Abstract: A method is described for the preparation of solutions containing little or no water of tertiary alkyl hydroperoxides in inert solvents by dewatering with sulfuric acid, according to which one or more inert organic solvents are added to an aqueous solution as well as sulfuric acid in such amount and concentration that in the aqueous phase forming after the mixing followed by separation of the phases there is at least 49% of H.sub.2 SO.sub.4 and the water content in the organic phase amounts to no more than 2.5%.

Abstract: A process for the distillative separation of tertiary alkyl hydroperoxides of the formulaR--OOHwhereinR is a tertiary alkyl group with 4 to 6 carbon atoms from the corresponding di-tertiary alkyl peroxides resulting during their preparation, which process comprises neutralizing the reaction mixture resulting during the preparation of the tertiary alkyl hydroperoxide, subjecting same to vacuum distillation in the presence of water at a temperature of less than about 45.degree. C. and recovering the purified tertiary alkyl hydroperoxide as a bottoms product.