Iodine-129 levels have been published for biological matrices that naturally accumulate iodine such as animal thyroid and kelp. However, published procedures have insufficient sensitivity to determine^^^l in other environmental and biological species. A unique procedure has been developed for the determination of^^^i which couples neutron activation with mass separation. The procedure results in a significant improvement in sensitivity, thus allowing analyses to be performed on a variety of matrices which heretofore had not been investigated. Method development and analytical procedures are presented and analytical results at the lO'^^-lO"^"* gram^^^I level are given.