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OAS accession Detail for 0292003
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Title: Flow through sediment core incubations for nitrogen concentration and isotopic fluxes collected in 2013 on the Island of Sylt, Germany in the North Sea (NCEI Accession 0292003)
Abstract: This dataset contains chemical data collectedat Wadden Sea Field Station, Sylt, Germany; Santa Catalina Island, California,USA from 2013-08-14 to 2013-08-22. These data include Ammonium, D17O_NO3, Dissolved Organic Nitrogen, Nitrate, Nitrite, Nitrogen, Nitrous Oxide, Total Dissolved Nitrogen, d15N, d18O_NO3, dN15_NO3, delta17O, and stable oxygen ration 18. The instruments used to collect these data include Chemiluminescence NOx Analyzer, Fluorometer, Mass Spectrometer, and Spectrophotometer. These data were collected by Wiebke Ziebis of University of Southern California and Scott Wankel of Woods Hole Oceanographic Institution as part of the "Collaborative Research: Nitrous Oxide Production and Fluxes in Coastal Sediments: Response to Environmental Change (Coastal_Nitrous_Oxide)" project. The Biological and Chemical Oceanography Data Management Office (BCO-DMO) submitted these data to NCEI on 2022-04-10.

The following is the text of the dataset description provided by BCO-DMO:

Acquisition Description:
Sediments were collected from three intertidal sites near Königshafen on the island of Sylt in the North Sea, Germany. The ‘Schlickwatt (CL)’ and ‘Mischwatt (SLT)’ sites were located inside a small lagoon, while the ‘Sandwatt (SD)’ site was more openly exposed to wind and waves. Thirty intact push cores (30cm length, 10cm OD) were taken using polycarbonate core liners having vertical lines of silicone sealed holes (ø 3mm) at 1-cm intervals to allow porewater collection. Cores were retrieved leaving ~10 cm of overlying water and sealed with double o-ring caps to minimize gas exchange during transport, and brought immediately back to the laboratory. The gas-tight sealed sediment cores were incubated in the dark at in situ temperatures (19˚C) while being continuously supplied with filtered seawater at a flow rate of 1.8 0.06 ml/min for ~8 days. For experimental manipulations, four different inflow seawater compositions were used: “Low nitrate” (air sparged; ~20uM; LN), “Low oxygen, low nitrate” (sparged with N 2 to 30-35% O 2 saturation; ~20uM; LOLN), “High nitrate” (amended with NaNO 3 to ~120uM (above background nitrate); HN) and “low oxygen, high nitrate” (combined treatments; LOHN). Samples of each sediment core effluent were taken twice per day.

Concentrations of NO 3 - + NO 2 - were measured by chemiluminescence after reduction in a hot acidic vanadyl sulfate solution on a NOx analyzer (Braman and Hendrix, 1989). Concentrations of NO 2 - were quantified by using the Griess-Ilosvay method followed by measuring absorption 540nm, and NO 3 - was quantified by difference (Grasshoff et al., 1999). Concentrations of NH 4 + were measured by fluorescence using the OPA method (Holmes et al., 1999). Concentrations of N 2 O were made using the integrated peak area of the m/z 44 beam on the IRMS, standardizing to analyses of known amounts of N 2 O (injected into N 2 sparged seawater in 160ml serum bottles) and normalizing to sample volume (158ml).

All N and O isotopic composition measurements (d15N and d18O (or d17O); where d15N = [( 15 R sample / 15 R Air )-1)*1000 in units of ‰, and 15 R = 15N/14N and where d18O = [( 18 R sample / 18 R VSMOW )-1)*1000 in units of ‰, and 18 R = 18O/16O (or 17O/16O) were made after conversion of analytes to nitrous oxide, followed by purification with a customized purge and trap system similar to that previously described (McIlvin and Casciotti, 2010) and analysis on a continuous flow IsoPrime 100 isotope ratio mass spectrometer (IRMS). D17O refers to the excess 17O beyond that defined by the terrestrial fractionation line for the oxygen isotope system and is defined as D17O = d17O*0.52 - d18O. Nitrate was converted to N 2 O using the denitrifier method (Casciotti et al., 2002; Sigman et al., 2001) after removal of nitrite by addition of sulfamic acid (Granger and Sigman, 2009). Corrections for drift, size and fractionation of O isotopes during bacterial conversion were carried out as previously described using NO 3 - standards USGS 32, USGS 34 and USGS 35 (Casciotti et al., 2002; McIlvin and Casciotti, 2011), with a typical reproducibility of 0.2‰ and 0.4‰ for d15N and d18O, respectively. Nitrate D17O measurements were made on separate aliquots by routing denitrifier-produced N 2 O through a gold tube (1/16” OD) held at 780˚C, thermally decomposing the N 2 O into N 2 and O 2 , which were chromatographically separated using a 2m column (1/16” OD) packed with molecular sieve (5Å) before being sent into the IRMS (Kaiser et al., 2007; Komatsu et al., 2008). Nitrate standards USGS 35 and USGS 34 were used to normalize any scale contraction during conversion, with typical reproducibility of D17O measurements of 0.8‰. All samples for nitrite N and O isotope measurements were converted to N 2 O within 2 hours of collection using the azide method (McIlvin and Altabet, 2005). Internal nitrite isotope standards (WILIS 10, 11 and 20) were run in parallel at 3 different sizes to correct for any variations in sample size and instrumental drift, with a typical reproducibility for both d15N and d18O is 0.2‰. Based on calibrations against isotope standards USGS 32, 34 and 35 for d15N (Böhlke et al., 2003) and N23, N7373, and N10129 for d18O (Casciotti et al., 2007), the values of internal standards WILIS 10, 11, and 20 are reported here as -1.7, +57.1, and -7.8‰ for d15N and +13.2, +8.6 and +47.6‰ for d18O, respectively. Nitrite D17O measurements were made after conversion to N 2 O using the azide method and normalized using a combination of NO 2 - and NO 3 - isotopic standards. D17O values of NO 2 - isotope standards WILIS 10 and WILIS 11 were calibrated previously against USGS 34 and USGS 35 using the denitrifier method followed by thermal decomposition of N 2 O to N 2 and O 2 as described above – yielding D17O values of 0‰ for both. For sample NO 2 - , raw d17O and d18O values were first normalized for oxygen isotopic exchange with water during the azide reaction (McIlvin and Altabet, 2005) using the calibrated d17O and d18O values of WILIS 10 and WILIS 11. During the same IRMS run, N 2 O produced from USGS 34 and USGS 35 via the denitrifier method was also thermally converted and analyzed as N 2 and O 2 . Because any isotope fractionation occurring during these reactions is mass dependent (e.g., D17O is unaffected), the D17O of NO 2 - can be calculated by normalizing to D17O values of these NO 3 - standards. We disregard the small amount of oxygen isotope exchange occurring during the denitrifier method, as this would have only a small impact on the calculated D17O values. Total reduced nitrogen (TRN, e.g., DON + NH 4 + ) was measured in a subset of incubation cores by oxidation of the total dissolved nitrogen (TDN) pool via persulfate digest – followed by d15N analysis using the denitrifier method, similar to that previously described (Knapp et al., 2005). The d15N of the TRN pool was then calculated by mass balance by subtracting the molar contribution of the measured d15N of NO 3 - and NO 2 - pools to the TDN pool. Based on the measurement of NH 4 + concentrations, the DON flux was generally of the same magnitude as the NH 4 + flux (not shown). For dissolved N 2 O, samples were extracted from the 160ml serum bottles using a purge and trap approach similar to that previously described (McIlvin and Casciotti, 2010). Liquid samples were quantitatively transferred from the sample bottle into a purging flask using a 20psi He stream, followed by He-sparging (~45 min) and cryogenic trapping using the same system described above for nitrate and nitrite derived N 2 O. Isotopic composition of the dissolved N 2 O was measured by direct comparison against the N 2 O reference tank. The composition of this tank (d15N bulk = -0.7‰; d18O = +39.1‰; site preference (SP) = -5.3‰, where SP = d15N alpha – d15N beta, and alpha and beta refer to the central and outer N atoms in the linear N 2 O molecule, respectively) was calibrated directly against aliquots of two previously calibrated N 2 O tanks from the Ostrom Lab at Michigan State University, having been calibrated by Tokyo Tech. Several sample analyses of tropospheric N 2 O from the study site using this system yielded isotope values of +6.8 0.7‰ for d15N bulk, +44.1 1.7‰ for d18O and +17.4 2.2‰ for SP. Reported values have been corrected for any size linearity of isotopic ratios (31/30, 45/44 and 46/44) by using a series of reference tank subsamples injected into 20ml headspace vials using a gastight syringe. Precision for replicate analyses of our reference gas analyzed as samples for d15N is 0.3‰, for d18O is 0.4‰ and for SP is 0.8‰. The D17O of N 2 O was calculated similar to that described above for NO 2 - . After extraction and cryotrapping, the N 2 O sample is thermally decomposed to N 2 and O 2 and chromatographically separated before measurement on the IRMS. Regular analyses of N 2 O converted from NO 3 - isotope standards (USGS 35 and USGS 34) via the denitrifier method were made to normalize D17O values.
Date received: 20220410
Start date: 20130814
End date: 20130822
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Observation types: chemical
Instrument types: fluorometer, mass spectrometer, spectrophotometer
Datatypes: AMMONIUM (NH4), DELTA NITROGEN-15, Delta Oxygen-18, Dissolved Organic Nitrogen, NITRATE, NITRITE, NITROGEN, nitrous oxide (N2O), OXYGEN ISOTOPES - OXYGEN-18, Total Dissolved Nitrogen (TDN)
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Submitting institution: Biological and Chemical Oceanography Data Management Office
Collecting institutions: University of Southern California, Woods Hole Oceanographic Institution
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Metadata version: 1
Keydate: 2024-04-29 15:36:39+00
Editdate: 2024-04-29 15:36:56+00