Controlled destruction of residual crosslinker in a silicone elastomer for drug delivery

In drug delivery systems that use silicone elastomers as a diffusion matrix for the active drug, it is common to crosslink the material by the hydrosilylation reaction. In this platinum‐catalyzed reaction, vinyl groups on a polymer add to the methyl siloxane hydride (MHS) groups on a low molecular mass crosslinker. With an excess of crosslinker, a fast curing is achieved and a fully crosslinked material is formed. Unreacted MHS groups were shown to remain in the elastomer after curing because of the excess crosslinker. In this work, a simple procedure was developed to eliminate the unreacted MHS groups from the final product. We found that storage of the product at +40°C and 75% relative humidity for a few weeks will effectively destroy the residual MHS groups in the elastomer. The effects of varying levels of humidity, oxygen, and temperature on this postcuring procedure were studied. The amount of MHS groups was measured with NMR and IR spectroscopy. We also found that the hardness of the material increased by approximately 25% as a consequence of this postcuring treatment. This increase is probably due to a secondary crosslinking reaction between MHS and silanol groups. Heat treatment at higher temperatures led to an even further increase in the hardness and compression modulus. Because no MHS groups remained in the elastomer when this heat treatment was started, it is apparent that another secondary crosslinking reaction is occurring, probably silanol condensation. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 84: 2254–2264, 2002     

The effect of synthesis gas composition on the Fischer–Tropsch synthesis over Co/γ-Al2O3 and Co–Re/γ-Al2O3 catalysts

The Fischer–Tropsch synthesis over Co/γ-Al₂O₃ and Co–Re/γ-Al₂O₃ was investigated in a fixed-bed reactor at 20 bar and 483 K using feed gases with molar H₂/CO ratios of 2.1, 1.5 and 1.0 simulating synthesis gas derived from biomass. With lower H₂/CO ratios in the feed, the CO conversion and the CH₄ selectivity decreased, while the C₅₊ selectivity and olefin/paraffin ratio for C₂–C₄ increased slightly. The water–gas shift activity was low for both catalysts, resulting in high molar usage ratios of H₂/CO (close to 2.0), even at the lower inlet ratios (i.e. 1.5 and 1.0). For both catalysts, the drop in the production rate of hydrocarbons when shifting from an inlet ratio of 2.1 to 1.5 was significant mainly because the H₂/CO usage ratio did not follow the change in the inlet ratio. The hydrocarbon selectivities were rather similar for inlet H₂/CO ratios of 2.1 and 1.5, while significantly deviating from those for an inlet ratio of 1.0. With the studied catalysts, it is possible to utilize the advantages of an inlet ratio of 1.0 (higher selectivity to C₅₊, lower selectivity to CH₄, no water–gas shifting of the bio-syngas needed prior to the FT reactor) if a low syngas conversion is accepted.     

Near Wall Studies of Pulp Suspension Flow Using LDA

A detailed study of the flow behaviour in the near wall region of pulp suspensions up to 4.7% have been performed using Laser Doppler Anemometry (LDA) in pipe flow. Axial mean velocity profiles show a distinct plug flow and an increase of the plug region as the flow rate decreases and fibre concentration increases. An attempt is made to relate the LDA data‐rate to fibre concentration, which indicates a dilution region at 1‐2 mm from the wall that is larger than the annulus region. The dilution region increases with increasing flow rate, decreasing concentration and when using longer pulp fibres.     

Oxidative dehydrogenation of ethane on Pt–Sn impregnated monoliths

The oxidative dehydrogenation of ethane was studied over Pt–Sn impregnated monoliths at 1 bar, 600–900 °C and with different contents of oxygen, hydrogen and steam in the feed gas. As expected a decrease in oxygen in the feed led to a decrease in the conversion of ethane due to lower temperatures in the reactor. Adding steam to the feed showed no effect on the ethane conversion or the ethene selectivity. When the hydrogen/ethane ratio in the feed was varied from 0 to 0.5 at 700 and 850 °C, it resulted in a significant increase in the selectivity to ethene while the ethane conversion remained relatively unchanged. At 700 °C the selectivity increased from about 50% to 93% (carbon basis) with only a small decrease in the conversion of ethane. The results clearly show that both Pt and Sn have a catalytic effect. Pt caused the ethane conversion to rise and addition of Sn resulted in much better ethene selectivity. However, even though Sn alone showed some catalytic effect at lower temperatures, it cannot explain the great difference between the Pt and Pt–Sn catalysts. A reasonable assumption is therefore that there exist interactions between Pt and Sn that gives the Pt–Sn catalysts excellent properties for oxidative dehydrogenation of ethane, in particular upon addition of hydrogen.     

Small-scale hydrogen production from propane

Partial oxidation and oxidative steam reforming of propane were investigated over 0.01 wt.% Rh/Al₂O₃ foam catalysts. High selectivity to hydrogen was obtained for both reactions, but addition of steam to the reactant mixture gave higher selectivity to hydrogen. Stability tests over 7 h revealed that the catalytic activity of Rh was quite stable under partial oxidation conditions. Higher loss in Rh activity was observed when steam was present in the reactant mixture. FE-SEM images showed that Rh particle size and distribution are modified under partial oxidation and oxidative steam reforming conditions. However, these changes were more distinct on the catalyst used for oxidative steam reforming.     

Rheological and extrusion characteristics of glass fiber-reinforced polycarbonate

An experimental investigation of the rheological properties of glass fiber-reinforced polycarbonate melts and the extrusion of such compounds through capillary and slit dies is presented. The viscosity–shear rate function seems independent of instrument for cone-plate and capillary investigations. The presence of fibers increases the level of the viscosity. Normal stresses at fixed shear stress are also increased by the presence of fibers. The extrudate swell is decreased by the presence of fibers and surface roughness is increased. Fiber orientation increases and surface roughness decreases with increasing extrusion rate.     

Comparison of different flowability tests for powders for inhalation

A series of placebo powders for inhalation was characterized regarding bulk density and powder flowability using different techniques. The powders were of the ordered mixture type and were prepared by mixing a pharmaceutical carrier grade of lactose with different fractions of intermediate sized and fine (i.e., micronized) lactose. A modified Hausner Ratio was obtained by measurement of the poured and the compressed bulk densities. Other tests investigated were the angle of repose, the avalanching behaviour using the AeroFlow, and the yield strength using the Uniaxial tester. Furthermore, the relation between ordered mixture composition and flowability was examined.Of the methods investigated, the modified Hausner Ratio discriminates well between the investigated powders and seems to have the widest measuring range. It was also found that the poured and compressed bulk densities provide information about the packing of the particles in the powders. A good correlation was obtained between the modified Hausner Ratio and the angle of repose. The AeroFlow was suitable for powders with a low percentage of fine particles, but could not discriminate between the more cohesive powders. The Uniaxial tester, on the other hand, seems to be better suited for more cohesive powders.Regarding the powder composition, addition of micronized particles has a strong influence on the flowability of ordered mixtures, while intermediate sized particles have little impact on the powder flow.     

Single-stage flowing liquid film impactor for continuous on-line particle analysis

A single-stage “wet impactor” is presented, where the impaction occurs on a regenerated water surface. The developed impactor is equipped with an impaction liquid support plate of etched glass and a drain spout providing a continuous liquid flow covering the impaction area. Subsequent transport of the impaction liquid makes an on-line determination possible. With multiple nozzles (74 holes, 0.3 mm i.d.) and an air flow of 101/min the cut-off was determined to 0.41 ± 0.02 μm. The impactor was also investigated for its particle loss. The cut-off function, regarding the consequences of letting impaction occur in a liquid film is discussed and compared to conventional impactors. The analysis technique was tested in an ambient air measurement study with an ion chromatograph attached to the sampling system.