[en] The present study aims to use the α-spectroscopy at Nuclear Materials Authority (NMA) of Egypt. A radiochemical technique for analysis uranium isotopes was carried out for ten mineralized granitic samples together with the International standards RGU-1 (IAEA) and St_4 (NMA). Several steps of sample preparation, radiochemical separation and source preparation were performed before analysis. Uranium was separated from sample matrix with 0.2 M TOPO in cyclohexane as an extracting agent with a chemical yield 98.95% then uranium was purified from lanthanides and actinides present with 0.2 M TOA in xylene as an extracting agent. The pure fraction was electrodeposited on a mirror-polished copper disc from buffer solution (NaHSO_4+H_2SO_4+NH_4OH). Rectangle pt-electrode with an anode-cathode distance of 2 cm was used. Current was 900 mA and the electrodeposition time reach up to 120 min. The achieved results show that the chemical yield ranged between 87.9±6.8 and 98±8.6. - Highlights: • Radiochemical technique for analysis uranium isotopes. • Alpha-particle spectrometry is performed after a radiochemical procedure. • Electrodeposition conditions for preparation of alpha uranium source. • Using "2"3"2U (t_1_/_2=70.6a, E_α=5320.24 keV, intensity=69.1%) as an internal tracer makes it a highly reliable technique