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     

AN EXPERIMENTAL EVALUATION OF THE GOVERNING MOISTURE MOVEMENT PHENOMENA IN THE PAPER COATING PROCESS. I. THEORETICAL ASPECTS

The most important issue when coating paper is the modelling of the moisture movement in the coating process, since the water movement pattern is strongly connected to binder movement and the final structure of fibres and coating colour, which in turn affects the final printing properties of the paper. Therefore, we are now studying a novel laboratory method to determine the dynamic water movement in a hygroscopic porous media, i.e. the liquid movement in the paper coating process. The experimentally determined physical properties yield information relevant to the mass and energy balances of a real paper coating process. We have also studied the widely used Lucas-Washburn capillary suction theory in combination with the build-up of a filter-cake in the coating colour. The study shows, that the water loss from the coating colour into a hygroscopic material can be well explained by applying vapour diffusion into the base paper as the governing mass transfer mechanism.     

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.     

An analysis of the use of electrical power measurements for process control in large‐scale stirred vessels

The mechanical power that is transferred to a liquid via the shaft of an agitator is obtained from a measurement of the electrical power flowing into the electric motor within an accuracy of less than 5%. The accuracy obtained is limited by the calibration procedure. As the implementation of an electric power measurement is both simple and comparatively inexpensive, the technique is suitable for a continuous monitoring of the power used by agitators in the process industries.     

Influence of seed polymer molecular weight on polymerization kinetics and particle morphology of structured styrene–butadiene latexes

Heterogeneous film‐forming latexes were prepared using two‐stage, seeded emulsion polymerization. The polymerization was performed in a calorimetric reactor with a control unit that monitored the reaction rate and controlled the charging rate of the monomers. Three types of styrene seed latexes were prepared at 70°C. The first was an unmodified polystyrene (PS) latex. The second had the molecular weight lowered by the use of carbon tetrachloride (CCl₄) as a chain‐transfer agent, added at the start of the polymerization. For the third one, divinylbenzene (DVB) was used as a comonomer. DVB was added under starved conditions near the end of the polymerization to achieve crosslinked particle shells and to introduce double bonds as possible grafting sites. The second polymerization step was performed at 80°C as a batch operation in a 200‐mL calorimeter reactor. The second‐stage polymer was poly(styrene‐co‐butadiene‐co‐methacrylic acid) (S/B/MAA). A fixed S/B ratio was used together with varying small amounts of MAA. Particle morphology and particle‐size distributions were examined after the second stage using TEM after staining with osmium tetroxide. The particle morphology was found to depend on both the seed composition and the amount of MAA used in the second stage. Molecular weight and crosslinking of the DVB‐containing seed influenced the internal particle viscosity, which gave differences in the polymerization rate and the particle morphology. Crosslinking of the second‐stage polymer decreased the monomer concentration in the particles, which could be detected as a change in the slope the pressure/conversion curve. This phenomenon was used to indicate the critical conversion for crosslinking of the second‐stage polymer. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 77: 297–311, 2000     

The influence of thermal annealing on residual stresses and mechanical properties of arc-evaporated TiCxN1−x (x=0, 0.15 and 0.45) thin films

We report the stress relaxation behavior of arc-evaporated TiC_xN_1−x thin films during isothermal annealing between 350 and 900°C. Films with x=0, 0.15, and 0.45, each having an initial compressive intrinsic stress σ_int=−5.4 GPa, were deposited by varying the substrate bias V_s and the gas composition. Annealing above the deposition temperature leads to a steep decrease in the magnitude of σ_int to a saturation stress value, which is a function of the annealing temperature. The corresponding apparent activation energies for stress relaxation are E_a=2.4, 2.9, and 3.1 eV, for x=0, 0.15, and 0.45, respectively. TiC_0.45N_0.55 films with a lower initial stress σ_int=−3 GPa, obtained using a high substrate bias, show a higher activation energy E_a=4.2 eV. In all the films, stress relaxation is accompanied by a decrease in defect density indicated by the decreased width of X-ray diffraction peaks and decreased strain contrast in transmission electron micrographs. Correlation of these results with film hardness and microstructure measurements indicates that the stress relaxation is a result of point-defect annihilation taking place both during short-lived metal-ion surface collision cascades during deposition, and during post-deposition annealing by thermally activated processes. The difference in E_a for the films of the same composition deposited at different V_s suggests the existence of different types of point-defect configurations and recombination mechanisms.     

Welding of stainless steels. Duplex and superduplex steels

In the pulsed MAG welding with highly precise periodic drop transfer, welding current was analysed by fast Fourier transform (FFT). By this analysis, peculiar frequency of the molten pool was detected by resonance phenomena with the base plate vibration and it was confirmed that peculiar frequency falls according to growth of the molten pool. Furthermore, natural frequency was detected at the natural welding state that is without vibration of the base plate and confirmed by the resonance method with the base plate vibration. To amplify natural vibration of the molten pool, drop transfer pulse was modulated consisting of regular pulse peak current and higher pulse peak current. The higher pulse peak current makes a change in the arc pressure and the molten pool is pushed down in the period of higher pulse. Because short circuit is apt to occur at the time that the molten pool is at the top of the front side, so it is effective for amplifying the molten pool oscillation that higher pulse phase begins at this time instantaneously or somewhat later. According to this, higher peak was gained at peculiar frequency by FFT analysis. It means that amplifying of the molten pool oscillation was successful. Appropriate period of higher pulse for maintaining stable oscillation is from about 1/4 to 1/2 of the oscillation cycle.     

Exploring agile values in method configuration

The Method for Method Configuration (MMC) has been proposed as a method engineering approach to tailoring information systems development methods. This meta-method has been used on a variety of methods, but none of these studies have focused on the ability to manage method tailoring with the intention to promote specific values and goals, such as agile ones. This paper explores how MMC has been used during three software development projects to manage method tailoring with the intention to promote agile goals and values. Through content examples of method configurations we have shown that it is possible to use MMC and its conceptual framework on eXtreme Programming and we report on lessons learned with regard to maintaining coherency with the overall goals of the original method.     

Assessing plastically dissipated energy as a condition for fatigue crack growth

The suitability of using a proposed condition for simulating cyclic crack propagation in a numerical scheme is qualitatively investigated, employing the finite element method. The propagation criterion is based on a condition that relates the plastically dissipated energy to a critical value. In the finite element simulation scheme, the crack is allowed to propagate when the criterion is satisfied, and the crack propagates until the condition is no longer fulfilled. Experimentally, it is well established that a negative load ratio increases the crack propagation rate, whereas a tensile overload tends to decrease the crack propagation rate. By simulating these load conditions, we show that the proposed propagation criterion closely captures these rate changes.     

Kinematics of the heart: strain-rate imaging from time-resolved three-dimensional phase contrast MRI

A four-dimensional mapping (three spatial dimensions + time) of myocardial strain-rate would help to describe the mechanical properties of the myocardium, which affect important physiological factors such as the pumping performance of the ventricles. Strain-rate represents the local instantaneous deformation of the myocardium and can be calculated from the spatial gradients of the velocity field. Strain-rate has previously been calculated using one-dimensional (ultrasound) or two-dimensional (2-D) magnetic resonance imaging) techniques. However, this assumes that myocardial motion only occurs in one direction or in one plane, respectively. This paper presents a method for calculation of the time-resolved three-dimensional (3-D) strain-rate tensor using velocity vector information in a 3-D spatial grid during the whole cardiac cycle. The strain-rate tensor provides full information of both magnitude and direction of the instantaneous deformation of the myocardium. A method for visualization of the full 3-D tensor is also suggested. The tensors are visualized using ellipsoids, which display the principal directions of strain-rate and the ratio between strain-rate magnitude in each direction. The presented method reveals the principal strain-rate directions without a priori knowledge of myocardial motion directions.