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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
Author(s) -
Fritzsche Florian,
Tichomirowa Marion
Publication year - 2006
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.2488
Subject(s) - chemistry , isotope , analytical chemistry (journal) , mass spectrometry , sulfur , spectrum analyzer , isotope analysis , isotope ratio mass spectrometry , matrix (chemical analysis) , chromatography , ecology , physics , organic chemistry , quantum mechanics , electrical engineering , biology , engineering
Abstract Elemental analyzer/continuous flow isotope ratio mass spectrometry (EA/CF‐IRMS) has become a standard procedure for the determination of δ 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‰ in δ 34 S (1 SD). The virtual absence of memory effects was established by analyzing adjacent samples exhibiting a large difference in δ 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 µg) 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 δ 34 S determination in small biological and mineral samples, minimizing matrix effects in various materials including sandstone, soil, and plant samples. Copyright © 2006 John Wiley & Sons, Ltd.