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Space-faring crews must have safe breathing air throughout their missions to ensure adequate performance and good health. Toxicological assessment of air quality depends on the standards that define acceptable air quality, measurements of pollutant levels during the flight, and reports from the crew on their in-flight perceptions of air quality. Air samples returned from ISS on flights 8A, UF2, 9A, and 11A were analyzed for trace pollutants. On average, the air during this period of operations was safe for human respiration. However, about 3 hours into the regeneration of 2 Metox canisters in the U.S. airlock on 20 February 2002 the crew reported an intolerable odor that caused them to stop the regeneration, take refuge in the Russian segment, and scrub air in the U.S. segment for 30 hours. Analytical data from grab samples taken during the incident showed that the pollutants released were characteristic of nominal air pollutants, but were present in much higher concentrations.