A method for determination of arsenite As (III) and arsenate As (V) in some sediments and water samples was developed by using Hydride Generation-Atomic Absorption Spectrometry (HG-AAS). Optimization of the signal was carried out for a number of experimental parameters, including the carrier gas flow rate, sample volume, concentration of reducing agent; sodium borohydride (NaBH_4), and the concentration of hydrochloric acid (HCl). The precision for nine sample replicates was better than 3.1% for all arsenic species. The accuracy of the method was determined by analysis of a lake sediment reference material (IAEA-SL-1). This method can be applied for sediments and water samples.