A quantitative spectrophotometric method using Pd(II) chloride as analytical reagent for the determination of polythiazide in pharmaceutical preparations is described in this study. It has been found that polythiazide reacts with Pd(II) chloride in the pH range 3.6-5.8, forming a red, water-soluble (1:1) complex with maximum absorbance at 527 nm. At the optimum pH of 4.8 and an ionic strength mu = 0.1 M, the conditional stability constant of the complex is found to be log K' = 4.77. The molar absorptivity at 527 nm is 3.2 x 10(3) l mol-1 cm-1. Good agreement with Beer's law was found for polythiazide concentrations up to 2.2 mmol l-1. The nominal percent recovery of polythiazide was 99.5% (n = 20). The simplicity, selectivity and sensitivity of the method described is suitable for rapid and accurate determinations of polythiazide in tablets.