A general introduction to ac conductivity and a specific introduction to Complex Impedance Spectroscopy (CIS) technique are dealt with in Chapter 1. To acquire information on the work done already in this direction, literature survey is being carried out. Chapter 2 comprises of the review of the literature, namely the various experimental techniques developed by earlier workers in this direction. The third chapter is divided into two parts. The first part deals with the instrumentation developed in the present study. The second part of this chapter comprises of the calibration of the developed circuit. Chapter 4 deals with the synthesis of new samples. Studies made and the results obtained using the developed circuit is discussed in Chapter 5. In essence, the thesis highlights the development of instrumentation for ac conductivity measurement and investigations made on certain polymers. The technique developed in the present work is cost effective since costly instruments such as impedance analysers, ac conductivity bridges are not used. A personal computer with interfacing hardware and suitable software is what is needed in carrying out the investigations.