The free fraction of pertechnetate in Tc-99(m) radiopharmaceuticals has to be tested for quality control reasons in line with the European Pharmacopoeia. Such quality control is often performed by miniaturized chromatographic methods. There are several recommended methods in the literature for quality control of the same radiopharmaceuticals, though it is unlikely that all methods are equivalent. Some of these methods were compared, taking into account different parameters (spot size, time required, analytical artifacts, true separation and shape of the chromatographic peaks, ease of handling), to verify the best method for the control of each radiopharmaceutical. It would appear that instant thin layer chromatography silica gel is the best support for these miniaturized methods, using MEK as solvent to check DTPA, DMSA, gluconate, pyrophosphate, medronate and phytate; NaCl 20% solution is the best solvent for IDA derivatives, human albumin and albumin particles (microspheres, macroaggregates).