In a typical synthesis of mesoporous Mn0.5Ce0.5Ox solid solution oxides, 6.16 g of cerium (IV) methoxyethoxide (18–20% in methoxyethoxide, Gesta), 0.63 g Mn(OOCCH3)2·6H2O (99%, Aldrich) and 1.0 g of ionic liquid (BmimTf2N) were dissolved in 5.0 ml of ethanol. The solution was stirred at room temperature for 2 h until Mn(OOCCH3)2·6H2O was completely dissolved. Subsequently, ethanol (5.0 ml) was added slowly with stirring. The mixed solution was gelled in an open petridish at 50 °C for 24 h and aged at 200 °C for 2 h, and a solid film was obtained. The ionic liquid was extracted by refluxing the sample with ethanol in a Soxhlet extractor for 24 h. The as-made sample (Mn0.5Ce0.5Ox@200) was thermally treated at 500 °C for 2 h with the heating rate of 1 K min−1 in air, and the final sample denoted as Mn0.5Ce0.5Ox@500. Other metal oxides were prepared by the same process except with different metal precursors. The materials were characterized by N2 adsorption (TriStar, Micromeritics) at 77 K, powder XRD (Panalytical Empyrean diffractometer with Cu Ka radiation k=1.5418 A° operating at 45 kV and 40 mA), thermogravimetric analysis (TGA 2950, TA Instruments), Fourier-transform infrared spectrum (PerkinElmer Frontier FTIR spectrometer) and H2-TPR (Auto chem II, Micromeritics).
Autochem 2
Manufactured by Micromeritics
Sourced in United States
The AutoChem II is a laboratory instrument designed for the characterization of solid materials. It is capable of performing temperature-programmed studies, such as chemisorption, physisorption, and temperature-programmed reduction, oxidation, and desorption analyses. The AutoChem II provides detailed information about the surface properties and catalytic behavior of solid samples.
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Lab products found in correlation
Tristar 3000, by Micromeritics (2 mentions)
Tga 2950, by TA Instruments (1 mentions)
Optima 4300dv spectrometer, by PerkinElmer (1 mentions)
X pert pro instrument, by Malvern Panalytical (1 mentions)
S 5200 microscope, by Hitachi (1 mentions)
Vista ax spectrometer, by Agilent Technologies (1 mentions)
Asap 2020, by Micromeritics (1 mentions)
17 protocols using autochem 2
1
Synthesis and Characterization of Mn0.5Ce0.5Ox Oxides
2
Catalyst Characterization via H2 Chemisorption
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Experiments were performed utilizing a Micromeritics AutoChem II instrument under the flow of He at 20 mL min−1. NAC-800 catalyst (200 mg) was mounted between quartz wool inside a quartz reactor assembled in a furnace. The temperature was measured at the sample position with a K-type thermocouple sealed in a quartz capillary. All samples were thermally pretreated at 400 °C for 4 h to remove any possible surface contamination such as carbon species or water present in air. In the pulsed chemisorption experiment, H2 consumption was monitored through a thermal conductivity detector that measures the signal difference of the desorbed gas versus a reference flow.
3
Acidity Determination of Catalysts
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This technique was used to determine the acidity of the catalysts, previously calcined. The Micromeritics® AutoChem II equipment was employed (Norcross, GA, USA) for the measurements. First, the samples were reduced at 700 °C with a 5 vol% H2/Ar mixture. After 30 min with He, it was cooled down to 100 °C, and NH3 adsorption was run for 30 min. Subsequently, the physically adsorbed NH3 was desorbed with He at 150 °C and the chemically adsorbed NH3 was desorbed between 150 °C and 900 °C, with a heating rate of 10 °C/min. The consistency of the acidity was differentiated as a function of the temperature required to desorb the adsorbed ammonia. In this way, three classes of acidity were differentiated: weak acidity below 250 °C, medium acidity between 250 °C and 450 °C and strong acidity between 450 °C and 900 °C. Once the signal emitted by the equipment was calibrated, the NH3 concentration was obtained in units of Ncm3/min. Subsequently, using the ideal gas equation and corrected with the mass of catalyst used in the analysis, the mmolNH3/(min·g) desorbed was obtained. Finally, by integrating over the desired time, adsorbed mmolNH3 per gram of catalyst were obtained.
4
Reduction Temperature Determination of Catalysts
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This technique was employed to determine the reduction temperature of the reducing species in the previously calcined catalysts. For this purpose, Micromeritics® AutoChem II equipment (Norcross, GA, USA) with a thermal conductivity detector was used. A 5 vol% H2/Ar mixture was used with approximately 0.1 g of catalyst from room temperature to 950 °C, with a heating rate of 5 °C/min.
5
Characterization of Heterogeneous Catalysts
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The Brunauer–Emmett–Teller
(BET) surface area40 (link) of the samples was
determined by N2 physisorption at −196 °C using
a BELSOPRP-mini instrument (MicrotracBEL, Osaka, Japan). Prior to
the analysis, the samples were degassed at 200 °C for 2 h.
The crystallinity of the catalyst components was assessed via XRD
using an X′Pert PRO instrument (PANalytical, Malvern, United
Kingdom). The patterns were recorded between 5 and 120° using
Cu Kα radiation (wavelength = 1.54 Å) with a step size
of 0.017°.
Temperature-programmed reduction with H2 (H2-TPR) was performed on an AutoChem II instrument
(Micromeritics,
Norcross, USA) by heating the sample at 10 °C/min from room temperature
to 900 °C while dosing 50 mL/min of 10%H2/Ar. Before
the reduction step, adsorbed species were removed by heating the sample
in 50 mL/min of He from room temperature to 200 °C.
For
all catalyst samples, Ni and Pt metal loadings were determined
by inductively coupled plasma optical emission spectroscopy (ICP-OES)
using an OPTIMA 4300 DV spectrometer (PerkinElmer, Waltham, USA).
(BET) surface area40 (link) of the samples was
determined by N2 physisorption at −196 °C using
a BELSOPRP-mini instrument (MicrotracBEL, Osaka, Japan). Prior to
the analysis, the samples were degassed at 200 °C for 2 h.
The crystallinity of the catalyst components was assessed via XRD
using an X′Pert PRO instrument (PANalytical, Malvern, United
Kingdom). The patterns were recorded between 5 and 120° using
Cu Kα radiation (wavelength = 1.54 Å) with a step size
of 0.017°.
Temperature-programmed reduction with H2 (H2-TPR) was performed on an AutoChem II instrument
(Micromeritics,
Norcross, USA) by heating the sample at 10 °C/min from room temperature
to 900 °C while dosing 50 mL/min of 10%H2/Ar. Before
the reduction step, adsorbed species were removed by heating the sample
in 50 mL/min of He from room temperature to 200 °C.
For
all catalyst samples, Ni and Pt metal loadings were determined
by inductively coupled plasma optical emission spectroscopy (ICP-OES)
using an OPTIMA 4300 DV spectrometer (PerkinElmer, Waltham, USA).
6
Catalyst Surface Area Analysis
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The active metal surface area (AMSA) and the metal dispersion were determined by chemical adsorption by CO in a Micromeritics® AutoChem II apparatus (Norcross, GA, USA). The samples were reduced prior to analysis at 700 °C in the presence of a 5 vol% H2-Ar mixture. Subsequently, the CO-chemisorption capacity was measured at 35 °C in the presence of a 5 vol% CO-He mixture.
7
Ammonia Temperature-Programmed Desorption
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The acidity of the samples
was determined in a Micromeritics AutoChem II equipment. The sample
(0.08 g) was first pretreated in N2 with a total flow rate
of 50 mL min–1 from room temperature to 550 °C
with a temperature ramp of 10 °C min–1. Then,
10% NH3/He was fed at 100 °C until saturation, followed
by a purge with 50 mL min–1 of He for 1 h to desorb
physisorbed NH3. Finally, the sample was heated from 100
to 550 °C with a temperature ramp of 10 °C min–1 in 50 mL min–1 of He. The effluent of the reactor
was continuously measured by a TCD detector to quantify the NH3 desorption profile.
was determined in a Micromeritics AutoChem II equipment. The sample
(0.08 g) was first pretreated in N2 with a total flow rate
of 50 mL min–1 from room temperature to 550 °C
with a temperature ramp of 10 °C min–1. Then,
10% NH3/He was fed at 100 °C until saturation, followed
by a purge with 50 mL min–1 of He for 1 h to desorb
physisorbed NH3. Finally, the sample was heated from 100
to 550 °C with a temperature ramp of 10 °C min–1 in 50 mL min–1 of He. The effluent of the reactor
was continuously measured by a TCD detector to quantify the NH3 desorption profile.
8
H2-TPR Analysis of Pt/CeO2 Catalysts
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H2-temperature-programmed reduction
(H2-TPR) curves
were obtained with 0.03 g of the sample using an Autochem II (Micromeritics)
equipped with a thermal conductivity detector (TCD). Typically, samples
were oxidized with 10% O2/He at 400 °C for 1 h to
remove impurities, cooled to 50 °C under O2, and purged
with Ar at 50 °C for 30 min and stabilized under 10% H2/Ar at 50 °C for 1 h, and then the temperature was increased
in a linear course to collect H2-TPR curves. The influence
of prereduction on the TPR behavior of pure CeO2 was assessed
by collecting H2-TPR curves after reduction with 10% H2/Ar at 450 °C for 1 h followed by re-oxidation with 10%
O2/He at 100 °C for 1 h. Similarly, the influence
of prereduction on the TPR behavior of Pt/CeO2 was studied
by collecting H2-TPR curves after reduction with 10% H2/Ar at 350 °C for 1 h followed by re-oxidation with 10%
O2/He at 350 °C for 1 h. To confirm that the change
in the oxidation state of Pt was not the only cause for the improved
H2 consumption rate following prereduction, Pt(2)/CeO2 was ex situ reduced with 10% H2/Ar at 400 °C
for 1 h, diluted with pure CeO2, and then re-oxidized in
situ with 10% O2/He at 350 °C for 1 h. The amount
of H2 consumed during the TPR runs was estimated by integrating
the TCD signals.
(H2-TPR) curves
were obtained with 0.03 g of the sample using an Autochem II (Micromeritics)
equipped with a thermal conductivity detector (TCD). Typically, samples
were oxidized with 10% O2/He at 400 °C for 1 h to
remove impurities, cooled to 50 °C under O2, and purged
with Ar at 50 °C for 30 min and stabilized under 10% H2/Ar at 50 °C for 1 h, and then the temperature was increased
in a linear course to collect H2-TPR curves. The influence
of prereduction on the TPR behavior of pure CeO2 was assessed
by collecting H2-TPR curves after reduction with 10% H2/Ar at 450 °C for 1 h followed by re-oxidation with 10%
O2/He at 100 °C for 1 h. Similarly, the influence
of prereduction on the TPR behavior of Pt/CeO2 was studied
by collecting H2-TPR curves after reduction with 10% H2/Ar at 350 °C for 1 h followed by re-oxidation with 10%
O2/He at 350 °C for 1 h. To confirm that the change
in the oxidation state of Pt was not the only cause for the improved
H2 consumption rate following prereduction, Pt(2)/CeO2 was ex situ reduced with 10% H2/Ar at 400 °C
for 1 h, diluted with pure CeO2, and then re-oxidized in
situ with 10% O2/He at 350 °C for 1 h. The amount
of H2 consumed during the TPR runs was estimated by integrating
the TCD signals.
9
Hydrogen Temperature-Programmed Reduction
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The reduction of the as-prepared
samples was analyzed by H2-TPR using a Micromeritics AutoChem
II setup equipped with a thermal
conductivity detector (TCD). Typically, about 100 mg of the sample
was loaded into a quartz U-tube between two quartz wool layers. The
sample was pretreated in a He flow (50 mL/min) at 120 °C for
1 h before the measurements. The TPR profile was recorded by heating
the sample from 40 to 800 °C at a 10 °C/min rate in a 4
vol % H2 in He flow (50 mL/min). H2 consumption
was monitored with a thermal conductivity detector (TCD). H2 consumption was determined by integrating the area under the H2-TPR profile in a specific temperature range, and this area
was compared to a reference H2-TPR experiment in which
a known amount of CuO was reduced, assuming the complete reduction
of all Cu2+ to Cu(0).
samples was analyzed by H2-TPR using a Micromeritics AutoChem
II setup equipped with a thermal
conductivity detector (TCD). Typically, about 100 mg of the sample
was loaded into a quartz U-tube between two quartz wool layers. The
sample was pretreated in a He flow (50 mL/min) at 120 °C for
1 h before the measurements. The TPR profile was recorded by heating
the sample from 40 to 800 °C at a 10 °C/min rate in a 4
vol % H2 in He flow (50 mL/min). H2 consumption
was monitored with a thermal conductivity detector (TCD). H2 consumption was determined by integrating the area under the H2-TPR profile in a specific temperature range, and this area
was compared to a reference H2-TPR experiment in which
a known amount of CuO was reduced, assuming the complete reduction
of all Cu2+ to Cu(0).
10
Comprehensive Characterization of Catalytic Materials
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TPR experiments (ca. 45 mg of sample) were performed on a Micromeritics Autochem II within a temperature range of 60–900 °C (10 °C/min heating rate) under flowing (50 mL/min) 10%H2/Ar. The specific surface areas of the samples were obtained by adsorption–desorption of N2 at 77 K on a Micromeritics ASAP 2020 following the multi-point Brunauer–Emmett–Teller (BET) method. The samples were previously degassed at 300 °C under vacuum for 100 min. Powder XRD analyses were carried out on a Rigaku UltimaIV diffractometer employing CuKα radiation and a scanning rate of 2°/min. SEM observations were carried out on a Hitachi S5200 microscope, and samples were used without any further modification. Inductively coupled plasma atomic emission spectroscopy (ICP–AES) was used to determine the actual oxide content of the different samples. This measurement was made on a Varian Vista AX spectrometer, and samples were previously dissolved in 5 mL of aqua regia (HNO3:HCl, 1:3 in volume).
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