double manifold apparatus fitted with refrigerant lines to circulate refrigerant through the cold plate and the exit port is connected to a gc ms instrument as well as any additional ports as needed upon adequate chilling of the solid reaction mixture within the reaction vessel placed upon the cold plate the discharge is energized to initiate the diamond unit cell forming reaction while the effluent is monitored by gc ms in one embodiment this process is conducted under vacuum in another embodiment this process is conducted in an inert gas when no more ejection products are observed spectroscopically energy to the discharge cell is discontinued and the reaction vessel is transferred to a spectrometer for product analysis in one embodiment the reaction vessel containing the solid reaction is placed on a cold plate and chilled to about u2212 20 u00b0 c to about u2212 45 u00b0 c within a microwave discharge cell under an inert atmosphere at higher temperatures the tetrahedroidal compound s have sufficient vapor pressure to alter the precision of the stoichiometry in one embodiment the cell is energized to effect the reaction which is over in about three to five seconds for a one mmol scale reaction in one embodiment the reaction is conducted under vacuum in.