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A new steady-state method for studying dynamic photochemical processes by EPR is discussed. The EPR spectra of some photolysed alkyl hydroperoxides are obtained and the free radical intermediates identified as alkoxy radicals. Recombination rate constants of ∼105 liters/mole sec were obtained with activation energies of ∼4 kcal. A new EPR spectrometer with improved sensitivity capable of photoirradiation in situ and variable temperatures is discussed.