Validity of particle size analysis techniques for measurement of the attrition that occurs during vacuum agitated powder drying of needle-shaped particles

Analysis of needle-shaped particles of cellobiose octaacetate (COA) obtained from vacuum agitated drying experiments was performed using three particle size analysis techniques: laser diffraction (LD), focused beam reflectance measurements (FBRM) and dynamic image analysis. Comparative measurements were also made for various size fractions of granular particles of microcrystalline cellulose. The study demonstrated that the light scattering particle size methods (LD and FBRM) can be used qualitatively to study the attrition that occurs during drying of needle-shaped particles, however, for full quantitative analysis, image analysis is required. The algorithm used in analysis of LD data assumes the scattering particles are spherical regardless of the actual shape of the particles under evaluation. FBRM measures a chord length distribution (CLD) rather than the particle size distribution (PSD), which in the case of needles is weighted towards the needle width rather than their length. Dynamic image analysis allowed evaluation of the particles based on attributes of the needles such as length (e.g. the maximum Feret diameter) or width (e.g. the minimum Feret diameter) and as such, was the most informative of the techniques for the analysis of attrition that occurred during drying

Formation of valine microcrystals through rapid antisolvent precipitation

In this work we have experimentally studied concentration effects on antisolvent precipitation of valine (an amino acid) from aqueous isopropanol solutions. Our experiments showed that the valine precipitation is very sensitive to both the supersaturation and to the water content in the final solution. Results from spectrophotometric measurements and supersaturation analysis showed that the crystal formation kinetics are strongly dependent on both mixing and concentration profiles in the early stages of the process, even though no visible change in the systems occurs immediately upon mixing with the antisolvent or subsequent dilution. Results from small-angle static light scattering measurements showed that the first visible crystals are of micron size and they grow only little over time, while their number increases gradually. Taken together, these experiments point to intermediate phase separation of (possible amorphous) precursors, being either very small nanoparticles or droplets with their refractive index closely matching that of the continuous phase, which subsequently assemble into micron size valine crystals

Dynamic response studies on aggregation and breakage dynamics of colloidal dispersions in stirred tanks

Aggregation and breakage of aggregates of fully destabilized polystyrene latex particles in turbulent flow was studied experimentally in both batch and continuous stirred tanks using small-angle static light scattering. It was found that the steady-state values of the root-mean-square radius of gyration are fully reversible upon changes of stirring speed as well as solid volume fraction. Steady-state values of the root-mean-square radius of gyration were decreasing with decreasing solid volume fraction as well as with increasing stirring speed. Moreover, it was found that the steady-state structure and shape of the aggregates is not influenced by the applied stirring speed

Effects of temperature and concentration on mechanism and kinetics of thermally induced deposition from coffee extracts

Production of soluble (instant) coffee powders typically involves extraction of roasted coffee by water followed by evaporation in order to concentrate extracts before spray or freeze drying to produce dry coffee powder. In the course of evaporation, deposition of dissolved material from coffee extracts is a major cause of fouling at the heat exchange surfaces of evaporators. Therefore, in order to improve the design and optimization of evaporation processes of coffee extracts, better understanding of the deposition mechanism and kinetics is needed. In this study, optical waveguide lightmode spectroscopy (OWLS) was used to monitor the initial formation of nanometer scale deposits on surfaces exposed to coffee extracts. OWLS measurements were complemented by light scattering from extract solutions, gravimetry of macroscopic deposits, and scanning electron microscopy imaging of deposited layers. Primary molecular-scale layers of about 1 mg m^−2 were rapidly formed in the first stage of deposition, even at ambient temperature, followed by the secondary deposition with kinetics strongly dependent on temperature. Secondary deposition rates were low and largely independent of the extract concentration at ambient temperature, but became strongly dependent on the extract concentration at elevated temperatures. In particular, activation energies for the deposition between 25◦C and 70◦C were much higher for the original extract (13.3 mass %, solids) than for diluted extracts (up to 1.3 mass %, solids). Furthermore, heating of the original extracts above 60◦C resulted in rapid aggregation of suspended macromolecules into large clusters, while only gradual aggregation was observed in diluted extracts

Analysis of strategies for improving uranium utilization in pressurized water reactors

Includes bibliographical references (pages 238-241)Systematic procedures have been devised and applied to evaluate core design and fuel management strategies for improving uranium utilization in Pressurized Water Reactors operated on a once-through fuel cycle. A principal objective has been the evaluation of suggested improvements on a self-consistent basis, allowing for concurrent changes in dependent variables such as core leakage and batch power histories, which might otherwise obscure the sometimes subtle effects of interest. Two levels of evaluation have been devised: a simple but accurate analytic model based on the observed linear variations in assembly reactivity as a function of burnup; and a numerical approach, embodied in a computer program, which relaxes this assumption and combines it with empirical prescriptions for assembly (or batch) power as a function of reactivity, and core leakage as a function of peripheral assembly power. State-of-the-art physics methods, such as PDQ-7, were used ! to verify and supplement these techniques.These methods have been applied to evaluate several suggested improvements: (1) axial blankets of low-enriched or depleted uranium, and of beryllium metal, (2) radial natural uranium blankets, (3) low-leakage radial fuel management, (4) high burnup fuels, (5) optimized H/U atom ratio, (6) annular fuel, and (7) mechanical spectral shift (i.e. variable fuel-to-moderator ratio) concepts such as those involving pin pulling and bundle reconstitution.The potential savings in uranium requirements compared to current practice were found to be as follows: (1) O0-3%, (2) negative, (3) 2-3%; possibly 5%, (4) "15%, (5) 0-2.5%, (6) no inherent advantage, (7) 10%. Total savings should not be assumed to be additive; and thermal/hydraulic or mechanical design restrictions may preclude full realization of some of the potential improvements

Analysis of strategies for improving uranium utilization in pressurized water reactors

Systematic procedures have been devised and applied to evaluate core design and fuel management strategies for improving uranium utilization in Pressurized Water Reactors operated on a once-through fuel cycle. A principal objective has been the evaluation of suggested improvements on a self-consistent basis, allowing for concurrent changes in dependent variables such as core leakage and batch power histories, which might otherwise obscure the sometimes subtle effects of interest. Two levels of evaluation have been devised: a simple but accurate analytic model based on the observed linear variations in assembly reactivity as a function of burnup; and a numerical approach, embodied in a computer program, which relaxes this assumption and combines it with empirical prescriptions for assembly (or batch) power as a function of reactivity, and core leakage as a function of peripheral assembly power. State-of-the-art physics methods, such as PDQ-7, were used to verify and supplement these techniques.These methods have been applied to evaluate several suggested improvements: (1) axial blankets of low-enriched or depleted uranium, and of beryllium metal, (2) radial natural uranium blankets, (3) lowleakage radial fuel management, (4) high burnup fuels, (5) optimized H/U atom ratio, (6) annular fuel, and (7) mechanical spectral shift (i.e. variable fuel-to-moderator ratio) concepts such as those involving pin pulling and bundle reconstitution.The potential savings in uranium requirements compared to current practice were found to be as follows: (1) O0-3%, (2) negative, (3) 2-3%; possibly 5%, (4) "15%, (5) 0-2.5%, (6) no inherent advantage, (7) 10%. Total savings should not be assumed to be additive; and thermal/hydraulic or mechanical design restrictions may preclude full realization of some of the potential improvements

Chain-end modifications and sequence arrangements of antimicrobial peptoids for mediating activity and nano-assembly

Poly(N-substituted glycine) “peptoids” are an interesting class of peptidomimics that can resist proteolysis and mimic naturally found antimicrobial peptides (AMPs), which exhibit wide spectrum activity against bacteria. This work investigates the possibility of modifying peptoid AMP mimics (AMPMs) with aliphatic lipid “tails” to generate “lipopeptoids” that can assemble into micellar nanostructures, and evaluates their antimicrobial activities. Two families of AMPMs with different distributions of hydrophobic and cationic residues were employed—one with a uniform repeating amphiphilicity, the other with a surfactant-like head-to-tail amphiphilicity. To further evaluate the interplay between self-assembly and activity, the lipopeptoids were variously modified at the AMPM chain ends with a diethylene glycol (EG2) and/or a cationic group (Nlys-Nlys dipeptoid) to adjust amphiphilicity and chain flexibility. Self-assembly was investigated by critical aggregation concentration (CAC) fluorescence assays and dynamic light scattering (DLS). The structure of a key species was also verified by small-angle X-ray scattering (SAXS) and cryo-electron microscopy (cryo-EM). To screen for antibacterial properties, we measured the minimum inhibitory concentrations (MIC) against S. aureus, E. coli, and P. aeruginosa. We found that certain combinations of lipid tail and AMPM sequences exhibit increased antibacterial activity (i.e., decreased MICs). Perhaps counter-intuitively, we were particularly interested in increased MICs in combination with low CACs. Concealing antimicrobial interactions due to packing of AMPMs in nano-assemblies could pave the way to AMPMs that may be “inert” even if unintentionally released and prevent microbes from gaining resistance to the lipopeptoids. Overall, incorporation of EG2 significantly improved lipopeptoids packing while the hydrophobic tail length was found to have a major influence over the MIC. One particular sequence, which we named C15-EG2-(kss)4, exhibited a very low CAC of 34 μM (0.0075 wt.%) and a significantly increased MIC above values for the unmodified AMPM. With the sequence design trends uncovered from this study, future work will focus on discovering more species such as C15-EG2-(kss)4 and on investigating release mechanisms and the potency of the released lipopeptoids

Scaling of glycine nucleation kinetics with shear rate and glass-liquid interfacial area

The scaling of the nucleation kinetics of glycine was investigated in supersaturated aqueous solutions under isothermal conditions. Induction times were measured in a Couette cell with a wide range of average shear rates γ_avg (25-250 s^-1) and a range of glass-liquid interfacial areas A (2.5-10 cm^2 per ml solution). The probability distributions of induction times were found to scale with shear rate and glass-liquid interfacial area, with the characteristic timescale (γ_avg.A)^-1. Primary nucleation rates and growth times to reach detection (estimated from the probability distributions) were both dependent on this timescale. In-situ dynamic light scattering revealed mesoscale clusters in the solutions that increased in size over time at rates which also depended on this timescale. The increase in size was thought to be due to the shear-enhanced aggregation or coalescence of mesoscale clusters leading to a higher number of larger mesoscale clusters, resulting in higher rates of primary nucleation