Journal of Physical Chemistry, Vol.100, No.13, 5426-5432, 1996
Small-Angle X-Ray-Scattering and Mass-Spectrometry Studies of Gamma-Irradiated C-60 in Cyclohexane
Intense (1.42 krad/min) gamma-radiolysis of C-60 dissolved in cyclohexane (weak magenta-colored solution) to a total dose of 51 krad resulted in the formation of a new compound (muddy red in color) with a solubility of more than 30 times that of saturated C-60 in toluene. Low-power, laser desorption Fourier transform mass spectrometry (LD-FTMS) of the product yielded two ions at m/z = 1539 and 1556, which correspond to [C-60(cyclohexane)(10)-xH](+) for x = 23 and 6, respectively. Higher power laser desorption conditions as well as collision-induced dissociation experiments of selected ions show the sequential loss of cyclohexene (C6H10) units. Small-angle X-ray scattering (SAXS) of the dissolved material supports the mass spectrometry results of cyclohexane additions to the sphere. Taken together, the mass spectrometry and SAXS data indicate that the identity of the gamma-radiolysis products of C-60 in cyclohexane most likely are cyclohexyl adducts of C-60, primarily Cao(cyclohexane)(10). The SAXS data further indicate that some of the C-60(C6H12)(x) entities aggregate into dimers in solution. A model is proposed in which cyclohexyl and hydrogen atom radiolysis products attach to C-60 across double bonds. These double bonds are possibly those associated with the two top and bottom 5-fold symmetry positions around two opposing pentagons.