Date of Award
Master of Science in Chemistry - (M.S.)
Chemical Engineering, Chemistry and Environmental Science
R. P. T. Tomkins
James M. Grow
A simple method, by High Performance Thin Layer Chromatography HPTLC), was developed for rapid determination of N-Nitrosohexamethyleneimine in Benzenesulfonamide, N-[((hexahydro-1 H Azepin-1-yl)amino]-Carbonyl]-4 methyl, (Tolazamide). Separation of N-Nitrosohe-xamethyleneimine from a Tolazamide solution in chloroform was obtained by precipitation of Tolazamide with n-heptane and by passing the resulting clear solution through a small silica column which was eluted with methanol.
Determination of the N-nitroso compound was achieved by ultraviolet irradiation of it on activated High Performance Silica Gel Plates. Detection was performed by spraying the plates with triethylamine and fluorescamine reagent giving a fluorescent product. Visual detection limits of 25 ppb were observed.
The method is recommended for rapid screening purposes.
Valdez, Anulfo A., "Detection and determination of N-Nitrosohexamethyleneimine in benzenesulfonamide, N-[[(hexahydro-1-H azepin-1-YL)amino]-carbonyl]-4 methyl by HPTLC" (1988). Theses. 1962.