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19 protocols using asap 2460

1

Biochar Characterization: Analytical Approach

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The carbon (C), hydrogen (H), and nitrogen (N) contents of each biochar sample were determined using an Element Analyzer (Elementar Vario EL III, Frankfurt, Germany). The yield data of biochar were calculated based on mass balance. The ash was analyzed according to the approach reported by He et al.16 (link) and its weight percent calculated using the following equation: Ash(%)=WfWi×100 where Wf and Wi represent the final and initial mass of the biochar sample, respectively. The biochar samples’ oxygen (O) content was calculated on the basis of the mass balance assuming that whatever was not ash, C, H, and N had to be O17 (link): O%=100%Ash%C%H%N%
The surface area and pore properties of biochar were analyzed using a surface area and pore size analyzer (Micrometrics ASAP 2460, Norcross, USA). The surface structure and morphology of all biochar samples were observed with a FIELD Scanning Electron Microscope (SEM, Hitachi S-4800, Tokyo, Japan). The pHpzc (pH at point of zero charges) values of biochar samples were measured using a Zeta potential analyzer (Nano Brook Zeta Plus, Suffolk, USA). Fourier-transform infrared (FTIR) spectra (recorded using a Bruker Vertex 80 spectrometer, Karlsruhe, Germany) were collected in the 400–4000 cm−1 wavenumber range to identify the functional groups present on the surface of biochar samples.
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2

Mesoporous Bioactive Glass Nanoparticle Synthesis

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Mesoporous BG NPs used in this study were prepared using a cetyl pyridine bromide (CPB) template method according to the previously published protocol (Sui et al., 2018 (link)). Briefly, 0.23 g NaOH and 1.0 g of polyvinylpyrrolidone (PVP) were dissolved in 120 ml ddH2O. After stirring for 10 min, 1.4 g of CPB (Sigma-Aldrich, St. Louis, United States) was dissolved in the solution and stirred continuously for one hour. Next, tetraethyl orthosilicate (TEOS), calcium nitrate tetrahydrate, and TEP (the molar ratio of Ca: P: Si = 15: 5: 80) were subsequently added and stirred for 24 h. The solution was collected and washed with ddH2O three times and then sealed in Teflon-lined autoclaves at 80°C for 48 h. Finally, the dispersion was dried at 80°C for 12 h and calcined at 550°C for five hours to obtain mesoporous BG NPs.
The structure and morphology of the BG NP sample were characterized by high-resolution transmission electron microscopy (TEM, JEM-2100, JEOL), and the size distribution was calculated by using ImageJ analysis software (Media Cybernetics Inc., United States). The Brunauer–Emmett–Teller (BET) specific surface area and pore size distribution of MBG were determined using a micromeritics porosimeter (ASAP 2460, Micrometrics Instrument).
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3

Comprehensive Material Characterization Protocol

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The X-ray diffraction (XRD) patterns were recorded on X’Pert–PRO, Panalytical, Almelo, The Netherlands, 2012 using Cu Kα radiation.
The N2 sorption isotherms were measured at −196 °C using an ASAP Sorption Surface Area and Pore Size Analyzer (ASAP 2460, Micrometrics, Norcross, GA, USA 2018).
Scanning electron microscopy was performed with an SU8020 Ultra-High Resolution Field Emission Scanning Electron Microscope (Hitachi Ltd., Ibaraki, Japan, 2012). The elemental analysis was conducted using Energy-Dispersive X-ray spectrometers (EDX) with the same instrument. The samples for SEM were sputter-coated with 40 nm of chromium in order to reduce charging.
FT-IR spectra of the catalyst were obtained using a Thermo Finnigan Nicolet 380 FT-IR instrument with an ATR Smart iTX attachment (Thermo Fisher Scientific Inc., Waltham, MA, USA) in the wavenumber range from 490 to 4000 cm−1.
Diffuse reflectance UV-Vis spectra of the catalyst in the wavelength range from 190 to 900 nm were obtained using a Jasco 650 (V-650, Jasco, Tokyo, Japan) spectrometer with a PIV-756 horizontal integrating sphere.
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4

Characterization of Graphitized Nanostructures

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X-ray diffraction (XRD) patterns were recorded on a D/MAX 2200 VPC equipment using Kα radiation as an X-ray source. Raman spectra were used to confirm the graphitized feature by a Renishaw inVia 2000 spectrometer. The morphology and nanostructure of the samples were observed by a scanning electron microscope (SEM; JSM-6330F) and a transmission electron microscope (TEM; JEOL JEM-2010). Nitrogen adsorption-desorption isotherms were measured at 77 K on a Micrometrics ASAP 2460 surface area and porosity analyzer. Brunauer-Emmett-Teller (BET) method was utilized to calculate the BET surface area (SBET). The micropore volume (Vmic), micropore surface area (Smic), mesopore volume (Vmes), mesopore surface area (Smes), and pore size distribution (PSD) curves of the samples were analyzed by t-plot, Barrett-Joyner-Halendar, and density functional theory (DFT), respectively.
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5

Comprehensive Characterization of Sr-Doped Mesoporous Bioactive Glass Nanoparticles

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Sr-MBGNs were characterized using field emission scanning electron microscopy (FE-SEM, Auriga, Carl Zeiss) under an accelerating voltage of 3 kV. X-ray diffraction (XRD) was performed using a D8 ADVANCE X-ray diffractometer (Bruker, USA) in a 2θ range of 10–80° with Cu K radiation. In addition, all samples were dispersed in ethanol and then dropped onto low-background silicon wafers (Bruker AXS, USA). A step size of 0.014° with a dwell time of 1 s per step was applied. To analyze the detailed porous structure of Sr-MBGNs, the particles were dispersed on a Cu net and analyzed with TEM (JEM 2100F, JEOL, Japan). The Brunauer-Emmett-Teller (BET) specific surface area (SSA) and pore size distribution of 0Sr-, 5Sr-, 15Sr-, and 30Sr-MBGNs were determined by using the nitrogen sorption analysis, conducted on a Micromeritics porosimeter (ASAP2460, Micrometrics Instrument, USA).
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6

Surface Area Analysis of Clays

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A Micrometrics ASAP 2460 (Norcross, Georgia, USA) was used for nitrogen gas sorption analysis of clay surface areas [11 (link),51 ]. Prior to the surface area measurement, clays were dried at 200 °C for 12 h under nitrogen. Data were calculated using MicroActive 2.01 analysis (Norcross, Georgia, USA).
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7

Comprehensive Structural and Compositional Analysis

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The X-ray diffraction (XRD) patterns of the powder samples were recorded using a BRUKER D8 ADVANCE diffractometer. X-ray photoelectron spectroscopy (XPS) data was measured using a Thermo ESCALAB 250Xi spectrometer. The specific surface area and porosity of the samples were obtained using a Micrometrics ASAP2460. The morphology of each sample was investigated using field emission scanning electron microscopy (SEM, SU8020), and the element mapping was performed using energy dispersive spectrometer (EDS). Transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM) images were obtained using a FEI Tecnai G2 F30. The Raman spectral profile was obtained using a Renishaw inVia at an excitation wavelength of 532 nm.
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8

Structural Characterization of Conductors

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The crystalline structures of the samples were characterized by X-Ray diffraction (XRD) on a Bruker AXS D8-Focus X-ray diffractometer with Cu-Kα (λ = 1.5405 Å) radiation. Morphologies of the samples were observed by scanning electron microscopy (SEM) with a Hitachi SU3500 scanning electron microscope. Brunauer-Emmett-Teller (BET) method (Micrometrics, ASAP 2460) was used to investigate the surface areas of the 4 kinds of conductors and the pore size distributions were determined by the Barret-Joyner-Halenda (BJH) method20 (link),21 (link).
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9

Characterization of Fe3O4@PB Nanocomposite

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The morphology and size of Fe3O4@PB were observed by scanning electron microscopy (SEM, Hitachi SU-8010, Japan) and high-resolution transmission electron microscopy (TEM, JEOL JEM-2100 F). The presence of PB-modified Fe3O4 was confirmed by powder X-ray diffraction (XRD, Rigaku Smart Lab, Tokyo, Japan). FTIR spectra of samples were recorded by a Bruker Vertex 70 (Germany) in the wavenumber range of 400–4000 cm−1 at a resolution of 4 cm−1 using the KBr pellet method. The specific surface area of Fe3O4@PB was determined by Brunauer-Emmett-Teller (BET, Micrometrics ASAP 2460 instrument, Norcross, GA, USA) method. The magnetic properties were measured by a superconducting quantum interference device (Quantum Design SQUID-VSM, San Diego, CA, USA) in 300 K. The zeta potentials for pH values from 2 to 11 were collected on SOE-070 nanoparticle size and Zeta potentiometer (Delsa Nano C/Z, Beckman Coulter, Brea, CA, USA).
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10

Advanced Characterization of Nanomaterials

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The inductively coupled plasma-optical
emission spectroscopy (ICP-OES) was carried out on an Agilent 720ES.
The Fourier transform infrared spectra of the samples were recorded
on a PerkinElmer Spectrum 100 instrument (wave number 400–4000
cm–1). X-ray diffraction (XRD) patterns of the prepared
materials were recorded on a PANalytical PW3040/60 X-ray diffraction
meter. The N2 adsorption–desorption isotherms at
77 K were measured using a Micrometrics ASAP2460 instrument and calculated
using the multipoint Brunauer–Emmett–Teller (BET) method.
The field emission scanning electron microscopy (FESEM) image was
taken on a JSM-7001F. The high-resolution transmission electron microscopy
(HRTEM) image was obtained using an instrument JEOL JEM-2100F. X-ray
photoelectron spectroscopy (XPS) spectra of the catalyst were recorded
on a Thermo XPS ESCALAB 250Xi spectrometer equipped with a monochromatic
Al Kα (1486.8 eV) X-ray source. Raman spectra were recorded
on a LabRAM HR Evolution using an argon ion laser with an excitation
wavelength of 532 nm.
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