Determination of trace analytes in nuclear grade Calcium Metal Samples by Axially Viewed Inductively Coupled Plasma – Atomic Emission Spectrometric technique

An Inductively Coupled Plasma – Atomic Emission Spectrometric (ICP-AES) method has been developed for the direct determination of 19 analytes namely, Al, B, Be, Cd, Co, Cr, Cu, Fe, Li, Mg, Mo, Mn, Ni, Pb, Pd, Si, Ta, V and W at trace concentration levels in calcium matrix. In nuclear industry, quality control and assurance of nuclear fuels and associated materials for trace metallic impurity contents form an integral part of the system for the smooth functioning of the reactor for the stipulated time span. In this context, it was required to determine trace analytes in nuclear grade Calcium which is used as a reducing agent for the production of U, Th, Pu, etc. in nuclear industry. Using axial ICP-AES, initially calibration curve for Ca with 396.847nm analytical line was obtained. Systematic studies were carried out to identify various analytical wavelengths of the analyte elements which are almost free from Ca, being the main matrix and calibration curves were obtained. For all analytes and Ca, detection limits and sensitivity values were calculated. To validate the method, three synthetic samples with analyte contents in the range of 0.1 - 5 g/mL and Ca at 1 mg/mL were analyzed, the % recovery being in the range of 80-120% with precision better than 5% RSD. The method was found to be useful for the direct determination of the elements of interest in calcium matrix and was applied for the analysis of two nuclear grade real life calcium metal samples.