A reliable and useful gas chromatography method for quantitative analysis of oxygen and nitrogen at room temperature and hydrogen and hydrogen deuteride at 77 K in high-purity deuterium was developed using 5 A molecular sieve and alumina as column packing materials respectively. The minimum detection limit was 150-200 ppm for hydrogen and hydrogen deuteride. The method is suitable for quantitative analysis of impurities during high-purity deuterium preparation. Copyright (C) 2011, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.