Three gas chromatographic systems a ppropriate for the reproducible rapid preparation and subsequent quantitative analysis of rum concentrates were developed and tested. The first and second systems employed preparative columns directly coupled to a capillary Golay column. Rum concentrates obtained in the preparative column were collected in a stainless steel trap of low dead space and simultaneously analyzed in the capillary system by flash heating of the trap. The third system used the same chromatographic equipment, with a 1/4-in o.d. trap to transfer an amount of concentrate to a 2-ml vial. These concentrates were subsequently analyzed with two Golay columns. In the first system, a 10-ft 20% Carbowax 20M packed preparative column coupled to a 150-ft Golay column through a 1/8-in o.d. trap gave excellent results in the analysis of the volatile fraction of rums. Ten congeners eluting before alcohol were detected in a commercial rum, six of which have not been identified. The second system, utilizing the 10-ft Carbowax 20M coupled to a 7-ft Porapak Q preparative column, was tested successfully with a 1/8-in o.d. trap. About 30 congeners were detected in the same commercial Puerto Rican rum. A 7-ft Porapak Q packed preparative column was investigated in the third system provided with a 1/4-in o.d. trap. About 40 congeners were detected in two commercial Puerto Rican rums utilizing a 50-ft SE-30 Golay column in series with a 150-ft Carbowax 20M Golay column. Results demonstrate the feasibility of obtaining a rapid and complete analysis of distilled alcoholic beverages.