Hydrogen--deuterium exchange in transition metal hydridocarbonyl cluster complexes. Standardization of a mass spectroscopic analytical technique

The facil exchange of H2Re2(CO)8 and H2Os3(CO)10 with D2O in the presence of Florisil chromatographic adsorbent was monitored by mass spectrometry. Owing to the possibility of an isotope effect in the ionization process and the presence of random errors in the recording system, a determination of the accuracy and precision of this analytical method was undertaken. As an extension of thermal hydrogenation synthesis, several of the compounds used in these studies were prepared by photolytic hydrogenation of Re2(CO)10