One of the prospective directions in the development of the generation IV reactors is the use of liquid metals as a coolant. At the same time, to ensure compliance with all the requirements, it is necessary to solve many practical problems and challenges. The subject of this work are radiochemical investigations required for licensing of the MYRRHA reactor conducted within the MYRTE-project as part of the EU-Programm for Research and Innovation “Horizon 2020” . The previous studies on the volatilization of radionuclides from liquid lead-bismuth eutectic (LBE) relevant for the safety of future accelerator driven systems will be extended to measuring the volatilization behaviour of fission products such as Cs, I and also the activation product Po from dilute solutions in LBE. Here, we describe the development and optimization of the samples preparation and experimental equipment for the transpiration method used for volatilization studies, through which it became possible to obtain reliable experimental data. Various series of experiments have been performed using the optimized setup, using 134Cs, 131I and 210Po tracers. In this report, we summarize the methodological development and show results in comparison with existing literature data determined by other authors.