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Determination of trace elements in rainwater by total-reflection X-ray fluorescence

Journal Article · · Anal. Chem.; (United States)
DOI:https://doi.org/10.1021/ac00291a031· OSTI ID:6445572
Three quasi-independent analytical procedures for the determination of trace elements in rainwater are presented, which are based on total-reflection X-ray fluorescence (TXRF), a special variant of energy-dispersive X-ray fluorescence. The three sample preparation techniques compared are (1) direct analysis, (2) preenrichment of the trace elements in rainwater by freeze-drying and redissolution in dilute nitric acid, and (3) a matrix removal and preconcentration procedure by metal chelation, chromatographic adsorption of the metal complexes, and subsequent elution of the metal chelates prior to TXRF measurement. The elements determined are S, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Pb, Se, Rb, Sr, Mo, Cd, and Ba. For a measuring time of 1000 s, detection limits down to 5-20 ng/L were achieved for the heavy-metal traces. The limits are slightly higher for iron, nickel, copper, zinc, and lead because of fluctuations in the blan values. The procedures were tested on rainwater samples from the Island of Pellworm (German Bight) containing comparatively low trace-metal contents. Systematic investigations for the characterization of the analytical procedures with regard to blanks, detection limits, precision, and accuracy are described and discussed. The accuracy was checked by independent analyses of duplicate samples using differential pulse anodic stripping voltammetry (KFA Juelich). 17 references, 4 figures, 2 tables.
Research Organization:
GKSS-Forschungszentrum, Geesthacht GmbH, West Germany
OSTI ID:
6445572
Journal Information:
Anal. Chem.; (United States), Journal Name: Anal. Chem.; (United States) Vol. 57:14; ISSN ANCHA
Country of Publication:
United States
Language:
English

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