Abstarct: A highly selective, rapid and sensitive spectrophotometric method for determination of Pd (II) is proposed in the acidic media. Pd (II) forms a complex with TAN which is soluble in aqueous sodium dodecyle sulfat (SDS) as a micellizing agent and can be monitored spectrophotometrically at 724 nm and 662nm. The linear range of calibration and detection limit at 724nm and 662nm are 0.100-6.00, 0.120-6.00 and 0.024, 0.023 µg.ml-1of Pd(II), respectively. The results show that many ions at high concentration did not interfere with Pd (II). The relative standard deviations for 6 determinations of 1.50, 3.00 and 5.00 µg.ml-1of palladium at 724nm and 662nm are 1.58%, 1.32%, 1.63% and 0.991%, 0.760%, 1.03% respectively. The capability of the method for the analysis of real samples was evaluated by determination of Pd (II) in tap water and alloy samples. A highly selective, rapid and simple spectrophotometric method for simultaneous determination of Pd(II) and Cu(II) by 1-(2-thiazolyl azo)-2-naphtol(TAN), using standard addition method(HPSAM) is described. The ligand and its mextal complexes (Pd(II)-TAN) and (Cu(II)-TAN) are water-soluble in aqueous sodium dodecyle sulfat (SDS) as a micellizing agent. The linear range was 0.100-6.00 µg.ml-1 for Pd(II) and 0.040-3.40 µg.ml-1 for Cu(II). The results show that Pd(II) and Cu(II) can be determined simultaneously with the concentration ratios of Pd(II) to Cu(II) varying from 7:1 to 1:5 in the mixed sample. The capability of the method for the analysis of real samples was evaluated by determination of Pd (II) and Cu(II) in tap water and alloy samples.