Abstract
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 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.
| Original language | English |
|---|---|
| Pages (from-to) | 2097-2103 |
| Number of pages | 7 |
| Journal | Rapid Communications in Mass Spectrometry |
| Volume | 22 |
| Issue number | 13 |
| DOIs | |
| Publication status | Published - Jul 2008 |
Fingerprint
ASJC Scopus subject areas
- Analytical Chemistry
- Spectroscopy
Cite this
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.
In: Rapid Communications in Mass Spectrometry, Vol. 22, No. 13, 07.2008, p. 2097-2103.Research output: Contribution to journal › Article
}
TY - JOUR
T1 - Simplified method for microlitre deuterium measurements in water and urine by gas chromatography-high-temperature conversion-isotope ratio mass spectrometry
AU - Gucciardi, Antonina
AU - Cogo, Paola E.
AU - Traldi, Umberto
AU - Eaton, Simon
AU - Darch, Tegan
AU - Simonato, Manuela
AU - Ori, Carlo
AU - Carnielli, Virgilio P.
PY - 2008/7
Y1 - 2008/7
N2 - 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 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.
AB - 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 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.
UR - http://www.scopus.com/inward/record.url?scp=46849090766&partnerID=8YFLogxK
UR - http://www.scopus.com/inward/citedby.url?scp=46849090766&partnerID=8YFLogxK
U2 - 10.1002/rcm.3593
DO - 10.1002/rcm.3593
M3 - Article
C2 - 18512843
AN - SCOPUS:46849090766
VL - 22
SP - 2097
EP - 2103
JO - Rapid Communications in Mass Spectrometry
JF - Rapid Communications in Mass Spectrometry
SN - 0951-4198
IS - 13
ER -