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An analytical control method was needed for the rapid determination of monoand dinitroxylenes in a commercial process for hydrogenation of nitroxylene to xylidine. A polarographic method was devised based on the reduction of mononitroxylene at about 0.9 volt and of dinitroxylene at about 0.5 and 0.9 volt in ethyl alcohol-benzene solvents. Sodium acetate was employed as the supporting electrolyte. Only a few minutes are required for a determination and the accuracy is within 4 and 10% for mono-

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