A significant amount of technetium in Hanford waste exists as unidentified, stable, reduced technetium complexes. In order to facilitate the identification of these non-pertechnetate species we have developed a separation scheme which involves three major steps: (1) pretreatment of the sample with Zn2+, (2) cation-exchange to remove gross activity (90Sr), and (3) size exclusion chromatography to remove residual activity and separate the technetium fractions. Addition of Zn2+ is used to compete for the complexants that bind strontium without perturbing the pH of the sample. Technetium recovery was ~50%. One technetium fraction was obtained free of residual gross activity.