Deactivation
of catalysts due to rapid blocking of active surfaces
and pores is a major problem for methane cracking. The removal of
the template using different calcination methods contributes to the
different characteristics of catalyst support. Therefore, silica supports
were prepared with the sol–gel method, where sodium silicate
and chitosan are a silica source and a template, respectively. Calcination
using a microwave muffle furnace (MWF) was preferred over the conventional
electric muffle furnace at the heating rates of 2 and 17 °C/min
(CEF2 and CEF17, respectively) in order to remove the chitosan template.
A nickel nitrate precursor was loaded onto the obtained silica supports
by the incipient wetness impregnation method. The properties of the
silica support and the Ni/SiO2 catalysts were characterized
by means of N2-sorption, X-ray diffraction, scanning electron
microscopy–energy-dispersive X-ray, field emission transmission
electron microscopy, and H2 temperature-programmed reduction.
The catalytic activity was evaluated using a fixed-bed reactor at
550 °C with a CH4/N2 ratio of 1:4 in the
feed. The amount and the allotropes of carbon deposited on the spent
catalysts were investigated using thermogravimetric/differential thermal
analysis. The results showed that the SiO2-MWF support
had a higher surface area and a larger pore volume of a mesoporous
structure with larger interparticle channels than that of the SiO2-CEF supports. This leads to the higher dispersion of Ni metal
particles over and inside the interparticle channels of the SiO2-MWF support. This provided a higher metal–support
interaction, resulting in lower rates of methane conversion and carbon
deposition on the catalyst surface than those of Ni/SiO2-CEF catalysts. However, it displayed a lower bed pressure. It was
found that the carbon fibers deposited on all the catalysts were multiwalled
carbon nanotubes (MWCNTs). Additionally, the base-growth mechanism
of MWCNTs was only exhibited by the Ni/SiO2-MWF catalyst.
A simple flow injection with flame photometric detection has been developed for determination of sodium, potassium, and total alkalies in portland cement, fly ash, admixtures, and water of concrete. A liquid sample or a digest of solid sample was injected into a water carrier stream which flowed to a flame photometer. A change in emission intensity at a selected wavelength was recorded as a peak. An amplifier circuit was fabricated, which helped improve sensitivity of the flame photometer. Calibration graphs in the range of 0.05–1.0 mg L−1 and 1.0–20.0 mg L−1 were obtained with a detection limit of 0.02 mg L−1, for both potassium and sodium determination. Relative standard deviations for 11 replicates of injecting of 10 mg L−1 potassium and sodium solutions were 1.69 and 1.79%, respectively. Sample throughput of 120 h−1 was achieved. The proposed method was successfully applied to portland cement, fly ash, admixtures, and water samples validated by the ASTM standard method and certified reference materials of portland cement.
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