Transmission Anisotropy Spectroscopy (TAS) or/and Reflection AnisotropyrnSpectroscopy (RAS) are a powerful non-destructive and sensitive optical probe ofrnsurface that is capable of operating with in a wide range of environments. In thisrnthesis, by applying these optical techniques attempt was made to determine the degreernof anisotropy of a biaxial Potassium Titanyl Phosphate (KTP) crystal and its valuernis of the order of 10−3 and 10−4 for reflection and transmission respectively. It isrnalso seen that the absorption correction of KTP crystal is very small. Thereforernthe coupled techniques are also powerful for the determination of absorption loss of arntransmitting probes. The methods used in this work can also be used in situ real-timernmeasurements