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Inter-laboratory comparison of cryogenic water extraction systems for stable isotope analysis of soil water

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Abstract
For more than two decades, research groups in hydrology, ecology, soil science, and biogeochemistry have performed cryogenic water extractions (CWEs) for the analysis of delta H-2 and delta O-18 of soil water. Recent studies have shown that extraction conditions (time, temperature, and vacuum) along with physicochemical soil properties may affect extracted soil water isotope composition. Here we present results from the first worldwide round robin laboratory inter comparison. We test the null hypothesis that, with identical soils, standards, extraction protocols, and isotope analyses, cryogenic extractions across all laboratories are identical. Two standard soils with different physicochemical characteristics along with deionized (DI) reference water of known isotopic composition were shipped to 16 participating laboratories. Participants oven-dried and rewetted the soils to 8 and 20 % gravimetric water content (WC), using the deionized reference water. One batch of soil samples was extracted via predefined extraction conditions (time, temperature, and vacuum) identical to all laboratories; the second batch was extracted via conditions considered routine in the respective laboratory. All extracted water samples were analyzed for delta O-18 and delta H-2 by the lead laboratory (Global Institute for Water Security, GIWS, Saskatoon, Canada) using both a laser and an isotope ratio mass spectrometer (OA-ICOS and IRMS, respectively). We rejected the null hypothesis. Our results showed large differences in retrieved isotopic signatures among participating laboratories linked to soil type and soil water content with mean differences compared to the reference water ranging from +18.1 to -108.4 parts per thousand for delta H-2 and +11.8 to -14.9 parts per thousand for delta O-18 across all laboratories. In addition, differences were observed between OA-ICOS and IRMS isotope data. These were related to spectral interferences during OA-ICOS analysis that are especially problematic for the clayey loam soils used. While the types of cryogenic extraction lab construction varied from manifold systems to single chambers, no clear trends between system construction, applied extraction conditions, and extraction results were found. Rather, observed differences in the isotope data were influenced by interactions between multiple factors (soil type and properties, soil water content, system setup, extraction efficiency, extraction system leaks, and each lab's internal accuracy). Our results question the usefulness of cryogenic extraction as a standard for water extraction since results are not comparable across laboratories. This suggests that defining any sort of standard extraction procedure applicable across laboratories is challenging. Laboratories might have to establish calibration functions for their specific extraction system for each natural soil type, individually.
Keywords
RATIO MASS-SPECTROMETRY, VACUUM EXTRACTION, PLANT-WATER, INFRARED-SPECTROSCOPY, SAMPLES, FRACTIONATION, DELTA-O-18, DELTA-H-2, OXYGEN, O-18

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MLA
Orlowski, Natalie et al. “Inter-laboratory Comparison of Cryogenic Water Extraction Systems for Stable Isotope Analysis of Soil Water.” HYDROLOGY AND EARTH SYSTEM SCIENCES 22.7 (2018): 3619–3637. Print.
APA
Orlowski, N., Breuer, L., Angeli, N., Boeckx, P., Brumbt, C., Cook, C. S., Dubbert, M., et al. (2018). Inter-laboratory comparison of cryogenic water extraction systems for stable isotope analysis of soil water. HYDROLOGY AND EARTH SYSTEM SCIENCES, 22(7), 3619–3637.
Chicago author-date
Orlowski, Natalie, Lutz Breuer, Nicolas Angeli, Pascal Boeckx, Christophe Brumbt, Craig S Cook, Maren Dubbert, et al. 2018. “Inter-laboratory Comparison of Cryogenic Water Extraction Systems for Stable Isotope Analysis of Soil Water.” Hydrology and Earth System Sciences 22 (7): 3619–3637.
Chicago author-date (all authors)
Orlowski, Natalie, Lutz Breuer, Nicolas Angeli, Pascal Boeckx, Christophe Brumbt, Craig S Cook, Maren Dubbert, Jens Dyckmans, Barbora Gallagher, Benjamin Gralher, Barbara Herbstritt, Pedro Alejandro Hervé Fernández, Christophe Hissler, Paul Koeniger, Arnaud Legout, Chandelle Joan Macdonald, Carlos Oyarzún, Regine Redelstein, Christof Seidler, Rolf Siegwolf, Christine Stumpp, Simon Thomsen, Markus Weiler, Christiane Werner, and Jeffrey J McDonnell. 2018. “Inter-laboratory Comparison of Cryogenic Water Extraction Systems for Stable Isotope Analysis of Soil Water.” Hydrology and Earth System Sciences 22 (7): 3619–3637.
Vancouver
1.
Orlowski N, Breuer L, Angeli N, Boeckx P, Brumbt C, Cook CS, et al. Inter-laboratory comparison of cryogenic water extraction systems for stable isotope analysis of soil water. HYDROLOGY AND EARTH SYSTEM SCIENCES. 2018;22(7):3619–37.
IEEE
[1]
N. Orlowski et al., “Inter-laboratory comparison of cryogenic water extraction systems for stable isotope analysis of soil water,” HYDROLOGY AND EARTH SYSTEM SCIENCES, vol. 22, no. 7, pp. 3619–3637, 2018.
@article{8620780,
  abstract     = {For more than two decades, research groups in hydrology, ecology, soil science, and biogeochemistry have performed cryogenic water extractions (CWEs) for the analysis of delta H-2 and delta O-18 of soil water. Recent studies have shown that extraction conditions (time, temperature, and vacuum) along with physicochemical soil properties may affect extracted soil water isotope composition. Here we present results from the first worldwide round robin laboratory inter comparison. We test the null hypothesis that, with identical soils, standards, extraction protocols, and isotope analyses, cryogenic extractions across all laboratories are identical. Two standard soils with different physicochemical characteristics along with deionized (DI) reference water of known isotopic composition were shipped to 16 participating laboratories. Participants oven-dried and rewetted the soils to 8 and 20 % gravimetric water content (WC), using the deionized reference water. One batch of soil samples was extracted via predefined extraction conditions (time, temperature, and vacuum) identical to all laboratories; the second batch was extracted via conditions considered routine in the respective laboratory. All extracted water samples were analyzed for delta O-18 and delta H-2 by the lead laboratory (Global Institute for Water Security, GIWS, Saskatoon, Canada) using both a laser and an isotope ratio mass spectrometer (OA-ICOS and IRMS, respectively). We rejected the null hypothesis. Our results showed large differences in retrieved isotopic signatures among participating laboratories linked to soil type and soil water content with mean differences compared to the reference water ranging from +18.1 to -108.4 parts per thousand for delta H-2 and +11.8 to -14.9 parts per thousand for delta O-18 across all laboratories. In addition, differences were observed between OA-ICOS and IRMS isotope data. These were related to spectral interferences during OA-ICOS analysis that are especially problematic for the clayey loam soils used. While the types of cryogenic extraction lab construction varied from manifold systems to single chambers, no clear trends between system construction, applied extraction conditions, and extraction results were found. Rather, observed differences in the isotope data were influenced by interactions between multiple factors (soil type and properties, soil water content, system setup, extraction efficiency, extraction system leaks, and each lab's internal accuracy). Our results question the usefulness of cryogenic extraction as a standard for water extraction since results are not comparable across laboratories. This suggests that defining any sort of standard extraction procedure applicable across laboratories is challenging. Laboratories might have to establish calibration functions for their specific extraction system for each natural soil type, individually.},
  author       = {Orlowski, Natalie and Breuer, Lutz and Angeli, Nicolas and Boeckx, Pascal and Brumbt, Christophe and Cook, Craig S and Dubbert, Maren and Dyckmans, Jens and Gallagher, Barbora and Gralher, Benjamin and Herbstritt, Barbara and Hervé Fernández, Pedro Alejandro and Hissler, Christophe and Koeniger, Paul and Legout, Arnaud and Macdonald, Chandelle Joan and Oyarzún, Carlos and Redelstein, Regine and Seidler, Christof and Siegwolf, Rolf and Stumpp, Christine and Thomsen, Simon and Weiler, Markus and Werner, Christiane and McDonnell, Jeffrey J},
  issn         = {1607-7938},
  journal      = {HYDROLOGY AND EARTH SYSTEM SCIENCES},
  keywords     = {RATIO MASS-SPECTROMETRY,VACUUM EXTRACTION,PLANT-WATER,INFRARED-SPECTROSCOPY,SAMPLES,FRACTIONATION,DELTA-O-18,DELTA-H-2,OXYGEN,O-18},
  language     = {eng},
  number       = {7},
  pages        = {3619--3637},
  title        = {Inter-laboratory comparison of cryogenic water extraction systems for stable isotope analysis of soil water},
  url          = {http://dx.doi.org/10.5194/hess-22-3619-2018},
  volume       = {22},
  year         = {2018},
}

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