This paper describes development work to prepare a method to measure absolute239Pu content and Pu-isotopics by ICP-MS in acidified Hanford DOE-site samples which are very high in90Sr,99Tc, and137Cs radioactivity and which are frequently high in organic carbon content. Samples with very large90Sr and137Cs contents have historically been difficult to analyze for Pu content by each of three alpha-counting techniques in use at
SRS, and analysis by ICP-MS in these samples is complicated by the high organics content. We report an ion exchange chemical
preparation to obtain fraction of Pu that does not contain any fission product contribution and no interfering organics to
allow measure of absolute239Pu and of239Pu through241Pu isotopics by ICP-MS. The method uses a242Pu spike to measure Pu recovery and is demonstrated in this paper with three distinct commercially available resins and with
over 300 samples. Measured absolute239Pu contents in sixty-three spiked/unspiked duplicates have agreed within 15% precision. Overall242Pu recoveries were near 90% with 25% precision. Comparisons of absolute239Pu contents measured directly on three samples agreed within the quoted 25% uncertainty.