A spectrophotometric determination of butadienefurfural condensation product, a carbonyl compound, can be made by reaction of the compound with 2,4dinitrophenylhydrazine in a two-phase system composed of iso-octane and an alcohol-water-phosphoric acid mixture.The 2,4-dinitrophenylhydrazone is selectively extracted into the iso-octane phase and its concentration determined by absorption measurement at 340 µ.The excess reagent remains in the aqueous phase and does not interfere.
readily and undergoes autoxidation on exposure to air (15).Acetanilide-Boron Trifluoride. A solution of acetanilide in chloroform was added to an excess of boron trifluoride dissolved in diethyl ether. The crystalline product was filtered, washed, while wet, with ether, and stored in vacuo over anhydrous calcium chloride for 48 hours before analysis. The product melted, with decomposition, at 143°to 149°C. [133°C . with decomposition ( 16)].
PROCEDUREThe combustion tube was conditioned in a stream of oxygen for 24 hours, after which a few unweighed samples of benzoic acid were burned to restore moisture equilibrium and activate the platinum gauze. The furnace temperature was maintained at 725°± 25°C. and the heating mortar at the boiling point of p-cymene.The sample contained in a platinum boat was placed 6 to 7 cm. in front of the platinum gauze (Figure 1) and the sample burner was placed 2 to 3 cm.
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