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Active gas atoms of N and O were produced in a flow system by subjecting N2 to a microwave discharge. The amount of N atoms produced was accurately measured by titration with NO. The O atoms were generated by titration reaction. The gas in the flow system was sampled through a leak by a time-of-flight mass spectrometer which was developed for upper atmosphere sampling. Various experiments were conducted to find the optimum conditions for the detection of these atoms. It was found that the O atom response of the mass spectrometer was most affected by the entrance geometry into the ion source, while the N atom response was hardly changed. The most sensitive mass spectrometer variable for atom determination in the presence of air gases was found to be the energy of the ionizing electron; the optimum electron energy range was found to be 16 eV to 24 eV. (Author)