Less than 1 ppb of Ni(CO)4 was detected, under STP [standard temperature and pressure] conditions, in the presence of a 106-fold excess of CO at 2 cm-1 resolution. Absorbance subtraction software was employed to minimize the interfering effects of the CO spectra. Using 20 m absorption length gas cells, Ni(CO)4 concentrations on the order of 0.01 ppb are detectable using this technique.