The objectives of this study were to identify and compare the composition, flavor, and volatile components of serum protein concentrate (SPC) and whey protein concentrate (WPC) containing about 34% protein made from the same milk to each other and to commercial 34% WPC from 6 different factories. The SPC and WPC were manufactured in triplicate with each pair of serum and traditional whey protein manufactured from the same lot of milk. At each replication, SPC and WPC were spray dried (SD) and freeze dried (FD) to determine the effect of the heat used in spray drying on sensory properties. A trained sensory panel documented the sensory profiles of rehydrated SD or FD powders. Volatile components were extracted by solid-phase microextraction (SPME) and solvent extraction followed by solvent-assisted flavor evaporation (SAFE) with gas chromatography-mass spectrometry and gas chromatography-olfactometry. Whey protein concentrates had higher fat content, calcium, and glycomacropeptide content than SPC. Color differences (Hunter L, a, b) were not evident between SPC and WPC powders, but when rehydrated, SPC solutions were clear, whereas WPC solutions were cloudy. No consistent differences were documented in sensory profiles of SD and FD SPC and WPC. The SD WPC had low but distinct buttery (diacetyl) and cardboard flavors, whereas the SD SPC did not. Sensory profiles of both rehydrated SD products were bland and lower in overall aroma and cardboard flavor compared with the commercial WPC. Twenty-nine aroma impact compounds were identified in the SPC and WPC. Lipid and protein oxidation products were present in both products. The SPC and WPC manufactured in this study had lower total volatiles and lower concentrations of many lipid oxidation compounds when compared with commercial WPC. Our results suggest that when SPC and WPC are manufactured under controlled conditions in a similar manner from the same milk using the same ultrafiltration equipment, there are few sensory differences but distinct compositional and physical property differences that may influence functionality. Furthermore, flavor (sensory and instrumental) properties of both pilot-scale manufactured protein powders were different from commercial powders suggesting the role of other influencing factors (e.g., milk supply, processing equipment, sanitation).