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8 protocols using asap 2020 volumetric adsorption analyzer

1

Characterization of HP-β-CD/CC and SBA-16 Samples

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SEM images of the prepared HP-β-CD/CC and SBA-16 samples were taken with S-4800 type microscope (Hitachi, Japan) in high-vacuum mode. Transmission electron microscopy (TEM) images of the particles were recorded on a Tecnai G2 microscope (FEI, the Netherlands) operated at an accelerating voltage of 200 kV. The particle size distribution was measured by DLS using a Zetasizer Nano sizer (Malvern, UK). Nitrogen sorption isotherms and pore characterization of the prepared samples were recorded at −196°C using an ASAP 2020 volumetric adsorption analyzer (Micromeritics, USA). The prepared HP-β-CD/CC and SBA-16 samples were degassed at 100°C for 6 hours prior to measurement, while the samples loaded with IRB and pure IRB powder were degassed at 40°C overnight in the degas port to avoid possible thermal degradation. The specific surface area was calculated by the standard Brunauer–Emmett–Teller (BET) model. The pore size distribution was determined according to the Barrett–Joyner–Halenda (BJH) method.
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2

Characterization of Electrode Materials

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Field emission scanning electron microscope (FESEM; JSM 6701F), transmission electron microscope (TEM; JEOL 2100 FEG), powder X-ray diffraction (XRD; Rigaku D/Max-2400, Cu-Kα radiation, λ = 0.15405 nm) and Raman spectroscope (JY-HR800, the excitation wavelength of 532 nm) were employed to investigate the morphology and structure of as-prepared electrode materials. X-ray photoelectron spectroscope (XPS, Physical Electronics, PerkinElmer PHI-5702) and Fourier transform infrared spectrometer (FTIR IFS120HR) were employed to examine the chemical species. Thermogravimetry (TG) measurements were performed by a thermo gravimetric analyser (TGA-STA 449C, from 30 °C to 800 °C in air). The nitrogen adsorption–desorption isotherm measurements were performed on a Micromeritics ASAP 2020 volumetric adsorption analyzer at 77 K. The Brunauer–Emmett–Teller (BET) method was utilized to calculate the specific surface area. The pore-size distribution was determined by a nonlocal density functional method using the adsorption data, and assuming a slit pore model.
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3

Structural and Compositional Characterization of Vanadium Compounds

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XRD measurements were performed using an x-ray diffractometer using Cu Kα radiation (D8 Advance PANalytical X’Pert Pro). The morphology and microstructures of the samples were observed by a field-emission scanning electron microscope (S-4800) and transmission electron microscope (Tecnai G2 F20 S-TWIN). The Raman spectra of the V2O5 NW/MWCNT and VN NW/MWCNT fibers were recorded using a micro-Raman spectroscope (LabRAM HR, with an excitation wavelength of 532 nm). XPS was performed on an ESCALab MKII X-ray photoelectron spectrometer with nonmonochromatized Mg-Ka x-ray as the excitation source. The binding energies in the XPS analysis were corrected by referencing C 1s to 284.6 eV. The nitrogen adsorption/desorption measurements were performed on an ASAP 2020 volumetric adsorption analyzer (Micromeritics, USA) at 77 K.
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4

Characterization of CuFe2O4 Nanoparticles

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N2 adsorption–desorption measurements were conducted using an ASAP 2020 volumetric adsorption analyzer (Micromeritics, Norcross, GA, USA). The specific surface areas were measured using the standard Brunauer-Emmett-Teller (BET) method. The surface morphology of the samples was characterized via a scanning electron microscope (SEM, ZEISS SUPRA 55, Jena, Germany). The composition and chemical oxidation state of the elements were determined by X-ray photoelectron spectroscopy (XPS, ESCALAB 250Xi, ThermoFisher Scientific, Waltham, MA, USA). Fourier-transform infrared spectroscopy (FTIR, VERTEX 70, Bruker, Karlsruhe, Germany) was used for the characterization of CuFe2O4 before and after the reaction. The pH values were measured via a pH meter (Starter-3100, Ohaus, Parsippany-Troy Hills, NJ, USA). The PAA concentration was measured according to the N, N-diethyl-p-phenylenediamine (DPD) colorimetric method [57 (link)]. The Rhodamine B concentration was measured via a UV-Vis spectrophotometer (Agilent, Santa Clara, CA, USA) at 553 nm.
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5

Comprehensive Structural Characterization of Materials

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Scanning electron microscopy (SEM, JSM-6701F, operating at 10 kV) and transmission electron microscopy (TEM, JEOL-2010, operating at 200 kV) were carried out to characterize morphologies and structures of the samples. Powder X-ray diffraction (XRD) measurements were performed on a RIGAK X-ray diffractometer (D/MAX2550 VB/PC, Japan) using a Cu Kα radiation (1.5418 Å) at a voltage of 40 kV. Raman spectra were measured on a Tri VistaTM 555CRS Raman spectrometer at 532 nm of excitation. X-ray photoelectron spectroscopy (XPS) measurements were operated with an ESCLAB 250 spectrometer using X-ray source of Al Kα (1486.6 eV photons). The specific surface area determination and pore size distribution analysis were carried out by the Brunauer-Emmett-Teller (BET) method and density functional theory (DFT) pore model, respectively, using an ASAP2020 volumetric adsorption analyzer (Micromeritics) at 77 K.
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6

Characterization of Bacterial Cellulose Composites

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The surface morphologies of all samples were studied by scanning electron microscopy (SEM). Prior to SEM observation, the samples were coated with spray-gold under high-vacuum conditions. The composition of BC and the BC/EVMT composite were analyzed using a PHI 5000 VersaProbe spectrometer (ULVAC-PHI, Chigasaki, Japan). FTIR spectra were reflected using a Thermo Scientific Nicolet iS5 spectrometer (Spectral range: 500 cm−1 to 4000 cm−1, resolution: 2 cm−1). The thermogravimetric analysis (TGA) was performed on a TA instrument (model no 300, EXSTAR, Fukuoka, Japan) with temperature ranging from 50 °C to 800 °C, a heating rate of 10 °C min−1, and under a nitrogen atmosphere. X-ray diffractometry (XRD) patterns were obtained using a Bruker AXS D8 advanced diffractometer with Cu Kα radiation (λ = 1.5418 Å) at 30 kV and 15 mA, with a scanning rate of 5° min−1 and a 2θ angle ranging from 5° to 70°. XPS analyses were carried out using X-ray photoelectron spectroscopy (ESCALAB 250Xi, Thermo Scientific Escalab, Waltham, MA, USA). The Brunauer–Emmett–Teller (BET) surface area and pore size were obtained by the N2 adsorption–desorption isotherm at 77 k with a Micromeritics ASAP 2020 volumetric adsorption analyzer.
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7

Characterization of Noria-POP-1 Nanomaterials

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All reagents were commercial products of high purity and were not further purified except noria, which was prepared according to a previously reported method.48 (link) Fourier transform infrared (FT-IR) spectra were measured in the 4000–400 cm−1 wavenumber range using a PerkinElmer model 580B IR spectrophotometer with the KBr pellet technique. Thermogravimetric analysis (TGA) was performed on an SDT2960 analyzer (Shimadzu, Japan) up to 750 °C at a heating rate of 10 °C min−1 under N2. UV-Vis spectra were recorded on Agilent 8453. The solid-state 13C cross-polarization/magic angle spinning nuclear magnetic resonance (13C CP/MAS) NMR spectrum was recorded on a Bruker SBAvance III 500 MHz spectrometer. Field-emission scanning electron microscopy (SEM) was performed on a JEOL JSM-7800F microscope under an accelerating scanning voltage of 3.0 kV. Surface area and pore size distribution of Noria-POP-1 were measured using nitrogen adsorption and desorption at 77 K on a Micromeritics ASAP2020 volumetric adsorption analyzer.
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8

Comprehensive Material Characterization Protocol

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The samples were characterized by different analytical techniques. Simultaneous TG/DSC analysis was performed on a NETZSCH STA 449 C Jupiter system. Optical image was captured on a Nikon Microphot-FXA microscope. SEM observations were made on a JEOL JSM-6700F field-emission SEM. TEM images, SAED pattern, EELS, and EDS were obtained on a JEOL JEM-2100F STEM (200 kV, field-emission gun) system equipped with an Oxford INCA x-sight EDS and an ENFINA 1000 EELS. XPS spectra were acquired on a Thermo Scientific Escalab 250Xi spectrometer. XRD measurement was conducted using a Rigaku SmartLab Intelligent X-ray diffraction system with filtered Cu Kα radiation (λ = 1.5406 Å, operating at 45 kV and 200 mA). Raman measurement was taken using a Horiba Jobin Yvon LabRAM HR system with a laser wavelength of 488 nm. The nitrogen adsorption and desorption isotherms were obtained at 77 K with a Micromeritics ASAP 2020 volumetric adsorption analyzer.
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