Electron paramagnetic resonance (EPR) reveals the presence of free radicals in raw shale, shale oil, and spent shale. Thirty-four samples of raw shale, and the spent shale and shale oil produced in the Fischer assay of these raw shale samples were studied. There is a significant correlation between the gallons per ton oil yield as estimated by Fischer assay and the spin density in the raw oil shale. However, the scatter in the data (due to uncertainties in sample preparation, Fischer assay results, and estimation of spins per gram of sample) limits the analytical utility of this finding. Sample preparation techniques affect the EPR signal.