A rapid, quantitative batch procedure for analysis of atmospheric nitrogen oxide samples (NO + NO2, commonly referred to as NOx) from mines, tunnels, and raw or dilute diesel exhaust is described. This modification of the phenoldisulfonic acid nitration procedure eliminates the time-consuming evaporation step and two transfer steps of the original procedure. Samples are collected in evacuated bottles containing an absorbent solution and hydrogen peroxide to completely oxidize the gas-phase NOx to nitric acid. After destruction of excess oxidant, an aliquot of the absorbed sample is added to the phenoldisulfonic acid reagent in a 25-ml. volumetric flask which is used as the reaction vessel for subsequent nitration and neutralization. This modified method can double or triple the number of analyses per day by the original method.
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