Microdetermination of organic peroxides: Comparison of iodometric and titanous chloride reduction methods

Abstract

Iodometric and titanous chloride micromethods are presented for determining peroxides. Sample weights for all determinations arranged from 3 to 15 mg. The iodometric microprocedure includes the use of a ferric catalyst for the determination of alkyl hydroperoxides, peroxyesters, diacyl peroxides, bicyclic peroxides, and ketone peroxides. The use of the catalyst enabled most of the peroxides tested to be determined in 5 min. at room temperature. This compares to a previous microiodometric procedure which required 15 hr. for a determination. The titanous chloride method employs a stabilized titanous reagent dispensed from a modified Machlett microburet. Reaction time required is also 5 min. It is shown by comparison of the micromethods that the iodometric procedure is preferred.