Simple Summary Acid oils and fatty acid distillates are by-products from the edible oil refining industry that are rich in free fatty acids. Their use as feed ingredients is a way to valorize them in order to increase the sustainability of the food chain; however, differences in the animal productive parameters when using them have been reported. The objective of this study is their characterization and the identification of their sources of variability. Results have revealed a high variability in their composition, being influenced both by the botanical origin of de crude oil and by the type of refining process. Thus, the analytical control and standardization of these by-products is of outmost importance to guarantee a standardized quality which would increase their value as feed ingredients. Remarkably, almost all samples showed some compositional values above the limits recommended by some feed fat guidelines, which suggests that the production of these by-products must be standardized and improved, and some of the thresholds should probably be revised. Abstract Acid oils (AO) and fatty acid distillates (FAD) are oil refining by-products rich in free fatty acids. The objective of this study is their characterization and the identification of their sources of variability so that they can be standardized to improve their use as feed ingredients. Samples (n=92) were collected from the Spanish market and the MIU value (sum of moisture, insoluble impurities, and unsaponifiable matter), lipid classes, fatty acid composition, and tocol content were analyzed. Their composition was highly variable even between batches from the same producer. As FAD originated from a distillation step, they showed higher free fatty acid amounts (82.5 vs 57.0 g/100 g, median values), whereas AO maintained higher proportions of moisture, polymers, tri-, di-, and monoacylglycerols. Overall, the MIU value was higher in AO (2.60–18.50 g/100 g in AO vs 0.63-10.44 g/100 g in FAD), with most of the contents of insoluble impurities being higher than those in the guidelines. Tocol and fatty acid composition were influenced by the crude oil’s botanical origin. The calculated dietary energy values were, in general, higher for AO and decreased when a MIU correction factor was applied. The analytical control and standardization of these by-products is of the outmost importance to revalorize them as feed ingredients.