A high-pressure fiber-optic light-scattering spectrometer has been constructed for in situ observation of molecular dissolution/association as well as the polymerization process in supercritical fluids. Single (or multiple) fiber-optic probes, each comprised of a single optical fiber (or multiple optical fibers) and a graded index microlens, are used to transmit the incident laser beam and to receive the scattered light as well as the transmitted light from the high pressure cell. The direct immersion in the scattering medium of the fiber-optic probes makes the spectrometer more compact and more flexible with an easier alignment process. With the miniaturization and flexibility, our high-pressure light-scattering cell can be transported and adapted in combination with other physical techniques, such as synchrotron small angle x-ray scattering which requires a different set of windows (e.g., made of diamond) suitable for x-ray transmissions. This spectrometer has been successfully used for the in situ study of the molecular association behavior of a diblock copolymer of 1,1-dihydroperfluorooctylacrylate and vinyl acetate in supercritical carbon dioxide under pressures up to 552 bar.
A fiber-optic probe employing two monomode optical fibers, one for transmitting a Gaussian laser beam to the scattering volume and the second, positioned at some backscatter angle, for receiving the scattered light is described. Performance and suitability of the system for a process control environment is assessed by studying a suspension of polystyrene latex particles over a wide range of sizes and concentrations. The results show that the probe is ideal for a process control environment in industrial and laboratory applications. Particle size is recovered, without any additional corrections for multiple light scattering, in concentrations containing up to 10% solids of 39-nm polystyrene latex spheres.
Cylindrical capillaries can be used as optical elements in a waveguide, where refraction will confine an appropriately focused light beam to pass through the interiors of successive capillaries in a flat parallel array. Such a capillary waveguide allows efficient illumination of samples in multiple capillaries with relatively little laser power. Analytical expressions derived under paraxial and thin-lens approximations provide guidance in selecting the capillary sizes and the refractive indices that will produce the waveguiding effect, but accurate predictions require exact ray tracing. Small reflective losses as the light passes through the capillary surfaces cause cumulative intensity decreases, but the resulting lack of uniformity can be compensated to a considerable extent by illuminating the capillary array from both sides. A 12-capillary waveguide illuminated from both sides in air has a difference of less than 10% from the strongest to the weakest illumination. By increasing the refractive index of both the external medium and the contents of the capillaries, a 96-capillary waveguide for DNA sequencing could be produced that would also provide nearly uniform illumination. A 12-capillary, bi-directionally illuminated waveguide system for DNA sequencing has been constructed. The two focused laser beams are delivered by integrated fiber optic transmitters (IFOTs), and fluorescence is collected by a set of optical fibers whose spacing exactly matches that of the capillaries in the waveguide. The system is easy to align and provides sensitive detection of fluorescence with minimal cross-talk between channels.
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