Abstract
Micromethods are described for the determination of nitro and nitroso groups by means of titanous chloride with samples of 3 to 9 mg. The apparatus consists of a modified Machlett microburet with a ground glass tip, and a reaction flask which has a ground glass neck and two side arms. Titanous chloride solution is stabilized with amalgamated zinc so that its normality remains practically constant for 3 weeks. Satisfactory results have been obtained for all aromatic nitro and nitroso compounds which were analyzed, and a relative precision of about ±0.3% has been established. Nitroso compounds can be determined in the presence of certain nitro compounds by replacing the buffer with concentrated hydrochloric acid.N-nitroso compounds could not be determined separately in mixtures containing nitro compounds.
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