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Gas chromatography/isotope ratio mass spectrometry of recalcitrant target compounds: performance of different combustion reactors and strategies for standardization

RATIONALE

Compound‐specific isotope analysis (CSIA) relies on continuous flow combustion of organic substances to CO2 and N2 in a miniature reactor to measure 13 C/12 C and 15 N/14 N stable isotope ratios. Accurate analysis is well established for many volatile hydrocarbons. In contrast, compounds which contain hetero and halogen atoms are less volatile and may be more recalcitrant to combustion.

METHODS

This study tested carbon and nitrogen isotope analysis of atrazine, desethylatrazine (DEA), dichlobenil and 2,6‐dichlorobenzamide (BAM) by gas chromatography/isotope ratio mass spectrometry (GC/IRMS) with multiple reactor tubes of two different kinds (conventional CuO/NiO/Pt and a NiO tube/CuO‐NiO reactor prototype).

RESULTS

The advantages of the NiO tube/CuO‐NiO reactor were the absence of an additional reduction reactor, the possibility of routine reoxidation in nitrogen isotope analysis, and reliable atrazine and DEA measurements over several hundred injections. In contrast, BAM analysis showed good accuracy for carbon, but notable variations in the trueness of nitrogen isotope ratios. Accurate carbon and nitrogen analysis was nevertheless possible by bracketing samples with external compound‐specific standards and subsequent offset correction.

CONCLUSIONS

We conclude that instrument data should never be taken at its 'face value', but must consistently be validated with compound‐specific standards of the respective analytes. Copyright © 2012 John Wiley & Sons, Ltd.

Authors:   Reinnicke, Sandra; Juchelka, Dieter; Steinbeiss, Sibylle; Meyer, Armin; Hilkert, Andreas; Elsner, Martin
Journal:   Rapid Communications in Mass Spectrometry
Volume:   26
Issue:   9
Year:   2012
Pages:   1053
DOI:   10.1002/rcm.6199
Publication date:   15-05-2012

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