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Liquid Chromatography / Mass Spectrometry / Mass Spectrometry (LC/MS/MS) is a powerful technique for identifying unknown non-volatile organic compounds dissolved in liquids. One type of LC/MS/MS that is gaining popularity is quadrupole-time-of-flight (QqTOF) mass spectrometry. This technique is now in use at the Johnson Space Center for identification of unknown nonvolatile organics in water samples from the space program. An example of the successful identification of an unknown peak in U.S. Lab Condensate is reviewed in detail in this paper. Each step of the procedure is described in the identification of triethylene glycol mono-n-butyl ether (TGBE) as the unknown analyte. The advantages of time-of-flight instrumentation are demonstrated through this example as well as the strategy employed in using time-of-flight data to identify unknowns. The use of the instrument for quantitative analysis is also demonstrated.