The use of radiotracers in the present study is intended to replace traditional steps of metal quantitative analysis (solution sampling and instrumental chemical analysis) and to allow real-time measurements of metal concentrations during the leaching process. In this study, 64Cu, an isotope of copper, was selected as a radiotracer. Samples of copper flotation tailings were irradiated in the Maria research reactor (Świerk, Poland) and mixed with an inactive portion of the milled fl otation waste. The leaching process was carried out in a glass reactor, and the radiation spectrum was measured using a gamma spectrometer. The material was then treated using various acids (sulphuric acid, nitric acid, acetic acid, citric acid, and ascorbic acid) in a wide range of their concentrations. Experiments with the radiotracer were conducted in sulphuric and nitric acids. The amount of the leached metal (copper) was calculated on the basis of the peak area ratio in the gamma-ray spectrum of the activated tailings and standard samples. Inductively coupled plasma mass spectrometry (ICP-MS) was also used to analyse the metal content. Maximum recovery of 56% Cu was achieved using 9 M HNO3, whereas the recovery was lowest for ascorbic acid (<1%). Both analytical methods were compared, and the results presented in this paper are in good agreement with radiometric measurements obtained using ICP-MS analysis.