Disposal of whey is an economic and environmental challenge for artisanal creameries and acid whey producers. One possible solution is to ferment and distill whey to produce an alcoholic beverage that may be sold at a premium. The objectives of our research were to evaluate the fermentation and distillation of acid and sweet whey and to compare aroma profiles of the distillates. Acid whey was obtained from cottage cheese production and sweet whey from cheddar production. Volatile compounds from the distillates were extracted using headspace solid-phase microextraction and identified via gas chromatography- mass spectrometry (GCMS). Several differences in volatile composition were identified. Methyl ketones: 2-heptanone, 2-pentadecanone, 2-tridecanone, and 2-undecanone were found to only be present in artisanal creamery’s distillate, whereas geraniol was found only to be present in the acid whey distillate. Significant differences in other compounds peak area were also identified. This research demonstrates that distilled spirits can be obtained from acid whey as well as sweet whey. Differences in aroma compounds likely have an effect upon the organoleptic qualities of spirits produced from whey.