Briefly, samples were acquired and kept frozen until analysis using the Denitrifier Method (Sigman et al. 2001; Casciotti et al. 2002) at Princeton University.
The following methods are further described in the Intercalibration Report (PDF) for this dataset (also provided under Supplemental Files).
Sampling and storage procedures followed the GEOTRACES cookbook: (1) seawater samples were collected from Niskin bottles into pre-rinsed square 60 mL high-density polyethylene (HDPE) bottles, (2) Each sample was filled to approximately ¾ the bottle height to prevent sample overflow during ice expansion, (3) Samples were stored immediately in upright position at -20°C. The one difference between the sampling for the PANDORA cruise and the GEOTRACES cookbook is that these samples were not filtered before freezing. As per the GEOTRACES cookbook, filtration is recommended, but prior tests showed no difference between filtered and non-filtered samples for nitrate isotope measurements (at least within 18 months of sampling).
Samples were analyzed by the Denitrifier Method (Casciotti et al., 2002; Sigman et al., 2001), with technical updates described by (Weigand et al., 2016). Specific protocols for these samples are described in (Marconi et al., 2015) and in detail along with extensive analysis of reference solution results in Weigand et al., 2016. All isotope analyses were performed on a MAT253 Thermo IRMS equipped with a custom-sample preparation system, described by Weigand et al. (2016). Nitrite was not removed from these samples, so they should be considered as possibly "Nitrate + Nitrite" measurements.
Raw data were calibrated to nitrate reference materials IAEA-NO3 and UGSS34, dissolved in low-nitrate seawater collected from the mixed layer at BATS. Samples were bracketed in nitrate concentration by the reference nitrate solutions. When nitrate reference solutions indicated a concentration trend in nitrate d18O, a correction was applied based on those results. These and other aspects of the data processing are described in detail by Weigand et al. (2016).
