A spectrophotometric method for the determination of palladium, iron and tellurium from nitric acid media after extraction of their p-[4-(3,5-dimethylisoxazolyl)azophenylazo]calix(4)arene [DMIAPAC] complexes has been developed and possible synergistic effects have been investigated. Chloroform, carbon tetrachloride, cyclohexane, 1,2-dichloroethane, toluene and xylene were used as the diluents. The maximum enhancement was obtained in the presence of 30% 1,2-dichloroethane. The trace amounts of metals were determined spectrophotometrically. Beer’s law obeyed in the concentration range of 5.0–95.0 μg, 8.0–120.0 μg and 10.0–140.0 μg/10 mL of the final solution of palladium, iron and tellurium, respectively. The molar absorptivities (l mol−1cm−1) and Sandell’s sensitivities (μg cm −1) were calculated: Pd(II) = 1.73 × 104 and 0.0061; Fe(III) = 1.08 × 104 and 0.0052; Te(IV) = 1.67 × 104 and 0.0077. Ten replicate analyses containing 20 μg of Pd(II), 12.5 μg of Fe(III) and 32 μg of Te(IV) gave mean absorbance of 0.326, 0.242 and 0.418 with relative standard deviation of 0.36, 0.65 and 0.82% for Pd(II), Fe(III) and Te(IV), respectively. The interference of various ions was studied and optimum conditions were developed for the determination of these metals in certain alloys and synthetic mixtures.