Simplified method for microlitre deuterium measurements in water and urine by gas chromatography-high-temperature conversion-isotope ratio mass spectrometry
Deuterium (2H) 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 2H/1H in water and urine samples by continuous flow IRMS, normally used for 2H/1H m...
Published in: | Rapid Communications in Mass Spectrometry |
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Online Access: | http://hdl.handle.net/11577/2445773 https://doi.org/10.1002/rcm.3593 |
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ftunivpadovairis:oai:www.research.unipd.it:11577/2445773 2024-04-14T08:02:20+00:00 Simplified method for microlitre deuterium measurements in water and urine by gas chromatography-high-temperature conversion-isotope ratio mass spectrometry GUCCIARDI, ANTONINA SIMONATO, MANUELA ORI, CARLO P. Cogo U. Traldi S. Eaton T. Darch V. Carnielli Gucciardi, Antonina P., Cogo U., Traldi S., Eaton T., Darch Simonato, Manuela Ori, Carlo V., Carnielli 2008 STAMPA http://hdl.handle.net/11577/2445773 https://doi.org/10.1002/rcm.3593 eng eng info:eu-repo/semantics/altIdentifier/wos/WOS:000257243800011 volume:22 firstpage:2097 lastpage:2103 numberofpages:7 journal:RAPID COMMUNICATIONS IN MASS SPECTROMETRY http://hdl.handle.net/11577/2445773 doi:10.1002/rcm.3593 info:eu-repo/semantics/altIdentifier/scopus/2-s2.0-46849090766 info:eu-repo/semantics/article 2008 ftunivpadovairis https://doi.org/10.1002/rcm.3593 2024-03-21T19:20:52Z Deuterium (2H) 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 2H/1H in water and urine samples by continuous flow IRMS, normally used for 2H/1H measurements in organic compounds. A deactivated column connected the split injector to a high-temperature conversion reactor (TC HD), and 0.5 mL 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. S72 up to 6323 delta per mil (dD %)) 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% dDVSMOW with a precision of W5%. 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. Article in Journal/Newspaper Antarc* Antarctic GISP Greenland Ice Sheet Padua Research Archive (IRIS - Università degli Studi di Padova) Antarctic Greenland Rapid Communications in Mass Spectrometry 22 13 2097 2103 |
institution |
Open Polar |
collection |
Padua Research Archive (IRIS - Università degli Studi di Padova) |
op_collection_id |
ftunivpadovairis |
language |
English |
description |
Deuterium (2H) 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 2H/1H in water and urine samples by continuous flow IRMS, normally used for 2H/1H measurements in organic compounds. A deactivated column connected the split injector to a high-temperature conversion reactor (TC HD), and 0.5 mL 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. S72 up to 6323 delta per mil (dD %)) 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% dDVSMOW with a precision of W5%. 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. |
author2 |
Gucciardi, Antonina P., Cogo U., Traldi S., Eaton T., Darch Simonato, Manuela Ori, Carlo V., Carnielli |
format |
Article in Journal/Newspaper |
author |
GUCCIARDI, ANTONINA SIMONATO, MANUELA ORI, CARLO P. Cogo U. Traldi S. Eaton T. Darch V. Carnielli |
spellingShingle |
GUCCIARDI, ANTONINA SIMONATO, MANUELA ORI, CARLO P. Cogo U. Traldi S. Eaton T. Darch V. Carnielli Simplified method for microlitre deuterium measurements in water and urine by gas chromatography-high-temperature conversion-isotope ratio mass spectrometry |
author_facet |
GUCCIARDI, ANTONINA SIMONATO, MANUELA ORI, CARLO P. Cogo U. Traldi S. Eaton T. Darch V. Carnielli |
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 |
publishDate |
2008 |
url |
http://hdl.handle.net/11577/2445773 https://doi.org/10.1002/rcm.3593 |
geographic |
Antarctic Greenland |
geographic_facet |
Antarctic Greenland |
genre |
Antarc* Antarctic GISP Greenland Ice Sheet |
genre_facet |
Antarc* Antarctic GISP Greenland Ice Sheet |
op_relation |
info:eu-repo/semantics/altIdentifier/wos/WOS:000257243800011 volume:22 firstpage:2097 lastpage:2103 numberofpages:7 journal:RAPID COMMUNICATIONS IN MASS SPECTROMETRY http://hdl.handle.net/11577/2445773 doi:10.1002/rcm.3593 info:eu-repo/semantics/altIdentifier/scopus/2-s2.0-46849090766 |
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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1796314184312422400 |