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ABSTRACT
An inductively coupled plasma optical emission spectrometry (ICP OES) method for Pb, Zr, Ti, Sr, Cr, Fe, Cu, Mn, and Al determination in PZT-ceramics is described. Careful analytical work was carried out in order to evaluate precision, accuracy, and matrix interference. Different procedures were investigated for the ceramics decomposition. Axially viewed plasma operating conditions were evaluated for trace elements (Al, Fe, Cu, Mn, and Cr) in presence of sample matrix. The relative standard deviation (RSD) ranged from 0.7 to 3.9%, whereas the analytes recoveries in the spiked samples ranged from 92 to 119%. The detection limits (LODs) of trace elements ranged from 2.4 to 2.6 µg g−1. The developed method is useful for evaluating the PZT-ceramics synthesis.
ACKNOWLEDGMENTS
The authors are grateful to CAPES from Brazil for the scholarship of Margarita Villanueva Tagle; Instituto de Química, UFRGS, Brazil, where the work was carried out; and PNCIT projects B7 and 10/04, of the Sciences Technologies and Environment Ministry, CITMA, Cuba for its financial contribution.
Notes
Note: a argon (from White Martins/Praxair, Brazil).
Note: Those wavelengths marked in bold were selected.
Note: Concentrations are the means of six replicates and respective interval of the means at 95% confidence level.
Note: Matrix II was used. It contained 297, 110, 15, and 7 mg L−1 of Pb, Zr, Ti, and Sr, respectively. Values shown are the average and the confidence interval (α = 0.05) of three independent determinations.
a the nebulizer gas-flow rate was 0.8 L min−1.
b the RF power was 1.5 kW.
c a solution containing 0.5 mg L−1of Al was used.
Note: External calibration was used, whereas six replicates of the samples were measured (n = 6).
a different from the predicted value (theoretical) with 95% of confidence.