Development of on-line electrochemical sample pretreatment methods for the analysis of thallium and uranium by ICP-MS
Anodic and adsorptive stripping voltammetry (AWV and AdSV, respectively) were performed on-line with a mercury thin-film electrode (MTFE) to effect the selective accumulation and detection of thallium and uranium, respectively. ASV-ICP-MS experiments using thallium as the test element were performed to characterize the behavior of the on-line system for low level and quantitative determinations. Excellent linearity in response was demonstrated for thallium standards ranging from 0.25 ng/L to 50 {micro}g/L. The 1.0 pg/L detection limit calculated from this data for thallium (3{sigma}/sensitivity) was 400 times lower than that of conventional ICP-MS. The ability to overcome sample matrix effects in quantitative determinations was demonstrated by the analysis of an undiluted synthetic urine sample. AdSV-ICP-MS experiments were performed using uranium as the test element to demonstrate the utility of this method for the determination of radiologically important elements. A uranium(VI)-cupferron complex was used to effect adsorptive accumulation of uranium from a 10 {micro}g/L standard solution onto the MTFE. The uranium was chemically stripped from the electrode for subsequent downstream detection by the ICP-MS. The quantitative nature of this method and a modest enhancement of signal levels ({approximately}X10) over those levels obtained with conventional ICP-MS for samples in the microgram/liter concentration range were demonstrated. Modifications to the current system to provide low flow rate operation will allow further optimization of the ASV-ICP-MS and AdSV-ICP-MS combinations.
- OSTI ID:
- 409717
- Report Number(s):
- CONF-9410207--; ISBN 0-8031-2034-6
- Country of Publication:
- United States
- Language:
- English
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