A new method with repetitive freezing thawing process was developed to separate authigenic clay minerals from sedimentary rocks. The aim of this process was to disaggregate rock samples using the volume expansion of water that impregnates into the samples. The results from X ray diffraction analysis show that in comparison to the conventional method there is no K feldspar pieces in the clay minerals (with clay mineral size 1?μm) separated from sedimentary rocks by the new method.