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Strategy of Sample Preparation for Arsenic Determination in Mineral Fertilizers

A method for determination of arsenic in mineral fertilizers by continuous flow hydride generation atomic absorption spectrometry (CF-HG-AAS) was developed by using diluted acid and digester block with perfluoroalkoxy (PFA) tubes to sample preparation. An additional sample preparation procedure using microwave-assisted digestion was evaluated and compared with the proposed procedure. A full factorial design was applied to investigate the effect of the variables and the best conditions found were 7 mol L−1 HNO3 + 30% (m/m) H2O2 as reagents, 4 h of digestion and concentration of reagents diluted 1:1. The effect of concomitants on the analytical signal of arsenic was investigated and no one significant interference was observed, with recoveries ranged from 97 to 103%. The accuracy of proposed method was evaluated by certified reference material (NIST SRM 695) and recovery of 95% was obtained. The arsenic concentration (8.9 ± 0.2 mg kg−1) found in the fertilizer is below of maximum concentration established by Brazilian legislation.

Keywords:
sample preparation; mineral fertilizers; arsenic; factorial design; CF-HG-AAS


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