Determination of Impurities in Isotopically Enriched Tetrakis(Trifluorophosphine) Nickel (58Ni(PF3)4) by Gas Chromatography-Mass Spectrometry (GC-MS)

The impurity composition of isotopically enriched tetrakis(trifluorophosphine) nickel 58Ni(PF3)4 was studied for the first time using the gas chromatography-mass-spectrometry. The possibilities of using GS-GasPro 60 m × 0.32 mm capillary columns with silica gel as a sorbent and DB-5MS 30 m × 0.32 mm × 0.25 μm with methylsiloxane for the separation of impurities were studied. Impurities were identified by comparing their mass spectra with those known from the literature. Impurities of permanent gases, a number of hydrocarbons from C1 to C9, dichloromethane, 1-propene-1-(2-furanyl) and an alkyl derivative of tetrakis(trifluorophosphine)nickel were detected, and their concentrations were determined. Detection limits for impurities at the level of 9 × 10–5–4 × 10–6 vol % were achieved. For the first time, the mass spectrum of Ni(PF3)3(PF2CH3), which is absent from literary sources, was obtained and described.