Multielement XRF Semimicroanalysis of Pb(Zr,Ti)O3 Type Ferroelectric Ceramic Materials Doped with Pb(Nb,Mn)O3 and Bi2O3 by the Thin Layer Method

A method of wavelength-dispersive XRF analysis of Pb(Zr,Ti)O3 type ferroelectric ceramics doped with Pb(Nb,Mn)O3 and Bi2O3 is presented. The major elements Pb, Zr, Ti and minor elements Nb, Mn, Bi were determined. Matrix effects were minimized by using the thin layer method. Standards of the same chemical composition but varied masses were prepared to simplify calibration. To minimize errors resulting from inhomogeneity of a mass per unit area, the internal standard was used. Preparation of the sample consisted in digesting 25 mg of the materials (with nickel as the internal standard) in sulfuric acid, evaporating to dryness and digesting in nitric acid and hydrogen peroxide, filling up to 25 mL, and dropping 0.5 mL of the solution onto a substrate. Standard samples were prepared by dropping different amounts of the multielement solution onto the substrate. The residual standard deviation for the reference sample of mass from 0.25 mg to 0.7 mg was within the range of 0.001–0.009 mg (correlation coefficient 0.998–0.999) for major elements and within the range of 0.00003–0.0009 mg (correlation coefficient 0.989–0.993) for minor elements. The detection limits for 0.5 mg samples were within the range of 0.015%–0.35% for manganese and zirconium, respectively.