Signal improvement in elemental analyzer/continuous flow isotope ratio mass spectrometry for samples with low sulfur contents using a pre-concentration technique for on-line concentration adjustment

Rapid Communications in Mass Spectrometry : RCM
Florian Fritzsche, Marion Tichomirowa

Abstract

Elemental analyzer/continuous flow isotope ratio mass spectrometry (EA/CF-IRMS) has become a standard procedure for the determination of delta(34)S values. Common procedures are, however, frequently less than satisfactory for organic as well as for mineral samples with very low concentrations of sulfur (<2000 ppm). Here we present a method which employs cold trapping of SO(2) to adjust the gas concentration for subsequent isotope signature determination. Analytical accuracy is comparable with common EA/CF-IRMS analysis without trapping, showing a precision of better than +/-0.4 per thousand in delta(34)S (1 SD). The virtual absence of memory effects was established by analyzing adjacent samples exhibiting a large difference in delta(34)S and by prolonged freezing of the carrier gas, yielding virtually no S concentration peak. The method was tested using less than 15% (6 microg) of the S required for a conventional isotope analysis at comparable signal intensity. Even smaller samples can be analyzed with high precision. This facilitates the on-line delta(34)S determination in small biological and mineral samples, minimizing matrix effects in various materials including sandstone, soil, and plant samples.

References

Jan 28, 2003·Isotopes in Environmental and Health Studies·L HanS Halas
Jan 9, 2004·Isotopes in Environmental and Health Studies·I TeaD Kleiber
May 10, 2005·Rapid Communications in Mass Spectrometry : RCM·Misuk YunStephen W Taylor

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Citations

Jan 31, 2007·Journal of Mass Spectrometry : JMS

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