Hydride generation (HG) coupled to a simultaneous multi-element axially viewed inductively coupled plasma atomic emission spectrometer (ICP-CCD-AES) was used to determine trace contaminants (<10 mg kg−1) of As, Bi, Se, Sn, and Te in chemically resistant high alloy steels and Ni alloys. These refractory and chemically resistant samples were quantitatively digested using a mixed acid microwave-assisted procedure. EDTA, tartaric acid and 2-pyridinecarbaldehyde oxime were evaluated as interference-retarding agents. Accuracy was evaluated using spiked synthetic steel solutions and CRM steel and Ni alloys. Limits of quantification (LOQs) calculated for the solid material varied from about 1–10 mg kg−1 and satisfactory data were obtained for As, Bi, Se, Sn and Te. However, the LOQs for Sb were degraded and, as a result, this LOQ could not be determined with satisfactory accuracy in the samples tested.
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