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The treatment of laboratory waste containing arsenic compounds should be part of the chemical analysis protocol in educational and research institutions. An alternative procedure for the treatment of these residues is proposed for the development of a didactic analytical route in the detection of As3+, As5+, MMA (monomethylarsonic acid) and DMA (dimethylarsinic acid). The treatment is based on the coprecipitation of inorganic arsenic species with a quaternary ammonium salt (tetra-n-butylammonium perchlorate) in suspension. Detection occurred by controlling the hydride generation reactions and Atomic Absorption Spectrometry. The methylated species MMA and DMA remain in the supernatant and can be monitored by adjusting the pH, concentration of the borohydride reducer, and the use of auxiliary reducers (hydroxylamine hydrochloride and KI). Satisfactory selective detectability was obtained for each arsenic species present in the waste sample. This work contributes to the development of experiments to be implemented in Qualitative Analytical Chemistry and Instrumental Analysis classes. The results allow to approach the chemical vapor generation, which is generally not well explored in undergraduate classes. Discussion of this procedure is supported by a teaching proposal based on the theory of nascent hydrogen for inorganic arsenic species and the nucleophilic performance of the hydride ion for methylated species. This approach allows the student to contextualize important concepts such as Lewis structure, oxidation state and kinetics of arsenic hydride generation reactions. This interdisciplinary contextualization forms a common theoretical basis, preparing and enabling the student to research speciation analysis by hydride generation and to understand the most accepted theories. [ABSTRACT FROM AUTHOR]

An ultrasound-assisted extraction procedure was developed for determination of inorganic arsenic (As) in phosphate fertilizer by hydride generation atomic absorption spectrometry. The variables that affect the hydride generation step were optimized, including the reducer, acid, sample low rate, and concentrations of the acid and reducer. The determination of As(III) was performed through the simple control of solution pH with a 0.5 M citric acid-sodium citrate buffer solution at pH 4.5, and total As was determined after a pre-reduction reaction with 1.0% (w/v) thiourea. Ultrasound-assisted acid extraction was performed, and the parameters sonication time and acid and Triton X-114 concentrations were optimized using a 2³ factorial design and central composite design. LODs for As(III) and total As were 0.029 and 0.022 µg/L, respectively. The accuracy of the method was conirmed with certiied reference materials. The method was successfully applied in the determination of inorganic As in phosphate fertilizer samples. [ABSTRACT FROM AUTHOR]