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The optimization and validation of a procedure for the determination of tritium from gaseous effluents from a nuclear power plant is described. Optimization included performance assessment of silica gel and a molecular sieve as a material for the adsorption of water moisture from air for continuous tritium sampling. In addition, the usability of such a system for monitoring tritium in laboratory air for low-level tritium measurements was assessed. The molecular sieve showed better performance, with an average desorption efficiency of 95% compared to 78% achieved with silica gel. The memory effect was also lower and more reproducible for the molecular sieve, amounting to 7% on average compared to 35% attained for silica gel. Measurement of low-level tritium in air showed the importance of prior checks of intrinsic tritium levels in the molecular sieve as due to that erroneous results could be produced.