The aim of this investigation was to determine if the rapid solvent removal evaporation that occurs during electrospinning enabled the gluten protein and poly( vinyl alcohol) (PVOH) chains to remain at least partially entangled in the final product. Natural and synthetic biopolymer blends are known to phase separate in the melt. Differential scanning calorimetry (DSC) was used to test our hypothesis, which we achieved by systematically comparing the thermal profiles of the nonwoven fibrous sheets comprising: 1) 100% commercial wheat gluten, 2) 100% PVOH, and 3) the (75/25) wheat gluten/PVOH blend. The DSC scans of the two PVOH-containing, nonwoven fibrous sheets exhibited differences in the characteristics and positions of the melting peaks (T(m)) of the PVOH crystalline phase, while the DSC scans of the nonwoven fibrous sheets comprising either 100% commercial wheat gluten or the wheat gluten/PVOH blend yielded neither a measurable glass transition temperature (T(g)) nor a Tm. Energy dispersive spectroscopy (EDS) was used to compare the elemental compositions of the individual fibers with the compositions of the spherical domains found in the nonwoven fibrous mats. These scans revealed that the mineral matter found in commercial wheat gluten ( roughly 1% by weight) had phase-separated from the bulk gluten protein as a result of electrospinning.