An integrated scheme has been developed for the separation of the oxygen and nitrogen compound types present in high boiling petroleum fractions into reasonably clean cut fractions for further analysis by other techniques. Cation and anion exchange are used in conjunction with adsorption chromatography on alumina, silica, and charcoal. The resulting separations are experimentally convenient, repeatable, and predictable, and sample recoveries are satisfactory. Sample reactions during separation appear to be generally minor and do not interfere with sample analysis. The use of this separation scheme-in whole or in part -by different workers should also serve to interrelate their findings on the analysis of different crude oil fractions. © 1968, American Chemical Society. All rights reserved.