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12 protocols using belsorp mini

1

Characterization of Polyoxotungstate-Polymer Catalysts

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The FTIR spectra of all the samples were recorded in the range of 4000–500 cm−1 using alpha T-Bruker spectrometer in transmission mode by KBr pellet technique to examine the formation of polyoxotungstate complex and also to confirm the successful anchoring of polyoxotungstate complex on to the mesoporous polymer.31P MAS NMR was recorded in ECX-JEOL 400(S), AVIII400(L) NMR spectrometer. The thermal stability of the polymeric catalyst is determined by thermogravimetric analysis (TGA). TGA analysis was performed using a Discovery TGA by TA Instruments-Waters Lab at a ramp rate of 10 °C min−1 under a flow of nitrogen. The nitrogen sorption measurements were performed using the BELSORP-mini instrument at 77 K temperature. Before the analysis, the samples were degassed at 100 °C for 2 h under a high vacuum. The amount of tungsten loaded on catalysts is estimated by Inductively Coupled Plasma Optical Emission Spectrometer (ICP-OES) by PerkinElmer-Optima 7000V instrument. Contact angle measurement was done by making a pellet of PW11/MP catalysts and placing a drop of 30% H2O2 on the pellet. The contact angle of H2O2 was captured using a digital camera and the image was analyzed.
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2

Biochar Microstructure Analysis

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The microstructure of biochar was observed by scanning electron microscopy (SEM, JSM-5610LV, Electron Optics Laboratory, Tokyo, Japan) after coating with Au for 2 min at 15 mA and 1 mbar. The specific surface areas of the specimens were determined by the Brunauer–Emmett–Teller (BET, BELSORP-mini, Osaka, Japan) method.
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3

Characterization of HPBG Powder by XRD, SAXS, SEM, and TEM

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The XRD spectrum of HPBG powder was obtained by Rigaku Smart Lab 3kW diffractometer, with Cu Kα radiation at 40 kV and 100 mA. Small angle X-ray scattering (SAXS) patterns were taken on Bruker NanoSTAR. The morphology and microstructure were characterized by field emission scanning electron microscope SEM (JEOL, JSM-7800F) with operating voltage at 15 kV, and transmission electron microscope TEM (Philips Tecnai F20) equipped with X-ray energy spectrometer (EDS) with operating voltage at 200 kV. All the samples characterized by TEM were first dispersed in ethanol and then dripped onto the carbon film. The specific surface area and pore volume were measured by nitrogen adsorption analyzer (BELSORP-mini) at 77 K. Samples were degassed at 350 °C under nitrogen flow for at least 4 h prior to testing. The specific surface area and total pore volume of the materials were calculated by the BET (Brunauer–Emmett–Teller) method, and the pore size distribution was calculated by the BJH (Barrett–Joyner–Halenda) method based on the adsorption data.
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4

Detailed Characterization of Materials

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Scanning electron microscopy (SEM) images were taken using a Hitachi SU9000 field emission SEM. XPS measurements were conducted using an ESCA-3400 apparatus (Shimadzu). The binding energies were determined by referencing the C 1s peak (284.5 eV) for each sample. UV-vis diffuse reflectance spectra were obtained using a spectrophotometer (V-670, JASCO). The BET surface area was measured using a gas adsorption apparatus (MICROTRAC MRB, BELSORP-mini) at liquid nitrogen temperature (77 K).
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5

Surface Area Analysis via N2 Adsorption

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Gas adsorption isotherms were collected by a BELSORP-mini with a cryostat system. The Brunauer−Emmett−Teller (BET) surface area was calculated using the N2 adsorption isotherm at 77 K. Each sample was activated at 70 °C under vacuum for 24 h.
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6

Comprehensive Materials Characterization Protocol

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X-ray diffraction
(XRD) patterns were collected on a Unisantis XMD300 powder diffractometer
unit using Cu Kα (λ = 1.5418 Å). FTIR spectra were
recorded using a Bruker α II spectrophotometer in the range
of 400–2000 cm–1. Thermal properties of the
ZHF nanohybrid were determined using an SDT Q600 V20.9 Build 20 instrument
operated under an argon atmosphere at a flow rate of 50 mL/min from
25 to 720 °C at a rate of 5 °C/min. The morphologies and
texture of the carbon materials were characterized using a field emission
scanning electron microscope (FESEM) (MIRA3, TESCAN) and a transmission
electron microscope (FEI Tecnai F20 at 200 kV). Elemental analysis
was also performed by using energy-dispersive X-ray spectroscopy (EDS,
XFlash 6130 detector, Bruker). The surface area and pore size distribution
of the carbon materials were determined using a BELSORP measuring
instrument (BELSORP-mini, Japan, Inc.) using nitrogen gas adsorption–desorption
technique at 77 K. X-ray photoelectron spectroscopic (XPS) measurement
was performed on a Thermo Scientific K-Alpha X-ray photoelectron spectroscope
using Al Kα and spot size 400 μm.
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7

Comprehensive Characterization of Nanoparticles

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Pore size distribution was calculated by the ASAP 2000 analysis program using the method by Barrett, Joyner and Halenda (BJH) [21 (link)]. The surface area was determined by a nitrogen adsorption analyzer (BELSORP-mini, Japan). X-ray diffraction (XRD, STOE, Germany) was used to physiochemically examine the nanoparticles. Nanoparticles were suspended in deionized water at 2, 4, 6, 8, and 10 pH values, and Zetasizer Nano Plus instruments were used for measurements of zeta potential. Cytotoxicity assay was performed by cell proliferation in vitro and H&E staining in vivo.
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8

Comprehensive Characterization of Synthesized Material

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The surface morphology of the synthesized
material was characterized
using a field-emission scanning electron microscope (JEOL JSM-7610-F)
and a high-resolution transmission electron microscope (JEOL JEM-ARM200F).
The powder diffraction pattern of the sample was obtained with the
Bruker (D8 advance) X-ray diffractometer using the Cu X-ray source
(1.5406 Å) with a Ni-filter. The laser Raman spectra of the synthesized
sample were collected using the dispersive Raman spectrometer (SENTERRA,
Bruker) using 532 nm as an excitation wavelength. The specific surface
area of the material was carried out by employing the BELSORP-mini
(MicrotracBEL Corp.), where the material was degassed at 120 °C
for 12 h before the analysis. The impurity present in the exfoliated
material was studied with the Linseis thermogravimetric analyzer (STA
PT1600) under an oxygen atmosphere.
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9

Comprehensive Material Characterization by XRD, TEM, XPS, and Adsorption

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X-ray diffraction (XRD) patterns were recorded on a Rigaku MiniFlex600 powder diffractometer employing monochromatic Cu Kα radiation and operating at 15 mA and 40 kV. Transmission electron microscopy (TEM) images were acquired using a JEM-2010F electron microscope (Jeol). X-ray photoelectron spectra (XPS) were acquired using an ESCA-3400 X-ray photoelectron spectrometer (Shimadzu). The binding energies determined using XPS were corrected with reference to the C 1s peak (284.6 eV) for each sample. N2 adsorption isotherms were measured using a BELSORP-mini instrument (MicrotracBEL) at liquid nitrogen temperature. H2O adsorption isotherms were acquired at 298 K using a BELSORP-max (MicrotracBEL) instrument. Samples were heated at 473 K for 1 h under vacuum prior to the measurements for both N2 and H2O adsorption isotherms.
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10

Comprehensive Structural and Compositional Analysis of Cu-MOF

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The morphology of the samples was examined by FESEM (JEOL-6700) and TEM (JEOL, JEM-2010). The crystal structure of the samples was examined by XRD on the Bruker D2 Phaser X-Ray Diffractometer with Cu Kα radiation (λ = 1.5406 Å). The theoretical XRD pattern of conductive Cu-MOF was calculated on the basis of the XRD simulation software of Mercury 4.1.0. The compositions of the samples were analyzed by the FESEM instrument equipped with an EDX spectroscope. The elemental mapping images of the samples were measured by using the EDX spectroscope attached to TEM (JEOL, JEM-2100F). The nitrogen adsorption-desorption isothermal curves of the samples were obtained at 77 K by using BELSORP-mini (MicrotracBEL Corp.) The electronic structure of the samples was studied by XPS (PHI Quantum 2000) with the adventitious carbon (C 1s) at the binding energy of 284.6 eV as the reference. The surface functional groups of the samples were determined by FTIR (Thermo-Smart-iTR). The XAFS spectroscopy of Cu and/or Fe K-edge was collected at the X-ray absorption fine structure for catalysis (XAFCA) beamline of the Singapore Synchrotron Light Source (SSLS), Singapore. The energy was calibrated using a copper foil. Quantitative curve fittings of the Fourier-transformed k3χ(k) in the R-space were carried out on the basis of the ARTEMIS module implemented in the IFEFFIT software packages.
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