The results of study of the content of rhenium and other valuable metals in the oil shales of the Volga basin are presented. The new data on precise determination of Re, Co, Ni, Cu, Zn, U and other metals by inductively coupled plasma mass spectrometry have been published. The content of the studied metals were compared with clarks in carbonaceous shales. The association of metals with rhenium (Mo, U, Co, Ni, Cu, Zn, Se, Ag, Sb) has been isolated in oil shales. The organic matter of oil shales acts as a rhenium concentrator, and apparently Mo, U. The preferred petrographic type of oil shales for the concentration of rhenium in them is the colloalginite-vitrinite-clay type. The rhenium-bearing and metalliferous content of the Volga shales is compared with the contents of rhenium and a number of other valuable metals in dictyonema shales of the Baltic sedimentary basin.