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Isotope fractionation during capillary leaking in an isotope ratio mass spectrometer.

Rationale When isotope composition is measured in dual-inlet mode with an isotope ratio mass spectrometer (IRMS), reference gas may be gradually enriched in heavy isotopes due to preferential loss of light ones from the bellow over time. Quantifying the degree of isotopic enrichment on the reference gas is imperative for high-precision isotopic analysis (i.e., at per meg level).


METHODS
O2 and CO2 leaking experiments were performed with the dual inlet system of an IRMS (Thermo Fisher® MAT 253 plus). During each experiment, the drop of gas pressure in bellow with time was recorded and isotope ratios of residual gas at different time intervals were analyzed.


RESULTS
Isotopic enrichment of residual O2 gas could be as large as 1‰ for δ18 O when a large fraction (>75%) of initial gas was lost. The evolution of isotope compositions of the remaining gas can be well described by a pressure-dependent Rayleigh fractionation equation. When the pressure in bellow is within 10-50 mbar, isotope fractionation factor (α18 O) for O2 leaking ranges from 0.99911 to 0.99982 and the characteristic relationship of α17 O and α18 O is from 0.5123 to 0.5124.


CONCLUSIONS
Isotope fractionation associated with capillary leaking from bellow is pressure-dependent. We recommend that the reference gas should be reloaded frequently, especially after a measurement with a low analyzing pressure for the analysis of small sample amount.