This study investigates the possibility of using a time-resolved Fluorescence and Diffuse Reflectance Spectroscopy (tr-FRS) system to define tumour surgical margins of invasive ducal carcinoma of breast. UV excitation light was used for the fluorescence component and data was collected from the 370-550 nm range. A broadband source was used for diffuse reflectance collection and the emitted response was in the 400-800 nm range. 40 matched pair cases were collected from patients undergoing breast conservation surgeries. Histological analysis was performed on each sample to determine the fat and tumour content within each normal and tumour sample respectively. Statistical analysis was performed on the optical data to reveal biochemical changes in the endogenous fluorophores collagen, reduced nicotinamide adenine dinucleotide (NADH), and flavin adenine dinucleotide (FAD) as well as changes in absorption and scattering properties attributed to variances in absorber concentrations and cell density respectively. Statistical significant differences in collagen, NADH, and FAD lifetimes, collagen, NADH, FAD and NADH/FAD intensity, diffuse reflectance and reduced scatter coefficient were observed between tumour and normal breast samples. These significant factors were used in Principle Component Analysis model construction and a binary classification scheme using Soft Independent Modeling of Class Analogy (SIMCA) was used as a classification tool to predict unknown breast samples as either normal or tumour with specificity of 60% and sensitivity slightly over 50%. / Thesis / Master of Science (MSc)