Simplified method for microlitre deuterium measurements in water and urine by gas chromatography–high‐temperature conversion–isotope ratio mass spectrometry
Abstract Deuterium ( 2 H) in water and urine can be measured by off‐line and, more recently, on‐line techniques using isotope ratio mass spectrometry (IRMS). We describe a new simple on‐line pyrolysis method for the analysis of 2 H/ 1 H in water and urine samples by continuous flow IRMS, normally us...
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crwiley:10.1002/rcm.3593 2024-06-02T07:57:39+00:00 Simplified method for microlitre deuterium measurements in water and urine by gas chromatography–high‐temperature conversion–isotope ratio mass spectrometry Gucciardi, Antonina Cogo, Paola E. Traldi, Umberto Eaton, Simon Darch, Tegan Simonato, Manuela Ori, Carlo Carnielli, Virgilio P. 2008 http://dx.doi.org/10.1002/rcm.3593 https://api.wiley.com/onlinelibrary/tdm/v1/articles/10.1002%2Frcm.3593 http://onlinelibrary.wiley.com/wol1/doi/10.1002/rcm.3593/fullpdf en eng Wiley http://onlinelibrary.wiley.com/termsAndConditions#vor Rapid Communications in Mass Spectrometry volume 22, issue 13, page 2097-2103 ISSN 0951-4198 1097-0231 journal-article 2008 crwiley https://doi.org/10.1002/rcm.3593 2024-05-03T10:40:05Z Abstract Deuterium ( 2 H) in water and urine can be measured by off‐line and, more recently, on‐line techniques using isotope ratio mass spectrometry (IRMS). We describe a new simple on‐line pyrolysis method for the analysis of 2 H/ 1 H in water and urine samples by continuous flow IRMS, normally used for 2 H/ 1 H measurements in organic compounds. A deactivated column connected the split injector to a high‐temperature conversion reactor (TC HD), and 0.5 µL of sample was injected. Accuracy and precision were determined with Vienna Standard Mean Ocean Water (VSMOW), Standard Light Antarctic Precipitation (SLAP), and Greenland Ice Sheet Precipitation (GISP). The range of linearity was measured with a calibration curve of enriched water from 0 up to 0.1 atom percent excess (APE) (i.e. −72 up to 6323 delta per mil ( δ D ‰)) with a precision of <5‰ and accuracy ranging between 1 and 55‰. Blinded reanalysis of urine samples by an equilibration device (Gas Bench) and by a dedicated pyrolysis system (TC/EA) was performed and results compared by the Bland‐Altman test. Enrichments ranged between 600 and 2400‰ δD VSMOW with a precision of ±5‰. Urine enrichments described by our method were strongly correlated with values obtained by Gas Bench and TC/EA ( p < 0.0001). There was a significant memory effect that was reduced by injecting the sample 15 times and discarding the first 10 injections, together with accurate furnace conditioning and appropriate cleaning of the syringe. Data indicate that the method is accurate, and that it can be used for water and urine deuterium determination when a Gas Bench or TC/EA instrument is not available and the amount of sample is limited. Copyright © 2008 John Wiley & Sons, Ltd. Article in Journal/Newspaper Antarc* Antarctic GISP Greenland Ice Sheet Wiley Online Library Antarctic Greenland Rapid Communications in Mass Spectrometry 22 13 2097 2103 |
institution |
Open Polar |
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Wiley Online Library |
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crwiley |
language |
English |
description |
Abstract Deuterium ( 2 H) in water and urine can be measured by off‐line and, more recently, on‐line techniques using isotope ratio mass spectrometry (IRMS). We describe a new simple on‐line pyrolysis method for the analysis of 2 H/ 1 H in water and urine samples by continuous flow IRMS, normally used for 2 H/ 1 H measurements in organic compounds. A deactivated column connected the split injector to a high‐temperature conversion reactor (TC HD), and 0.5 µL of sample was injected. Accuracy and precision were determined with Vienna Standard Mean Ocean Water (VSMOW), Standard Light Antarctic Precipitation (SLAP), and Greenland Ice Sheet Precipitation (GISP). The range of linearity was measured with a calibration curve of enriched water from 0 up to 0.1 atom percent excess (APE) (i.e. −72 up to 6323 delta per mil ( δ D ‰)) with a precision of <5‰ and accuracy ranging between 1 and 55‰. Blinded reanalysis of urine samples by an equilibration device (Gas Bench) and by a dedicated pyrolysis system (TC/EA) was performed and results compared by the Bland‐Altman test. Enrichments ranged between 600 and 2400‰ δD VSMOW with a precision of ±5‰. Urine enrichments described by our method were strongly correlated with values obtained by Gas Bench and TC/EA ( p < 0.0001). There was a significant memory effect that was reduced by injecting the sample 15 times and discarding the first 10 injections, together with accurate furnace conditioning and appropriate cleaning of the syringe. Data indicate that the method is accurate, and that it can be used for water and urine deuterium determination when a Gas Bench or TC/EA instrument is not available and the amount of sample is limited. Copyright © 2008 John Wiley & Sons, Ltd. |
format |
Article in Journal/Newspaper |
author |
Gucciardi, Antonina Cogo, Paola E. Traldi, Umberto Eaton, Simon Darch, Tegan Simonato, Manuela Ori, Carlo Carnielli, Virgilio P. |
spellingShingle |
Gucciardi, Antonina Cogo, Paola E. Traldi, Umberto Eaton, Simon Darch, Tegan Simonato, Manuela Ori, Carlo Carnielli, Virgilio P. Simplified method for microlitre deuterium measurements in water and urine by gas chromatography–high‐temperature conversion–isotope ratio mass spectrometry |
author_facet |
Gucciardi, Antonina Cogo, Paola E. Traldi, Umberto Eaton, Simon Darch, Tegan Simonato, Manuela Ori, Carlo Carnielli, Virgilio P. |
author_sort |
Gucciardi, Antonina |
title |
Simplified method for microlitre deuterium measurements in water and urine by gas chromatography–high‐temperature conversion–isotope ratio mass spectrometry |
title_short |
Simplified method for microlitre deuterium measurements in water and urine by gas chromatography–high‐temperature conversion–isotope ratio mass spectrometry |
title_full |
Simplified method for microlitre deuterium measurements in water and urine by gas chromatography–high‐temperature conversion–isotope ratio mass spectrometry |
title_fullStr |
Simplified method for microlitre deuterium measurements in water and urine by gas chromatography–high‐temperature conversion–isotope ratio mass spectrometry |
title_full_unstemmed |
Simplified method for microlitre deuterium measurements in water and urine by gas chromatography–high‐temperature conversion–isotope ratio mass spectrometry |
title_sort |
simplified method for microlitre deuterium measurements in water and urine by gas chromatography–high‐temperature conversion–isotope ratio mass spectrometry |
publisher |
Wiley |
publishDate |
2008 |
url |
http://dx.doi.org/10.1002/rcm.3593 https://api.wiley.com/onlinelibrary/tdm/v1/articles/10.1002%2Frcm.3593 http://onlinelibrary.wiley.com/wol1/doi/10.1002/rcm.3593/fullpdf |
geographic |
Antarctic Greenland |
geographic_facet |
Antarctic Greenland |
genre |
Antarc* Antarctic GISP Greenland Ice Sheet |
genre_facet |
Antarc* Antarctic GISP Greenland Ice Sheet |
op_source |
Rapid Communications in Mass Spectrometry volume 22, issue 13, page 2097-2103 ISSN 0951-4198 1097-0231 |
op_rights |
http://onlinelibrary.wiley.com/termsAndConditions#vor |
op_doi |
https://doi.org/10.1002/rcm.3593 |
container_title |
Rapid Communications in Mass Spectrometry |
container_volume |
22 |
container_issue |
13 |
container_start_page |
2097 |
op_container_end_page |
2103 |
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1800740837263409152 |