Natural gamma ray well logging, an effective tool in geophysical prospecting, is used to investigate the radioactive and phosphatic layers in the Khneifiss mine in Syria. The interpretation of the gamma ray measurements, using numerical methods of analysis developed previously and applied successfully in some phosphatic areas in Syria, make it possible to define precisely the phosphate thickness from place to place in the study area. This technique has been successfully applied while studying seven boreholes in the area. Sixty-three core samples from phosphatic layers in the boreholes have been analyzed, using gamma ray spectrometry for the determination of P2O5 , U, Th, and K. Good correlation between P2O5 content and U concentration has been found. The total count gamma logs correlate reasonably well with the U core analysis, suggesting that radioactive equilibrium exists in the U decay series. These gamma logs can be therefore used effectively to quantitatively map the distribution of P2O5 and U. The characteristics of both subsurface phosphatic sand and phosphatic rocks have been investigated and outlined using a statistical approach. The affinity of uranium to some trace elements such as V, Sr, Cu, and Ni has been verified using correlation matrices of these elements.