The optimum extraction conditions have been evaluated by studying various parameters such as acidity, reagent concentration, equilibration period, diluent effect and effect of diverse ions for the separation of palladium(II) using 2-oxo-4'-hydroxy-phenylacetaldehyde oxime (HOHPO). Palladiuni(II) was quantitatively extracted with HOHPO from 0.2 M acetic acid medium into chloroform. The extracted yellow coloured complex showed maximum absorption at 420 nm. The nature of the extracted species was determined by the plot of log D versus log [HOHPO]. Palladium(II) was separated from number of elements with which it is generally associated. The method was extended for the analysis of synthetic mixtures and sonic real samples.