Separation of macro amount of gold(III) from a small amount of Pd(II) was investigated by ion exchange. From the screening experiments, a nonionic resin Amberlite XAD7HP was selected for this purpose. The adsorption behavior of Au(III) onto Amberlite XAD7HP followed Langmuir isotherm. The loading capacity obtained from the isotherm agreed well with that experimentally measured. Au(III) solution with 99.99% purity was obtained by eluting the loaded Amberlite XAD7HP with the mixture of HCl and acetone. Comparative studies on the synthesis of gold particles were done from the eluate by adding ascorbic acid and K2CO3 in presence and absence of acetone.