We implemented a laboratory apparatus based on a NaI(TI) gamma-ray spectrometer for the assessment of naturally occurring radioactive materials. This apparatus is devoted to the quantitative determination of U, Th and K in rock and soil samples. We analysed the calibration procedures with particular emphasis to factors which affect accuracy and detection limits. A first series of measurements were compared to those obtained by means of high energy gamma-ray spectrometry. A discussion was made on factors restricting the approach based on scintillation spectrometry, such as secular equilibrium and radon encapsulation.