^Primary nitroparaffins have been determined spectrophotometrically by means of their coupling reaction with p-diazobenzenesulfonic acid. Secondary nitroparaffins and 2-nitro-2a Iky 1-1 -alkanols do not interfere, but 2-nitro-2-alkyl-1,3-alkenediols react with p-diazobenzenesulfonic acid. Nitromethane can be determined at 440 mp in the concentration range up to 50 per ml.,'while nitromethane and 1 -nitropropane can be determined at 395 mp up to 80 and 100 per ml., respectively.