The goal of this research was to quantify the degradation experienced by a polymer electrolyte fuel cell after storage at subzero temperatures ranging from 0 to -40°C. The performance loss was determined by comparing the polarization and other applicable power curves before and after the subzero storage cycle. The causes of this performance degradation were investigated by the use of Scanning Electron Microscope, Energy Dispersive x-ray Spectroscopy, and porosity scanning technologies. It was found that there are two distinct types of degradation experienced by the membrane. The first type was identified as a variance of the actual voltage - current relationship of the cell. The membrane experienced a 2 - 15% power reduction depending on the load applied to the cell. This mode of degradation only pertained to the initial freeze/thaw cycle and was not observed after any number of subsequent cycles. The cause of this type of degradation has been hypothesized to be related to the delamination of the proton exchange, gas diffusion, and micro porous layers. The second type of degradation was only observed during the subsequent cycles, and mainly affected the high power regions of the operating range. A 5% reduction in current density and power output was observed as a result of further freeze/thaw cycles. Mass transport limitations may have been caused by the destruction of the meso-porous gas diffusion and micro-porous layers. The pore size, volume, and membrane surface area were quantified using a B.E.T. porosity scanner. The results showed that the pore diameter of the catalyst and proton exchange layer did not increase significantly. The porosity scanner did indicate that a pore volume increased by a factor of ten and was confirmed by the surface area measurements of the membrane. The S.E.M. investigations allowed visual inspection of the membrane's structural integrity. Physical separation of the catalyst and gas diffusion layers was observed in the experimental sample, while a more homogeneous assembly was seen in the control sample.