[en] By the end of 1996, the tests of the radiochemical purity (RCP) of preparation of HMDP-^99mTc at Necker hospital were effected by means of 'Tech-Kit' technique which allowed making evident only one radiochemical impurity, the free TcO₄^-. So, the aim of this work has been the search for another technique able to detect also the reduced hydrolyzed ^99mTc, and then, to optimize, validate and standardize this new technique. Several methods have been tested and compared on different points (the chemical species identified, practical difficulties, duration, reproducibility) in order to chose 'the best' one, consisting in associating two TLC (migration time, 3 minutes): - TLC no.1, ITLC-SG/Methyl-ethyl-ketone; - TLC no.2, ITLC-SG/1M Sodium acetate. This method has been subsequently: - optimized, concerning the quantity of deposed sampling, way of deposit drying, migration range, reading protocol by radio-chromatograph; - validated, by verifying the migration of radiochemical impurities by means of controls and by evaluating its sensitivity; - standardized, by defining the interest zones for interpreting the radio-chromatograms, by evaluating the reproducibility and by calculating the 'normal values' of RCP percentages. This method has been adopted as routine and with current recoil (40 preparations) and our conditions of realizations, the extreme values of the percentages obtained for the impurity zones of interests, have been the following: - TcO₄^- zone, [0.39%-1.07%]; - hydrolyzed reduced Tc zone, [0.96%-5.09%]. By taking into account their distribution we calculated a minimum RCP value of 94% to accept the preparation (the RCP being defined as equal to 100% - % TcO₄^- % hydrolyzed reduced Tc)