Graduate Thesis Or Dissertation
 

Controlled potential coulometry in non-aqueous solvents--application to the Karl Fisher determination of water and to aromatic nitro compounds in dimethyl-sulfoxide

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  • Aromatic Nitro Compounds. The n-values for the reduction of the isomers of nitrophenol and nitrobenzoic acid and for several other nitro compounds are determined in dimethylsulfoxide by controlled potential coulometry. A procedure is given in which one mole of nitro compound may be determined with errors of less than one percent. The associated background currents are quantitatively evaluated, and electrolysis conditions for their minimization are discussed. Controlled potential polarographic determinations are given for these nitro compounds in dimethylsulfoxide, and reaction schemes are proposed for the stepwise reductions. Water. Microgram quantities of water are determined by rapid, controlled potential coulometry. Excess iodine is produced and removed coulometrically in a Karl Fischer system. By means of a special cell design, two μmoles of iodine in methanol may be reduced in 96 seconds. Ten to 74 μg. of water in methanol and 18 to 82 μg. of water in dimethylsulfoxide may be determined with an absolute standard deviation of ± 0.2 and 0.3 μg. of water, respectively.
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