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Two spectrophotometric methods for the trace determination of hydroperoxides in benzenemethanol medium are compared. The first is based on complex formation between Fell and 1,lO-phenanthroline (tentatively denoted by FellP), and the other makes use of the complex formed between Fell1 and the thiocyanate anion (tentatively denoted by FelllT). The thiocyanate method, when modified by adding more benzene to the system and employing active silver to suppress the blank values, proved to be less laborious, more sensitive and faster than the determination with 1,IO-phenanthroline. The yield of FelIlT is almost stoicheiometric, which is not so for the Fe"P complex. Owing to its simplicity, great sensitivity and reproducibility, the modified thiocyanate method is suitable for series determinations.