extractant on the chromatographic separation was also studied. Complete recoveries of arsenic species required several repetitive extractions. Results obtained for CRM 320 River Sediment, certified for total arsenic concentration, were low, which indicated the influence of the matrix composition on the final extraction.