Manual preparation of polymer samples for molecular weight characterization by solution methods such as gel permeation chromatography (GPC) is a time-consuming, labor-intensive, and redundant task. Preparation of samples for high-temperature GPC characterization further complicates the procedure. A typical manual high-temperature sample preparation exposes the analyst to both hot surfaces and solvent vapors. An automated system to prepare samples for high temperature GPC analysis has been developed. The system is based on a Zymark laboratory robotic system, and custom hardware peripherals developed at The Dow Chemical Company. The automated procedure performs all the steps required to prepare samples for high-temperature GPC analysis, including the hot steps. The samples were analyzed using the Waters 150-C GPC in combination with the differential refractive index (DRI) and low-angle laser light scattering (LALLS) detectors to demonstrate the reproducibility and reliability of the automated procedure. The system hardware, software options, and performance are presented in this paper.