A laboratory test setup for in situ measurements of the dielectric properties of catalyst powder samples under reaction conditions by microwave cavity perturbation: Set up and initial tests

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Abstract

The catalytic behavior of zeolite catalysts for the ammonia-based selective catalytic reduction (SCR) of nitrogen oxides (NOX) depends strongly on the type of zeolite material. An essential precondition for SCR is a previous ammonia gas adsorption that occurs on acidic sites of the zeolite. In order to understand and develop SCR active materials, it is crucial to know the amount of sorbed ammonia under reaction conditions. To support classical temperature-programmed desorption (TPD) experiments, a correlation of the dielectric properties with the catalytic properties and the ammonia sorption under reaction conditions appears promising. In this work, a laboratory test setup, which enables direct measurements of the dielectric properties of catalytic powder samples under a defined gas atmosphere and temperature by microwave cavity perturbation, has been developed. Based on previous investigations and computational simulations, a resonator cavity and a heating system were designed, installed and characterized. The resonator cavity is designed to operate in its TM010 mode at 1.2 GHz. The first measurement of the ammonia loading of an H-ZSM-5 zeolite confirmed the operating performance of the test setup at constant temperatures of up to 300 °C. It showed how both real and imaginary parts of the relative complex permittivity are strongly correlated with the mass of stored ammonia.

Figures

  • Figure 1. Schematic setup of the developed test bench including the sample tube, the double-walled and evacuated tube, the sealing mechanism, the resonator with waveguide extensions, loop antennas and two thermocouples. The gas heater, the Fourier transform infrared (FTIR) gas analyzer and the network analyzer (all external components) are not shown.
  • Figure 2. Absolute value of the transmission parameter S21 between 1 and 3 GHz: measurement (black) and simulation (red) (a). The simulated electric (red: High and blue: Zero) and magnetic (white arrows) field distribution of the TM010 mode (b).
  • Figure 3. Thermal simulation model of the heating mechanism: Scheme of the model (a) and temperature distribution of a simulation (b).
  • Figure 4. Results of the heating simulation: temperature of the sample as a function of the heating gas inlet temperature and the heating gas flow. The red line indicates the expected temperature using the available heating system.
  • Figure 5. Results of the heating tests with and without resonator and preheating.
  • Figure 6. Temperature distribution inside the sample tube along its axis at a heating gas temperature of 430 °C. The sample tube is enclosed by the resonator in the gray area.
  • Table 1. Influence of the heating on the microwave measurement: heating gas temperature, frequency shift and quality factor. The resonator temperature is calculated from the frequency shift.
  • Figure 7. First measurement with the test setup: Upstream (inlet) and downstream (outlet) ammonia concentration (a), calculated stored amount of ammonia (b), resonance frequency and unloaded quality factor of the TM010 mode (c) and calculated effective values of the complex permittivity (d).

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CITATION STYLE

APA

Dietrich, M., Rauch, D., Porch, A., & Moos, R. (2014). A laboratory test setup for in situ measurements of the dielectric properties of catalyst powder samples under reaction conditions by microwave cavity perturbation: Set up and initial tests. Sensors (Switzerland), 14(9), 16856–16868. https://doi.org/10.3390/s140916856

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