Major anions ( , , , and Cl−) of the samples were measured with an ion chromatograph (Dionex, USA). Total Fe, Mg, Co, Ni, B, and Cu were determined by atomic absorbance spectrometer (AAnalystTM 200, ParkinElmer, USA). Levels of Na, Ca, and K were quantified by using flame photometer (52A Flame Photometer Perkin–Elmer, USA). Total organic carbon (TOC), total nitrogen (TN), total dissolved solids (TDS), total phosphorus (TP), and NH3 were analyzed using standard methods (APHA, 1998 ).
Ion chromatograph
Manufactured by Thermo Fisher Scientific
Sourced in United States
An ion chromatograph is an analytical instrument used for the separation, identification, and quantification of ionic species in a solution. It operates by passing the sample through an ion exchange column, where different ions are separated based on their affinity to the column material. The separated ions are then detected and measured, providing information about the composition and concentration of the sample.
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Lab products found in correlation
810 icp ms system, by Agilent Technologies (1 mentions)
Gc fid, by Agilent Technologies (1 mentions)
Carbopac pa20 column, by Thermo Fisher Scientific (1 mentions)
Chromeleon software, by Thermo Fisher Scientific (1 mentions)
Ec meter, by Mettler Toledo (1 mentions)
High speed amino acid analyzer, by Hitachi (1 mentions)
Ph meter, by Mettler Toledo (1 mentions)
8 protocols using ion chromatograph
1
Comprehensive Analytical Methods for Environmental Samples
2
Characterization of Water and Sediment
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Major anions (SO42−, NO3−, PO43−, HCO3−, F− and Cl−) and cations (Ca2+, Na+, K+ and NH4+) in the water samples were estimated with an ion chromatograph (Dionex, USA). Total As, Fe and Mn were determined by atomic absorbance spectrometer (AAnalystTM 200, ParkinElmer, USA). Trace element concentration including As was measured with an inductively coupled plasma mass spectrometer (ICP-MS) (Varian 810 ICP-MS System, California). Total organic carbon, nitrogen, phosphorous and sulphur from the samples were assessed by following standard procedures as described APHA-AWWA-WPCF [34 ].
Mineralogy of the sediment sample (orange sand) was characterized by powder X-ray diffraction (XRD) using Panalytical high resolution XRD-I, PW 3040/60 diffractrometer (Almelo, Netherlands) with Cu-Kα1 radiation. Concentration of major and trace elements within the orange sand were determined by X-ray fluorescence spectrometry (PANalytical AXIOS, Almelo, Netherlands).
Mineralogy of the sediment sample (orange sand) was characterized by powder X-ray diffraction (XRD) using Panalytical high resolution XRD-I, PW 3040/60 diffractrometer (Almelo, Netherlands) with Cu-Kα1 radiation. Concentration of major and trace elements within the orange sand were determined by X-ray fluorescence spectrometry (PANalytical AXIOS, Almelo, Netherlands).
3
Sediment Porosity and Porewater Chemistry
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Sediment porosity was measured by mass after drying at 80°C, according to the equation
Here mw represents mass lost after drying, ρw represents the density of pure water, md represents the mass of the dry sediment, S represents salinity in grams per kilogram, and ρds represents the density of dry sediment (assumed to be 2.5 g cm−3). Using an ion chromatograph (Dionex, Sunnyvale, CA), sulfate concentrations in porewater that was separated by centrifugation in 15-ml centrifuge tubes at 5,000 × g for 5 min, filtered at 0.2 μm, and acidified with 10% HCl were measured. Methane was measured using 3-ml sediment subsamples that were collected from a cutoff syringe, entering through the side of a core section, immediately after core extrusion. Subsamples were deposited immediately in 20-ml serum vials containing 1 ml 0.1 M KOH. These were immediately stoppered and shaken to mix sediment with KOH. Methane was later measured by injecting 500 μl bottle headspace into a gas chromatograph-flame ionization detector (GC-FID; Agilent, Santa Clara, CA) using a headspace equilibrium method (62 ).
Here mw represents mass lost after drying, ρw represents the density of pure water, md represents the mass of the dry sediment, S represents salinity in grams per kilogram, and ρds represents the density of dry sediment (assumed to be 2.5 g cm−3). Using an ion chromatograph (Dionex, Sunnyvale, CA), sulfate concentrations in porewater that was separated by centrifugation in 15-ml centrifuge tubes at 5,000 × g for 5 min, filtered at 0.2 μm, and acidified with 10% HCl were measured. Methane was measured using 3-ml sediment subsamples that were collected from a cutoff syringe, entering through the side of a core section, immediately after core extrusion. Subsamples were deposited immediately in 20-ml serum vials containing 1 ml 0.1 M KOH. These were immediately stoppered and shaken to mix sediment with KOH. Methane was later measured by injecting 500 μl bottle headspace into a gas chromatograph-flame ionization detector (GC-FID; Agilent, Santa Clara, CA) using a headspace equilibrium method (62 ).
4
Groundwater Geochemical Analysis
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All collected groundwater was filtered through 0.45 μm PVDF filters before being preserved by addition of concentrated nitric acid. Groundwater samples were analyzed for δ 238 U and dissolved U concentrations on a Nu Plasma HR MC-ICPMS,(26,36) δD on a Los Gatos Research liquid water isotope analyzer, (7) and anion concentrations on a Dionex ion chromatograph(6) (see the Supporting Information for details).
5
Analysis of Monosaccharide Composition by Ion Chromatography
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Monosaccharide components were tested using ion chromatograph (ThermoFisher, America) according to the approach we used previously (Li et al., 2022 (link)). Samples were hydrolyzed thoroughly using trifluoroacetic acid (TFA, 3 mol/L) at 120 °C for 3 h, and then dried by nitrogen blowing. The residue obtained was fully dissolved in 5 mL of pure water through vortexing, and diluted to 20 times the volume of the sample, then centrifuged at 12000 rpm for 5 min. Next, the supernatant was washed out at 30 °C with a Dionex Carbopac TMPA20 column (3.0 mm × 150 mm) at an elution speed of 0.3 mL/min. A volume of 5 µL of the sample was injected, and the eluent was composed of A, H2O; B, 15 mM NaOH; C, 15 mM NaOH and 100 mM NaOAC. The samples were detected using an electrochemical detector. Standard monosaccharide mixture containing fucose; galactose hydrochloride, rhamnose, arabinose, glucosamine hydrochloride galactose; glucose, N-acetyl-d -glucosamine, xylose, mannose, fructose, ribose, galactose acid, guluronic acid, glucuronic acid, and mannuronic acid. The amount of each monosaccharide was calculated based on peak aera of each standard.
6
Monosaccharide Composition Analysis of Fucoidan
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Monosaccharide composition was determined using an ion chromatograph (ThermoFisher, America) according to the method reported by Li et al. [54 (link)], with minor modifications. Specifically, the fucoidan was hydrolyzed completely using trifluoroacetic acid (TFA, 3 mol/L) at 120 °C for 3 h. The hydrolysate was desiccated to remove excess TFA. Then, 5 mL of distilled water was added into the sample and vortexed, and 50 µL of the sample was pipetted into 950 µL of distilled water, then centrifuged at 12000 rpm for 5 min; the supernatant was used for ion chromatographic analysis with a Dionex Carbopac TMPA20 column (3.0 mm × 150 mm) at a flow rate of 0.3 mL/min and a column temperature of 30 °C. The mobile phase was consisted of A, H2O; B, 15 mM NaOH; C, 15 mM NaOH and 100 mM NaAc. A 5 µL sample was injected, and the testing process was monitored through an electrochemical detector.
7
Quantification of Plant Sugars
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Approximately 100 mg of leaf or stem tissues were powdered using liquid nitrogen. Total sugar extraction was performed and quantified through an ion chromatograph (Thermo Fisher, USA), following a previously outlined protocol with minor adaptations (Xu Q, et al., 2018 (link)). The separation column employed was a CarboPac PA 10 column, and the mobile phase comprised a 200 mM NaOH solution, running at a flow rate of 1 mL min-1. For amperometric detection, a gold electrode served as the working electrode, and an Ag/AgCl electrode functioned as the reference electrode. The elution time spanned 40 min. Standard curves were generated using a combination of three sugars (i.e., Glc, Fru, and Suc). The relative concentrations of these distinct sugars were quantified through the peak area normalization method, executed within the Chromeleon software (Thermo Fisher, USA).
8
Chemical Analysis of Fermented Products
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The pH and electrical conductivity (EC) value was measured every week during the whole fermentation period. The pH value was measured with the pH meter (METTLER TOLEDO) and EC value was measured with the EC meter (METTLER TOLEDO). The contents of free amino acids (Aa) in the fermented products were determined by the High Speed Amino Acid Analyzer (Hitachi, Japan) [20 (link)]. The contents of main ions in the fermentation products were determined by the Ion Chromatograph (Thermo Fisher, Germany) [21 (link)]. The content of available N in the fermentation products was determined by Alkaline Hydrolysis Diffusion method [22 (link)]. The content of total phenol was determined by Folin-Ciocalteu colorimetric method [23 (link)] and the content of total acids were determined by Acid-base Titration method.
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