The work reported in this thesis has been carried out in the following two areas of Optical metrology: 1. Measurement and correction of prism angles 2. Measurement of refractive indices using a spectrograph. The prism angles are conventionally tested by mechanical bevel protractors, autocol-limators (angle dekkors), simple interference techniques and interferometers. All these methods have their own limitations either in accuracy or in terms of cost. Mechanical methods are usually employed to measure the angles of prisms. Interference techniques and interferometers are also used but they need optically polished components. For both mechanical and simple interference methods of testing, it is essential to fabricate more than a single component in number. The process of building interferometers or purchasing interferometers, angle dekkors and standard angle gauges is not cost effective for many research laboratories, and medium scale industries. To overcome these difficulties simple and inexpensive methods without sacrificing the accuracy in the bargain are suggested for the measurement of prism angles, based on the principles of reflection of light. The refractive indices of prism materials for invisible and weaker spectral lines are usually determined from spectrograms using dispersion formulae and numerical interpolation techniques. In these methods, the accuracy of the results depends on the accuracy of determining the constants of the dispersion formulae. A simple experimental technique, using a spectrograph, is devised for the measurement of refractive indices of solids and liquids both for visible and invisible spectral lines (wavelengths). The thesis has been divided into six chapters. The first chapter starts with the general introduction. The second chapter presents the literature review of the existing methods for angle and refractive index measurements. The third chapter describes the proposed new techniques for prism angle measurements. The fourth chapter presents the experimental results of angle measurements, and the discussion of the accuracy of the results. This chapter also gives the scope for further research. The fifth chapter describes a newly proposed technique for measuring refractive indices and the experimental results. This chapter also gives the scope for further research. The summary of the results, conclusions, and suggestions for further work are presented in chapter six.