Nondestructive determination of lead, cadmium, tin, antimony, and barium in ceramic glazes by radioisotope X-ray fluorescence spectrometry
1996
Anderson, D.L. | Cunningham, W.C.
Quantitation capabilities of radioisotope X-ray fluorescence spectrometry (RXRFS) for determining lead, cadmium, tin, antimony, and barium in ceramic glazes were investigated. Twenty-one air-dried glazes and 85 fired glazes on test tiles were analyzed by using (109)Cd and (57)Co excitation sources. Accurate Pb determinations, with limits of detection (LODs) of about 0.3 mg/cm2 for 5 min counting times, were achieved by using the 75 keV K alpha 1 X-ray photopeak and a Pb foil calibration procedure. Cd, Sn, Sb, and Ba concentrations were determined with LODs from about 0.5 to 1.5 mg/cm2. For Pb and Ba, results obtained by using absorption corrections based only on element concentrations determined by RXRFS and an iterative approach led to analytical biases of less than or equal to 4% relative to results obtained by using corrections based on known total element compositions. Biases were more severe for Cd, Sn, and Sb because lower X-ray energies were involved and sensitivities varied as a function of matrix Pb content. Pb concentrations were above LODs (1.3-40 mg/cm2) in 39 of 47 fired "food-safe" glazes and in 33 of the other 38 fired glazes (0.4-39 mg/cm2).
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