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PubMed1999

Biodegradable polymeric microcellular foams by modified thermally induced phase separation method.

Thermally induced phase separation (TIPS) for the fabrication of porous foams based on various biodegradable polymers of poly(L-lactic acid) and its copolymers with D-lactic acid and/or glycolic acid is presented. Diverse foam morphologies were obtained by systematically changing several parameters involved in the TIPS process, such as polymer type and concentration, coarsening conditions, solvent/nonsolvent composition, and the presence of an additive. The produced foams had microcellular structures with average pore diameters ranging from 1 to 30 microns depending on the process parameters, which were characterized by scanning electron microscopy (SEM) and mercury intrusion porosimetry. Additionally, Pluronic F127 was used as an additive porogen to control the pore geometry and size.

Biocompatible Materials↗

PubMed2004

Breakdown of dynamic scaling in thin film binary liquids undergoing phase separation.

The kinetics of phase separation in thin polymer blend films displaying discrete and bicontinuous domain morphologies are examined. For discrete domains, the correlation length xi grows as t(1/3), in agreement with a coalescence model. By plotting xi/d vs t/t(i) (initiation time), universal growth behavior is obtained for thickness values (d) from 1000 to 190 nm. In contrast, bicontinuous domains grow with a decreasing exponent, 0.62 to 0.28, as d decreases from 900 to 90 nm (i.e., no universal growth). This slowing down with reduced dimensionality suggests suppression of lateral hydrodynamic pumping.

Journal Article↗

PubMed1999

Influence of Component Ratio on Adsorption of Polymer Mixtures under Phase Separation of Solutions.

The influence of the component ratio on polymer mixture adsorption in the two-phase condition is estimated. Transition toward the two-phase condition was attained by increasing the solution concentration up to phase separation. For solutions that have separated into two phases with increasing component concentration, the adsorption from each phase has been studied separately and the total adsorption from two phases has been calculated. The polystyrene-poly(butyl methacrylate)-CCl(4) system was investigated using fumed silica as adsorbent. Simultaneously, the fraction of segments of each type that were immobilized by the surface was determined from NMR spectra. In all cases, poly(butyl methacrylate) is characterized by preferential adsorption. The main features of adsorption are similar in both one-phase and two-phase states; however, the values for adsorption and fraction of immobilized segments are different in the case of adsorption from two separated phases because of the difference between the phases in the ratio of components and their concentration in each phase. The distinctions between adsorption from one-phase solutions before phase separation and from solutions modeling separated phases are connected with the redistribution of components between upper and lower phases. As a result, their ratio does not correspond to the initial ratio, and therefore the thermodynamic conditions of solutions, responsible for adsorption, are changed. Because of this, the shape of isotherms of adsorption and the adsorption values are determined by the different levels of aggregation in solutions with various ratios of components. Copyright 1999 Academic Press.

Journal Article↗

PubMed2003

Depletion-induced phase separation in colloid-polymer mixtures.

Phase separation can be induced in a colloidal dispersion by adding non-adsorbing polymers. Depletion of polymer around the colloidal particles induces an effective attraction, leading to demixing at sufficient polymer concentration. This communication reviews theoretical and experimental work carried out on the polymer-mediated attraction between spherical colloids and the resulting phase separation of the polymer-colloid mixture. Theoretical studies have mainly focused on the limits where polymers are small or large as compared to the colloidal size. Recently, however, theories are being developed that cover a wider colloid-polymer size ratio range. In practical systems, size polydispersity and polyelectrolytes (instead of neutral polymers) and/or charges on the colloidal surfaces play a role in polymer-colloid mixtures. The limited amount of theoretical work performed on this is also discussed. Finally, an overview is given on experimental investigations with respect to phase behavior and results obtained with techniques enabling measurement of the depletion-induced interaction potential, the structure factor, the depletion layer thickness and the interfacial tension between the demixed phases of a colloid-polymer mixture.

Journal Article↗

PubMed2001

Mechanisms of phase separation and aggregation in colloid-polymer mixtures.

The final structure of a colloidal system is greatly influenced by the mechanisms by which phase separation and aggregation occur. The drive to phase separate can be altered in colloid-polymer mixtures (which phase separate due to the depletion interaction) by varying the polymer concentration. Here, we use small angle light scattering to follow the phase separation in such mixtures and analyze the results within a framework indicated by previous results from microscopy investigations. The mechanisms of diffusion-limited cluster aggregation, reaction-limited cluster aggregation, and nucleation and growth are found to provide good descriptions of the phase separation regimes. The growth rate in the nucleation and growth regime is shown to be dependent on the polymer concentration.

Journal Article↗

PubMed2006

Lipid fluorination enables phase separation from fluid phospholipid bilayers.

To probe the effect of lipid fluorination on the formation of lipid domains in phospholipid bilayers, several new fluorinated and non-fluorinated synthetic lipids were synthesised, and the extent of phase separation of these lipids from phospholipid bilayers of different compositions was determined. At membrane concentrations as low as 1% mol/mol, both fluorinated and non-fluorinated lipids were observed to phase separate from a gel-phase (solid ordered) phospholipid matrix, but bilayers in a liquid disordered state caused no phase separation; if the gel-phase samples were heated above the transition temperature, then phase separation was lost. We found incorporation of perfluoroalkyl groups into the lipid enhanced phase separation, to such an extent that phase separation was observed from cholesterol containing bilayers in the liquid ordered phase.

Hydrocarbons, Fluorinated↗

PubMed1993

Phase separation inhibitors and lens transparency.

A phase separation inhibitor, WR77913 [S-3(amino-2-hydroxypropyl) phosphorothioate], was tested for its effects on lens opacification in the radiation (RAD), selenite (SEL), galactose (GAL), streptozotocin (STZ), and Royal College of Surgeons (RCS) models for cataract. A single i.p. injection of WR77913, approximately 15 min before induction of cataract formation by RAD, SEL, STZ delayed or inhibited opacification. Repeated administration was necessary to delay or inhibit opacification in the GAL or RCS models for cataracts. The results suggest that phase separation inhibitors such as WR77913 have the potential to delay or inhibit lens opacification resulting from a variety of physiological or biochemical mechanisms.

Amifostine↗

PubMedDate not supplied

Phase separation in a sheared gelatin/maltodextrin mixture studied by small-angle light scattering.

The influence of shear on the structure of a gelatin/maltodextrin mixture was investigated using small-angle light scattering both during phase separation and after phase separation was allowed to occur quiescently. In all cases, phase separation occurred via spinodal decomposition to form a droplet morphology, and a characteristic length scale was formed in the structure that was prevalent during shear, as well as in quiescent conditions. Below the critical shear rate for droplet breakup, shear accelerated the coarsening rate of the droplets. A transient regime of rapid hydrodynamic coarsening was present when shear was initiated after phase separation and at late times in all cases once the droplets attained a certain size. At the critical shear rate for droplet breakup (1 s(-1)), the rapid repetition of breakup and coarsening was postulated to occur, which enabled a microstructure consisting of elongated droplets with a narrow size distribution to form. When the shear rate enabled droplets to extend to such an extent that a percolated structure could form (10 s(-1)), then the structure was relatively stable and changed very slowly over time. At very high shear rates (100 s(-1)), droplet breakup was suppressed and a highly fibrillar morphology formed that was stable only while the system was under shear. Cessation of shear at high rates led to fiber breakup and the formation of many small droplets. For a given shear rate, the final microstructure appeared to be independent of the time that shear was started when the structure consisted of discrete droplets or fibers. When a percolated structure could form, however, the shear history appeared to be important.

Gelatin↗

PubMed2004

Viscoelastic phase separation in polymer blends.

In this paper, the dynamics and morphology of viscoelastic phase separation in polymer blends is investigated based on the two-fluid model in two dimensions. At critical composition, we have carefully checked the role of shear modulus, without taking account of bulk modulus. The results show that the higher shear modulus component tends to form a dispersed phase in the intermediate stage of phase separation, if the difference between the shear moduli of the components is large enough. This is opposite to the role of bulk modulus, that the higher bulk modulus component forms a networklike pattern without taking account of the shear modulus even if it is the minority phase. The morphological formation is determined by the competition of opposite effects of shear modulus and bulk modulus. For polymer blends at critical composition, the bulk modulus difference leads to a networklike pattern formed by the higher modulus component in the intermediate stage of phase separation. But if the difference between the shear moduli of the components is large enough, a co-continuous structure is observed, resulting from the competition between shear and bulk moduli. For off-critical composition, difference in bulk modulus also leads to a networklike pattern of the component with higher bulk modulus in the intermediate stage of phase separation, but phase inversion is observed rapidly. A small difference between the shear moduli of the components can support the networklike pattern to continue for longer time. But the networklike pattern does not occur for large difference between shear moduli.

Journal Article↗

PubMed1999

Application of a thermodynamic model to the prediction of phase separations in freeze-concentrated formulations for protein lyophilization.

Many of the compounds considered for use in pharmaceutical formulations demonstrate incompatibilities with other components at high enough concentrations, including pairs of polymers, polymers and salts, or even proteins in combination with polymers, salts, or other proteins. Freeze concentration can force solutions into a region where incompatibilities between solutes will manifest as the formation of multiple phases. Such phase separation complicates questions of the stability of the formulation as well as labile components, such as proteins. Yet, phase separation events are difficult to identify by common formulation screening methods. In this report, we use the osmotic virial expansion model of Edmond and Ogston (1) to describe phase-separating behavior of ternary aqueous polymer solutions. Second osmotic virial coefficients of polyethylene glycol 3350 (PEG) and dextran T500 were measured by light scattering. Assuming an equilibrium between ice and water in the freeze-concentrated solution, a degree of freeze concentration can be estimated, which, when combined with the phase separation spinodal, describes a "phase separation envelope" in which phase separation tendencies can be expected in the frozen solution. The phase separation envelope is bounded at low temperatures by the glass transition temperature of the freeze-concentrated solution. Scanning electron microscopic images and infrared spectroscopy of protein structure are provided as experimental evidence of the phase separation envelope in a freeze-dried system of PEG, dextran, and hemoglobin.

Dextrans↗

PubMed2003

Miniaturized sample preparation combined with liquid phase separations.

Miniaturized sample preparation methods designed as the sample pretreatment for liquid phase separations, such as liquid chromatography, capillary electrophoresis and capillary electrochromatography, have been reviewed especially for the on-line coupling of the sample preparation process and the separation process. The development of the desorption interfaces for the effective combining of the sample preparation and subsequent liquid phase separations is briefly described along with the applications of the combined analytical systems to the analysis of complex sample mixtures such as biological and environmental matrices. Novel use of fine polymeric filaments as the extraction medium for microscale liquid phase separation methods are investigated and a comparison is made with other sample preparation techniques. Polymer coating onto the fibrous material is also introduced to further develop microscale sample preparation methods with improved extraction performance. Several other microscale sample preparation methods having a potential compatibility to the liquid phase separations are also described for future applications of these techniques.

Chromatography, Liquid↗

PubMed2005

Kinetics of phase separation in systems exhibiting simple coacervation.

The kinetics of phase separation of a homogeneous polyelectrolytic solution into a dense polymer-rich coacervate and the dilute supernatant phase is discussed through statistical thermodynamics. It has been shown that the coacervate phase is associated with higher internal pressure, consequently giving rise to syneresis. Physical conditions for phase separations has been deduced explicitly which reveals that sigma(2)/qrt[I] > or = constant (where sigma is polyelectrolyte charge density and I is solution ionic strength), consistent with experimental observations. In the lattice model, r is the number of sites occupied by the polymer having a volume critical fraction psi(2c), it was found that phase separation would ensue when sigma(3)r > or = (64/9 alpha(2)) [psi(2c)/(1 - omega(2c))(2)], which reduces to (sigma(3)r/psi(2c)) > or = (64/9 alpha(2)) approximately 0.45 at 20 degrees C for psi(2c) < 1. The separation kinetics mimics a spinodal decomposition process. Rate of release of supernatant due to syneresis was found to be independent of the initial coacervate mass. Syneresis results are discussed in the context of temporal evolution of self-organization in polymer melts through Avrami model.

Journal Article↗

PubMed1999

Protein formulation and lyophilization cycle design: prevention of damage due to freeze-concentration induced phase separation.

Hemoglobin has been previously shown to unfold during freeze drying when lyophilized from formulations that undergo freeze-concentration induced phase separation (Heller et al. 1997. Biotechnol Prog 13:590-596). In this report, we show that such damage may be avoided using kinetic strategies to arrest the phase separation. By rapidly cooling samples during liquid nitrogen spray-freeze drying, the time that the formulation spends in temperature regimes (ca. -3 to -23 degrees C) in which phase separation is both thermodynamically favorable and kinetically realizable is minimized. Increased protein damage with decreasing cooling rates and/or longer annealing periods at -7 degrees C is observed by FTIR spectroscopy. Phase separation and concomitant protein damage may also be avoided by addition of mannitol at concentrations sufficient to cause crystallization. Mannitol crystals segregate the freeze concentrated solution into microscopic domains that block propagation and nucleation of phase separating events. Addition of noncrystallizing sugars, such as sucrose and trehalose, or nonionic surfactants, such as Tween 80 and Triton X-100, has little protective effect against phase separation induced damage during freezing drying.

Calorimetry, Differential Scanning↗

PubMed1979

Disappearance of calcium-induced phase separation in phosphatidylserine-phosphatidylcholine membranes caused by protonation and by electric current.

Disappearance of Ca2+-induced phase separation in phosphatidylserine-phosphatidylcholine membrane has been studied under several conditions by monitoring electron spin resonance spectrum of spin-labeled phosphatidylcholine. The membranes were prepared in Millipore filters. Electron micrographs of the pre parations showed formation of multilayered structures lined on the pore surface. The phase separation was disappeared when the membrane was soaked in non-buffered salt solution (100 ml KCl, pH 5.5). It was markedly contrasting that when the bathing salt solution was buffered no disappearance was observed. Disappearance of the phase separation was also observed when the Ca2+-treated membrane was transferred to acidic salt solutions (less than or equal to pH 2.5) or to low ionic strength media (less than or equal to mM) buffered at pH 5.5, and then to the buffered salt solution (100 mM KCl, pH 5.5). These are due to replacement of Ca2+ by proton, proton-induced separation, followed by disappearance of the phase separation in the buffered salt solution. Biological significance of the competition between Ca2+ and proton for the phase separation or domain formation in the membranes was emphasized.

Calcium↗

PubMed2002

Relation between aggregation and phase separation: three-dimensional Monte Carlo simulations.

We study phase separation of particles in solution using Monte Carlo simulations of reversible aggregation on a cubic lattice. Two stages of the phase separation can be clearly distinguished: initial random aggregation and subsequent densification. Step one leads to a distribution of fractal aggregates close to the binodal and to a temporary gel for large attractive interaction. Step two leads to isolated spherical dense domains close to the binodal and branched wormlike strands for large attractive interactions. The transition between the two types of structure is gradual and there is no clear feature that shows the existence of a spinodal. The first stage of the phase separation is metastable very close to the binodal or at very large interaction energy. In the latter case, the second step can be viewed as an aging process of the gel formed in the first step.

Biophysical Phenomena↗

PubMed2005

Critical polymer-polymer phase separation in ternary solutions.

We study polymer-polymer phase separation in a common good solvent by means of Monte Carlo simulations of the bond-fluctuation model. Below a critical, chain-length-dependent concentration, no phase separation occurs. For higher concentrations, the critical demixing temperature scales nonlinearly with the total monomer concentration, with a power law relatively close to a renormalization-group prediction based on "blob" scaling arguments. We point out that earlier simulations and experiments have tested this power-law dependence at concentrations outside the validity regime of the scaling arguments. The critical amplitudes of the order parameter and the zero-angle scattering intensity also exhibit chain-length dependences that differ from the conventional predictions but are in excellent agreement with the renormalization-group results. In addition, we characterize the variation of the average coil shape upon phase separation.

Journal Article↗

PubMed2005

Viscoelastic phase separation of protein solutions.

In addition to the known behavior of normal phase separation and gelation, we report novel phase-separation behavior of protein solutions as their intermediate case. A network structure of the protein-rich phase may be formed even if it is the minority phase, contrary to the conventional wisdom. This behavior is characteristic of viscoelastic phase separation found in polymer solutions. This kinetic pathway may play crucial roles in the complex phase ordering of protein solutions, in particular, protein network formation in biological systems and foods.

Elasticity↗

PubMed2007

Phase separation in liquid crystalline mesophases of [Co(H2O)6]X2:P65 Systems (X = NO3-, Cl-, or ClO4-).

Transition-metal aqua complex salts [M(H2O)6]X2 (where M is Mn(II), Co(II), Ni(II), Zn(II), or Cd(II) and X is NO3-, Cl-, or ClO4-) can be dissolved in triblock poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) copolymers (Pluronics, such as P65) to form homogeneous liquid crystalline (LC) mesophases. However, the [Co(H2O)6]X2:P65 LC mesophases slowly undergo phase separation into a disordered ion-free phase and an ordered ion-rich LC mesophase. The phase separation also takes place in the two-salt systems [Co(H2O)6](NO3):[Co(H2O)6](ClO4)2:P65 in which the ion-free disordered domains separate out from the initially ordered homogeneous mesophase. The phase separation results in a physical mixture of a hexagonal nitrate-rich and cubic perchlorate-rich LC and disordered ion-free domains in the mixed salt systems. The driving force in the phase separation in the [Co(H2O)6]X2:P65 system is Co(II)-catalyzed aerobic oxidation of P65 into ester and/or other oxidation products. The separation of ions in the [Co(H2O)6](NO3)2:[Co(H2O)6](ClO4)2:P65 system is related to the mesostructures of the two-salt systems that are different, hexagonal in the [Co(H2O)6](NO3)2:P65 system and cubic in the [Co(H2O)6](ClO4)2:P65 system. There is no visible phase separation in the other transition-metal salt:P65 systems. The phase separation in the [Co(H2O)6]X2:P65 systems can also be eliminated by keeping the mesophase under a N2 atmosphere.

Journal Article↗