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  • 1
    In: Hydrology and Earth System Sciences, Copernicus GmbH, Vol. 26, No. 13 ( 2022-07-08), p. 3573-3587
    Abstract: Abstract. Using water-stable isotopes to track plant water uptake or soil water processes has become an invaluable tool in ecohydrology and physiological ecology. Recent studies have shown that laser absorption spectroscopy can measure equilibrated water vapour well enough to support inference of liquid-stable isotope composition of plant or soil water, on-site and in real-time. However, current in situ systems require the presence of an instrument in the field. Here we tested, first in the lab and then in the field, a method for equilibrating, collecting, storing, and finally analysing water vapour for its isotopic composition that does not require an instrument in the field. We developed a vapour storage vial system (VSVS) that relies on in situ sampling into crimp neck vials with a double-coated cap using a pump and a flow metre powered through a small battery and measuring the samples in a laboratory. All components are inexpensive and commercially available. We tested the system's ability to store the isotopic composition of its contents by sampling a range of water vapour of known isotopic compositions (from −95 ‰ to +1700 ‰ for δ2H) and measuring the isotopic composition after different storage periods. Samples for the field trial were taken in a boreal forest in northern Sweden. The isotopic composition was maintained to within 0.6 ‰ to 4.4 ‰ for δ2H and 0.6 ‰ to 0.8 ‰ for δ18O for natural-abundance samples. Although 2H-enriched samples showed greater uncertainty, they were sufficient to quantify label amounts. We detected a small change in the isotopic composition of the sample after a long storage period, but it was correctable by linear regression models. We observed the same trend for the samples obtained in the field trial for δ18O but observed higher variation in δ2H than in the lab trial. Our method combines the best of two worlds, sampling many trees in situ while measuring at high precision in the laboratory. This provides the ecohydrology community with a tool that is not only cost efficient but also easy to use.
    Type of Medium: Online Resource
    ISSN: 1607-7938
    Language: English
    Publisher: Copernicus GmbH
    Publication Date: 2022
    detail.hit.zdb_id: 2100610-6
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  • 2
    Online Resource
    Online Resource
    American Geophysical Union (AGU) ; 2012
    In:  Water Resources Research Vol. 48, No. 3 ( 2012-03)
    In: Water Resources Research, American Geophysical Union (AGU), Vol. 48, No. 3 ( 2012-03)
    Type of Medium: Online Resource
    ISSN: 0043-1397
    Language: English
    Publisher: American Geophysical Union (AGU)
    Publication Date: 2012
    detail.hit.zdb_id: 2029553-4
    detail.hit.zdb_id: 5564-5
    SSG: 13
    SSG: 14
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  • 3
    In: Hydrology and Earth System Sciences, Copernicus GmbH, Vol. 25, No. 9 ( 2021-09-27), p. 5219-5235
    Abstract: Abstract. The direct vapor equilibration laser spectrometry (DVE-LS) method has been developed for obtaining matrix-bound water stable isotope data in soils, the critical zone, and bedrock, deriving therefrom subsurface water flow and transport processes and, ultimately, characterizing, for example, groundwater recharge and vulnerability. Recently, DVE-LS has been increasingly adopted due to its possible high sample throughput, relative simplicity, and cost-efficiency. However, this has come at the cost of a non-unified standard operation protocol (SOP), and several contradictory suggestions regarding protocol details do exist which have not been resolved to date. Particularly, sample container material and equilibration times have not yet been agreed upon. Beside practical constraints, this often limits DVE-LS applicability to interpreting relative isotope dynamics instead of absolute values. It also prevents data comparability among studies or laboratories, and several previous comparisons of DVE-LS with other, more traditional approaches of water extraction and subsequent stable isotope analysis yielded significant discrepancies for various sample matrices and physical states. In a series of empirical tests, we scrutinized the controversial DVE-LS protocol details. Specifically, we tested 10 different easily available and cost-efficient inflatable bags previously employed or potentially suitable for DVE-LS sample collection and equilibration. In storage tests similar to the DVE-LS equilibration process but lasting several weeks, we quickly found heat-sealed bags made of laminated aluminum (Al) sheets to be superior by several orders of magnitude over more frequently used freezer bags in terms of evaporation safety and accompanying adverse isotope effects. For the first time, Al-laminated bags allow the applied equilibration time to be adapted exclusively to sample requirements instead of accepting reduced data quality in a trade-off with material shortcomings. Based on detailed physical considerations, we further describe how to calculate the minimum available container headspace and sample-contained liquid water volume and how their ratio affects analytical precision and accuracy. We are confident that these guidelines will expand DVE-LS applicability and improve data quality and comparability among studies and laboratories by contributing to a more unified, physically well-founded SOP based on more appropriate components.
    Type of Medium: Online Resource
    ISSN: 1607-7938
    Language: English
    Publisher: Copernicus GmbH
    Publication Date: 2021
    detail.hit.zdb_id: 2100610-6
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  • 4
    In: Hydrology and Earth System Sciences, Copernicus GmbH, Vol. 22, No. 7 ( 2018-07-06), p. 3619-3637
    Abstract: 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 δ2H and δ18O 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 intercomparison. 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 δ18O and δ2H 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 ‰ for δ2H and +11.8 to −14.9 ‰ for δ18O 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.
    Type of Medium: Online Resource
    ISSN: 1607-7938
    Language: English
    Publisher: Copernicus GmbH
    Publication Date: 2018
    detail.hit.zdb_id: 2100610-6
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  • 5
    Online Resource
    Online Resource
    Copernicus GmbH ; 2019
    In:  Hydrology and Earth System Sciences Vol. 23, No. 7 ( 2019-07-17), p. 3007-3019
    In: Hydrology and Earth System Sciences, Copernicus GmbH, Vol. 23, No. 7 ( 2019-07-17), p. 3007-3019
    Abstract: Abstract. The water isotopic composition of throughfall is affected by complex diffusive exchange with ambient water vapour, evaporative enrichment of heavy isotopes, and mixing processes in the tree canopy. All interception processes occur simultaneously in space and time, generating a complex pattern of throughfall depth and water isotopic composition. This pattern ultimately cascades through the entire hydrologic system and is therefore crucial for isotope studies in catchment hydrology, where recharge areas are often forested, while reference meteorological stations are generally in the open. For the quasi real-time observation of the water isotopic composition (δ18O and δ2H) of both gross precipitation and throughfall, we developed an approach combining a membrane contactor (Membrana) with a laser-based Cavity Ring-Down Spectrometer (CRDS, Picarro), obtaining isotope readings every 2 s. A setup with two CRDS instruments in parallel analysing gross precipitation and throughfall simultaneously was used for the continuous observation of the temporal effect of interception processes on the stable isotopes of water. All devices were kept small to minimize dead volume with time lags of only 4 min for water from the rainfall collectors to the isotope analysers to increase the temporal resolution of isotope observations. Complementarily, meteorological variables were recorded at high temporal resolution at the same location. The achieved evolution from discrete liquid or event-based bulk samples to continuous measurements allows for direct comparison of water stable isotope data with common meteorological measurements. Future improvements of the spatial representativeness will make our approach an even more powerful tool towards detailed insight into the dynamic processes contributing to interception during rainfall events.
    Type of Medium: Online Resource
    ISSN: 1607-7938
    Language: English
    Publisher: Copernicus GmbH
    Publication Date: 2019
    detail.hit.zdb_id: 2100610-6
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  • 6
    Online Resource
    Online Resource
    American Chemical Society (ACS) ; 2016
    In:  Environmental Science & Technology Vol. 50, No. 13 ( 2016-07-05), p. 7074-7081
    In: Environmental Science & Technology, American Chemical Society (ACS), Vol. 50, No. 13 ( 2016-07-05), p. 7074-7081
    Type of Medium: Online Resource
    ISSN: 0013-936X , 1520-5851
    RVK:
    Language: English
    Publisher: American Chemical Society (ACS)
    Publication Date: 2016
    detail.hit.zdb_id: 280653-8
    detail.hit.zdb_id: 1465132-4
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  • 7
    In: Vadose Zone Journal, Wiley, Vol. 17, No. 1 ( 2018-01), p. 1-10
    Abstract: Observed biases were gas matrix effects exclusively caused by biogenic headspace CO 2 . Observed biases exceeded 30× (δ 2 H) and 65× (δ 18 O) accepted measurement uncertainties. The proposed correction scheme uses data from repeated analyses of soil samples only. Post‐correction quality of isotope data matches accepted measurement uncertainties. The presented method helps to avoid grave misinterpretations of soil water isotope data. The isotopic composition (δ 2 H, δ 18 O) of pore water is an invaluable tracer for the minimally invasive study of subsurface water flow and transport processes. Here, we evaluated a method for pore water isotope analysis that combines laser‐based isotope analyzers and water‐vapor isotope equilibration using evaporation‐proof metalized sample bags. We tested inflation atmospheres (dry air vs. pure N 2 ) and the impact of biogenic gas (CO 2 , CH 4 ) accumulation for storage times of up to 4 wk. Samples were analyzed with a water isotope analyzer (Picarro L2120‐ i ) and a gas chromatograph. Air‐inflated water vapor samples showed a greater range of gas matrix effects (δ 18 O: 9.63‰; δ 2 H: 21.7‰) than N 2 –inflated samples (δ 18 O: 7.49‰; δ 2 H: 10.6‰) induced by nonuniform buildup of biogenic CO 2 , starting immediately after sample preparation. However, only air‐inflated samples could be reliably corrected using instrument‐specific sensitivity factors that were empirically determined by interpretation of periodically repeated isotope measurements. Corrected water isotope data were confirmed by similarity with local precipitation and suction cup isotope data. Residual uncertainties were well below the natural variations of soil water isotope values and independent of storage time, thus allowing for consistently reliable interpretations of soil water isotope profiles. We conclude that, especially for pore water sampling that requires small sample volumes and/or long storage times, metalized sample bags should be used to prevent evaporation notwithstanding the enhanced buildup of biogenic gases. Further, if gas matrix effects cannot be excluded, air inflation is preferred over pure N 2 , as only in that case can reliable postcorrections be performed by using internal data only.
    Type of Medium: Online Resource
    ISSN: 1539-1663 , 1539-1663
    Language: English
    Publisher: Wiley
    Publication Date: 2018
    detail.hit.zdb_id: 2088189-7
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