Fluorine-containing siloxane oligomers were made from bis(aminopropyl)tetramethyldisiloxane and trimethyltris(trifluoropropyl)cyclotrisiloxane. These materials were characterized by IR spectroscopy, size exclusion chromatography, nonaqueous colorimetric end group titration, and H-1-NMR. The end groups of one oligomer were chemically modified for an increased NMR signal for molecular weight determination. The cyclic trimeric siloxane starting material was additionally studied via C-13-, Si-29, and F-19-NMR. Two forms of it were used: a white solid obtained at room temperature, and a colorless liquid isolated at low temperature.