The procedure for the preparation of NiZn-ferrite powder with average particle size of 10 nm and saturation magnetization of 50 emu/g by using precipitation reaction between acidified sulphate precursor salts and NH4OH as the precipitating agent in the water-in-oil domain of the microemulsion CTAB/1-hexanol/water at 45 degrees C is presented herein. TEM measurements have revealed relatively uniform morphology of the particles, which are associated in coral-like agglomerates. EDS measurements have been used for qualitative analysis of the sample, whereby FAAS measurement has been performed in order to reveal the proportion of the cations in the sample - Ni : Zn : Fe = 0.17 : 0.18 : 2.64.