| Processing Steps |
- Parameter or Variable: pH (measured); Units: pH scale; Observation Category: laboratory analysis; Sampling Instrument: Ross pH electrode; Sampling and Analyzing Method: Pore water was extracted from sediments using a manual press. Measurements on small pore water volumes carried out using a flow-through cell. Ross electrode (Thermo Fisher, Prod. No. 8103BNUWP) was calibrated with buffers of pH 4, 7, and 10. Water column pH measured while continuously stirring.
- Parameter or Variable: SALINITY (measured); Units: psu; Observation Category: laboratory analysis; Sampling Instrument: handheld refractometer
- Parameter or Variable: NITRITE (measured); Units: micromole/liter; Observation Category: laboratory analysis; Sampling Instrument: Shimadzu UV1601; Sampling and Analyzing Method: Pore water was extracted from sediments using a manual press. Pore water and water column samples were filtered through a pre-rinsed 0.2 micron cellulose filter and frozen until time of analysis. Nitrite was measured colorimetrically using method of Bendschneider and Robinson, 1952; reproduced by Parsons et al. 1984. Absorbance was measured on a Shimadzu UV1601 spectrophotometer.
- Parameter or Variable: nitrate + nitrite content (concentration) (measured); Units: micromole/liter; Observation Category: laboratory analysis; Sampling Instrument: CTD, Antek Instruments 7050 NO detector; Sampling and Analyzing Method: Pore water was extracted from sediments using a manual press. Pore water and water column samples were filtered through a pre-rinsed 0.2 micron cellulose filter and frozen until time of analysis. NOx (nitrite + nitrate) was chemically reduced and measured with a nitric oxide detector according to the method of Garside 1981 using an Antek Instruments 7050 Nitric Oxide Detector with 745 Nitrate/Nitrite Reduction Assembly.
- Parameter or Variable: NITRATE (calculated); Units: micromole/liter; Observation Category: laboratory analysis; Sampling Instrument: CTD; Sampling and Analyzing Method: Calculated by subtracted measured nitrite concentration from measured NOx (nitrite + nitrate) concentration
- Parameter or Variable: AMMONIUM (NH4) (measured); Units: micromole/liter; Observation Category: laboratory analysis; Sampling Instrument: CTD, Shimadzu UV1601; Sampling and Analyzing Method: Pore water was extracted from sediments using a manual press. Water column and pore water samples were filtered through a pre-rinsed 0.2 micron cellulose filter and frozen until time of analysis. Ammonium measured colorimetrically using the phenolhypochlorite method developed by Solorzano, 1969, on a Hach Company DR 2800 spectrophotometer.
- Parameter or Variable: Dissolved Inorganic Nitrogen (DIN) (calculated); Units: micromole/liter; Observation Category: laboratory analysis; Sampling Instrument: CTD; Sampling and Analyzing Method: Calculated by adding measured NOx (nitrite + nitrate) concentration and measured NH4 concentration
- Parameter or Variable: Total Dissolved Nitrogen (TDN) (measured); Units: micromole/liter; Observation Category: laboratory analysis; Sampling Instrument: CTD, Shimadzu TOC-Vcph TNM Total Nitrogen Analyzer; Sampling and Analyzing Method: Pore water was extracted from sediments using a manual press. Water column and pore water samples were filtered through a pre-rinsed 0.2 micron cellulose filter and frozen until time of analysis. Samples analyzed using a Shimadzu Instruments TOC-Vcph Total Organic Carbon Analyzer with ASI-V Autosampler and TNM Total Nitrogen Analyzer, according to method of Watanabe et al. 2007.
- Parameter or Variable: Dissolved Organic Nitrogen (calculated); Units: micromole/liter; Observation Category: laboratory analysis; Sampling Instrument: CTD; Sampling and Analyzing Method: DON concentrations calculated by subtracted the calculated dissolved inorganic nitrogen concentration from the total dissolved nitrogen concentration
- Parameter or Variable: phosphate (measured); Units: micrmole/liter; Observation Category: laboratory analysis; Sampling Instrument: CTD, Shimadzu UV1601; Sampling and Analyzing Method: Pore water was extracted from sediments using a manual press. Water column and pore water samples were filtered through a pre-rinsed 0.2 micron cellulose filter and frozen until time of analysis. Phosphate was measured on a Shimadzu UV1601 spectrophotometer according to the colorimetric method of Strickland and Parsons, 1972.
- Parameter or Variable: Total Dissolved Phosphorus (measured); Units: micromole/liter; Observation Category: laboratory analysis; Sampling Instrument: CTD, Shimadzu UV1601; Sampling and Analyzing Method: Pore water was extracted from sediments using a manual press. Water column and pore water samples were filtered through a 0.2 micron cellulose filter and frozen until time of analysis. TDP concentrations measured on a Shimadzu UV1601 spectrophotometer according to the colorimetric method of of Solorzano and Sharp, 1980.
- Parameter or Variable: Dissolved Organic Phosphorus (calculated); Units: micromole/liter; Observation Category: laboratory analysis; Sampling Instrument: CTD; Sampling and Analyzing Method: Calculated by subtracting the measured phosphate concentrations from the measured total dissolved phosphorus concentrations
- Parameter or Variable: DIN:DIP (calculated); Units: molar ratio (unitless); Observation Category: laboratory analysis; Sampling Instrument: CTD; Sampling and Analyzing Method: Calculated by dividing the calculated DIN concentration by the measured phosphate concentration.
- Parameter or Variable: DON:DOP (calculated); Units: molar ratio (unitless); Observation Category: laboratory analysis; Sampling Instrument: CTD; Sampling and Analyzing Method: Calculated by dividing the calculated dissolved organic nitrogen concentration by the calculated dissolved organic phosphorus ratio.
- Parameter or Variable: DISSOLVED ORGANIC CARBON (measured); Units: micromole/liter; Observation Category: laboratory analysis; Sampling Instrument: Shimadzu TOC-Vcph TOC Analyzer; Sampling and Analyzing Method: Pore water was extracted from sediments using a manual press. Water column and pore water samples were filtered through a pre-rinsed 0.2 micron cellulose filter and frozen until time of analysis. DOC was measured on a Shimadzu Instruments TOC-Vcph Total Organic Carbon Analyzer with ASI-V Autosampler and TNM Total Nitrogen Analyzer according to the method of Sugimura and Suzuki, 1988.
- Parameter or Variable: LATITUDE (measured); Units: decimal degrees; Observation Category: other; Sampling Instrument: shipboard GPS
- Parameter or Variable: LONGITUDE (measured); Units: decimal degrees; Observation Category: other; Sampling Instrument: shipboard GPS
- Parameter or Variable: Sample depth (measured); Units: meters; Observation Category: in situ; Sampling Instrument: CTD
- Parameter or Variable: DEPTH - BOTTOM (measured); Units: meters; Observation Category: in situ; Sampling Instrument: multibeam sonar
- Parameter or Variable: Date (measured); Units: mo/day/year; Observation Category: other; Sampling Instrument: none
- Parameter or Variable: Local time (measured); Units: hh:mm; Observation Category: other; Sampling Instrument: none; Sampling and Analyzing Method: Time of sample collection in Eastern Daylight Time (UTC-4:00)
- Parameter or Variable: redox potential (Eh) (sediments) (measured); Units: mV; Observation Category: laboratory analysis; Sampling Instrument: Eh probe; Sampling and Analyzing Method: Whole sediment Eh was measured during core sectioning.
- Parameter or Variable: minimum section depth (sediments) (measured); Units: centimeters below surface (cmbsf); Observation Category: laboratory analysis; Sampling Instrument: ruler; Sampling and Analyzing Method: The distance between sediment-water interface and the top of the sediment core section.
- Parameter or Variable: maximum section depth (sediments) (measured); Units: centimeters below surface (cmbsf); Observation Category: laboratory analysis; Sampling Instrument: ruler; Sampling and Analyzing Method: The distance between the sediment-water interface and the bottom of the sediment core section.
- Parameter or Variable: section midpoint depth (sediments) (calculated); Units: centimeters below surface (cmbsf); Observation Category: laboratory analysis; Sampling Instrument: ruler; Sampling and Analyzing Method: The distance between the sediment-water interface and the midpoint of the sediment core section, or, the average of the section minimum depth and section maximum depth
- Parameter or Variable: total alkalinity (pore water) (measured); Units: millimoles/liter; Observation Category: laboratory analysis; Sampling Instrument: Shimadzu UV1601 spectrophotometer; Sampling and Analyzing Method: Pore water was extracted using a manual press. Water was filtered through a 0.2 micron pre-rinsed cellulose filter. Alkalinity was determined using the spectrophotometric method described by Sarazin et al., 1999.
- Parameter or Variable: DISSOLVED INORGANIC CARBON (DIC) (pore water) (calculated); Units: millimoles/liter; Observation Category: laboratory analysis; Sampling Instrument: calculated; Sampling and Analyzing Method: DIC concentrations were calculated from the measured alkalinity values as follows: DIC = Alkalinity * (alpha1 + 2*alpha2) where alpha1 = [HCO3] * [DIC] alpha2 = [CO3] * [DIC] alpha1 and alpha2 were determined using K1 and K2 of carbonic acid dissolution pK1 and pK2 were determined from temperature and salinity according to Luecker et al. 2001: pK1 = 3633.86/T – 61.2172 + 9.67770 * ln(T) – 0.011555 * S + 0.0001152 * S2 pK2 = 471.178/T + 25.9290 – 3.1697 * ln(T) – 0.01781 * S + 0.0001122 * S2
- Parameter or Variable: Methane (CH4) (measured); Units: micromole/liter; Observation Category: laboratory analysis; Sampling Instrument: SRI 8610 GC-FID; Sampling and Analyzing Method: Sediment samples (3 cubic centimeters) were collected into a glass serum vial, preserved with N2-purged 2M NaOH (3 milliliters), crimp-sealed with a butyl rubber stopper and stored at room temperature until analysis. Concentrations were determined by headspace analysis using an SRI 8610C gas chromatograph equipped with a flame ionization detector and SRI Hayesep D 6’x1/8” column (Prod. No. 8600-PKDB). Water column gas samples were collected by overflowing a 1 L PETG bottle and closing headspace-free with a silicone septum cap. A modified 1 L glass media bottle was evacuated to a pressure of 0.2 Torr or below. A 0.7 L aliquot of sample from the PETG was pulled into the evacuated bottle. The 0.7 L sample was shaken and sonicated 3x before the pressure was equilibrated by the addition of brine purged with UHP nitrogen. Extracted gases were collected from the top of the modified media bottle using a syringe and stored in 20 mL serum vials filled with brine. Methane concentrations were determined by injecting gas samples from the brine vials onto an SRI 8610 GC-FID and SRI Hayesep D 6’x1/8” column (Prod. No. 8600-PKDB). See Schmitt, 1991 and Lammers, 1994.
- Parameter or Variable: Mean delta 13C of methane (measured); Units: permil; Observation Category: laboratory analysis; Sampling Instrument: Picarro G2201-i CRDS; Sampling and Analyzing Method: Methane isotopic ratios were measured out of the same vials as methane concentrations. 2 mL (sediments) or 5 ml (water column) of headspace from the methane vials (3 cc sediment preserved with 3 mL UHP N2 purged 2 M NaOH for sediments, 20 mL vials of brine for water column) was injected into the Small Sample Introduction Module of the Picarro CRDS.
- Parameter or Variable: Standard deviation delta 13C of methane (measured); Units: permil; Observation Category: laboratory analysis; Sampling Instrument: Picarro G2201-i CRDS; Sampling and Analyzing Method: Standard deviation of several measurements taken over the course of 4 minutes by the Picarro G2201-i CRDS.
- Parameter or Variable: Hydrogen Sulfide (H2S) (pore water) (measured); Units: millimoles/liter; Observation Category: laboratory analysis; Sampling Instrument: Shimadzu UV1601 spectrophotometer; Sampling and Analyzing Method: Pore water was extracted using a manual press. 2 mL unfiltered porewater was collected into a 15 mL centrifuge tube containing 100 uL or 500 uL 20% zinc acetate w/v solution and stored at 5°C until analysis. H2S was determined using the colorimetric method described by Cline, 1969.
- Parameter or Variable: Sulfate (SO4 2-) (pore water) (measured); Units: millimoles/liter; Observation Category: laboratory analysis; Sampling Instrument: Dionex Integrion HPIC; Sampling and Analyzing Method: Pore water was extracted from sediments using a manual press. Water was filtered through a pre-rinsed 0.2 micron cellulose filter. Samples were collected in 7 ml glass vials and preserved with 10 ul HNO3 per ml of sample. Samples were diluted for analysis on a Dionex Integrion HPIC with AS-AP autosampler and AS19 guard and analytical columns; Data Quality Method: Data were corrected for analytical bias and for evaporation using the ratio of measured chloride concentration to expected chloride concentration.
- Parameter or Variable: Iron II (pore water) (measured); Units: micromole/liter; Observation Category: laboratory analysis; Sampling Instrument: Shimadzu UV1601 spectrophotometer; Sampling and Analyzing Method: Pore water was extracted from sediments using a manual press. Pore water was filtered through a pre-rinsed 0.2 micron cellulose filter. Samples were collected in 7 ml glass vials and preserved with 10 ul HNO3 per ml of sample. Iron (II) was measured using the spectrophotometric method described by Stookey, 1970.
- Parameter or Variable: Anarobic Methane Oxidation Rate (sediments) (measured); Units: nanomoles per cubic centimeter per day; Observation Category: laboratory analysis; Sampling Instrument: Beckmann-Coulter LS6500; Sampling and Analyzing Method: Live sediment (3 cc) was transferred into a modified Hungate tube with a Hungate stopper and cap on one end and a modified, movable blue butyl chloride stopper at the other end. Three replicates were sampled per depth, with one kill control sampled per core. Kill controls were killed using 2M NaOH. UHP methane was added to samples expected to have high in situ methane concentrations for a target concentration of 15 mM. Samples were injected with 100 microliters of 14C-methane tracer (1 million dpm). Samples were incubated at in situ pressure and temperature for 1-3 days before termination by addition of 3 mL 2 M NaOH. Samples were later transferred to Erlenmeyer flasks, acidified with 5 mL 30% sulfuric acid, and distilled for 6-8 hours. Evolved carbon dioxide was captured using 3-methoxypropylamine and counted on a Beckman-Coulter 6500 liquid scintillation counter. Rates were calculated using the ratio of counted 14C carbon dioxide to the injected tracer activity and the measured in situ methane concentration. Method described in Bowles et al. 2011 and Joye et al. 2004, adapted from Iversen and Blackburn 1981.
- Parameter or Variable: Experimental anaerobic methane oxidation rate (sediments) (measured); Units: nanomoles per cubic centimeter per day; Observation Category: laboratory analysis; Sampling Instrument: Beckmann-Coulter LS6500; Sampling and Analyzing Method: Method the same as for Anaerobic Methane Oxidation Rate, except that the added methane (15 mM) plus in situ methane concentration was used in the rate calculation.
- Parameter or Variable: Sulfate Reduction Rate (sediments) (measured); Units: nanomoles per cubic centimeter per day; Observation Category: laboratory analysis; Sampling Instrument: Beckmann-Coulter LS6500; Sampling and Analyzing Method: Live sediment (3 cc) was transferred into a modified Hungate tube with a Hungate stopper and cap on one end and a modified, movable blue butyl chloride stopper at the other end. Three replicates were sampled per depth, with one kill control sampled per core. Kill controls were killed using 3 mL 20% zinc acetate. Samples were injected with 100 microliters of 35S sodium sulfate tracer (10 million dpm). Samples were incubated at in situ pressure and temperature for 1-3 days before termination by addition of 3 mL 20% zinc acetate. Samples were later spin down in a centrifuge at 5000 rpm for 2 min twice. The supernatant was subsampled and counted to determine the activity of injected sulfate. Sediments were then distilled in hot hydrochloric acid and reduced chromium chloride (TRIS distillations). Evolved hydrogen sulfide was captured in zinc acetate traps and counted on a Beckman-Coulter 6500 liquid scintillation counter. Rates were calculated using the ratio of captured 35S sulfide to injected sulfate activity, the measured pore water sulfate concentration, and the sediment porosity. Method described in Bowles et al. 2011, and Joye et al. 2004, adapted from Fossing and Jorgensen 1989.
- Parameter or Variable: CORE - POROSITY (measured); Units: percent; Observation Category: laboratory analysis; Sampling Instrument: analytical balance; Sampling and Analyzing Method: Sediment samples were collected into glass scintillation vials, capped and stored at 4°C until analysis. Porosity was determined by drying a sample of known mass at 80°C, weighing, and calculating the moisture content.
- Parameter or Variable: Sediment organic matter - loss on ignition (measured); Units: percent; Observation Category: laboratory analysis; Sampling Instrument: analytical balance; Sampling and Analyzing Method: Sediment samples were collected into glass scintillation vials, capped and stored at 4°C until analysis. SOM was determined by drying a sample at 80°C, weighing, ashing at 500°C, weighing and calculating weight lost on ignition.
- Parameter or Variable: Total Particulate Nitrogen (sediments) (measured); Units: percent; Observation Category: laboratory analysis; Sampling Instrument: ThermoFinnigan FlashEA 1112 series NC Soil Analyzer; Sampling and Analyzing Method: A pressed sediment sample (mud-cake, removed from pore water press after extraction) was dried at 60°C and then homogenized via grinding. TPN was determined by the method described by Gordan, Jr., 1969 as reproduced by Sharp, 1974. Samples were analyzed on a ThermoFinnigan FlashEA 1112 series NC Soil Analyzer.
- Parameter or Variable: CARBON - TOTAL PARTICULATE - SEDIMENT (measured); Units: percent; Observation Category: laboratory analysis; Sampling Instrument: Thermofinnigan FlashEA 1112 series NC Soil Analyzer; Sampling and Analyzing Method: A pressed sediment sample (mud-cake, removed from pore water press after extraction) was dried at 60°C and then homogenized via grinding. TPC was determined by the method described by Gordan, Jr., 1969 as reproduced by Sharp, 1974. Samples were analyzed on a ThermoFinnigan FlashEA 1112 series NC Soil Analyzer.
- Parameter or Variable: PARTICULATE ORGANIC CARBON (sediments) (measured); Units: percent; Observation Category: laboratory analysis; Sampling Instrument: ThermoFinnigan FlashEA 1112 series NC Soil Analyzer; Sampling and Analyzing Method: A pressed sediment sample (mud-cake, removed from pore water press after extraction) was acidified with 1 N HCl, dried at 60°C, and then homogenized via grinding. POC was determined by the method described by Gordan, Jr., 1969 as reproduced by Sharp, 1974. Samples were analyzed on a ThermoFinnigan FlashEA 1112 series NC Soil Analyzer.
- Parameter or Variable: Total particulate phosphate (sediments) (measured); Units: micromole/gram sediment; Observation Category: laboratory analysis; Sampling Instrument: Shimadzu UV1601 spectrophotometer; Sampling and Analyzing Method: A pressed sediment sample (mud-cake, removed from pore water press after extraction) was dried at 80°C, ground, and distributed into 20 mL scintillation vials. The samples were prepared using the method described by Zhou et. al., 2003. TPP and TPP percent were determined using the colormetric method described by Solorzano and Sharp, 1980.
- Parameter or Variable: Aerobic Methane Oxidation (water column) (measured); Units: picomoles/liter/day; Observation Category: laboratory analysis; Sampling Instrument: Beckmann Coulter LS6500; Sampling and Analyzing Method: Four technical replicates were collected from each sampled depth by filling 16.6 mL Hungate tubes headspace-free and sealing with exetainer septa. Tubes were stored at 4 °C until injection. One of the four replicates was killed by displacing 1.6 ml sample with 1.6 ml 37% formalin. All samples, including the killed abiotic control, were injected with ~2000000 dpm tritiated methane tracer. Samples were incubated at near-in situ temperature for 1-4 days. Immediately before incubation termination, a 100 ul subsample was removed from each tube and measured on a liquid scintillation counter to determine total dissolved 3H-methane addition. Incubations were terminated by killing with 1.6 ml 37% formalin and purging with air for 1 hour to remove remaining tracer. A 5 ml aliquot of each killed replicate was measured on a liquid scintillation counter to determine the ratio of tracer turnover. The turnover ratio was multiplied by the measured in situ methane concentration to obtain the MOx rate. Killed controls were subtracted and the replicates averaged to obtain the final rate number. See Rogener, 2018
- Parameter or Variable: Process Date (measured); Units: mo/day/year; Observation Category: other; Sampling Instrument: none; Sampling and Analyzing Method: Date of sediment core processing
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