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...
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Online Access: | http://hdl.handle.net/11390/1100600 https://doi.org/10.1002/rcm.3593 |
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ftunivudineiris:oai:air.uniud.it:11390/1100600 2023-07-30T03:57:48+02:00 Simplified method for microlitre deuterium measurements in water and urine by gas chromatography-high-temperature conversion-isotope ratio mass spectrometry Gucciardi, Antonina Traldi, Umberto Eaton, Simon Darch, Tegan Simonato, Manuela Ori, Carlo Carnielli, Virgilio P. COGO, Paola Gucciardi, Antonina Cogo, Paola Traldi, Umberto Eaton, Simon Darch, Tegan Simonato, Manuela Ori, Carlo Carnielli, Virgilio P. 2008 http://hdl.handle.net/11390/1100600 https://doi.org/10.1002/rcm.3593 eng eng info:eu-repo/semantics/altIdentifier/wos/WOS:000257243800011 volume:22 issue:13 firstpage:2097 lastpage:2103 numberofpages:7 journal:RAPID COMMUNICATIONS IN MASS SPECTROMETRY http://hdl.handle.net/11390/1100600 doi:10.1002/rcm.3593 info:eu-repo/semantics/altIdentifier/scopus/2-s2.0-46849090766 info:eu-repo/semantics/closedAccess Chromatography High Pressure Liquid Deuterium Equipment Design Equipment Failure Analysi Hot Temperature Mass Spectrometry Microchemistry Online System Reproducibility of Result Sensitivity and Specificity Urinalysi Water Analytical Chemistry Spectroscopy info:eu-repo/semantics/article 2008 ftunivudineiris https://doi.org/10.1002/rcm.3593 2023-07-18T20:18:17Z 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 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 (δD ‰)) 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‰ δDVSMOW 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. Article in Journal/Newspaper Antarc* Antarctic GISP Greenland Ice Sheet Università degli Studi di Udine: CINECA IRIS Antarctic Greenland Rapid Communications in Mass Spectrometry 22 13 2097 2103 |
institution |
Open Polar |
collection |
Università degli Studi di Udine: CINECA IRIS |
op_collection_id |
ftunivudineiris |
language |
English |
topic |
Chromatography High Pressure Liquid Deuterium Equipment Design Equipment Failure Analysi Hot Temperature Mass Spectrometry Microchemistry Online System Reproducibility of Result Sensitivity and Specificity Urinalysi Water Analytical Chemistry Spectroscopy |
spellingShingle |
Chromatography High Pressure Liquid Deuterium Equipment Design Equipment Failure Analysi Hot Temperature Mass Spectrometry Microchemistry Online System Reproducibility of Result Sensitivity and Specificity Urinalysi Water Analytical Chemistry Spectroscopy Gucciardi, Antonina Traldi, Umberto Eaton, Simon Darch, Tegan Simonato, Manuela Ori, Carlo Carnielli, Virgilio P. COGO, Paola Simplified method for microlitre deuterium measurements in water and urine by gas chromatography-high-temperature conversion-isotope ratio mass spectrometry |
topic_facet |
Chromatography High Pressure Liquid Deuterium Equipment Design Equipment Failure Analysi Hot Temperature Mass Spectrometry Microchemistry Online System Reproducibility of Result Sensitivity and Specificity Urinalysi Water Analytical Chemistry Spectroscopy |
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 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 (δD ‰)) 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‰ δDVSMOW 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. |
author2 |
Gucciardi, Antonina Cogo, Paola Traldi, Umberto Eaton, Simon Darch, Tegan Simonato, Manuela Ori, Carlo Carnielli, Virgilio P. |
format |
Article in Journal/Newspaper |
author |
Gucciardi, Antonina Traldi, Umberto Eaton, Simon Darch, Tegan Simonato, Manuela Ori, Carlo Carnielli, Virgilio P. COGO, Paola |
author_facet |
Gucciardi, Antonina Traldi, Umberto Eaton, Simon Darch, Tegan Simonato, Manuela Ori, Carlo Carnielli, Virgilio P. COGO, Paola |
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/11390/1100600 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 issue:13 firstpage:2097 lastpage:2103 numberofpages:7 journal:RAPID COMMUNICATIONS IN MASS SPECTROMETRY http://hdl.handle.net/11390/1100600 doi:10.1002/rcm.3593 info:eu-repo/semantics/altIdentifier/scopus/2-s2.0-46849090766 |
op_rights |
info:eu-repo/semantics/closedAccess |
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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1772819406165901312 |