PubMed · 14101592
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A R ROGERS. 1963. AN ACCELERATED STORAGE TEST WITH PROGRAMMED TEMPERATURE RISE.. https://doi.org/10.1111/j.2042-7158.1963.tb11194.x
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This paper illustrates the application of a combined discrete- and finite-element simulation to the compaction of assemblies comprising both ductile and brittle particles. Through case studies, the results demonstrate the importance of using a fine mesh on the particle boundary, the effect of fragmentation and its impact on the form of the compression curve, and the effect of inclusion of ductile particles at ca. 25% by volume suppressing brittle failure mechanisms. Although, the calculations can be extended to three dimensions, the computational cost is a current limitation on such calculations. The novelty of this approach is in its ability to predict material yield surfaces for the compaction of a mixture of particles. The initial results are optimistic, but there is a need for model improvement, principally through the ability to capture the random packing of irregular particles since this will eliminate a key problem in defining an initial density for the simulation. The main advantage of this technology is in its ability to minimize the need for expensive triaxial testing of samples to develop the yield-surface history.
The objectives of this work were to develop a robust procedure for assessing powder flow using a commercial avalanche testing instrument and to define the limits of its performance. To achieve this a series of powdered pharmaceutical excipients with a wide range of flow properties was characterized using such an instrument (Aeroflow, TSI Inc., St. Paul, MN, USA). The experimental conditions (e.g., sample size, rotation speed) were rationally selected and systematically evaluated so that an optimal standard-operating-procedure could be identified. To evaluate the inherent variability of the proposed methodology samples were tested at multiple sites, using different instruments and operators. The ranking of the flow properties of the powders obtained was also compared with that obtained using a conventional shear-cell test. As a result of these experiments a quick, simple, and rugged procedure for determining the flow properties of pharmaceutical powders in their dilated state was developed. This procedure gave comparable results when performed at four different testing sites and was able to reproducibly rank the flow properties of a series of common pharmaceutical excipient powders. The limits of the test method to discriminate between different powder samples were determined, and a positive correlation with the results of a benchmark method (the simplified shear cell) was obtained.
In order to develop a radiopharmaceutical for hepatobiliary scintigraphy with better hepatobiliary properties new ligand for complexation of 99mTc, 4-iodo-2,6-dimethylphenylcarbamoylmethyl iminodiacetic acid (METHYLIODIDA), was synthesized. Acid-base equilibria of METHYLIODIDA were studied potentiometrically, because these data are important for determination of complex formation conditions. It was established that METHYLIODIDA undergoes a complex acid-base equilibrium due to its zwitterionic nature and four proton-binding sites. The stoichiometric ionization constants were determined at 25 degrees C and constant ionic strength 0.1M (NaClO(4)): pK1=1.7+/-0.1; pK2=2.44+/-0.07; pK3=6.29+/-0.02 and pK4=10.91+/-0.06, respectively.