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Online characterization of particle based reactions by laser backscattering Open Access


Other title
In-situ particle characterization
Laser backscattering
Diffuse wave spectroscopy
High Temperature
Online particle reaction sizing
Type of item
Degree grantor
University of Alberta
Author or creator
Medina Messina, Miguel A
Supervisor and department
McCaffrey, William C (Chemical and Materials Engineering)
Examining committee member and department
Gupta, Manisha (Electrical and Computer Engineering)
Gupta, Rajender (Chemical and Materials Engineering)
Rajendran, Arvind (Chemical and Materials Engineering)
Department of Chemical and Materials Engineering
Chemical Engineering
Date accepted
Graduation date
2016-06:Fall 2016
Master of Science
Degree level
A fiber optic dynamic light scattering device was successfully developed for the in-situ characterization of particle size in turbid media. Currently available techniques are only capable of performing characterizations at room temperature and are highly limited by the turbidity of the sample. In-situ particle size characterization was accomplished using the diffuse wave spectroscopy theory and time-dependent autocorrelation analysis. Using this basis for the interpretation, information regarding the particle morphology was obtained from the backscattering signals using two simultaneous lasers, of 532 and 655nm wavelength, at elevated pressures up to 5 MPa, and at temperatures up to 420 °C. Validation of the analytical technique was achieved by studying a stable particulate dispersion of Carbon Lampblack (CB) in water and 1-methylnaphthalene. The 162 nm average particle size of the dispersion was characterized ex-situ with transmission electron microscopy and a commercial laser diffraction apparatus. The average particle size obtained by this technique was 275±39 nm at room temperature and 216±23 nm at 280 °C, showing a good agreement compared with the ex-situ values. Ultimately, the goal of this work is to develop a technique capable to track on-line the size and concentration of nanoscale particles. For this purpose, sulfidation reaction of iron naphthenate was selected to study the in-situ generation of iron based nanoparticles. Particles of 202±33 nm average size were characterized by this technique, finding good agreement with ex-situ characterization of the collected reaction products. Further study of this reaction with the developed technique allowed to determine the temperature on-set for the particle generation at 274.6±0.7 °C. While simultaneous determination of particle size and concentration was not possible in this work, several modifications of the current design are presented in the end of this manuscript aiming to solve the issues encountered during this work.
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