I. Eguiarte et al., DETERMINATION OF TOTAL ARSENIC IN SOILS BY DIFFERENTIAL-PULSE CATHODIC STRIPPING VOLTAMMETRY, Analyst, 121(12), 1996, pp. 1835-1838
A procedure which permits the determination of total arsenic in soils
using differential-pulse cathodic stripping voltammetry at a hanging m
ercury drop in the presence of copper after the acid digestion of soli
d samples in a closed-vessel microwave digester was developed. Optimiz
ed conditions include accumulation potential -0.5 V, accumulation time
120 s, 0.05 mol l(-1) of KI to reduce As-V to As-III, 10 mu g ml(-1)
of copper and both 3.8 mol l(-1) HCl and 0.24 mol l(-1) NaHCO3 as elec
trolyte. The detection limit was 50 pg ml(-1) and the reproducibility
was 3.8% intra-day and 4.5% inter-day for 10 determinations at a conce
ntration of 2.6 ng ml(-1). The method was applied to a reference certi
fied soil sample, obtaining a relative error of 0.7%, Results for 12 s
oil samples from a zone of the Basque Country mere compared with those
obtained by hydride generation atomic absorption spectrometry.