Crystal structures of Ni–Fe nanoparticles were analyzed with the X-ray diffraction (XRD) method. Stoe theta/2theta diffractometer in Bragg–Brentano geometry with Cu K Kα1/2 radiation was used to obtain XRD diagrams. Since surface area and porosity of the catalyst are essential parameters to correlate with catalytic performance, Ni–Fe particles were examined with N2 sorption with 3Flex Micrometrics at 77 K. Samples were degassed at 150 °C for 10 h before the measurement. Brunauer–Emmett–Teller (BET) surface areas were determined from the relative pressure range between 0.06 and 0.2. Transmission electron microscopy (TEM) images of samples were taken at 100 kV with Hitachi H-7100 electron microscope. High-resolution TEM (HRTEM) and scanning electron microscopy (SEM) images were obtained with HF-2000 and Hitachi S-5500 microscopes, respectively. Thermogravimetric analysis-mass spectroscopy (TG-MS) was performed in order to analyze possible carbon contamination in the catalyst under synthetic air until 900 °C with 10 K/min heating rate. TG-MS result was obtained with Netzsch STA 449 F3 Jupiter connected to QMS 403D (Netzsch) mass spectrometer.
Qms 403d
Manufactured by Netzsch
The QMS 403D is a compact and robust quadrupole mass spectrometer designed for analytical applications. It features a high-performance mass analyzer and a sensitive detector to provide accurate and reliable mass analysis. The core function of the QMS 403D is to measure the mass-to-charge ratio of ionized molecules or atoms in a sample, enabling the identification and quantification of chemical species.
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3 protocols using qms 403d
1
Characterization of Ni-Fe Nanoparticles
2
Thermal Analysis and Mass Spectrometry
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Thermal analysis and differential scanning calorimetry (TG/DSC)
were
carried out with a Netzsch Jupiter F449 system being combined with
MS (mass spectroscopy) for the simultaneous analysis of gaseous compounds
being released during TG/DSC measurements. A heating rate of 10 K/min
was preselected for the heating regime, which was set to a maximum
temperature of 1250 °C. The Proteus software 6.1 by Netzsch was
used to evaluate the recorded data.
Parallel to the TG/DSC measurement,
mass spectra of the gaseous emissions were also simultaneously recorded
during heating with a quadrupole mass spectrometer QMS 403 D Aëolos
from Netzsch. The maximum atom mass units (amu) of the ion key fragments
were set to 100 in the MS operating Quadstar software, i.e. a range
from 1 to 100 amu was covered with 0.5 s as detection time for each
mass. Hence, 145 cycles were recorded during the 2 h heating regime
with a channeltron-type detector featuring a SEM (second electron
multiplier) voltage of 1.2 kV.
were
carried out with a Netzsch Jupiter F449 system being combined with
MS (mass spectroscopy) for the simultaneous analysis of gaseous compounds
being released during TG/DSC measurements. A heating rate of 10 K/min
was preselected for the heating regime, which was set to a maximum
temperature of 1250 °C. The Proteus software 6.1 by Netzsch was
used to evaluate the recorded data.
Parallel to the TG/DSC measurement,
mass spectra of the gaseous emissions were also simultaneously recorded
during heating with a quadrupole mass spectrometer QMS 403 D Aëolos
from Netzsch. The maximum atom mass units (amu) of the ion key fragments
were set to 100 in the MS operating Quadstar software, i.e. a range
from 1 to 100 amu was covered with 0.5 s as detection time for each
mass. Hence, 145 cycles were recorded during the 2 h heating regime
with a channeltron-type detector featuring a SEM (second electron
multiplier) voltage of 1.2 kV.
3
Thermogravimetric and Calorimetric Analysis
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Thermogravimetric analysis (TGA) coupled differential scanning calorimetry (DSC) was performed using Netzsch STA449 F1 at 20 °C min -1 , using argon as the purge gas. The gases evolved were analyzed by Fourier transform infrared spectroscopy using Bruker Tensor 37 (liquid nitrogen cooled) and mass spectroscopy using Netzsch QMS 403D. Samples were heated from 40 °C to 800 °C, a blank run was performed and subtracted from the sample run to compensate for thermally induced mass drift.
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