After irradiation, the oil was equilibrated with the Hg-poisoned, filtered seawater (125 ml) in the dark, on a shaker table for 24 hours at 30°C and 100 rpm. To remove the water-insoluble oil, each leachate was filtered through a Milli-Q–rinsed, 0.22-μm Sterivex filter into three separate precombusted glass 40-ml vials (Thermo Fisher Scientific). Samples were acidified with trace metal–grade HCl, and DOC was quantified as CO2 after high-temperature combustion using the Shimadzu 5000A TOC Analyzer (58 ). To test whether DOC was saturated in our experimental system, we determined DOC production as a function of oil-to-water ratio and found that it was not limited by saturation (section S7 and fig. S4). To test whether biodegradation could have contributed to DOC production, we monitored how two well-established indicators of biological oxidation, the heptadecane (n-C17)–to–pristane ratio and the octadecane (n-C18)–to–phytane ratio (59 (link)), changed in the dark throughout the longest exposure period (7.5 days). Stable n-C17/pristane and n-C18/phytane ratios throughout the exposure period indicate that biological activity did not contribute to DOC production in our experimental system (section S8).
Toc 5000a analyzer
Manufactured by Shimadzu
Sourced in Japan
The TOC-5000A analyzer is a laboratory instrument designed to measure the Total Organic Carbon (TOC) content in water samples. It provides accurate and reliable analysis of organic carbon levels in various water types, including industrial, environmental, and research applications.
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Lab products found in correlation
Vario el 3 elemental analyzer, by Elementar (4 mentions)
Fiastar 5000 analyzer, by Foss (3 mentions)
Aa 7000, by Shimadzu (2 mentions)
Fe20 fiveeasy ph, by Mettler Toledo (2 mentions)
Prominence lc 20a, by Shimadzu (1 mentions)
Kjeltec 2300 analyzer unit, by Foss (1 mentions)
Delta ph meter, by Mettler Toledo (1 mentions)
Uv 3700 uv vis spectrometer, by Shimadzu (1 mentions)
Chi 660e, by CH Instruments (1 mentions)
Agilent 5110 icp oes, by Agilent Technologies (1 mentions)
Toc analyzer, by Elementar (1 mentions)
Chnso elemental analyzer, by PerkinElmer (1 mentions)
Finnigan mat253 mass spectrometer, by Thermo Fisher Scientific (1 mentions)
High performance liquid chromatography (hplc), by Waters Corporation (1 mentions)
20 protocols using toc 5000a analyzer
1
Quantifying DOC Release from Irradiated Oil
2
Dissolved Organic Carbon Optical Characterization
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Dissolved organic carbon concentration (DOC) was quantied as CO 2 aer high-temperature combustion using a Shimadzu 5000A TOC analyzer. 20 Absorption spectra were collected using a 1 cm pathlength UV-visible spectrophotometer (Aqualog; Horiba Scientic). Naperian absorption coefficients were calculated by multiplying absorbance (A) by 2.303 and dividing by the pathlength (m) of the quartz cuvette. Specic UV-visible absorbance as 254 nm (SUVA 254 ; L mg C À1 m À1 ) were calculated as previously described. 21 The spectral slope ratio was calculated as the ratio of the slope from 275 to 295 nm to the slope from 350 to 400 nm. 22 Protocols for collecting DOM uorescence excitation-emission matrices are previously described. [23] [24] [25] All bulk measurements (DOC and optical spectroscopy) were conducted prior to PPL solid-phase extraction for FT-ICR MS analysis.
3
Soil Physical and Chemical Analysis
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After sampling for 1 week, the soil was air dried for 5 days and sieved through 2-mm mesh to remove plant residues. Then, soil physical and chemical properties were measured according to previous studies (92 (link), 93 (link)). In general, soil pH was determined using a pH meter (FE20-FiveEasypH, Mettler Toledo, Germany) in soil water suspension (5:1 water-to-soil ratio). Total nitrogen (TN) was determined using a UV spectrophotometer (UV-1800, Suzhou, China). Total potassium (TK) in soil was measured using a flame atomic absorption spectrometer (AA-7000, Shimadzu, Japan). Soil organic carbon (SOC) content was assessed using a TOC-5000A analyzer (Shimadzu, Kyoto, Japan). The content of NH4+, NO3−, TP, and Olsen P in soil was determined by a continuous flow analytical system (Skalar San++, Netherlands). The effects of waterlogging on soil chemical properties are summarized in Table S1 in the supplemental material.
4
Nutrient Analysis of Water Samples
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Samples were filtered through glass fiber filters with 0.4 µm nominal porosity (GF-5, Macherey-Nagel, Düren, Germany). Concentrations of soluble reactive phosphorus (SRP) were determined spectrophotometrically [17 , 18 ]. Concentrations of nitrate and ammonium were measured according to Procházková [19 ] and Kopáčkek and Procházková [20 ]. Dissolved organic carbon (DOC) and dissolved nitrogen (DN) were measured with a TOC 5000 A analyzer (Shimadzu, Kyoto, Japan).
5
Soil Physical and Chemical Analysis
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After sampling for 1 week, the soil was air dried for 5 days and sieved through 2-mm mesh to remove plant residues. Then, soil physical and chemical properties were measured according to previous studies (92 (link), 93 (link)). In general, soil pH was determined using a pH meter (FE20-FiveEasypH, Mettler Toledo, Germany) in soil water suspension (5:1 water-to-soil ratio). Total nitrogen (TN) was determined using a UV spectrophotometer (UV-1800, Suzhou, China). Total potassium (TK) in soil was measured using a flame atomic absorption spectrometer (AA-7000, Shimadzu, Japan). Soil organic carbon (SOC) content was assessed using a TOC-5000A analyzer (Shimadzu, Kyoto, Japan). The content of NH4+, NO3−, TP, and Olsen P in soil was determined by a continuous flow analytical system (Skalar San++, Netherlands). The effects of waterlogging on soil chemical properties are summarized in Table S1 in the supplemental material.
6
Soil Carbon, Nitrogen, and Vegetation Dynamics
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Total soil organic carbon and nitrogen (TOC and TN) at the depths of 0–10 and 10–20 cm were measured by a TOC-5000A analyzer (Shimadzu Corp, Kyoto, Japan) and a Vario EL III Elemental Analyzer (Elementar, Hanau, Germany). The supernatant of soil solution was used for NH4+-N and NO3−-N measurement through a FIAstar 5000 Analyzer (FOSS, Hillerd, Denmark) as previously described (Yang et al. 2013 ).
Aboveground vegetation properties were measured by indices of species number, abundance, diversity, aboveground biomass, and average height based on common protocols (Yang et al. 2013 ). Among these, the species number and abundance were counted during field sampling. Plant biomass was weighed after mowing. The diversity was calculated by the Shannon–Weaver index (Liu et al. 2014 ). To measure the average height and coverage of the vegetation canopy, the 1 × 1 m quadrat was divided into 100 0.1 × 0.1 m small squares, then touched species were measured by 0.1 cm marks along a vertical ruler held behind the pin. The canopy height of shrub in 1 × 1 m quadrat was calculated by the average of all species in the zone.
Aboveground vegetation properties were measured by indices of species number, abundance, diversity, aboveground biomass, and average height based on common protocols (Yang et al. 2013 ). Among these, the species number and abundance were counted during field sampling. Plant biomass was weighed after mowing. The diversity was calculated by the Shannon–Weaver index (Liu et al. 2014 ). To measure the average height and coverage of the vegetation canopy, the 1 × 1 m quadrat was divided into 100 0.1 × 0.1 m small squares, then touched species were measured by 0.1 cm marks along a vertical ruler held behind the pin. The canopy height of shrub in 1 × 1 m quadrat was calculated by the average of all species in the zone.
7
Monitoring Antibiotic Ozonation Efficiency
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To monitor the ozonation efficiency of the selected antibiotics in the model effluent, TOC concentrations (mg L−1) were determined according to DIN EN 1484 [43 ] using Shimadzu TOC 5000A analyzer (Shimadzu, Kyoto, Japan).
8
Soil Nutrient Extraction and Analysis
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Soil samples were collected in August outside the metal frame, but inside the treated plot. A soil corer (3‐cm diameter) was pressed 5 cm down into the soil three times in each plot. The cores were divided into two depths, 0–2 cm and 2–5 cm, and the three subsamples were pooled together as one sample per plot, per depth.
To analyze carbon and nutrients, 5 g of soil was extracted with 25 ml of distilled water for 1 h. The extracts were left to settle for an hour and then filtered using a vacuum pump (KNF Laboport) through Whatman GF/D glass microfiber filters. The filtered extracts were kept frozen until analysis. Total dissolved organic carbon (DOC) was analyzed on a Shimadzu TOC5000A analyzer (Shimadzu). Total dissolved nitrogen (TN), NH4+, and NO32− concentrations were measured with a flow injection analyzer (5000 FIASTAR).
To analyze carbon and nutrients, 5 g of soil was extracted with 25 ml of distilled water for 1 h. The extracts were left to settle for an hour and then filtered using a vacuum pump (KNF Laboport) through Whatman GF/D glass microfiber filters. The filtered extracts were kept frozen until analysis. Total dissolved organic carbon (DOC) was analyzed on a Shimadzu TOC5000A analyzer (Shimadzu). Total dissolved nitrogen (TN), NH4+, and NO32− concentrations were measured with a flow injection analyzer (5000 FIASTAR).
9
Quantification of Benzoic Acid by HPLC
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The concentration of benzoic acid was evaluated by a high performance liquid chromatograph (HPLC, Shimadzu Prominence LC-20A) equipped with a UV detector and a C18 reverse phase column (4.6 × 250 mm, 5 μm). The mobile phase was methanol/ammonium acetate (5/95), flow rate was 1.0 mL min−1, injection volume was 10 μL, and detection wavelength was 230 nm. The solution pH was monitored by a PHC-3C pH meter. The leaching amount of Fe and Ce from Fe3O4@CeO2 catalyst to the solution during oxidation was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES, ICPE-9000, Thermo Electron Corporation, USA). The total organic carbon (TOC) was measured using a Shimadzu TOC-5000A analyzer.
10
Soil Physicochemical Property Analysis
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The soil samples were sieved through a 2-mm mesh to remove roots and then ground and homogenized with a mill (MM400, Retsch, Germany). 15 g of fresh soil was weighed before and after dried at 105 °C for 24 h to calculate the soil water content (SWC). The soils were subjected to Kjeldahl digestion, and the soil total nitrogen (TN) concentration was determined using a semi-autoanalyzer (Kjeltec 2300 Analyzer Unit, Foss Tecator, Sweden). Soil total phosphorus (TP) concentration was measured by persulfate oxidation followed by colorimetric analysis (Schade et al., 2003 (link)). Soil total organic carbon (TOC) was determined with a TOC-5000A analyzer (Shimadzu Corp., Kyoto, Japan). Soil pH was measured using a ratio of soil:water = 1g:2.5 ml with a Delta pH-meter (Mettler-Toledo Instruments, Columbus, OH, USA).
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