Zirconium sponge production. An integrated approach for chemical characterization of process intermediates using ICP-OES

The present paper discusses about the method developed for complete chemical characterization of Zirconium Washed and Dried Frit (WDF) and Reactor Grade ZrO${}_2$ powder which includes nonmetallic element sulphur using Inductively Coupled Plasma Optical Emission Spectrometer (ICP-OES). Studies have been carried-out on several important aspects of method development such as effect of matrix on determination of analytes, removal of matrix using different solvents, selection of interference free & sensitive wavelengths, calibration strategies like internal standard & standard addition, optimization of several instrumental parameters which includes RF power, plasma gas flow, nebulizer gas flow, nitrogen purging etc., and are discussed. A % RSD of less than 1 % for Zr and up to 3 % for other elements has been achieved in this method. The developed method has been validated using standard recovery of spiked real time samples with known amount of reference materials. Integrated approach adopted in the development of this method has resulted in reduction of analytical waste generated and also enabled to give quick analytical feedback to production plant for downstream processing.