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40 protocols using axis nova

1

X-ray Photoelectron Spectroscopy Analysis

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UPS spectra (AXIS-NOVA, Kratos. Inc.) were obtained with the samples biased at −15.0 V to clear the secondary cut-off. An energy resolution of 0.05 eV from the slope of the Fermi edge of a cleaned polycrystalline Au surface was utilized. XPS (AXIS-NOVA, Kratos. Inc.) with monochromatic Al-Kα (1486.6 eV) radiation as a photon source with a hemispherical analyzer was employed to investigate the chemical bonding nature of the species in the sample (base pressure = 1 × 10−9 Torr). High-resolution XPS patterns were obtained using an analysis area of 400 μm of the 40 eV pass energy with an energy step of 0.05 eV.
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2

Nanocomposite Characterization Techniques

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The surface morphology of the nanocomposite was analyzed through field emission scanning microscopy (FESEM, S7400, Hitachi, Chiyoda, Tokyo, Japan) operated at an acceleration voltage of 5 kV as well as transmission electron microscopy (TEM-2010, Orius SC10002, JEOL Ltd., Akishima, Tokyo, Japan). The crystalline nature and phase of nanocomposite were investigated by X-ray diffraction (XRD) with Cu Kα, λ Å = 1.540 (Rigaku, Tokyo, Japan). Similarly, Fourier transform infrared (FTIR) spectra were taken by an Bomen MB100 spectrometer (ABB, Zürich, Switzerland), and X-ray photoelectron spectra(XPS) were collected with an A1–Kα irradiation source (Kratos AXIS-NOVA, Shimadzu, Kyoto, Japan). Nitrogen adsorption–desorption was conducted to analyze the specific surface area of the sample through Brunauer-Emmett-Teller (BET) adsorption/desorption isotherm measurements at 77 K (ASAP 2420, Micromeritics, Norcross, GA, USA).
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3

Adsorbent Preparation and Characterization

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Lignin (Lig) was purchased from Tokyo Chemical Industry Co., Ltd. (Tokyo, Japan). Calcined Lig at 200, 400, 600, 800, and 1000 °C was prepared by keeping it in a muffle furnace for 2 h (denoted as Lig200, Lig400, Lig600, Lig800, and Lig1000, respectively). Cadmium chloride was purchased from FUJIFILM Wako Pure Chemical Co. (Osaka, Japan).
The morphologies of each adsorbent were measured by scanning electron microscopy SU1510 (SEM, Hitachi High-Technologies Co., Tokyo, Japan). The specific surface area and pore volumes were analyzed using a specific surface analyzer NOVA4200e (Quantachrome Instruments Japan G.K., Kanagawa, Japan). The surface functional groups were analyzed by the Fourier-transform infrared (FT-IR) spectroscopy system 460Plus (JASCO Co., Tokyo, Japan). The binding energy and elemental distribution of the adsorbent surface were measured by the X-ray photoelectron spectroscopy system AXIS-NOVA (Shimadzu Co., Ltd., Kyoto, Japan) and electron microanalyzer JXA-8530F (JEOL, Tokyo, Japan), respectively.
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4

Comprehensive Physicochemical Analysis of Sterile Filters

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Scanning Electron Microscopy (SEM), X-ray photoelectron spectroscopy (XPS), attenuated total reflection-Fourier-transform infrared (ATR-FTIR) spectroscopy, contact angle analysis using a sessile drop method, and gas–liquid porometry (GLP) were used to analyze the physicochemical properties of the sterile filter surface. Scanning electron microscopy (SEM, SNE-4500 M, SEC, Seoul, Korea) was used to investigate the surface and cross-sectional morphologies of the model sterile filters. An applied voltage of 15 kV and 1000× magnification was adjusted to obtain clear morphologies. For cross-section images, the samples were cut in liquid nitrogen using a sharp knife.
Surface characteristics were further investigated using Fourier-transform infrared spectroscopy (ATR-FTIR, Alpha-P FTIR spectrometer, Bruker, Billerica, MA, USA) and X-ray photoelectron spectroscopy (XPS, Axis Nova, Shimadzu, Japan) for functional group and surface chemical composition analysis. The average pore size and PSD of sterile filters were analyzed using a capillary flow porometer (Porolux 1000, Porometer NV, Nazareth, Belgium) with Porefil (15 mN/m, Alfa Wessemann Inc., West Caldwell, NJ, USA). To analyze the surface hydrophilicity of model filters, the sessile drop method was used to measure the water contact angle on the filter surface. The contact angle was measured after 5 s and 60 s of the water drop.
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5

Characterization of LCO Samples using Advanced Techniques

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X-ray diffraction (XRD) patterns of the LCO samples were recorded on a D2 Phaser X-ray diffractometer (Bruker) using Cu Kα radiation. For recording the XRD patterns of the carbons, liquid paraffin was used to fix the carbon on the sample holder. X-ray photoelectron spectroscopy (XPS) was performed on an AXIS-NOVA (Shimadzu) with a monochromatic Al Kα source at 15 kV and 20 mA. C 1s binding energy (284.8 eV) was used as the reference for charge correction. Field-emission scanning electron microscopy (FE-SEM) was conducted on an S-4800 microscope (Hitachi High-Technologies) at 15 kV. Transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM), and energy-dispersive X-ray (EDX) spectroscopy were performed on a JEM-ARM200F-B equipment (JEOL Ltd., Japan) operated at 200 kV. Nitrogen adsorption/desorption measurements were performed on a Belsorp II (MicrotracBEL) sorption analyzer at 77 K. Before the measurements, carbon and LCO samples were degassed under vacuum at 403 K. The specific surface area of the samples was calculated using the Brunauer–Emmett–Teller equation. Thermogravimetry/differential thermal analysis (TG/DTA) was performed on a TA-60 (Shimadzu) under flowing air (100 mL min−1) using a ramp rate of 10 K min−1.
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6

Cadmium Ion Adsorption by Mesoporous Graphene Sponge

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Several adsorption experiments were performed to determine the impact of operational factors on the removal of cadmium ions using the prepared MGS samples. Initially, samples (0.05 g) were soaked in 50 mL of 10 mg/L cadmium ion solution (pH was 2, 5, and 8) for 24 h to clarify the impact of pH on adsorption. The adsorption temperature was maintained at 25 °C. Second, samples (0.05 g) were soaked with 50 mL of 10 mg/L cadmium ion solution (pH = 5) for 1, 1.5, 2, 3, 4, 5, 6, 16, 20, and 24 h to investigate the effect of contact time on adsorption. Third, adsorption isotherms were obtained. Samples (0.05 g) were soaked in 50 mL of 0.1, 0.5, 1, 5, 10, 20, 30, 40, and 50 mg/L cadmium ion solutions (pH 5) for 24 h. The adsorption temperatures were 5, 25, and 45 °C. Subsequently, the equilibrium concentration of cadmium ions in the sample solutions after the adsorption process, which was filtered, was determined using an iCAP 7600 Duo instrument (ICP-OES, Thermo Fisher Scientific Inc., Japan). The number of adsorbed cadmium ions was measured from the different numbers before and after adsorption. Additionally, the mechanism of calcium ion adsorption by the prepared MGS samples was evaluated using an electron probe microanalyzer JXA-8530 F (JEOL, Japan) and AXIS-NOVA (Shimadzu, Japan).
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7

Comprehensive Materials Characterization Protocol

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1H NMR spectra were measured with a JEOL JNM ECA-500 using tetramethylsilane (TMS) as an internal standard; δ values are given in parts per million (ppm). IR spectra were measured with a SHIMADZU FTIR IRPrestige-21 spectrometer, and the values are provided in cm1. Flame atomic absorption spectrometry was conducted with a Hitachi Z-2310 polarized Zeeman atomic absorption spectrometer (AAS). X-ray photoelectron spectroscopy (XPS) was performed with a Kratos AXIS-NOVA instrument. Scanning electron microscopy (SEM) was performed using a HITACHI S-2500 instrument at an acceleration voltage of 1.5 kV. Energy-dispersive X-ray analysis (EDX/SEM) was conducted using a HITACHI S-3400N/BRUKER Quantax 200 System. Transmission electron microscopy (TEM) was conducted using a HITACHI HT-7700 instrument at an acceleration voltage of 20 kV. Samples for TEM analysis were deposited onto a Cu grid. Atomic force microscopy (AFM) was conducted with a KEYENCE VN-8010 instrument using a silicon substrate in the high amplitude mode (tapping mode) under an ambient condition.
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8

X-ray Photoelectron Spectroscopy of GONs and o-SWNTs

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To confirm the chemical compositions of GONs and o-SWNTs, C1s X-ray photoelectron spectroscopy (XPS) spectra were collected using an X-ray photoelectron spectrometer (AXIS NOVA, Kratos Analytical, Manchester, UK). The samples were prepared by dropping a dispersion of GONs or o-SWNTs onto a silicon wafer (4 WAFER P-100, Sehyoung Wafertech, Seoul, Korea) and then drying repeatedly.
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9

X-ray Photoelectron Spectroscopy of TMDSO Films

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The chemistry of the TMDSO films was analysed by XPS with an AXIS Nova (Kratos Analytical Inc., Manchester, UK) with a monochromated Al Kα X-ray source (λ = 1486.6 eV). The X-ray spot size was a slot with dimensions of 700 μm × 300 μm. The pressure within the analysis chamber during analysis was typically below 10−8 mbar. The photoemission angle of 0° corresponded to a 90° take-off angle respective to the surface. The survey and high-resolution C 1s spectra were collected at pass energies of 160 eV and 20 eV, respectively, and scan times of two minutes with two sweeps each. Three spots were analysed per sample with the electron gun used for charge neutralization. The acquired spectra were analysed using Casa XPS software version 2.3.15 (Casa Software Ltd., Cheshire, UK), with element quantification based on the standard relative sensitivity factors provided by the manufacturer. The spectra were calibrated using the hydrocarbon (C-C) to 285 eV.
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10

XPS Analysis of Ni/Ti Coating

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The XPS analysis before and after use of the file (n = 3/group) and Ni/Ti control was performed using Axis-NOVA (Kratos, UK) with a monochromatic Al Kα X-ray source (1486.6 eV) and an aluminum mode. A pass energy of 20 eV with energy steps of 0.2 eV step−1 was maintained for the photoelectron spectra. The photoelectron take-off angle was 90° between the sample surface and the axis of the analyzer lens with the aperture of spectrometer set at 300 × 700 µm2. Charging effect compensation was done using the magnetic immersion lens of a flood gun, in the XPS instrument. Depth profiling was done using Ar ions at 3000 eV in each 10 s cycles. Data was fit using Smart peak ground parameters in Avantage 5.9 software. Calibration was done by setting the C 1 s signal peak from impurities (284.8 eV.).
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