Abstract: A new method was introduced for determination of arsenic in fluorspar powder by atomic absorption spectrometry with hydride generation.The effect of different acid mediums and reductants and flow-rate of carrier gas on the determination of arsenic was studied.The operating conditions were optimized.The limit of detection of the proposed method was found as 0.052 μg·g-1 .The linear relationship between the absorbence and concentration of arsenic was in the range of 0.10-6.00 μg·L-1.Recovery in range of 90.0%-102.0% and its RSD of 9.8% were obtained.