| Summary: | In this article, inductively coupled plasma mass-spectrometry (ICP-MS) and inductively coupled plasma optical-emission spectrometry (ICP-OES) were used for the development of an analytical procedure for analysis of the waste of Sm-Co magnets. Experimental parameters related to microwave digestion processes and acid concentrations were optimized. Microwave digestion was carried out in mixtures of HF, HCl, HNO<sub>3</sub> and H<sub>2</sub>SO<sub>4</sub>. The complete dissolution of the samples occurred in the system: 10 mL H<sub>2</sub>O, 2 mL HNO<sub>3</sub>, 10 mL HCl and 1 mL H<sub>2</sub>SO<sub>4</sub>. The dependence of the matrix effect on the ICP-MS analysis of waste Sm-Co magnets was studied and optimal instrumental parameters were investigated (nebulizer gas flow, sampling depth and potential at the extractor lens). The optimal conditions were a nebulizer gas flow of 0.85–0.90 L/min, a sampling depth of 101, potential at the extractor lens of −400 V and a sample flow rate of 50 rpm. A recovery test and inter-method experiments were performed to verify the accuracy of the proposed method.
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