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Title: Preconcentration and analysis of trace elements

Thesis/Dissertation ·
OSTI ID:6177779

Two major topics have been addressed in this work: (1) optimization and evaluation of an ICP-Echelle spectrometer system for simultaneous multi-element trace analysis and (2) preconcentration of trace elements via reduction and precipitation using sodium borohydride. The elements Al, B, Ba, Be, Ca, Cd, Cr, Cu, K, Mg, Mn, Mo, Na, Ni, P, Pb, Si, and Sr were used as analytes in the optimization and evaluation of the ICP-Echelle spectrometer system. Problems with radio-frequency interference and source drift were encountered and dealt with. The Echelle spectrometer system was optimized for signal-to-noise ratio as a function of RF power and plasma viewing height. The preconcentration procedure was optimized at a preconcentration factor of 50 X for the amount of borohydride reductant employed, the solution aging time, and the use of iron and palladium as recovery enhancers, among other factors. The optimized procedure effected the preconcentration of all 18 of the test elements, 12 of which were recovered at levels not significantly below 95%, while 15 were recovered at levels not below 90%. The mean of the relative standard deviations observed for the standard recoveries of all 18 analytes was only 4.4%.

Research Organization:
Colorado State Univ., Fort Collins (USA)
OSTI ID:
6177779
Resource Relation:
Other Information: Thesis (Ph. D.)
Country of Publication:
United States
Language:
English