Gamma spectrometric measurements to determine the isotopic composition and total uranium mass in UO pellets (D = 7.5 mm; H = 3.5 mm, ρ = 10 g/cm) were carried out. The required efficiency curve was obtained by applying the efficiency transfer method from a calibration standard (D = 65 mm; H = 20 mm) of a slightly acidified water solution. The average isotopic composition of ten UO pellets was consistent with values of natural uranium given by IUPAC. The average relative bias for the U/U amount ratio was -0.73% using the 1001 keV gamma line for U and 0.50% using the 63 keV gamma line (186 keV was always used for U). For the total uranium mass, the mean deviation as compared to mass determinations using a balance was 5.5% using the 1001 keV gamma line for U and 4.3% using the 63 keV gamma line.
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