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Matrix-assisted laser desorption/ionization coupled with time-of-flight mass spectrometry (MALDI/TOF-MS) was used for the analysis of low-molecular phosphate compounds found in Hanford tank wastes. The mass spectra of these compounds indicate protonated peaks as well as sodium adducts. Analytical methods presently utilized for the analysis of the phosphate-related organics are both time consuming and labor intensive. A promising alternative is MALDI/TOFMS. The MALDI process produces both positive and negative ions directly and very little sample is required. In addition, there is limited sample preparation and minimal hazardous waste production.