Differential scanning calorimetry (DSC) was used to investigate the influence of resin synthesis parameters on the thermal behavior of low molecular weight phenol-formaldehyde (PF) resol resins prepared with different formaldehyde/phenol (F/P) molar ratios, different sodium hydroxide/phenol (NaOH/P) molar ratios, and different catalysts. As the F/P molar ratio increased, the molecular weight and activation energy increased while the gel time, peak temperature, resin pH, and nonvolatile solids content decreased. By contrast, the molecular weight, gel time, resin pH, resin solids content, and peak temperature increased with an increasing NaOH/P molar ratio. However, the activation energy decreased with an increasing NaOH/P molar ratio. The polydispersity increased with both F/P and NaOH/p ratios. Calcium hydroxide gave a faster curing resin compared to sodium and potassium hydroxides. All DSC thermograms of this study showed just a single exothermic peak for the resins that were used.