A novel sorbent, chitosan-immobilized pumice, has been prepared for the sorption of As(V) from waters prior to its determination by hydride generation atomic absorption spectrometry. The success of the immobilization has been checked with such characterization techniques as scanning electron microscopy, thermal gravimetric analysis, and elemental analysis. Points of zero charge of the sorbents were determined with potentiometric mass titration. Batch-type equilibration studies have shown that the novel sorbent can be employed at a wide pH range resulting in quantitative sorption (>90 %) at pH 3.0-7.0 and greater than 70 % sorption at pH >8.0. These results demonstrate the advantage of immobilizing chitosan onto pumice, because, under the same conditions, pumice displays <20 % sorption toward As(V), whereas chitosan gives approximately 90% sorption only at pH 3.0. The validity of the method was verified through the analysis of ultrapure, bottled drinking, and tap water samples spiked with arsenate; the respective sorption percentages of 93.2 (+/- 0.7), 89.0 (+/- 1.0), and 80.9 (+/- 1.3) were obtained by batch-type equilibration. Arsenic sorption was also examined in the presence of common interfering ions resulting in competing effects of PO43- and NO3- on As(V) adsorption.