Diclofenac is a Non-steroidal anti-inflammatory drugs (NSAIDs) are the group most widely used in human and veterinary medicine, since it is available without prescription for treatment of fever and minor pain. The clinical and pharmaceutical analysis of these drugs requires effective analytical procedures for quality control and pharmacodynamics and pharmacokinetic studies. An extensive survey of the literature published in various analytical and pharmaceutical chemistry related journals has been conducted and the instrumental analytical methods which were developed and used for determination of diclofenac (an aryl acetic acid derivative) in bulk drugs, formulations and biological fluids have been reviewed. This review covers the time period from 1989 to 2010 during which 43 methods including spectroscopic, chromatographic titrimetric methods were reported. The application of these methods for the determination of diclofenac in pharmaceutical formulations and biological samples has also been discussed.