We have developed charged particle activation analysis to determine light elements at a sub-ppb level. This analytical method is characterized by sample bombardment with charged particles at a few tens of mA and substoichiometric separation for13N,11C and18F within two half-life times and with decontamination factors of more than 108. Nuclear reactor interference is also estimated with this method. This analytical method is confirmed to be useful for characterizing highly purified materials from analytical results for boron, carbon, nitrogen and oxygen in Nb refined by the floating zone melting method.