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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.

Analytical Chemistry
|June 8, 2011
PubMed
Summary

A new cocondensation method synthesizes volatile iron(0) pentakis(trifluorophosphine) [Fe(PF3)5] from small iron samples. This technique enables more precise iron isotope ratio measurements using gas source mass spectrometry compared to traditional methods.

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Area of Science:

  • Analytical Chemistry
  • Inorganic Chemistry
  • Geochemistry

Background:

  • Accurate iron isotope ratio measurements are crucial for various scientific disciplines.
  • Existing methods like thermal ionization mass spectrometry (TIMS) have limitations in precision and sample requirements.
  • A need exists for a more sensitive and precise method for iron isotope analysis.

Purpose of the Study:

  • To describe a down-scaled cocondensation method for producing volatile iron(0) pentakis(trifluorophosphine) [Fe(PF3)5].
  • To enable precise iron isotope ratio measurements using gas source mass spectrometry (GSMS).
  • To demonstrate the application of this method for analyzing real-life samples.

Main Methods:

  • Down-scaling a cocondensation technique.
  • Synthesis of volatile Fe(PF3)5 from small iron samples (starting from 10 mg).
  • Analysis of iron isotope ratios using gas source mass spectrometry.

Main Results:

  • Successful synthesis of sufficient Fe(PF3)5 for isotopic analysis from minimal iron starting material.
  • Achieved higher precision in iron isotope ratio measurements compared to TIMS.
  • Reproducibilities for n(54Fe)/n(56Fe) and n(57Fe)/n(56Fe) were in the (1-3) × 10(-4) range, superior to TIMS's 10(-3) level.

Conclusions:

  • The down-scaled cocondensation method provides a highly precise technique for iron isotope analysis.
  • This method is advantageous for analyzing small or precious samples.
  • Fe(PF3)5 produced via this method is suitable for accurate iron content and isotope ratio determination by GSMS.