The present speciation method reports the determination of inorganic arsenic forms, using metallic furnace hydride generation atomic absorption spectrometry. The inorganic As speciation is carried out using mild conditions for hydride formation, such as slightly acid pH media (4.50) and low tetrahydridoborate(1-) concentration (0.1% (w/v)). Limits of detection and quantification of 2.0 and 6.6 μg L(-1) of iAs(III) are obtained using optimized conditions. Additionally, microwave-assisted extraction using water as solvent is carried out to provide the appropriate environment for As species extraction as well as impeding inter-conversion between species. With these analytical strategies, As was accurately determined (at 99.9% confidence level) in water and plankton samples.104187-92