Study of ammonium molybdate to minimize the phosphate interference in the selenium determination by electrothermal atomic absorption spectrometry with deuterium background correction

Abstract

The use of ammonium molybdate to minimize the phosphate interference when measuring selenium by electrothermal atomic absorption spectrometry (ETAAS) with deuterium background correction was evaluated. Ammonium molybdate did not produce a selenium thermal stabilization; however, the presence of ammonium molybdate decreased the phosphate interference. The study was carried out with mussel acid digests and mussel slurries. Pd–Mg(NO 3) 2 was used as a chemical modifier at optimum concentrations of 300 and 250 mg l −1, respectively, yielding optimum pyrolysis and atomization temperatures of 1200 and 2100 °C, respectively. A yellow solid (ammonium molybdophosphate) was obtained when adding ammonium molybdate to mussel acid digest solutions. This precipitate can be removed after centrifugation prior to ETAAS determination. Additionally, studies on the sampling of the solid ammonium molybdophosphate (AMP) together with the liquid phase, as a slurry, were also developed. The volatilization of the solid AMP was not reached at temperatures lower than 2500 °C. By this way, phosphate, as AMP, is not present in the vapor phase at the atomization temperature (2100 °C), yielding a reduction of the spectral interference by phosphate. The proposed method was validated analyzing three reference materials of marine origin (DORM-1, DOLT-1 and TORT-1). Good agreement with the certified selenium contents was reached for all cases.