The Separation and Determination of Molybdenum by Electron Paramagnetic Resonance

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Abstract
A procedure is described for the separation and quantitative determination of molybdenum by means of EPR. Molybdenum(VI) was precipitated from a hydrochloric acid solution (1.5 Molar) with α-benzoinoxime. The precipitate was separated by centrifugation and then the sample was dried in an oven at 105°C. Nitrogen was passed over the sample to complete the drying procedure. The precipitate was dissolved in acetonitrile which was 0.5 M in lithium perchlorate. Electrochemical reduction of the sample produced the molybdenum(V) species. The concentration of molybdenum(V) was determined directly from the intensity of the first derivative EPR signal. The range of linearity of the analytical curve was 1.00 × 10−2 M to 1.00 × 10−4 M, and a routine accuracy of less than 6% was obtained.