This document discusses the analysis of polyvinylidene fluoride (PVDF) on Agilent PLgel 10 µm MIXED-B and GPC/SEC. PVDF is an important material with a wide range of uses from non-stick coatings to inert packaging materials. However, PVDF can be difficult to analyze by gel permeation chromatography due to its low solubility in common solvents. This challenge can be overcome by using dimethyl sulfoxide as a solvent, Agilent PLgel MIXED-B columns, and operating the GPC system at elevated temperature with appropriate high temperature sample preparation. In this study, three samples of PVDF were analyzed in dimethyl sulfoxide at 95 °C using the Agilent PL-GPC 220 instrument with two Agilent PLgel 10 µm MIXED-B, 300 × 7.5 mm columns. By operating the GPC system at a flow rate of 1.0 mL/min and heating the samples for 4 hours to dissolve them and reduce the solvent viscosity, satisfactory chromatographic separation was achieved.