A combined hydride-generation/gas-phase chemiluminescence (HGGPCL) method for the determination of arsenic(III) and antimony(III) by using a conventional luminometer is proposed. The method was optimized in terms of the type of reaction chamber, the instrumental settings, and the hydride generation and reaction conditions used. It provides a linear response to As(III) and Sb(III) above a concentration of 0.05 and 0.50 mg L<sup>-1</sup>, respectively, with a relative standard deviation of ∼3% for both species. Arsenic and antimony can thus be determined simultaneously by (1) their differential effect on the signal obtained with an optical filter placed between the reaction chamber and detector, or (2) the difference between the peak height/peak area ratio of the transient signal for their hydrides. Both procedures were applied to the determination of arsenic and antimony in various synthetic aqueous samples with good accuracy and precision. The effect of potential interferences including anionic and hydride-forming inorganic species was investigated.

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