The analysis of red mud’s composition was carried out by X-ray fluorescence (XRF) spectrometer (Philips, Netherland) based on ISO/IEC 17025:2005 standard. Philips Expert System X-ray diffractometer (XRD) was employed for the mineralogical study with CuKa radiation and Ni-filter at 40 kV and 30 mA, at 2Ɵ range of 5°–80° with a scanning rate of 2°/min, an anti-scatter and receiving slit of 1° and 0.01 mm, respectively. Dynamic light scattering (DLS) technique was employed to find the distribution of particle size of red mud, using a scatteroscope I device (DLS, Nanotrac Wave from Microtrac Company). To study the morphology of samples, FESEM (SIGMA VP-500, ZEISS, Germany) was applied at an accelerating voltage of 15 kV. The elemental mapping and energy-dispersive X-ray spectroscopy (EDX) spectra were accomplished using Energy Dispersive X-ray Spectroscopy probe (Oxford Instruments, England). Transmission electron microscopy (TEM, Tecnai F30, Philips, Netherland) and scanning electron microscopy (SEM, TESCAN MIRA3 Microscope, Netherland) were utilized to investigate the morphology. The specific surface area and porosity of red mud, γ-Al2O3 and α-Fe2O3 were determined by nitrogen sorptometry analysis at 77 K performed with the BELSORP MINI II, Japan. Before any nitrogen sorptometry test, the samples were degassed at 180 °C for 3 h.
Mini 2
Manufactured by Microtrac
Sourced in Japan
The MINI II is a compact and versatile particle size analyzer designed for rapid and accurate particle size measurements. The instrument utilizes laser diffraction technology to determine the particle size distribution of a wide range of materials, including powders, suspensions, and emulsions.
Automatically generated - may contain errors
Lab products found in correlation
Mira3, by TESCAN (4 mentions)
Mira3 microscope, by TESCAN (2 mentions)
Pw1730, by Philips (2 mentions)
D5000, by Siemens (2 mentions)
Sta449f3, by Netzsch (2 mentions)
Cary 100 spectrophotometer, by Agilent Technologies (2 mentions)
Jem 2100 transmission electron microscope, by JEOL (2 mentions)
Pw1830 diffractometer, by Philips (2 mentions)
Sigma 500 vp, by Zeiss (1 mentions)
Tecnai f30, by Philips (1 mentions)
Jsm it200, by JEOL (1 mentions)
K alpha, by Thermo Fisher Scientific (1 mentions)
Jsm it200 intouchscope, by JEOL (1 mentions)
Vector 22, by Bruker (1 mentions)
Supra 55vp, by Zeiss (1 mentions)
D8 advance, by Bruker (1 mentions)
X pert pro diffractometer, by Malvern Panalytical (1 mentions)
Ultra dld, by Shimadzu (1 mentions)
Ultra 55 field emission scanning electron microscope, by Zeiss (1 mentions)
Flash 2000, by Thermo Fisher Scientific (1 mentions)
29 protocols using mini 2
1
Comprehensive Analysis of Red Mud Composition
2
Surface Area and Pore Analysis
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N2 adsorption–desorption isotherms were measured at 77 K with liquid nitrogen on a BELSORP-mini II high precision surface area and pore size analyzer. The specific surface area was calculated using the Brunauer–Emmett–Teller (BET) equation.57 (link) Pore volume and mean pore diameter were determined by Barrett–Joyner–Halenda (BJH) equations.58 (link)
3
Comprehensive Characterization of Photocatalytic Materials
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The composition of elements and surface configuration of samples were studied by utilizing a JSM-IT200 In Touch Scope with a fully integrated EDS which includes “live EDS analysis” (JSM-IT200, JEOL, Akishima, Tokyo).
The photocatalyst crystal structures were indicated by X-ray diffraction (XRD) analysis (Bruker MeasSrv (D2-205,530)/D2-205,530) with CuKa1 radiation (wavelength = 1.54060 A°) at 30 kV voltage and 10 mA current. The wide-angle diffraction pattern was taken over a 2θ angle range extending from 20° to 80°.
FT-IR spectra of photocatalysts ZnO, TiO2, NZB, and NTB were scanned from 4000 cm−1 to 500 cm−1 on a Bruker Vector 22 (AVATAR 360, Nicolet, Madison, USA) with KBr powder (sample/KBr = 1/200).
Nitrogen adsorption/desorption isotherms were determined by a Belsorp Mini II (Japan) at 77 K. BET and BJH isotherm models are used to determine specific surface area and physical characteristics of pores.
X-ray photoelectron spectroscopy (XPS) was investigated by K-ALPHA (Thermo Fisher Scientific, USA) with monochromatic X-ray Al K-ALPHA radiation − 10 to 1350 eV at pressure 10−9 mbar with full-spectrum pass energy 200 eV and narrow-spectrum 50 eV.
To investigate the optical characteristics, the diffuse absorbance spectra of samples were measured by JASCO V-570 UV–vis absorption spectrophotometer in the range from 250 and 850 nm.
The photocatalyst crystal structures were indicated by X-ray diffraction (XRD) analysis (Bruker MeasSrv (D2-205,530)/D2-205,530) with CuKa1 radiation (wavelength = 1.54060 A°) at 30 kV voltage and 10 mA current. The wide-angle diffraction pattern was taken over a 2θ angle range extending from 20° to 80°.
FT-IR spectra of photocatalysts ZnO, TiO2, NZB, and NTB were scanned from 4000 cm−1 to 500 cm−1 on a Bruker Vector 22 (AVATAR 360, Nicolet, Madison, USA) with KBr powder (sample/KBr = 1/200).
Nitrogen adsorption/desorption isotherms were determined by a Belsorp Mini II (Japan) at 77 K. BET and BJH isotherm models are used to determine specific surface area and physical characteristics of pores.
X-ray photoelectron spectroscopy (XPS) was investigated by K-ALPHA (Thermo Fisher Scientific, USA) with monochromatic X-ray Al K-ALPHA radiation − 10 to 1350 eV at pressure 10−9 mbar with full-spectrum pass energy 200 eV and narrow-spectrum 50 eV.
To investigate the optical characteristics, the diffuse absorbance spectra of samples were measured by JASCO V-570 UV–vis absorption spectrophotometer in the range from 250 and 850 nm.
4
Comprehensive Characterization of Zeolite Samples
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Morphology of the samples was observed with Field Emission Scanning Electron Microscopy (FESEM) (VP-FESEM, Zeiss Supra 55 VP). The XRD patterns of the samples was obtained via X-ray Diffraction (XRD) (Bruker D8 Advance) diffractometer with CuKα radiation in the 2θ range of 5–60°. Percentage of crystallinity of samples were calculated by using Eq. (1 ) at main XRD peaks with 2θ angles of 8.3°, 18.6° and 25.1°. The detailed equation for the calculation of percentage of crystallinity can be found as Supplementary Equation S1 .
Framework vibration spectra of the samples was determined by Fourier Transform Infrared Spectroscopy (FTIR) (Perkin Elmer Frontier) within a wavelength from 4000 cm−1 to 400 cm−1. Thermogravimetric Analysis (TGA) of the samples was performed by heating from room temperature to 900 °C with a heating rate of 10 °C/min and flow rate of 20 mL/min under nitrogen atmosphere using Perkin Elmer Pyris. Nitrogen adsorption-desorption of the samples were conducted at 77 K by using Belsorp mini-II to measure the pore characteristics of the samples. The specific surface areas of the samples were determined by Brunauer-Emmett-Teller (BET) method.
Framework vibration spectra of the samples was determined by Fourier Transform Infrared Spectroscopy (FTIR) (Perkin Elmer Frontier) within a wavelength from 4000 cm−1 to 400 cm−1. Thermogravimetric Analysis (TGA) of the samples was performed by heating from room temperature to 900 °C with a heating rate of 10 °C/min and flow rate of 20 mL/min under nitrogen atmosphere using Perkin Elmer Pyris. Nitrogen adsorption-desorption of the samples were conducted at 77 K by using Belsorp mini-II to measure the pore characteristics of the samples. The specific surface areas of the samples were determined by Brunauer-Emmett-Teller (BET) method.
5
Characterization of Novel Materials
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The samples were
characterized by X-ray diffraction (XRD) using a PANalytical X’pert
pro diffractometer (Cu Kα radiation, secondary graphite monochromator,
scanning rate of 1° 2θ/min). IR spectroscopic studies were
carried out in a PerkinElmer FTIR spectrophotometer (spectrum two)
in the range from 4000 to 550 cm–1 with a resolution
of 4 cm–1. X-ray photoelectron spectra (XPS) of
the samples were recorded using a Kratos axis Ultra DLD. Scanning
electron microscopy (SEM) images were recorded using a Zeiss, Ultra
55 field emission scanning electron microscope. A PerkinElmer LS 35
spectrometer was used to record the UV–visible spectra. The
catalytic oxidation of benzyl alcohol was monitored by HPLC (Jasco)
using a C18 column and a UV detector at 253 nm. A mixture of water
and acetonitrile in a 70:30 volume ratio and 0.2 M phosphoric acid
was used as the mobile phase. The mobile phase flow rate was maintained
at 0.8 mL min–1. The nitrogen sorption analysis
was performed in a BELsorp mini-II instrument at liquid nitrogen temperature.
The surface area of the material was determined by employing the Brunauer–Emmett–Teller
equation. The pore sizes and pore volumes of the materials were obtained
by the Barrett–Joyner–Halenda (BJH) method.
characterized by X-ray diffraction (XRD) using a PANalytical X’pert
pro diffractometer (Cu Kα radiation, secondary graphite monochromator,
scanning rate of 1° 2θ/min). IR spectroscopic studies were
carried out in a PerkinElmer FTIR spectrophotometer (spectrum two)
in the range from 4000 to 550 cm–1 with a resolution
of 4 cm–1. X-ray photoelectron spectra (XPS) of
the samples were recorded using a Kratos axis Ultra DLD. Scanning
electron microscopy (SEM) images were recorded using a Zeiss, Ultra
55 field emission scanning electron microscope. A PerkinElmer LS 35
spectrometer was used to record the UV–visible spectra. The
catalytic oxidation of benzyl alcohol was monitored by HPLC (Jasco)
using a C18 column and a UV detector at 253 nm. A mixture of water
and acetonitrile in a 70:30 volume ratio and 0.2 M phosphoric acid
was used as the mobile phase. The mobile phase flow rate was maintained
at 0.8 mL min–1. The nitrogen sorption analysis
was performed in a BELsorp mini-II instrument at liquid nitrogen temperature.
The surface area of the material was determined by employing the Brunauer–Emmett–Teller
equation. The pore sizes and pore volumes of the materials were obtained
by the Barrett–Joyner–Halenda (BJH) method.
6
Characterization of Silicon Quantum Dot Clusters
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Field-emission transmission
electron microscopy (FE-TEM) was performed using a JEM-2100F electron
microscope (JEOL, Japan) with an accelerating voltage of 400 kV. For
TEM sampling, 0.1 wt % solution of the Si QD cluster in toluene was
drop-cast onto a lacey carbon-coated copper grid, and the solvent
was evaporated in vacuum. Proton nuclear magnetic resonance (H NMR)
data were collected with the superconducting FT-NMR at 300 MHz (Varian
Inc., Palo Alto, California). Chemical shifts were reported in parts
per million (ppm) in a solvent of chloroform-d (99.8 atom % D). Fourier-transform
infrared (FT-IR) spectroscopy was performed using a Nicolet 380 spectrometry
system (Waltham, MA) operated in the mid-IR range of (4000–400)
cm–1, with the spectra obtained at a spectral resolution
of 2 cm–1 in the transmittance mode. Carbon, hydrogen,
nitrogen, sulfur, and oxygen contents were measured using a Thermo
Scientific Flash 2000 organic elemental analyzer and vario MICRO cube
elemental analyzer. Nitrogen adsorption–desorption isotherms
were recorded using Belsorp mini II surface area and porosimetry analyzer.
Prior to the measurements, the Si QD cluster was degassed under vacuum
at 70 °C for 6 h.
electron microscopy (FE-TEM) was performed using a JEM-2100F electron
microscope (JEOL, Japan) with an accelerating voltage of 400 kV. For
TEM sampling, 0.1 wt % solution of the Si QD cluster in toluene was
drop-cast onto a lacey carbon-coated copper grid, and the solvent
was evaporated in vacuum. Proton nuclear magnetic resonance (H NMR)
data were collected with the superconducting FT-NMR at 300 MHz (Varian
Inc., Palo Alto, California). Chemical shifts were reported in parts
per million (ppm) in a solvent of chloroform-d (99.8 atom % D). Fourier-transform
infrared (FT-IR) spectroscopy was performed using a Nicolet 380 spectrometry
system (Waltham, MA) operated in the mid-IR range of (4000–400)
cm–1, with the spectra obtained at a spectral resolution
of 2 cm–1 in the transmittance mode. Carbon, hydrogen,
nitrogen, sulfur, and oxygen contents were measured using a Thermo
Scientific Flash 2000 organic elemental analyzer and vario MICRO cube
elemental analyzer. Nitrogen adsorption–desorption isotherms
were recorded using Belsorp mini II surface area and porosimetry analyzer.
Prior to the measurements, the Si QD cluster was degassed under vacuum
at 70 °C for 6 h.
7
Comprehensive Characterization of Nanohybrids
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To study the crystallography of the samples, X-pert Philips pw 1730 (Netherland) X-ray diffractometer operating at current of 30 mA and accelerating voltage of 40 kV, using Cu-Kα1 (wavelength of 1.54056 Å) radiation in scanning range of 2θ = 10°–70° was utilized at a scanning speed of 1 s/0.05◦. Fourier transform infrared (FTIR) spectroscopy analyses was conducted using THERMO AVATAR (USA) FT-IR Spectrometer with the wavelength range of 400–4000 cm−1. The surface morphology of synthesized nanohybrids was observed by using FESEM–MIRA3 TESCAN (Czech). N2-physisorption experiments were carried out at 77 K in using BELSORP MINI II (Japan) instrument. Photoluminescence (PL) spectra were evaluated using Varian Cary Eclipse Fluorescence Spectrophotometer.
8
Heterogeneous Nanocatalyst for Humic Acid Degradation
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Merck Company (Germany) supplied silver nitrate (AgNO3). Degussa (Germany) provided the P25 titania (TiO2), while Sigma-Aldrich provided the Na3PO4 for the catalyst production. Sigma-Aldrich was also used to purchase the humic acid, sodium hydroxide (NaOH), and hydrogen chloride (HCl). The pH of the solutions was adjusted with HCl and NaOH (1 N), and the pH was detected with a pH meter (Wegtech Mi 151 22, UK). At a maximum wavelength of 254 nm, a UV–vis spectrophotometer (Model Optima SP3000 Plus, Japan) was utilized to measure the concentration of HA. The structure of this yellow nanocomposite, which acts as a heterogeneous catalyst, was studied using XRD, SEM, and EDS tools. XRD (Bourevestnik-Dron8) was used to characterize the shape and phase of a nano-crystal catalyst, SEM (TESCAN-Vega3) was used to study the structure, morphology, and surface characteristics of the nano-catalyst on the nanoscale, and EDS (TESCAN-Vega3) was used to evaluate the component mass percentages at the nano-catalyst and BET to quantify the size of a particular area in the nanocatalyst (BELSORP MINI II). After validating the physical and chemical composition of the heterogeneous nanocatalyst, it was utilized to degrade HA in an aqueous media.
9
Morphological and Surface Analysis of Activated Carbon
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The morphological information of the samples was obtained via field emission scanning electron microscopy (FE-SEM, Hitachi S-4800, Japan) at the National Nanofab Center, Daejeon, Republic of Korea. The Brunauer–Emmett–Teller (BET) surface areas of the AC samples were determined by nitrogen adsorption measurements at −196 °C (BELSORP MINI II, Japan) under a preheat treatment of 150 °C for 3 h with a vacuum of 10−2 kPa. The surface elemental composition of ACLA-C and ACLA-C_PEI layer was analyzed via X-ray photoelectron spectroscopy (XPS, MULTILAB 2000, Thermo Fisher Scientific, USA). The ionic concentration of the condensed water obtained after the desalination experiment was analyzed via inductively coupled plasma atomic emission spectroscopy (ICP-AES, ELAN DRC II, Perkin Elmer, USA). The light absorption of photothermal layer was measured via a diffuse reflectance UV-VIS-NIR spectrophotometer with an integrating sphere (SolidSpec-3700, Shimadzu, Japan). The contact angle measurements were carried out using DSA100B-Basic (KRÜSS, Germany).
10
Characterization of Powder Materials
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Nitrogen adsorption at −196 °C was carried out with Belsorp Mini-II (Osaka, Japan) for determining surface areas, pore volumes, and pore diameters of the powders. Prior to the measurement, the sample was kept in a vacuum at 100 °C for 3 h. The Brunauer–Emmet–Teller (BET) method was used to calculate a specific surface area. The pore diameter was derived from the isothermal adsorption branch using the Barrett–Joyner–Halande (BJH) method. The pore volume was estimated from the amount of gas adsorbed at relative pressure, p/p0 = 0.99. X-ray diffraction (XRD) was measured by the Multiplex (Rigaku, Japan) at room temperature in the range of 2θ = 2–20° using CuKα radiation (λ = 1.5406 Å). The Fourier-transform infrared spectroscopy (FT-IR) spectrum of the powder was recorded in attenuated total reflection mode on diamond crystals using the Vertex70 (Bruker, Germany) in the range of 400–4000 cm−1. Field emission scanning electron microscope (FE-SEM, JSM-6701F, JEOL, Tokyo, Japan) was used to investigate particle size and shape of the powder.
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