Belcat 2
Manufactured by Microtrac
Sourced in Japan
The BELCAT II is a laser particle size analysis instrument designed to measure the size distribution of particles in a sample. It utilizes the principle of laser diffraction to determine the particle size distribution.
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11 protocols using belcat 2
1
Thermal Decomposition of Nb2O5 and K2CO3
2
Comprehensive Characterization of Catalyst Materials
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XRD patterns were obtained using X-ray diffractometer (SmartLab SE, Rigaku) at 40 kV and 40 mA. N2 adsorption-desorption isotherms were measured with Micromeritics ASAP 2460 instrument at −196°C. TEM micrographs were obtained on FEI Tecnai G2 F20 S-TWIN at an acceleration voltage of 200 kV, and SEM observations were performed on Carl Zeiss Sigma with a field-emission gun operated at 5.0 kV. 27Al and 29Si MAS NMR experiments were performed on Bruker AVANCE III 600 spectrometer at a resonance frequency of 156.4 MHz and 119.2 MHz, respectively. NH3-TPD measurements were performed using a BELCAT II (MicrotracBEL) instrument. Chemical compositions were determined with ICP-OES on an Optima 7000DV (PerkinElmer) spectrometer. FTIR spectroscopy with 2,6-di-tert-butyl-pyriding (DTBP) adsorption were obtained on Bruker Vertex 70 instrument. The band at 1615 cm−1 corresponding to the protonated DTBP was used to estimate the amount of external Brønsted acid sites.
3
Comprehensive Characterization of Vanadium Slag
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The mineral composition
of vanadium slag and roasted clinker was characterized by using an
X-ray powder diffractometer (XRD, D/MAX-2500, Rigaku, Japan). The
chemical composition of vanadium slag was analyzed by an X-ray fluorescence
spectrometer (XRF, ARL Perform’X, Thermo Fisher Scientific
CDLtd, Switzerland). The morphology and element distribution of vanadium
slag and roasted clinker were analyzed by scanning electron microscopy
(SEM, Ultra Plus, Carl Zeiss, Germany) and X-ray energy dispersion
spectroscopy (EDS, Oxford X-MAX, Carl Zeiss, Germany). Thermogravimetric
(TG) and differential scanning calorimetry (DSC) analyses were performed
using a synchronous thermal analyzer (TG-DSC, TGA/DSC1/1600LF, Mettler
Corporation, Switzerland). The changes in the valence states of V
and Fe during roasting were analyzed by X-ray photoelectron spectroscopy
(XPS, Escalab-250Xi, ThermoFisher Corporation, Britain). The content
of the V element in the leaching solution of calcined clinker was
determined by an inductively coupled plasma emission spectrometry
system (ICP-OES, ICAP6300, ThermoFisher Scientific, Britain). The
oxygen adsorption capacity of the vanadium slag mixture was analyzed
by an automatic chemisorbent analyzer (TPD, Belcat II, MicrotracBEL,
Japan).
of vanadium slag and roasted clinker was characterized by using an
X-ray powder diffractometer (XRD, D/MAX-2500, Rigaku, Japan). The
chemical composition of vanadium slag was analyzed by an X-ray fluorescence
spectrometer (XRF, ARL Perform’X, Thermo Fisher Scientific
CDLtd, Switzerland). The morphology and element distribution of vanadium
slag and roasted clinker were analyzed by scanning electron microscopy
(SEM, Ultra Plus, Carl Zeiss, Germany) and X-ray energy dispersion
spectroscopy (EDS, Oxford X-MAX, Carl Zeiss, Germany). Thermogravimetric
(TG) and differential scanning calorimetry (DSC) analyses were performed
using a synchronous thermal analyzer (TG-DSC, TGA/DSC1/1600LF, Mettler
Corporation, Switzerland). The changes in the valence states of V
and Fe during roasting were analyzed by X-ray photoelectron spectroscopy
(XPS, Escalab-250Xi, ThermoFisher Corporation, Britain). The content
of the V element in the leaching solution of calcined clinker was
determined by an inductively coupled plasma emission spectrometry
system (ICP-OES, ICAP6300, ThermoFisher Scientific, Britain). The
oxygen adsorption capacity of the vanadium slag mixture was analyzed
by an automatic chemisorbent analyzer (TPD, Belcat II, MicrotracBEL,
Japan).
4
Characterization of Pd Catalysts by CO Pulse and XAFS
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The dispersion ratio and particle diameter of Pd catalysts were characterized using CO pulse (BEL CAT II; Microtrac-Bel Japan Inc.). Before measurements, the catalyst sample was pre-treated under He flow at 473 K for 1 h. After the treatment, the temperature was decreased to 323 K with He, and 10% CO was pulsed. The results of CO pulse are presented in Supplementary Materials Table S9 . TOF-s and TOF-p were calculated with the number of surface Pd atoms and that of interfacial Pd atoms. Detailed procedures are presented in Supplementary Materials . Pd and Ce K-edge in-situ X-ray adsorption fine structure (in-situ XAFS) spectra were recorded on BL14B2 in SPring-8 (Hyogo, Japan). The 3 wt% Pd/CeO2 catalyst was pressed into a pellet. Then the pellet was attached to a cell prepared for in-situ measurements, as shown in Figure S18 . The pellet sample was pre-treated with Ar flow at 723 K for 30 min. Measurements were conducted with 5 mA current and CH4: H2O: Ar = 1: 2: 117, total 120 SCCM flow at 473 K. Software (Athena ver. 0.8.056, Artemis ver. 0.8.012) was used to analyze the obtained XAFS spectra. Phase and morphology of CeO2 disc for AC impedance measurements were analyzed by X-ray diffraction (XRD, MiniFlex 600, Cu Kα1, Rigaku) and scanning electron microscopy (FE-SEM, Quanta 200 FEG, FEI Company).
5
Ethanol Desorption on Au-WO3 Catalyst
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The temperature-programmed desorption (TPD) of ethanol on Au-WO3 were carried out by an automated catalyst analyzer (BELCAT II, MicrotracBEL, Osaka, Japan) connected to a mass spectrometer (BELMass, MicrotracBEL, Osaka, Japan). Before TPD experiments, samples were treated with 20% O2 in He for 30 min at 300 °C, followed by purging with He for 15 min. The adsorption of ethanol was performed by introducing 50 ppm ethanol in synthetic air to a chamber where samples were loaded for 30 min at room temperature. After purging the system with He, the samples were heated to 300 °C with a heating rate of 10 °C·min−1 in He. Gas molecules desorbed from the samples were monitored by the mass spectrometer.
6
CO2 Temperature-Programmed Desorption
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CO2-TPD is conducted on the Microtrac BEL Cat II instrument. The catalyst (50 mg) is pretreated at 450 °C for 180 min in 20% H2 (heating rate of 5 °C/min), followed by cooling to 50 °C and purge with He for 30 min. Then, the catalyst is treated in CO2/He (10/90) for 60 min, followed by a 40-min purge with He to remove unabsorbed and physically adsorbed CO2. After the baseline has been stabilized, the temperature is gradually increased from room temperature to 800 °C at a heating rate of 10 °C/min in order to facilitate the desorption of CO2.
7
Pt Metal Dispersion and Surface Area
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Dispersion and metal surface area of Pt metal was estimated using CO pulse measurements (BELCAT II; MicrotracBEL Corp.). Pre-treatment was conducted at 623 K in He gas to vaporize the adsorbed water. In addition, the state of supported Pt was confirmed with STEM images and EDX mapping results from scanning transmission electron microscopy (STEM; HF-2210; Hitachi Ltd.). The specific surface area of the catalyst was investigated based on N2 adsorption using the BET method (Gemini VII; Micromeritics Instrument Corp.). Pre-treatment was conducted at 473 K in a N2 atmosphere for 2 h.
8
Structural and Acidic Analysis of Catalysts
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N2 physisorption was used to analyze
the structural characteristics
of catalysts at about −196 °C (nitrogen saturation temperature)
in an Autosorb-1 apparatus (TriStar II 3020M, Micromeritics, USA).
Powder X-ray diffraction (XRD, D8 ADVANCE, Bruker, Germany) was employed
to identify the crystalline phases of catalysts using Cu Kα
radiation (λ = 0.15406 nm) at 40 kV and 150 mA. NH3–TPD (BELCAT II, MicrotracBEL Japan) was used to determine
the acidities of catalysts. The testing conditions were referenced
from the literature.27 (link)
the structural characteristics
of catalysts at about −196 °C (nitrogen saturation temperature)
in an Autosorb-1 apparatus (TriStar II 3020M, Micromeritics, USA).
Powder X-ray diffraction (XRD, D8 ADVANCE, Bruker, Germany) was employed
to identify the crystalline phases of catalysts using Cu Kα
radiation (λ = 0.15406 nm) at 40 kV and 150 mA. NH3–TPD (BELCAT II, MicrotracBEL Japan) was used to determine
the acidities of catalysts. The testing conditions were referenced
from the literature.27 (link)
9
Catalytic Activity Tests for DRM
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Catalytic activity tests for the DRM were performed using a flow-type reactor, MicrotracBEL BELCAT II. Prior to reaction, the catalyst (100 mg) was loaded in a tubular reactor (inner diameter = 7.5 mm) and fixed with quartz wool on both sides. Then, the catalyst was reduced by H2 at 30 mL/min flow at 450 °C for 2 h. The DRM was conducted at 550 °C under a mixed gas stream of CO2/CH4/N2 = 10/10/5 (v/v/v) with a total gas flow rate of 25 mL/min. The temperature of the reactor was maintained at 550 °C for 15 h. The gaseous products were analyzed using a gas chromatograph (GL Sciences GC3200) with an active carbon column equipped with a TCD.
The CH4 and CO2 turnover frequencies (TOFs) were calculated by the moles of CH4 or CO2 converted per second per the moles of catalysts with the following equation: where N (gas), N (catalyst), and conversion represent gas flow rate (mol/s), amount of catalyst (mol), and conversion of reactant gas, respectively.
The CH4 and CO2 turnover frequencies (TOFs) were calculated by the moles of CH4 or CO2 converted per second per the moles of catalysts with the following equation: where N (gas), N (catalyst), and conversion represent gas flow rate (mol/s), amount of catalyst (mol), and conversion of reactant gas, respectively.
10
Hydrogen Temperature-Programmed Reduction
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H2-temperature-programmed
reduction (H2-TPR) was performed in a BELCAT II catalyst
analyzer from Microtrac MRB using a thermal conductivity detector.
The calcined samples were placed into a fixed-bed microreactor and
pretreated at 120 °C for 60 min with Ar (99.999%, Air Liquide).
After cooling to 40 °C, H2-TPR was carried out in
10% H2/Ar at a flow rate of 80 mL min–1 and the catalysts were heated to 900 °C at 10 K min–1. For 10 and 20% Ni/MgO WI samples, the catalyst amounts used were
65 mg. The amount of the used catalyst for 10 and 20% Ni/MgO CP was
300 and 150 mg, respectively.
reduction (H2-TPR) was performed in a BELCAT II catalyst
analyzer from Microtrac MRB using a thermal conductivity detector.
The calcined samples were placed into a fixed-bed microreactor and
pretreated at 120 °C for 60 min with Ar (99.999%, Air Liquide).
After cooling to 40 °C, H2-TPR was carried out in
10% H2/Ar at a flow rate of 80 mL min–1 and the catalysts were heated to 900 °C at 10 K min–1. For 10 and 20% Ni/MgO WI samples, the catalyst amounts used were
65 mg. The amount of the used catalyst for 10 and 20% Ni/MgO CP was
300 and 150 mg, respectively.
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