An Environmental Protection Agency (EPA) approved sampling and analysis protocol was developed and executed to verify atmospheric emissions compliance for the new Savannah River Site (SRS) F/H area Effluent Treatment Facility. Sampling equipment was fabricated, installed, and tested at stack monitoring points for filtrable particulate radionuclides, radioactive iodine, and tritium. The only detectable anthropogenic radionuclides released from Effluent Treatment Facility stacks during monitoring were iodine-129 and tritium oxide. This paper only examines the collection and analysis of tritium oxide.