Analytical Control over the Preparation of Pure Antimony

A multielement inductively coupled plasma atomic emission spectrometry (ICP-AES) technique has been proposed for high-speed monitoring of the preparation of pure antimony, and analytical lines of analytes with the weakest spectral effects have been chosen. We have studied the effect of matrix component concentration (5 to 40 g/L) on the analytical signals of impurity elements. Changes in excitation conditions in the plasma at a varied antimony concentration in solution and varied ICP power have been assessed using the ICP robustness. The robustness was evaluated from the intensity ratio of the magnesium ionic and atomic lines. The presence of 40 g/L of antimony in solution has been shown to reduce the ICP robustness by up to 5%. The adequacy of the proposed technique has been confirmed by the standard addition method and comparison with results obtained by an independent method. The proposed technique for analysis of antimony allows one to determine 56 impurity elements with detection limits from n × 10^–7 to n × 10^–4 wt %.