An HN03-HC104 dissolution procedure followed by evaporation, re-dissolution and dilution with a CH3C02H-KN03 electrolyte is shown to be effective for the treatment of soil samples prior to the determination of trace amounts of lead by differential-pulse anodic stripping voltammetry.
A measurement system capable of continuous on-line matrix removal, pre-concentration and analysis of 226Ra using pre-packed columns coupled to a flow injection system and an ICP-MS was developed. Full instrumental control of both the ICP-MS and the flow injection system provided automatic integration of the transient signals. The flow injection system was programmed to control column conditioning, sample loading, column rinsing, analyte elution and column cleaning operations employing appropriate solutions. The application of this system to the 226Ra analysis of an industrial liquid effluent was demonstrated. Using this particular instrument together with pre-concentration and matrix removal procedures, a limit of detection of 5.4 fg L−1 (2 mBq L−1) and a method detection limit of 16.2 fg L−1 (6 mBq L−1) were achieved for the measurement of 226Ra using a 25 mL sample volume. Total time for sample handling and analysis is approximately 10 minutes. The concentration of 226Ra in a discharged effluent sample was 0.73 pg L−1 (27 mBq L−1), which is in good agreement with the value of 0.81 pg L−1 (30 mBq L−1) measured using conventional alpha counting techniques.
ANGELO RANSIRIMAL FERNANDO, and BYRON KRATOCHVIL. Can. J. Chem. 69,755 (1991).The use of lead and cadmium as internal standards for each other in anodic stripping analysis was investigated. Although accuracy was not affected, precision was significantly improved. The surface active agents Triton-X 100 and starch affected the sensitivity of the anodic stripping procedure for lead and cadmium, leading to error if a calibration curve is used. Data for applicationof the procedure to the analysis of the marine biological reference material LUTS-1 and soil reference materials SO-2, SO-3, and SO-4 are provided.
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