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101 protocols using icpe 9000

1

Multielemental Analysis of Environmental Samples

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The surface and groundwater samples were filtered by filter papers (Qualitative, circle, 90 mm Ø, WhatmanTM, New Jersey, US) to obtain a 100-mL solution, to which 1 mL of HNO3 (65%) was added and then heated for 2 h without boiling at 80–90 ℃. The samples were cooled to room temperature and then filtered with 0.2-μm syringe filters [29 ]. The waters were analyzed using a multitype inductively coupled plasma emission spectrometer (ICP-ES) and ICPE-9000 (Shimadzu, Tokyo, Japan).
Five grams of soil were added to 20 mL of HNO3 (7 mol/L), stirred for 1 h, and then placed in an autoclave at 120 °C for 30 min. The mixture was cooled to room temperature, filtered by filter papers, and diluted by deionized water [30 ]. The samples were filtered again by a 0.2-μm syringe filter and transferred to tubes for analyses by ICPE-9000 (Shimadzu, Tokyo, Japan).
The roots, stems, and leaves of the plant samples were dried and ground into powder. An amount of 0.5 g of each sample was added to 6 mL of concentrated HNO3 (65%) and 2 mL of concentrated HCl (30%) and stood until the reaction was completed. The mixture was moved to an autoclave for 66 min at 132 °C for digestion [30 ]. The plant samples were analyzed by ICPE-9000 (Shimadzu, Tokyo, Japan).
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2

Mineral Quantification in Plant Samples

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Total of ten minerals (Na, K, Ca, Mg, Fe, Zn, Cu, Cr, Se, and Mn) were determined in the plant samples using inductively coupled plasma spectrometry (ICP, ICPE-9000; Shimadzu Corporation, Kyoto, Japan) according to standard procedures (Antonious et al., 2011) . Exactly 1 g of sample ash was weighed into a conical flask, and 10 mL concentrated nitric (HNO 3 ) acid was added. The mixture was gently swirled, sealed with aluminium foil and allowed to digest overnight at room temperature. The mixture was heated for 1 h at 160 °C in an oil bath (Ratek; Ratek Pty Ltd, Boronia, Vic., Australia), cooled to room temperature and then diluted with 50 mL Milli-Q water. The mixture was filtered through cellulose filter paper No. 1 (pore size of between 5 and 10 µM). The filtrate was tenfold serially diluted and the minerals detected by spectrometry using Shimadzu plasmic atomic emission spectrometer (ICPE-9000; Shimadzu Corporation). The sample minerals were tested and quantified by use of standard curves generated from a set of serially diluted reference standards of Ca, Mg, Na, K, Fe, Cu, Zn, Mn, Cr and Se (r-value = 0.999).
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3

Nutrient Content Analysis of Transplanted Crops

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On weeks 3, 6, 10, 16, 25, and 33 after transplanting, stems, leaves and fruits were sampled, washed with distilled water, and then dried in a ventilated oven at 75°C to constant weight. Nutrient contents in leaves and fruits samples were analyzed. The contents of K, Ca, Mg, and P were assayed after digestion with H2SO4-HNO3-HClO4 (H2SO4:HNO3:HClO4 = 1 ml:5 ml:1 ml) by inductively coupled plasma spectrometry (ICPE-9000, Shimazu, Japan; ICP-MS 7900, Agilent Technologies, United States). The N content was assayed after digestion with H2SO4-H2O2 by continuous flowing analyzer (AA3, Seal, Germany). The S content was assayed after digestion with HNO3 by inductively coupled plasma spectrometry (ICP-MS 7900, Agilent Technologies, United States) (Zhou et al., 2000 ).
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4

Comprehensive Structural Characterization

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Synchrotron XRD was measured at the BL02B2 beamline, SPring-8, Japan. The Rietveld refinement was performed using Pearson VII function35 (link),36 (link) with TOPAS3 software developed by Bruker AXS GmbH. The atomic percentages were determined by XRF (ZSX Primus IV, Rigaku, Japan). Bright-field TEM images were taken using an HT7700 microscope (Hitachi, Japan) operated at 100 kV. HAADF-STEM images and EDS were recorded on a JEM-ARM200F STEM instrument (JEOL, Japan) with an aberration corrector operated at 200 kV. ICP-MS was conducted on an ICPE-9000 (Shimazu, Japan). Lab XPS was performed on a Shimadzu ESCA-3400 X-ray photoelectron spectrometer (Shimazu, Japan). The HAXPES experiments were performed with a photon energy of 5.95 keV at the National Institute for Materials Science contract undulator beamline BL15XU at SPring-8, Japan. The binding energies were calibrated with respect to the Fermi edge of the Au reference. Both XPS and HAXPES spectra were calibrated by the C 1s peak at 284.5 eV.
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5

Nutrient Monitoring in Hydroponic Systems

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From 4 weeks after transplanting, root-zone solution and drainage were sampled every 2 or 3 weeks. Root-zone solution (100 ml) was collected with a root solution extractor installed between the crops, while drainage (100 ml) was collected from the drainage tank. The samples were stored at 2°C until further analyzing. The EC and pH were measured by using a multi meter (Multi 3420 SET C., WTW, Germany). NO3- was assayed by a continuous flowing analyzer (AA3, Seal, Germany). K+, Ca2+, Mg2+, and H2PO4- were assayed by inductively coupled plasma spectrometry (ICPE-9000, Shimazu, Janpan). SO42- was assayed by inductively coupled plasma spectrometry (ICP-MS 7900, Agilent Technologies, United States).
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6

BPA Boron Uptake and Cell Digestion

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After the incubation of the tumor cells (2.0 × 105) with 1 mM BPA for 30 min, cells were rapidly washed twice with cold (4°C) Hanks’ Balanced Salt Solution without Ca2+ and Mg2+, and digested with perchloric acid (60%) and hydrogen peroxide (30%) for 3 h at 75°C. In the BCH-treated group, cells were pre-treated with 1 mM BCH before BPA administration for 10 min. After the pre-treatment, cells were incubated with medium containing 1 mM BPA and 1 mM BCH. The boron concentration of the cell lysate was assessed via inductively coupled plasma atomic emission spectrometry (ICP-AES) (ICPE-9000, Shimazu, Shimazu, Tokyo, Japan) and was normalized as 10B μg per 107 cells.
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7

Elemental Analysis of Plant and Soil

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The dried plant shoots (leaves, stems and pod walls) and seeds were ground to a powder. Nitrogen content and atom% 15N in the ground samples were determined using the elemental analyzer (FlashEA 1112, Thermo Scientific, Italy) coupled with the isotope ratio mass spectrometer Delta V Advantage (Thermo Scientific, Dreieich, Germany) and the continuous flow interface ConFlo III following manufacturer’s instructions. To determine Al and nutrient (B, Ca, Co, Cu, Fe, K, Mg, Mn, Mo, Ni, S, P and Zn) contents, the ground shoot samples were digested in a mixture of concentrated HNO3 and 38% H2O2 at 70 °C using DigiBlock digester (LabTech, Sorisole, Italy). Rhizosphere soil samples (80 DAP) were incubated in deionized water (5 g soil + 25 mL water) at continuous shaking for 1 h. Soil samples were centrifuged at 10,000 g for 10 min and supernatants tested for pHH2O using pH meter F20 (Mettler-Toledo, Schwerzenbach, Switzerland). Then soil supernatants were acidified with concentrated HNO3 up to 1% to suppress microbial activity. Elemental content of digested plant samples and soil supernatants were determined using an inductively coupled plasma emission spectrometer ICPE-9000 (Shimadzu, Kyoto, Japan) following manufacturer’s instructions.
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8

Characterization of Synthesized Carbon Quantum Dots

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Transmission electron microscopy (TEM) images of the synthesized CQDs were recorded using a JEOL 2010 TEM equipped with a SC1000 ORIUS charge-coupled device operating at 120 kV. Optical extinction spectra were recorded using a Perkin Elmer Lambda 950 UV/Vis/NIR spectrophotometer. Elemental analysis of the CQDs was conducted using a Shimadzu ICPE-9000 inductively coupled plasma-optical emission spectrometer. The crystal structure of the CQDs was examined with a high-resolution X-ray diffractometer (Bede D1 System, Jordan Valley Semiconductors).
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9

Soil Characterization: Moisture, pH, and Elemental Analysis

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Air-dried soils were prepared as described by Bao.24 Moisture was determined using a gravimetric method by drying air-dried soils at 105 °C to a constant weight. The pH was measured in the slurry (with a 1 : 2.5, w/v ratio of soil to deionized water) using a digital pH meter (PB-10 Basic Meter, Sartorius). Water-soluble sulfate was extracted by vibrating the mixture of soil and deionized water with a ratio of 1 : 5 (w/v) at 25 °C, 150 rpm overnight. Besides, acid-soluble sulfate was prepared according to the standard of state environmental protection of HJ635-2012. Subsequently, the samples were centrifuged and then, the supernatant was used for sulfate measurement using an ICS-900 ion chromatographic system (Dionex, Sunnyvale, CA, USA).25 (link) The organic carbon was determined with the potassium dichromate titration method.24 The total iron element was detected using inductively coupled plasma atomic emission spectroscopy (ICPE-9000, Shimadzu), and the soil solution was prepared by the melting method using sodium carbonate as flux.24
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10

Elemental Analysis of Plant Biomass

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Above-ground organs were oven-dried at 60 °C, weighed for dry biomass, and homogenized in agate grinding jars with a mixer mill (MM200, Retsch GmbH, Haan, Germany); 0.5 g of the sample was digested with 1 mL HNO3 within Teflon vessels oven-heated to 160 °C for 4 h. Samples were left to rest overnight [53 ]. Concentrations of Ca, Mg, K, Na, P, Fe, Zn, Cu, and Mn were determined with a multitype ICP emission spectrometer (ICPE-9000, Shimadzu Co., Kyoto, Japan).
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