We describe the design and operation of a modified commercial rheometer to simultaneously perform rheological measurements and structural studies by small angle neutron scattering (SANS). The apparatus uses a Couette geometry shear cell allowing two of the three scattering planes to be observed by performing experiments in either the radial or tangential geometries. The device enables small angle neutron scattering patterns to be obtained simultaneously with a wide variety of rheological measurements such as stress/strain flow curves, oscillatory deformations, and creep, recovery and relaxation tests, from -20 °C to 150 °C, for samples with viscosities varying by several orders of magnitude. We give a brief report of recent experiments performed on a dispersion of acicular nanoparticles and biopolymer network under stress demonstrating the utility of such measurements. This device has been developed at the National Institute of Standards and Technology's Center for Neutron Research (NCNR) and made available to the complex fluids community as part of the standard sample environment equipment.
Liquid crystal lipid-based formulations are an effective approach to prolong pharmacokinetics and reduce burst release of a drug on subcutaneous delivery. The objective of this paper was to investigate the influence of phase structures of a lipid-based liquid crystal delivery system and its associated mechanical properties on the release profile of a peptide. It was hypothesized that release of drug molecules are closely related to the mechanical properties that are controlled by phase structures. Experimentally, the relationship between phase structures of lipid liquid crystal system-soy phosphatidyl choline (SPC) and glycerol dioleate (GDO) in water were characterized by polarized light microscopy and small angle X-ray diffraction. Their rheological properties were evaluated with a rheometer and the in vitro release of the peptide as a measure drug release from the LC-depot injection. Three phases: disordered phase, lamellar phase, mixtures of cubic, lamellar, and hexagonal phases were detected by varying formulation compositions. A significant difference in rheological behavior was observed. The disordered phase displayed some attributes of typical Newtonian fluid with lowest viscosity while the lamellar phase showed a shear thinning behavior. Regarding the mechanical strength, the lamellar phase presents the highest storage modulus due to its layer structure followed by mixed phases. Comparing release profiles, the lamellar phase produced a fast release followed by the mixture of phases. In conclusion, this study demonstrates the ability to characterize LC phase structures with microscopy, small angle X-ray diffraction, and rheological measurements and their link to modulating a peptide release profile.
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