In polyethylene microencapsulation, low-level mixed waste (LLMW) is homogenized with molten polyethylene and extruded into containers, resulting in a lighter, lower-volume waste form than cementation and grout methods produce. Additionally, the polyethylene-based waste form solidifies by cooling, with no risk of the waste interfering with cure, as may occur with cementation and grout processes. We have demonstrated real-time monitoring of the polyethylene encapsulation process stream using a noncontact device based on transient infrared spectroscopy (TIRS). TIRS can acquire mid-infrared spectra from solid or viscous liquid process streams, such as the molten, waste-loaded polyethylene stream that exits the microencapsulation extruder. The waste loading in the stream was determined from the TIRS spectra using partial least squares techniques. The monitor has been demonstrated during the polyethylene microencapsulation of nitrate-salt LLMW and its surrogate, molten salt oxidation LLMW and its surrogate, and flyash. The monitor typically achieved a standard error of prediction for the waste loading of about 1% by weight with an analysis time under 1 minute.