Development of HPLC Techniques for the Analysis of Trace Metal Species in the Primary Coolant of a Pressurised Water Reactor
The need to monitor corrosion products in the primary circuit of a pressurised water reactor (PWR), at a concentration of 10pg ml-li s discussed. A review of trace and ultra-trace metal analysis, relevant to the specific requirements imposed by primary coolant chemistry, indicated that high performance liquid chromatography (HPLC), coupled with preconcentration of sample was an ideal technique. A HPLC system was developed to determine trace metal species in simulated PWR primary coolant. - In order to achieve the desired detection limit an online preconcentration system had to be developed. Separations were performed on Aminex A9 and Benson BC-XI0 analytical" columns. Detection was by post column reaction with Eriochrome Black T and Calmagite Linear calibrations of 2.5-100ng of cobalt (the main species of interest), were achieved using up to 200ml samples. The detection limit for a 200ml sample was 10pg ml-¹. In order to achieve the desired aim of on-line collection of species at 300°ᶜ, the use of inorganic ion-exchangers is essential. A novel application, utilising the attractive features of the inorganic ion-exchangers titanium dioxide, zirconium dioxide, zirconium arsenophoshate and pore controlled glass beads, was developed for the preconcentration of trace metal species at temperature and pressure. The performance of these exchangers, at ambient and 300°ᶜ was assessed by their inclusion in the developed analytical system and by the use of radioisotopes. The particular emphasis during the development has been upon accuracy, reproducibility of recovery, stability of reagents and system contamination, studied by the use of radioisotopes and response to post column reagents. This study in conjunction with work carried out at Winfrith, resulted in a monitoring system that could follow changes in coolant chemistry, on deposition and release of metal species in simulated PWR water loops. On-line detection of cobalt at 11pg ml-¹ was recorded, something which previously could not be performed by other techniques.||Atomic Energy Establishment Winfrith, Winfrith, Dorchester, Dorset DT2 SDH
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