On March 15, 1968, at 1411 LMT, a Nike Tomahawk was launched from Wallops Island, Virginia, carrying a quadrupole mass spectrometer for measurements of positive ion composition in the ionosphere. The instrument was enclosed in a vacuum system principally controlled by a titanium getter pump and marks the first attempt to use this technique for rocket experiments. A CW radio propagation experiment plus ground‐based ionosonde results enabled the reduction of the data to absolute values. On upleg, the spectrometer was opened at 98 km and provided well‐resolved spectra in the ram direction up to an apogee of 303 km, slightly above the F2 peak. The sweep range from 13 to 49 amu enabled all major constituents to be determined, and the high sensitivity of the spectrometer allowed many minor constituents, having densities as low as 2‐5/cm³, to be detected. On downleg, measurements were restricted to wake composition, but values obtained at higher altitudes were similar to those seen on upleg. Upon entry into the D region, the vacuum system permitted spectra to be obtained to 68 km. D‐region results between 80 and 68 km show a predominance of 19+ and 37+ ions, possibly due to complex water clusters, marking the first independent observation in agreement with the earlier results of others.