An accurate X-ray fluorescence spectrometric method is described for the determination of lead, zirconium and titanium in lead zirconate-titanate ceramics. Careful matching of samples and standards by a borax fusion method resulted in a relative standard deviation of about 0.2% for the major constituents. The determination, after separation, of the unreacted oxide of lead by atomic absorption spectrometry, and of the unreacted oxides of zirconium and titanium by X-ray fluorescence spectrometry is also described. An X-ray fluorescence spectrometric method is proposed for the determination of dope elements (K, La, Sm, Yb) with internal standards (Ca, Ce, Cr, Ni respectively). The magnesium dope is determined by atomic-absorption spectrometry with standard addition.