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Microscale Synthesis of Fe(PF(3))(5) for Gas Source Mass Spectrometry
P D Taylor1, S Lehto, S Valkiers
1Institute for Reference Materials and Measurements, European Commission, JRC, Retieseweg, B-2440 Geel, Belgium, and Institut für Anorganische Chemie, Universität Köln, Greinstrasse 6, D-50939 Universität Köln, Germany.
Abstract:
Down-scaling of a cocondensation method to produce volatile pentakis(trifluorophosphine)iron(0) for measuring isotope ratios by gas source mass spectrometry is described. Starting from 10 mg of iron, this method allows synthesis of a sufficient amount of Fe(PF(3))(5) that can be used to measure iron content and/or isotope ratios in real-life samples. The advantage over thermal ionisation mass spectrometry is that more precise determinations of ratios/amounts are possible. Reproducibilities for n((54)Fe)/n((56)Fe) and n((57)Fe)/n((56)Fe) are (1-3) × 10(-4), while those obtained by thermal ionization mass spectrometry are at the 10(-3) level.
