An optical fiber probe has been constructed in order to obtain real-time measurements of fluorescence radiation during twin screw mixing and extrusion of plasticized polybutadiene and calcium carbonate particulate. The probe consists of an optical fiber bundle which was inserted along the axis of a half-inch sensor bolt, and it was used to transmit optical excitation energy to the processed material and to detect the subsequent fluorescence. The source of fluorescence radiation was a fluorescent dye which was doped into the processed ingredients at very low concentrations. Although most of our measurements were taken with the probe positioned close to the exit die, the sensor bolt can be placed in any instrumentation port along the extruder line. Experiments were carried out to measure residence time distribution, quality-of-mix, and mix concentrations as a function of processing conditions. Product mix changes in response to variations in material feed rates and screw RPM were also observed. Values of residence time were obtained by measuring the transit times for the dye to travel from an upstream injection port to the measurement probe, a distance of 63 cm. Flow instabilities, such as mat formation of the solids, were observed by noting the abrupt changes and discontinuities in the fluorescence signal.