SYMPOSIA PAPER Published: 01 January 1995

Development of On-Line Electrochemical Sample Pretreatment Methods for the Analysis of Thallium and Uranium by ICP-MS


Anodic and adsorptive stripping voltammetry (ASV 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 μg/L. The 1.0 pg/L detection limit calculated from this data for thallium (3σ/sensitivity) was 400 times lower than that of our 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 μg/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 (∼ × 10) over those levels obtained with our conventional ICP-MS for samples in the microgram/litre 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.

Author Information

Zhou, F
Oak Ridge National Laboratory, Oak Ridge, TN
Van Berkel, GJ
Oak Ridge National Laboratory, Oak Ridge, TN
Morton, SJ
Oak Ridge National Laboratory, Oak Ridge, TN
Duckworth, DC
Oak Ridge National Laboratory, Oak Ridge, TN
Adeniyi, WK
North Carolina A&T State University, Greensboro, NC
Keller, JM
Oak Ridge National Laboratory, Oak Ridge, TN
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Developed by Committee: C26
Pages: 82–98
DOI: 10.1520/STP15982S
ISBN-EB: 978-0-8031-5315-8
ISBN-13: 978-0-8031-2034-1