RESUMO
Controlling production online is an important issue for chemical companies. Visible and near-infrared (NIR) spectroscopy offers a number of important advantages for process monitoring, and has been used since the 1980s. For complex media such as silica precipitation samples, it is interesting to be able to study independently the scattering and absorption effects. From the scattering coefficient it is possible to extract information on the physical structure of the medium. In this work, the physical changes were monitored during a silica precipitation reaction by simple measurement of collimated transmittance NIR spectra. It is shown that it is possible to differentiate samples before and after the gel point, which is a key parameter for monitoring the process. From these NIR spectra the scattering coefficients were simply extracted, allowing a global vision of the physical changes in the medium. Then principal component analysis of the spectra allowed refinement of the understanding of the scattering effects, in combination with particle size monitoring.
RESUMO
In order to analyze light hydrocarbons mixtures with silica monolithic columns, a conventional gas chromatograph was modified to work with carrier gas pressure as high as 60bar. To understand hydrodynamic flow and retention with short columns (less than 30cm), special attention was required due to the temperature difference between the oven area and the FID detector which contain a significant length of the column. Efficiency and selectivity using various carrier gases (helium, nitrogen and carbon dioxide) at different inlet pressure for different oven temperature were studied. Carrier gas nature was a very significant parameter: on one side, linked to adsorption mechanism for gases like nitrogen and carbon dioxide onto the stationary phase modifying retention and selectivity, on the other side in relation to the minimum theoretical plate height which was as low as 15µm (66 000 platem(-1)) using carbon dioxide as carrier gas. The chromatographic system was then used to separate methane, ethane, ethylene, acetylene, propane, cyclopropane, and butane in less than 30s.
