A method using gas chromatography for the analysis of carbon dioxide, carbon monoxide, and nitric oxide in diesel exhaust was developed. A gas chromatograph containing a liquid phase column in series with a molecular sieve column, each of which eluted into thermal conductivity detectors, was utilized. Activation of the molecular sieve column was achieved by heat-treating and purging with nitric oxide. The chromatograph was calibrated by introducing sample mixtures of known concentration and measuring the responses. The exhaust gases of a diesel engine were analyzed while the engine operated at constant speed and load. Engine speed was kept at 1400 rpm while several different loads were applied. The results of these tests indicated that carbon dioxide, carbon monoxide, and nitric oxide concentrations all increased with load in the load range studied. Carbon monoxide exhibited a greater dependence on load than did the other compounds. Additionally, water was injected into the intake air stream to study its effect on nitric oxide concentration. Nitric oxide levels were reduced by 15% when a water/fuel mass ratio of 0.75 lb/lb was used. / Master of Science