The mechanism of "self-spin-probing'' reactions between carbanion of nitroalkanes (1) and omega-hydroperfluorodiacyl peroxides (2) initiated by electron transfer has been verified by EPR detection of new bis(omega-hydroperfluoro-dialkyl) nitroxides (11) and omega-hydroperfluoroalkyl nitroalkyl nitroxides (12) - spin adducts of radical intermediates H(CF2CF2)(n).(n=1,2,3) and (RRC)-R-1-C-2 . NO2 to the nitroso trap H(CFCF)(n)NO (9) generated in the reactions.