Measurement of 210Po by alpha-spectrometry and 210Pb by beta-spectrometry provide accurate methods of determination at low levels of activity, however, both techniques are time consuming and provide no scope for “in-line' evaluation. The main objective of this work was to investigate the suitability of liquid scintillation counting (LSC) to provide a fast analytical procedure for the determination of these radionuclides in hydrometallurgical process samples which are typically acidic, coloured and contain many different matrix ions.