Molecular and isotopic analysis of sediments from archaeological combustion features is a relatively new area of study. Applications can inform us about ancient pyrotechnologies and patterns of animal exploitation in a wide range of human contexts, but may be particularly informative with regard to ancient hunter-gatherers. Our analyses of sediments from experimental bone and wood fires, and from controlled laboratory heating sequences, provide fine-grained data on the formation and location of biomarkers from pyrolyzed animal fats in hearths. Integrating microstratigraphic, molecular, and isotopic data can improve recognition of bone fires in archaeological contexts, perhaps even where bone preservation is poor. Experimental bone fires produced an upper layer of calcined bone above a thin layer of tarry black amorphous material coating mineral sediments. Mineral sediments beneath the black layer showed little alteration but high lipid content. Sampling for molecular and isotopic analysis should target the black layer as the bulk of pyrolyzed biomarkers are located here and stable isotope values are less affected than in the overlying layer of ash or calcined bone. The combined presence of certain symmetric and slightly asymmetric saturated long-chain ketones (14-nonacosanone, 16-hentriacontanone 16-tritriacontanone, and 18-pentatriacontanone), especially together with heptadecane (C 17 n-alkane), are molecular indicators of the thermal degradation of terrestrial animal fat. Formation and relative dominance of these molecules in hearth sediments relates to the initial prevalence of specific precursor fatty acids and can provide broad separations between sources. We suggest that separations could be further supported and expanded by combining stable isotope analysis of the same compounds.Thermal processing and combustion of animal bone, fat, and oil for food and fuel has been critical to human survival in a wide range of contexts. Fat is an important source of energy and allows for efficient use of protein in carbohydrate-poor environments (Outram 2002;