The microstructures of the catalystswere analyzed using scanning electron microscopy (SEM, HITACHI S-4800) and transmission electron microscopy (TEM, JEOL JEM-2100F) equipped with EDS. X-ray photoelectron spectroscopy (XPS) was carried out on the Thermo Scientific ESCALab 250Xi using a 200W Al-Kα radiation. The base pressure in the analysis chamber was maintained at about 3 × 10-10 mbar to ensure accurate results. The hydrocarbon C1s line at 284.8 eV was utilized for energy referencing. X-ray diffraction (XRD) analysis was performed on the samples using a Rigaku D/max-2500 X-ray diffractometer with Cu-Kα radiation (y = 0.15406 nm) at a scan speed of 5o min−1. The Raman spectra of the samples were obtained on an FT Bruker RFS 106/S spectrometer equipped with a 514 nm laser in the region from 4000 to 100 cm−1 with a resolution of 2 cm−1, in a flame-sealed capillary at room temperature. The N2 adsorption/desorption isotherms were determined using a Micromeritics ASAP 2020 sorptometer operated at 77 K, and BET surface areas and pore volumes were obtained.
Asap 2020 sorptometer
Manufactured by Micromeritics
Sourced in United States
The ASAP 2020 sorptometer is a surface area and pore size analyzer that measures the physical adsorption of gases on solid or porous materials. It provides precise data on surface area, pore volume, and pore size distribution. The instrument uses nitrogen adsorption at cryogenic temperatures to generate adsorption and desorption isotherms, which are then analyzed to determine the material's physical properties.
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Lab products found in correlation
Phi 5300 esca, by PerkinElmer (2 mentions)
Escalab 250xi, by Thermo Fisher Scientific (2 mentions)
D max 2500, by Rigaku (1 mentions)
Jem 2100f, by JEOL (1 mentions)
S 4800, by Hitachi (1 mentions)
Jsm 6700f, by JEOL (1 mentions)
Jem 2010f, by JEOL (1 mentions)
Invia raman microspectrometer, by Renishaw (1 mentions)
Icps 7500 spectrometer, by Shimadzu (1 mentions)
Vg escalab 250 x ray photoelectron spectrometer, by Thermo Fisher Scientific (1 mentions)
Thermal analyzer, by PerkinElmer (1 mentions)
Tecnai g2 20, by Thermo Fisher Scientific (1 mentions)
Zetasizer nano zs90, by Malvern Panalytical (1 mentions)
Pw1710 diffractometer, by Philips (1 mentions)
H 8100 tem, by Hitachi (1 mentions)
Feg 650, by Thermo Fisher Scientific (1 mentions)
9 protocols using asap 2020 sorptometer
1
Comprehensive Catalyst Characterization Techniques
2
Comprehensive Characterization of Electrosynthesized Materials
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The morphology of the electrosynthesized products was characterized using a JEOL JSM-6700F field-emission-type scanning electron microscope (FESEM), and using a JEOL JEM-2010F high-resolution transmission electron microscope (HRTEM) operating at 200 kV. The elemental composition of the samples was analyzed by energy-dispersive X-ray spectroscopy (EDS) attached to the SEM and TEM. Powder X-ray diffraction (XRD) patterns were collected on a Rigaku D/Max-2550 diffractometer using Cu Kα radiation (λ = 0.15406 nm) operated at a voltage of 40 kV and 100 mA. Digital optical photograph of the sample was taken by a KEYENCE VHX-1000C digital optical microscope. X-ray photoelectron spectroscopy (XPS) analysis was performed on an ESCALAB 250Xi spectrometer with Al Kα radiation. Raman spectroscopy of the sample was performed on a Renishaw InVia Raman microspectrometer using an Ar ion laser (514.5 nm). Fourier transform infrared spectroscopy (FTIR) spectrum was recorded on a Nicolet Avatar 380 spectrometer. N2 adsorption and desorption isotherm was measured using a Micromeritics ASAP 2020 sorptometer at liquid nitrogen temperature (−196 °C). Before the measurement, the sample was degassed at 200 °C for 6 h. The specific surface area was evaluated using the Brunauer-Emmett-Teller (BET) method.
3
Structural Characterization of Ru Catalysts
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XRD patterns of Ru-x samples were measured on the D8ADVANCE diffractometer equipped with a Kα radiation. The morphologies and particle size of different Ru crystals were investigated by high-angle annular dark-field scanning transmission electron microscopy (HADDF-STEM) images on a JEOL-2100F FETEM. XPS spectra were conducted over a Thermo VG ESCALAB250 X-ray photoelectron spectrometer. UPS measurements were performed on a UV/VIS spectrometer Lambada 25. The mass loadings of Ru on the porous carbon substrate were measured by ICP-AES (Shimadzu ICPS-7500 spectrometer). BET surface area was determined through low-temperature N2 adsorption-desorption experiments on a Micromeritics ASAP 2020 sorptometer.
4
Characterization of Novel Material
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Thermogravimetric (TG) and differential scanning calorimetry (DSC) analysis were measured with PerkinElmer Thermal Analyzer. Scanning electron microscope (SEM) and transmission electron microscope (TEM) were performed to characterized morphology structure using a ZEISS EVO18 and JEM-2100 (HR), respectively. Nitrogen adsorption/desorption isotherms were measured at −195.68 °C by means of a Micromeritics model ASAP 2020 sorptometer. X-ray diffraction (XRD) was performed with a SmartLab X-ray diffractometer operated at 45 kV and 200 mA. An InVia-Reflex apparatus was used to measure Raman spectrum with 532 nm laser. Fourier transform infrared (FTIR) spectroscopy analysis was measured by Nexus 870 FT-IR. X-ray photoelectron spectroscopy (XPS) was performed with Escalab 250xi.
5
Nanoparticle Characterization: Size, Zeta, Morphology
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The size and zeta potential of nanoparticles were determined in aqueous suspension by using dynamic light scattering (DLS; Zetasizer Nano-ZS 90; Malvern Instruments, Malvern, UK). The morphology of nanoparticles was observed by transmission electron microscopy (Tecnai G2 20; FEI, Eindhoven, the Netherlands). Thermogravimetric analysis (TGA) of nanoparticles was performed by Pyris TG Analyzer (PerkinElmer Inc., Waltham, MA, USA) using nitrogen as an oxidant with continuous heating rate of 10°C/min from 30°C to 796.84°C. N2-absorption/desorption analysis was performed by using an ASAP 2020 sorptometer (Micromeritics, Norcross, GA, USA) at a constant temperature of 77 K.
6
Material Characterization Techniques for Sample Analysis
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Transmission electron micrograph (TEM) of the samples was taken on a Hitachi H-8100 TEM, operated at 200 kV. Powder X-ray diffraction (XRD) patterns were recorded on a Philips PW1710 diffractometer using Cu Kα radiation. Nitrogen adsorption–desorption isotherms were measured at 77 K on a Micromeritics ASAP 2020 sorptometer, with the samples outgassed for 16 h at 110 °C and 10−6 Torr prior to measurement. X-ray photoelectron spectroscopy (XPS) of the above mentioned samples were recorded on a spectrometer (Perkin-Elmer PHI-5300/ESCA, USA) with an Al Kα X-ray source. All the binding energies were referenced to the neutral C 1s peak at 284.6 eV to compensate for the surface charging effects. The XPS results were collected as binding energy forms and fitted using a curve-fitting program (XPSPEAK41 software).
7
Characterization of GAC and GACox Adsorbents
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Prior to characterization, GAC and GACox were dried at 105 °C for 24 h to remove the adsorbed moisture and were kept sealed under dry air in a desiccator. The surface acidic functional groups and acidic/basic sites were determined by Boehm titrations as described previously.27 (link) The pH of the point of zero charge (pHpzc) of samples was established using a method suggested by Noh and Schwarz.28 (link) Nitrogen adsorption–desorption isotherms were measured at 77 K on a Micromeritics ASAP 2020 sorptometer following the manufacture's introduction. Prior to measurement, the samples were outgassed for 16 h at 110 °C and 10−6 Torr. FTIR spectra were performed on the Spectrum One spectrometer from 400 to 4000 cm−1 by dried KBr pellet. XPS of the above mentioned samples were recorded on a spectrometer (Perkin-Elmer PHI-5300/ESCA, USA) with an Al Kα X-ray source. All the binding energies were referenced to the neutral C 1s peak at 284.6 eV to compensate for the surface charging effects. The XPS results were collected as binding energy forms and fitted using a curve-fitting program following the data analysis guide of XPSPEAK41 software.
8
Ruthenium Catalyst Characterization by XRD, N2 Adsorption, and TEM
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X-ray diffraction (XRD) patterns were obtained using a Rigaku D/MAX-2200 apparatus with a Cu Kα radiation (λ = 0.15418 nm) at a voltage of 40 kV and a current of 40 mA. N2 adsorption–desorption carried out using a Micromeritics ASAP 2020 Sorptometer at −196 °C. Before the measurement, the sample was degassed at 200 °C for 10 h. The Brunauer–Emmett–Teller (BET) method was utilized to calculate the specific surface areas (SBET) using adsorption data in a relative pressure range from 0.05 to 0.25. By using the Barrett–Joyner–Halenda (BJH) model, the pore volumes and size distributions were derived from the adsorption branches of isotherms, and the pore size (Dp) was obtained from the maximum of the pore distribution curve. The pore volume (Vp) was taken at P/P0 = 0.990 single point Transmission electron microscopy (TEM) micrographs were performed with a JEOL JEM-2010F field emission microscope operating at 200 kV. The weight percentage of Ru deposited was analyzed by inductively coupled plasma atomic emission spectrometry (ICP-AES).
9
Characterization of Porous Carbon Materials
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Scanning electron microscopy (SEM) images were recorded on a Quanta FEG650 (FEI) instrument. The particle size histograms were obtained by measuring ~ 300 particles in the SEM images. The nitrogen sorption isotherms of the carbon samples were measured at 196 °C using a Micromeritics ASAP 2020 sorptometer. The apparent surface area (S BET ) was calculated from the N 2 isotherms using the Brunauer-Emmett-Teller (BET) method. An appropriate relative pressure range was selected to ensure that a positive line intersect of multipoint BET fitting (C > 0) would be obtained and that the V ads (1 p/p o ) would increase with p/p o. [55, 56] The total pore volume (V p ) was determined from the amount of nitrogen adsorbed at a relative pressure (p/p o ) of 0.95. The micropore volume (V m ) was obtained by applying the Dubinin-Radushkevich equation. [57] The micropore size distributions were determined by applying the Quenched-Solid Density Functional Theory (QSDFT) method to the nitrogen adsorption data and assuming a slit pore model. Elemental analysis (C, N and O) of the samples was carried out on a LECO CHN-932 microanalyzer.
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