X1 1 For part IX see ref. 34.. Thermogravimetric and quantitative studies of the oxidative decarbonylation of tungsten hexacarbonyl

Abstract

Thermogravimetric and Derivative Thermogravimetric Analyses have been carried out on different stoichiometric mixtures of W(CO)6 and (CH3)3NO·2H2O (TMNO) under nitrogen. The stuides indicate that the optimum reactant ratio (W:TMNO) is close to 1:4, at which there is a single-step weight loss in the region 50-90°C and a residue (ca. 13%) is left. The rapid loss in weight is attributed to the ready decomposition of the primary product W(CO)6-n(Me3N)n (n>1). At W : TMNO ratios, 1 : n, where n is smaller or greater than four, unchanged W(CO)6 on TMNO, respectively, were observed from the thermal profiles. The liberation of CO2 was quantified during separate experiments. The amount of gas released is proportional to the concentration of TMNO present. When the latter is present in a 15-fold excess, four moles of CO2 are released per mole of the parent hexacarbonyl. © 1989.