A method has been developed to permit the simultaneous sampling of S02 and N02 from ambient air. Sulfur dioxide and N02 are collected on triethanolamine-impregnated glass fiber filters. After sampling, the filters are extracted, and the extract Is analyzed for sulfate, nitrite, and nitrate using Ion chromatography. Ambient concentrations are computed from the recovered nitrogen and sulfur and the sampled air volume. Laboratory tests were conducted to evaluate the performance of the method under various species concentrations and loadings, sampling rates, humidities, temperatures, flushing conditions, and Interferences. Results of these tests are described. Field measurements using the developed method compared favorably with other established methods. On the basis of the precision of field blanks, S02 and N02 detection limits of 0.3 and 0.2 ppb for 24-h samples and 0.04 and 0.03 ppb for 7-day samples were estimated. Precision estimates of better than ±15% were found, and accuracy within ±10% was observed.