Poly(vinyl alcohol) stabilization of acrylic emulsion polymers using the miniemulsion approach

NASA Astrophysics Data System (ADS)

Kim, Noma

Miniemulsion approach was employed to obtain stable acrylic latexes of n-butyl acrylate and methyl methacrylate (50/50 wt%) stabilized with poly(vinyl alcohol) (PVA) and to enhance the grafting reaction between PVA and acrylic monomers at the water/droplet interface. The stability of miniemulsions were studied in terms of the type and concentration of' the stabilizer, and the PVA partitioning were determined as a function of the PVA concentration. Using the comparison of PVA partitioning at droplet surface and grafted PVA as a function of concentration, it was suggested that the water/monomer interface is the main grafting site in the miniemulsion polymerization. Seeded emulsion and miniemulsion copolymerizations initiated with water-soluble (hydrogen peroxide, HPO), partially water-soluble (t-butyl peroxide, TBHP), and oil-soluble (t-butyl peroxyoctoate, TBPO) initiators were carried out to further investigate the oil/water interface as the grafting site for PVA. The interaction between the capillary wall in the CHDF (capillary hydrodynamic fractionation) chromatographic particle sizer and the water-soluble polymers adsorbed on the particle surface was studied using different types of water-soluble polymers and eluants. Different grafting architectures depending on the initiation site were suggested based on the CHDF results. The amounts of grafted PVA produced in miniemulsion polymers initiated with TBHP and TBPO were substantially less than those in the corresponding seeded emulsion polymerizations. The effect on the internal viscosity at the interface was proposed to explain the difference in grafting in terms of polymerization methods. Aqueous phase and interface grafting were studied using the measurement of the degree of hydrolysis (DH) of the serum PVA and adsorbed PVA after miniemulsion polymerizations. Based on the results, it was found that aqueous phase and interface grafting occurred in the HPO system; however, interface grafting dominated the TBHP system. Colloidal instability in conventional emulsion polymerizations was investigated and compared with the corresponding miniemulsion polymerization. It was found that the grafted PVA in conventional emulsion polymerizations was more hydrophobic presumably due to a greater amount of grafted chains than that in similar miniemulsion polymerizations and this could be correlated with the colloidal instability during conventional emulsion polymerizations.

Versatile Methodology to Encapsulate Gold Nanoparticles in PLGA Nanoparticles Obtained by Nano-Emulsion Templating.

PubMed

Fornaguera, Cristina; Feiner-Gracia, Natàlia; Dols-Perez, Aurora; García-Celma, Maria José; Solans, Conxita

2017-05-01

Gold nanoparticles have been proved useful for many biomedical applications, specifically, for their use as advanced imaging systems. However, they usually present problems related with stability and toxicity. In the present work, gold-nanoparticles have been encapsulated in polymeric nanoparticles using a novel methodology based on nano-emulsion templating. Firstly, gold nanoparticles have been transferred from water to ethyl acetate, a solvent classified as class III by the NIH guidelines (low toxic potential). Next, the formation of nano-emulsions loaded with gold nanoparticles has been performed using a low-energy, the phase inversion composition (PIC) emulsification method, followed by solvent evaporation giving rise to polymeric nanoparticles. Using this methodology, high concentrations of gold nanoparticles (>100 pM) have been encapsulated. Increasing gold nanoparticle concentration, nano-emulsion and nanoparticle sizes increase, resulting in a decrease on the stability. It is noteworthy that the designed nanoparticles did not produce cytotoxicity neither hemolysis at the required concentration. Therefore, it can be concluded that a novel and very versatile methodology has been developed for the production of polymeric nanoparticles loaded with gold nanoparticles. Graphical Abstract Schematic representation of AuNP-loaded polymeric nanoparticles preparation from nano-emulsion templating.

Localized in situ polymerization on graphene surfaces for stabilized graphene dispersions.

PubMed

Das, Sriya; Wajid, Ahmed S; Shelburne, John L; Liao, Yen-Chih; Green, Micah J

2011-06-01

We demonstrate a novel in situ polymerization technique to develop localized polymer coatings on the surface of dispersed pristine graphene sheets. Graphene sheets show great promise as strong, conductive fillers in polymer nanocomposites; however, difficulties in dispersion quality and interfacial strength between filler and matrix have been a persistent problem for graphene-based nanocomposites, particularly for pristine graphene. With this in mind, a physisorbed polymer layer is used to stabilize graphene sheets in solution. To create this protective layer, we formed an organic microenvironment around dispersed graphene sheets in surfactant solutions, and created a nylon 6, 10 or nylon 6, 6 coating via interfacial polymerization. Technique lies at the intersection of emulsion and admicellar polymerization; a similar technique was originally developed to protect luminescent properties of carbon nanotubes in solution. These coated graphene dispersions are aggregation-resistant and may be reversibly redispersed in water even after freeze-drying. The coated graphene holds promise for a number of applications, including multifunctional graphene-polymer nanocomposites. © 2011 American Chemical Society

Evaluation of rotating-cylinder and piston-cylinder reactors for ground-based emulsion polymerization

NASA Technical Reports Server (NTRS)

Vanderhoff, J. W.; El-Aasser, M. S.

1987-01-01

The objectives of this program are to apply ground-based emulsion polymerization reactor technology to improve the production of: monodisperse latex particles for calibration standards, chromatographic separation column packing, and medical research; and commercial latexes such as those used for coatings, foams, and adhesives.

Synthetic Polymers at Interfaces: Monodisperse Emulsions Multiple Emulsions and Liquid Marbles

NASA Astrophysics Data System (ADS)

Sun, Guanqing

The adsorption of polymeric materials at interfaces is an energetically favorable process which is investigated in much diversified fields, such as emulsions, bubbles, foams, liquid marbles. Pickering emulsion, which is emulsion stabilized by solid particles has been investigated for over one century and preparation of Pickering emulsion with narrow size distribution is crucial for both the theoretical study of the stabilization mechanism and practical application, such as templated fabrication of colloidosomes. The precise control over the size and functionality of polymer latices allows the preparation of monodisperse Pickering emulsions with desired sizes through SPG membrane emulsification at rather rapid rate compared to microfludic production. Double or multiple emulsions have long been investigated but its rapid destabilization has always been a major obstacle in applying them into practical applications. The modern living polymerization techniques allow us to prepare polymers with designed structure of block copolymers which makes it possible to prepare ultra-stable multiple emulsions. The precise tuning of the ratio of hydrophobic part over the hydrophilic can unveil the stabilization mechanism. Liquid marble is a new type of materials of which liquid droplets are coated by dry particles. The coating of an outer layer of dry particles renders the liquid droplets non-sticky at solid surface which is useful in transportation of small amount of liquid without leakage at extreme low friction force. The property of liquid marbles relies largely on the stabilizers and the drying condition of polymeric latices is shown to have great influence on the property of liquid marbles. Firstly, an introduction to the interfacial and colloidal science with special attention to topics on emulsions, multiple emulsion and liquid marbles is given in Chapter 1. The unique features of an interface and a discussion on the definition of colloids are introduced prior to the discussion of emulsion stabilization and preparation. A historical review of multiple emulsions is presented subsequently and the stability mechanism is discussed in details with regard to the transportation kinetics of small molecules through the separating membrane of double emulsions. The principle, property and applications of liquid marbles are then summarized. Secondly, the preparation of monodisperse Pickering emulsions stabilized by soft PNIPAM-co-MAA microgels through SPG membrane emulsification is described. The influence of the membrane pore size, pH of the particle dispersion, particle size and the operating parameters of the membrane emulsification device on the size of the emulsion droplets was investigated systematically. The improvement in monodispersity of the emulsion droplets allows us to measure the release profiles of a small molecular dye and a larger nanoparticle through the colloidosomes. It is further demonstrated that the preparation of monodisperse emulsions stabilized by other types of soft particles allows us control the stability of the emulsion with a pH trigger and improved biocompatibility. Thirdly, the preparation of multiple emulsions stabilized by a special designed PEG-b-PS diblock copolymer with desired hydrophobicity by one-step method was presented. The ultra-stability of the as-obtained multiple emulsions was ascribed to the effective steric stabilization of the two interfaces with different polymer configurations at the interfaces. A series of diblock copolymer with increasing PS chain length was then synthesized to investigate the influence of asymmetry ratio on the type of emulsions prepared. It is found that the diblock copolymers with the asymmetry ratio of approximately 1 had the highest power to stabilize multiple emulsions. The multiple emulsions were demonstrated to be a promising platform for controlled release. In the end, particle-stabilized water-in-air liquid marbles were investigated. PSco-MAA nanoparticles synthesized from surfactant-free emulsion polymerization were proved to be effective liquid marble stabilizers. The influence of drying conditions on the properties of liquid marbles was investigated through a macroscopic way. The pH value of the particle dispersion, which influences the protonation states of the particles before freeze-drying, has a profound influence on the property of the stabilized liquid marbles. A brief comment to the future of work of these investigated systems is delivered in the last part.

One-step formation of multiple Pickering emulsions stabilized by self-assembled poly(dodecyl acrylate-co-acrylic acid) nanoparticles.

PubMed

Zhu, Ye; Sun, Jianhua; Yi, Chenglin; Wei, Wei; Liu, Xiaoya

2016-09-13

In this study, a one-step generation of stable multiple Pickering emulsions using pH-responsive polymeric nanoparticles as the only emulsifier was reported. The polymeric nanoparticles were self-assembled from an amphiphilic random copolymer poly(dodecyl acrylate-co-acrylic acid) (PDAA), and the effect of the copolymer content on the size and morphology of PDAA nanoparticles was determined by dynamic light scattering (DLS) and transmission electron microscopy (TEM). The emulsification study of PDAA nanoparticles revealed that multiple Pickering emulsions could be generated through a one-step phase inversion process by using PDAA nanoparticles as the stabilizer. Moreover, the emulsification performance of PDAA nanoparticles at different pH values demonstrated that multiple emulsions with long-time stability could only be stabilized by PDAA nanoparticles at pH 5.5, indicating that the surface wettability of PDAA nanoparticles plays a crucial role in determining the type and stability of the prepared Pickering emulsions. Additionally, the polarity of oil does not affect the emulsification performance of PDAA nanoparticles, and a wide range of oils could be used as the oil phase to prepare multiple emulsions. These results demonstrated that multiple Pickering emulsions could be generated via the one-step emulsification process using self-assembled polymeric nanoparticles as the stabilizer, and the prepared multiple emulsions have promising potential to be applied in the cosmetic, medical, and food industries.

Shedding light on the different behavior of ionic and nonionic surfactants in emulsion polymerization: from atomistic simulations to experimental observations.

PubMed

Magi Meconi, Giulia; Ballard, Nicholas; Asua, José M; Zangi, Ronen

2017-12-06

Although surfactants are known to play a vital role in polymerization reactions carried out in dispersed media, many aspects of their use are poorly understood, perhaps none more so than the vastly different action of ionic and nonionic surfactants in emulsion polymerization. In this work, we combine experimental measurements of emulsion polymerization of styrene with atomistic molecular dynamics simulations to better understand the behavior of surfactants at monomer/polymer-water interfaces. In a batch emulsion polymerization of styrene, the nonionic surfactant Disponil AFX 1080 leads to two nucleation periods, in contrast to the behavior observed for the ionic surfactant SDS. This can be explained by the absorption of the nonionic surfactant into the organic phase at the early stages of the polymerization reaction which is then released as the reaction progresses. Indeed, we find that the partition coefficient of the surfactant between the organic phase and water increases with the amount of monomer in the former, and preferential partitioning is detected to organic phases containing at least 55% styrene. Results from molecular dynamics simulations confirm that spontaneous dissolution of the non-ionic surfactant into a styrene-rich organic phase occurs above a critical concentration of the surfactant adsorbed at the interface. Above this critical concentration, a linear correlation between the amount of surfactant adsorbed at the interface and that absorbed inside the organic phase is observed. To facilitate this absorption into a completely hydrophobic medium, water molecules accompany the intruding surfactants. Similar simulations but with the ionic surfactant instead did not result in any absorption of the surfactant into a neat styrene phase, likely because of its strongly hydrophilic head group. The unusual partitioning behavior of nonionic surfactants explains a number of observable features of emulsion polymerization reactions which use nonionic surfactants and should help with future development of processes for improved control over polymerization.

Intriguing Morphology Evolution from Noncrosslinked Poly(tert-butyl acrylate) Seeds with Polar Functional Groups in Soap-Free Emulsion Polymerization of Styrene.

PubMed

Wang, Lu; Pan, Mingwang; Song, Shaofeng; Zhu, Lei; Yuan, Jinfeng; Liu, Gang

2016-08-09

Herein, we demonstrate a facile approach to prepare anisotropic poly(tert-butyl acrylate)/polystyrene (PtBA/PS) composite particles with controllable morphologies by soap-free seeded emulsion polymerization (SSEP). In the first step, noncrosslinked PtBA seeds with self-stabilizing polar functional groups (e.g., ester groups and radicals) are synthesized by soap-free emulsion polymerization. During the subsequent SSEP of styrene (St), PS bulges are nucleated on the PtBA seeds due to the microphase separation confined in the latex particles. The morphology evolution of PtBA/PS composite particles is tailored by varying the monomer/seed feed ratio, polymerization time, and polymerization temperature. Many intriguing morphologies, including hamburger-like, litchi-like, mushroom-like, strawberry-like, bowl-like, and snowman-like, have been acquired for PtBA/PS composite particles. The polar groups on the PtBA seed surface greatly influence the formation and further merging of PS/St bulges during the polymerization. A possible formation mechanism is proposed on the basis of experimental results. These complex composite particles are promising for applications in superhydrophobic coatings.

Synthesis of dodecylamine-functionalized graphene quantum dots and their application as stabilizers in an emulsion polymerization of styrene.

PubMed

Xuan, Wang; Ruiyi, Li; Zaijun, Li; Junkang, Liu

2017-11-01

Pickering emulsions have attracted considerable interest due to their potential applications in many fields, such as the food, pharmaceutical, petroleum and cosmetics industries. The study reports the synthesis of dodecylamine-functionalized graphene quantum dots (d-GQDs) and their implementation as stabilizers in an emulsion polymerization of styrene. First, d-GQDs are prepared by thermal pyrolysis of citric acid and dodecylamine in 0.1M ammonium hydroxide. The resulting d-GQDs consist of small graphene sheets with abundant amino, carboxyl, acylamino, hydroxyl and alkyl chains on the edge. The amphiphilic structure gives the d-GQDs high surface activity. The addition of d-GQDs can reduce the surface tension of water to 30.8mNm -1 and the interfacial tension of paraffin oil/water to 0.0182mNm -1 . The surface activity is much better than that of previously reported solid particle surfactants for Pickering emulsions and is close to that of sodium dodecylbenzenesulfonate, which is, a classical organic surfactants. Then, d-GQDs are employed as solid particle surfactants for stabilizing styrene-in-water emulsions. The emulsions exhibit excellent stability at pH 7. However, stability is lost when the pH is more than 9 or less than 4. The pH-switchable behaviour can be attributed to the protonation of amino groups in a weak acid medium and dissociation of carboxyl groups in a weak base medium. Finally, 2,2'-azobis(2-methylpropionitrile) is introduced into the Pickering emulsions to trigger emulsion polymerization of styrene. The as-prepared polystyrene spheres display a uniform morphology with a narrow diameter distribution. The fluorescent d-GQDs coated their surfaces. This study presents an approach for the fabrication of amphiphilic GQDs and GQDs-based functional materials, which have a wide range of potential applications in emulsion polymerization, as well as in sensors, catalysts, and energy storage. Copyright © 2017 Elsevier Inc. All rights reserved.

A Robust Oil-in-Oil Emulsion for the Nonaqueous Encapsulation of Hydrophilic Payloads.

PubMed

Lu, Xiaocun; Katz, Joshua S; Schmitt, Adam K; Moore, Jeffrey S

2018-03-14

Compartmentalized structures widely exist in cellular systems (organelles) and perform essential functions in smart composite materials (microcapsules, vasculatures, and micelles) to provide localized functionality and enhance materials' compatibility. An entirely water-free compartmentalization system is of significant value to the materials community as nonaqueous conditions are critical to packaging microcapsules with water-free hydrophilic payloads while avoiding energy-intensive drying steps. Few nonaqueous encapsulation techniques are known, especially when considering just the scalable processes that operate in batch mode. Herein, we report a robust oil-in-oil Pickering emulsion system that is compatible with nonaqueous interfacial reactions as required for encapsulation of hydrophilic payloads. A major conceptual advance of this work is the notion of the partitioning inhibitor-a chemical agent that greatly reduces the payload's distribution between the emulsion's two phases, thus providing appropriate conditions for emulsion-templated interfacial polymerization. As a specific example, an immiscible hydrocarbon-amine pair of liquids is emulsified by the incorporation of guanidinium chloride (GuHCl) as a partitioning inhibitor into the dispersed phase. Polyisobutylene (PIB) is added into the continuous phase as a viscosity modifier for suitable modification of interfacial polymerization kinetics. The combination of GuHCl and PIB is necessary to yield a robust emulsion with stable morphology for 3 weeks. Shell wall formation was accomplished by interfacial polymerization of isocyanates delivered through the continuous phase and polyamines from the droplet core. Diethylenetriamine (DETA)-loaded microcapsules were isolated in good yield, exhibiting high thermal and chemical stabilities with extended shelf-lives even when dispersed into a reactive epoxy resin. The polyamine phase is compatible with a variety of basic and hydrophilic actives, suggesting that this encapsulation technology is applicable to other hydrophilic payloads such as polyols, aromatic amines, and aromatic heterocyclic bases. Such payloads are important for the development of extended pot or shelf life systems and responsive coatings that report, protect, modify, and heal themselves without intervention.

Various aspects of ultrasound assisted emulsion polymerization process.

PubMed

Korkut, Ibrahim; Bayramoglu, Mahmut

2014-07-01

In this paper, the effects of ultrasonic (US) power, pulse ratio, probe area and recipe composition were investigated on two process responses namely, monomer (methyl methacrylate, MMA) conversion and electrical energy consumption per mass of product polymer (PMMA). Pulsed mode US is more suitable than continuous mode US for emulsion polymerization. The probe (tip) area has little effect on the yield of polymerization when comparing 19 and 13 mm probes, 13 mm probe performing slightly better for high conversion levels. Meanwhile, large probe area is beneficial for high conversion efficiency of electric energy to US energy as well as for high radical generation yield per energy consumed. The conversion increased slightly and electrical energy consumption decreased substantially by using a recipe with high SDS and monomer concentrations. Conclusions presented in this paper may be useful for scale-up of US assisted emulsion polymerization. Copyright © 2014 Elsevier B.V. All rights reserved.

A new type of polymeric heavy metal complexing precipitant used as fishery disinfectant and antiparasitic drug

NASA Astrophysics Data System (ADS)

Liu, Y. C.; Zhang, A. N.; Wang, X. B.; Xu, J.; Zeng, X. H.; Wang, H. M.

2017-08-01

This paper presents a technique to produce a new kind of fishery drug that is water emulsion suspending agent containing polymeric calcium-iron-dithiocarbamate with heavy metal complexing precipitate ability, good disinfection and auxiliary insecticidal efficacy. The product has good dispersion, high efficiency and low toxicity, as well as no pollution and no harmful residues. It not only can be used in the pond waters and ornamental waters, but also can meet the high requirements of the aquaculture waters. There is non-pollutant emission in the production, which is a green environment-friendly technique without three waste discharges. This technology belongs to the ecological and environmental protection.

Fine-tuning of process conditions to improve product uniformity of polystyrene particles used for wind tunnel velocimetry

NASA Technical Reports Server (NTRS)

Ray, Asit K.

1990-01-01

Monodisperse polymer particles (having uniform diameter) were used for the last two decades in physical, biological, and chemical sciences. In NASA Langley Research Center monodisperse polystyrene particles are used in wind tunnel laser velocimeters. These polystyrene (PS) particles in latex form were formulated at the Engineering Laboratory of FENGD using emulsion-free emulsion polymerization. Monodisperse PS latices particles having different particle diameters were formulated and useful experimental data involving effects of process conditions on particle size were accumulated. However, similar process conditions and chemical recipes for polymerization of styrene monomer have often yielded monodisperse particles having varying diameters. The purpose was to improve the PS latex product uniformity by fine-tuning the process parameters based on the knowledge of suspension and emulsion polymerization.

In situ functionalization and PEO coating of iron oxide nanocrystals using seeded emulsion polymerization.

PubMed

Kloust, Hauke; Schmidtke, Christian; Feld, Artur; Schotten, Theo; Eggers, Robin; Fittschen, Ursula E A; Schulz, Florian; Pöselt, Elmar; Ostermann, Johannes; Bastús, Neus G; Weller, Horst

2013-04-16

Herein we demonstrate that seeded emulsion polymerization is a powerful tool to produce multiply functionalized PEO coated iron oxide nanocrystals. Advantageously, by simple addition of functional surfactants, functional monomers, or functional polymerizable linkers-solely or in combinations thereof-during the seeded emulsion polymerization process, a broad range of in situ functionalized polymer-coated iron oxide nanocrystals were obtained. This was demonstrated by purposeful modulation of the zeta potential of encapsulated iron oxide nanocrystals and conjugation of a dyestuff. Successful functionalization was unequivocally proven by TXRF. Furthermore, the spatial position of the functional groups can be controlled by choosing the appropriate spacers. In conclusion, this methodology is highly amenable for combinatorial strategies and will spur rapid expedited synthesis and purposeful optimization of a broad scope of nanocrystals.

Design and Synthesis of Multigraft Copolymer Thermoplastic Elastomers: Superelastomers

DOE PAGES

Wang, Huiqun; Lu, Wei; Wang, Weiyu; ...

2017-09-28

Thermoplastic elastomers (TPEs) have been widely studied because of their recyclability, good processibility, low production cost, and unique performance. The building of graft-type architectures can greatly improve mechanical properties of TPEs. This review focuses on the advances in different approaches to synthesize multigraft copolymer TPEs. Anionic polymerization techniques allow for the synthesis of well-defined macromolecular structures and compositions, with great control over the molecular weight, polydispersity, branch spacing, number of branch points, and branch point functionality. Progress in emulsion polymerization offers potential approaches to commercialize these types of materials with low production cost via simple operations. Moreover, the use ofmore » multigraft architecturesprovides a solution to the limited elongational properties of all-acrylic TPEs, which can greatly expand their potential application range. The combination of different polymerization techniques, the introduction of new chemical compositions, and the incorporation of sustainable sources are expected to be further investigated in this area in coming years.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Huiqun; Lu, Wei; Wang, Weiyu

Thermoplastic elastomers (TPEs) have been widely studied because of their recyclability, good processibility, low production cost, and unique performance. The building of graft-type architectures can greatly improve mechanical properties of TPEs. This review focuses on the advances in different approaches to synthesize multigraft copolymer TPEs. Anionic polymerization techniques allow for the synthesis of well-defined macromolecular structures and compositions, with great control over the molecular weight, polydispersity, branch spacing, number of branch points, and branch point functionality. Progress in emulsion polymerization offers potential approaches to commercialize these types of materials with low production cost via simple operations. Moreover, the use ofmore » multigraft architecturesprovides a solution to the limited elongational properties of all-acrylic TPEs, which can greatly expand their potential application range. The combination of different polymerization techniques, the introduction of new chemical compositions, and the incorporation of sustainable sources are expected to be further investigated in this area in coming years.« less

Purified phenolics from hydrothermal treatments of biomass: ability to protect sunflower bulk oil and model food emulsions from oxidation.

PubMed

Conde, Enma; Moure, Andrés; Domínguez, Herminia; Gordon, Michael H; Parajó, Juan Carlos

2011-09-14

The phenolic fractions released during hydrothermal treatment of selected feedstocks (corn cobs, eucalypt wood chips, almond shells, chestnut burs, and white grape pomace) were selectively recovered by extraction with ethyl acetate and washed with ethanol/water solutions. The crude extracts were purified by a relatively simple adsorption technique using a commercial polymeric, nonionic resin. Utilization of 96% ethanol as eluting agent resulted in 47.0-72.6% phenolic desorption, yielding refined products containing 49-60% w/w phenolics (corresponding to 30-58% enrichment with respect to the crude extracts). The refined extracts produced from grape pomace and from chestnut burs were suitable for protecting bulk oil and oil-in-water and water-in-oil emulsions. A synergistic action with bovine serum albumin in the emulsions was observed.

Synthesis of amphipathic block copolymers based on polyisobutylene and polyoxyethylene and their application in emulsion polymerization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sar, B.

1992-12-31

Polymer colloids stabilized by polymeric surfactants are of great interest both commercially and academically. It has been found that these materials enhance latex stabilization in a number of applications. The polymeric surfactants are amphipathic block and graft copolymers containing both hydrophilic and hydrophobic moieties. The current study involved the synthesis of a series of amphipathic triblock copolymers, polyisobutylene-block-polyoxyethylene-block-polyisobutylene (PIB-b-POE-b-PIB), for use in the emulsion polymerization of styrene (STY), methyl methacrylate (MMA), and vinyl acetate (VAc). The stabilizing effectiveness of these triblock copolymers was studied as a function of their blocklength. When the molecular weight of the POE center block wasmore » changed from M{sub n} = 2,000 to 20,000 g/mole, stable lattices were obtained in emulsion polymerization with MMA, STY, and VAc as the monomers. In all cases, the polymerization rates remained constant, while the number of particles/volume decreased with increasing POE chain length. When the molecular weight of the PIB end blocks was changed from M{sub n} = 400 to 2,600 g/mole keeping the molecular weight of the POE center block constant at M{sub n} = 20,000 g/mole, the poly(methyl methacrylate) and poly(vinyl acetate) lattices exhibited similar behavior, i.e., the number of particles and particle sizes remained the same, but the rate of polymerization reached a maximum at 87 wt% POE content. In the case of poly(styrene) both the rate of polymerization and the number of particles remained constant. The emulsion polymerization of other monomers such as butadiene, acrylonitrile, methyl acrylate, ethyl acrylate, and butyl acrylate was carried out by using one triblock copolymer, i.e., PIB(400)-b-POE (8,000)-b-PIB-(400). Stable lattices were also formed in all cases.« less

21 CFR 175.210 - Acrylate ester copolymer coating.

Code of Federal Regulations, 2014 CFR

2014-04-01

... polymerized copolymer of ethyl acrylate, methyl methacrylate, and methacrylic acid applied in emulsion form to... of the polymer and in the preparation and application of the emulsion may include substances named in... amount required as a preservative in emulsion defoamer. Disodium hydrogen phosphate Do. Formaldehyde...

Aspects of droplet and particle size control in miniemulsions

NASA Astrophysics Data System (ADS)

Saygi-Arslan, Oznur

Miniemulsion polymerization has become increasingly popular among researchers since it can provide significant advantages over conventional emulsion polymerization in certain cases, such as production of high-solids, low-viscosity latexes with better stability and polymerization of highly water-insoluble monomers. Miniemulsions are relatively stable oil (e.g., monomer) droplets, which can range in size from 50 to 500 nm, and are normally dispersed in an aqueous phase with the aid of a surfactant and a costabilizer. These droplets are the primary locus of the initiation of the polymerization reaction. Since particle formation takes place in the monomer droplets, theoretically, in miniemulsion systems the final particle size can be controlled by the initial droplet size. The miniemulsion preparation process typically generates broad droplet size distributions and there is no complete treatment in the literature regarding the control of the mean droplet size or size distribution. This research aims to control the miniemulsion droplet size and its distribution. In situ emulsification, where the surfactant is synthesized spontaneously at the oil/water interface, has been put forth as a simpler method for the preparation of miniemulsions-like systems. Using the in situ method of preparation, emulsion stability and droplet and particle sizes were monitored and compared with conventional emulsions and miniemulsions. Styrene emulsions prepared by the in situ method do not demonstrate the stability of a comparable miniemulsion. Upon polymerization, the final particle size generated from the in situ emulsion did not differ significantly from the comparable conventional emulsion polymerization; the reaction mechanism for in situ emulsions is more like conventional emulsion polymerization rather than miniemulsion polymerization. Similar results were found when the in situ method was applied to controlled free radical polymerizations (CFRP), which have been advanced as a potential application of the method. Molecular weight control was found to be achieved via diffusion of the CFRP agents through the aqueous phase owing to limited water solubilities. The effects of adsorption rate and energy on the droplet size and size distribution of miniemulsions using different surfactants (sodium lauryl sulfate (SLS), sodium dodecylbenzene sulfonate (SDBS), Dowfax 2A1, Aerosol OT-75PG, sodium n-octyl sulfate (SOS), and sodium n-hexadecyl sulfate (SHS)) were analyzed. For this purpose, first, the dynamics of surfactant adsorption at an oil/water interface were examined over a range of surfactant concentrations by the drop volume method and then adsorption rates of the different surfactants were determined for the early stages of adsorption. The results do not show a direct relationship between adsorption rate and miniemulsion droplet size and size distribution. Adsorption energies of these surfactants were also calculated by the Langmuir adsorption isotherm equation and no correlation between adsorption energy and miniemulsion droplet size was found. In order to understand the mechanism of miniemulsification process, the effects of breakage and coalescence processes on droplet size distributions were observed at different surfactant concentrations, monomer ratios, and homogenization conditions. A coalescence and breakup mechanism for miniemulsification is proposed to explain the size distribution of droplets. The multimodal droplet size distribution of ODMA miniemulsions was controlled by the breakage mechanism. The results also showed that, at a surfactant concentration when 100% surface coverage was obtained, the droplet size distribution became unimodal.

Physical Immobilization Liposomes in Uniform Zwitterionic Microgel Particles Fabricated in Microcapillary Device

NASA Astrophysics Data System (ADS)

Jeong, Eun Seon; Byun, Aram; Kim, Jin Woong

2014-03-01

Lipid molecules have both hydrophilic and hydrophobic properties. Since their packing parameter ranges from 0.5 to 1, they self-assemble to form a vesicle structure, liposome. Thanks to the vesicle structure, liposome is able to encapsulate both hydrophilic and hydrophobic active ingredients, thus widening its applicability to pharmaceutical, cosmetic, and food industry. However, its vesicular structure is readily transferred to micelle in the presence of amphiphilic additives with low packing parameters. Therefore, it is critical to developing a technique to overcome this drawback. This study introduces a microfluidic approach to physically immobilize liposome in microgel particles. For this, we generate a uniform liposome-in-oil-in-water emulsion in a capillary-based microfluidic device. Basically, we observe how the flows in micro-channels affect generation of embryo emulsion drops. Then, the uniform emulsion is solidified by using photo-polymerization. Finally, we characterize the particle morphology, membrane fluidity, and mesh property, encapsulation efficiency and releasing.

Preparation of polystyrene/SiO2 microsphere via Pickering emulsion polymerization: Synergistic effect of SiO2 concentrations and initiator sorts

NASA Astrophysics Data System (ADS)

Zhou, Haiou; Shi, Tiejun; Zhou, Xun

2013-02-01

In this paper, polystyrene (PS)/SiO2 microspheres were successfully prepared via Pickering emulsion polymerization stabilized solely by ethacryloxypropyltrimethoxysilane (MPTMS) modified SiO2 nanoparticles. The formation mechanisms of PS/SiO2 microspheres with different morphology were investigated under various Pickering emulsion polymerization conditions. The results showed that SiO2 concentrations and initiator sorts would synergistically impact on the morphology of products corresponding to distinct formation mechanisms. When SiO2 concentrations was low and water-solute initiator potassium persulfate (KPS) was used, aqueous nucleation was dominant, which was deduced to the formation of dispersive microspheres sparsely anchored by SiO2 particles. When SiO2 concentrations was increased and oil-solute initiator azobisisobutyronitrile (AIBN) was applied, nucleation in oil phase prevailed which lead to the formation of microspheres densely packed by SiO2 particles.

The Effect of Surfactant and Compatibilizer on Inorganic Loading and Properties of PPO-based EPMM Membranes

NASA Astrophysics Data System (ADS)

Bissadi, Golnaz

Hybrid membranes represent a promising alternative to the limitations of organic and inorganic materials for high productivity and selectivity gas separation membranes. In this study, the previously developed concept of emulsion-polymerized mixed matrix (EPMM) membranes was further advanced by investigating the effects of surfactant and compatibilizer on inorganic loading in poly(2,6-dimethyl-1,4-phenylene oxide) (PPO)-based EPMM membranes, in which inorganic part of the membranes originated from tetraethylorthosilicate (TEOS). The polymerization of TEOS, which consists of hydrolysis of TEOS and condensation of the hydrolyzed TEOS, was carried out as (i) one- and (ii) two-step processes. In the one-step process, the hydrolysis and condensation take place in the same environment of a weak acid provided by the aqueous solution of aluminum hydroxonitrate and sodium carbonate. In the two-step process, the hydrolysis takes place in the environment of a strong acid (solution of hydrochloric acid), whereas the condensation takes place in weak base environment obtained by adding excess of the ammonium hydroxide solution to the acidic solution of the hydrolyzed TEOS. For both one- and two-step processes, the emulsion polymerization of TEOS was carried out in two types of emulsions made of (i) pure trichloroethylene (TCE) solvent, and (ii) 10 w/v% solution of PPO in TCE, using different combinations of the compatibilizer (ethanol) and the surfactant (n-octanol). The experiments with pure TCE, which are referred to as a gravimetric powder method (GPM) allowed assessing the effect of different experimental parameters on the conversion of TEOS. The GPM tests also provided a guide for the synthesis of casting emulsions containing PPO, from which the EPMM membranes were prepared using a spin coating technique. The synthesized EPMM membranes were characterized using 29Si nuclear magnetic resonance (29Si NMR), differential scanning calorimetry (DSC), inductively coupled plasma mass spectrometry (ICP-MS), and gas permeation measurements carried out in a constant pressure (CP) system. The 29Si NMR analysis verified polymerization of TEOS in the emulsions made of pure TCE, and the PPO solution in TCE. The conversions of TEOS in the two-step process in the two types of emulsions were very close to each other. In the case of the one-step process, the conversions in the TCE emulsion were significantly greater than those in the emulsion of the PPO solution in TCE. Consequently, the conversions of TEOS in the EPMM membranes made in the two-step process were greater than those in the EPMM membranes made in the one-step process. The latter ranged between 10 - 20%, while the highest conversion in the two-step process was 74% in the presence of pure compatibilizer with no surfactant. Despite greater conversions and hence the greater inorganic loadings, the EPMM membranes prepared in the two-step process had glass transition temperatures (Tg) only slightly greater than the reference PPO membranes. In contrast, despite relatively low inorganic loadings, the EPMM membranes prepared in the one-step process had Tgs markedly greater than PPO, and showed the expected trend of an increase in Tg with the inorganic loading. These results indicate that in the case of the one-step process the polymerized TEOS was well integrated with the PPO chains and the interactions between the two phases lead to high Tgs. On the other hand, this was not the case for the EPMM membranes prepared in the two-step process, suggesting possible phase separation between the polymerized TEOS and the organic phase. The latter was confirmed by detecting no selectivity in the EPMM membranes prepared by the two-step process. In contrast, the EPMM membranes prepared in the one-step process in the presence of the compatibilizer and no surfactant showed 50% greater O2 permeability coefficient and a slightly greater O2/N2 permeability ratio compared to the reference PPO membranes.

SOURCE ASSESSMENT: POLYVINYL CHLORIDE

EPA Science Inventory

This report summarizes data on air emissions from the polyvinyl chloride (PVC) industry. PVC is manufactured by 20 companies at 35 plants. Each plant uses one or more of four possible polymerization processes: (1) suspension polymerization, (2) emulsion polymerization, (3) bulk p...

Liquid-liquid two phase systems for the production of porous hydrogels and hydrogel microspheres for biomedical applications: A tutorial review

PubMed Central

Elbert, Donald L.

2010-01-01

Macroporous hydrogels may have direct applications in regenerative medicine as scaffolds to support tissue formation. Hydrogel microspheres may be used as drug delivery vehicles or as building blocks to assemble modular scaffolds. A variety of techniques exist to produce macroporous hydrogels and hydrogel microspheres. A subset of these relies on liquid-liquid two phase systems. Within this subset, vastly different types of polymerization processes are found. In this review, the history, terminology and classification of liquid-liquid two phase polymerization and crosslinking are described. Instructive examples of hydrogel microsphere and macroporous scaffold formation by precipitation/dispersion, emulsion and suspension polymerizations are used to illustrate the nature of these processes. The role of the kinetics of phase separation in determining the morphology of scaffolds and microspheres is also delineated. Brief descriptions of miniemulsion, microemulsion polymerization and ionotropic gelation are also included. PMID:20659596

Bio-Functional, Lanthanide-Labeled Polymer Particles by Seeded Emulsion Polymerization and their Characterization by Novel ICP-MS Detection.

PubMed

Thickett, Stuart C; Abdelrahman, Ahmed I; Ornatsky, Olga; Bandura, Dmitry; Baranov, Vladimir; Winnik, Mitchell A

2010-01-01

We present the synthesis and characterization of monodisperse, sub-micron poly(styrene) (PS) particles loaded with up to and including 10(7) lanthanide (Ln) ions per particle. These particles have been synthesized by seeded emulsion polymerization with a mixture of monomer and a pre-formed Ln complex, and analyzed on a particle-by-particle basis by a unique inductively coupled plasma mass cytometer. Seed particles were prepared by surfactant-free emulsion polymerization (SFEP) to obtain large particle sizes in aqueous media. Extensive surface acid functionality was introduced using the acid-functional initiator ACVA, either during seed latex synthesis or in the second stage of polymerization. The loading of particles with three different Ln ions (Eu, Tb, and Ho) has proven to be close to 100 % efficient on an individual and combined basis. Covalent attachment of metal-tagged peptides and proteins such as Neutravidin to the particle surface was shown to be successful and the number of bound species can be readily determined. We believe these particles can serve as precursors for multiplexed, bead-based bio-assays utilizing mass cytometric detection.

Bio-Functional, Lanthanide-Labeled Polymer Particles by Seeded Emulsion Polymerization and their Characterization by Novel ICP-MS Detection

PubMed Central

Thickett, Stuart C.; Abdelrahman, Ahmed I.; Ornatsky, Olga; Bandura, Dmitry; Baranov, Vladimir; Winnik, Mitchell A.

2010-01-01

We present the synthesis and characterization of monodisperse, sub-micron poly(styrene) (PS) particles loaded with up to and including 107 lanthanide (Ln) ions per particle. These particles have been synthesized by seeded emulsion polymerization with a mixture of monomer and a pre-formed Ln complex, and analyzed on a particle-by-particle basis by a unique inductively coupled plasma mass cytometer. Seed particles were prepared by surfactant-free emulsion polymerization (SFEP) to obtain large particle sizes in aqueous media. Extensive surface acid functionality was introduced using the acid-functional initiator ACVA, either during seed latex synthesis or in the second stage of polymerization. The loading of particles with three different Ln ions (Eu, Tb, and Ho) has proven to be close to 100 % efficient on an individual and combined basis. Covalent attachment of metal-tagged peptides and proteins such as Neutravidin to the particle surface was shown to be successful and the number of bound species can be readily determined. We believe these particles can serve as precursors for multiplexed, bead-based bio-assays utilizing mass cytometric detection. PMID:20396648

Self-Assembled Colloidal Particle Clusters from In Situ Pickering-Like Emulsion Polymerization via Single Electron Transfer Mechanism.

PubMed

Yuan, Jinfeng; Zhao, Weiting; Pan, Mingwang; Zhu, Lei

2016-08-01

A simple route is reported to synthesize colloidal particle clusters (CPCs) from self-assembly of in situ poly(vinylidene fluoride)/poly(styrene-co-tert-butyl acrylate) [PVDF/P(St-co-tBA)] Janus particles through one-pot seeded emulsion single electron transfer radical polymerization. In the in situ Pickering-like emulsion polymerization, the tBA/St/PVDF feed ratio and polymerization temperature are important for the formation of well-defined CPCs. When the tBA/St/PVDF feed ratio is 0.75 g/2.5 g/0.5 g and the reaction temperature is 35 °C, relatively uniform raspberry-like CPCs are obtained. The hydrophobicity of the P(St-co-tBA) domains and the affinity of PVDF to the aqueous environment are considered to be the driving force for the self-assembly of the in situ formed PVDF/P(St-co-tBA) Janus particles. The resultant raspberry-like CPCs with PVDF particles protruding outward may be promising for superhydrophobic smart coatings. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Silicone-containing aqueous polymer dispersions with hybrid particle structure.

PubMed

Kozakiewicz, Janusz; Ofat, Izabela; Trzaskowska, Joanna

2015-09-01

In this paper the synthesis, characterization and application of silicone-containing aqueous polymer dispersions (APD) with hybrid particle structure are reviewed based on available literature data. Advantages of synthesis of dispersions with hybrid particle structure over blending of individual dispersions are pointed out. Three main processes leading to silicone-containing hybrid APD are identified and described in detail: (1) emulsion polymerization of organic unsaturated monomers in aqueous dispersions of silicone polymers or copolymers, (2) emulsion copolymerization of unsaturated organic monomers with alkoxysilanes or polysiloxanes with unsaturated functionality and (3) emulsion polymerization of alkoxysilanes (in particular with unsaturated functionality) and/or cyclic siloxanes in organic polymer dispersions. The effect of various factors on the properties of such hybrid APD and films as well as on hybrid particles composition and morphology is presented. It is shown that core-shell morphology where silicones constitute either the core or the shell is predominant in hybrid particles. Main applications of silicone-containing hybrid APD and related hybrid particles are reviewed including (1) coatings which show specific surface properties such as enhanced water repellency or antisoiling or antigraffiti properties due to migration of silicone to the surface, and (2) impact modifiers for thermoplastics and thermosets. Other processes in which silicone-containing particles with hybrid structure can be obtained (miniemulsion polymerization, polymerization in non-aqueous media, hybridization of organic polymer and polysiloxane, emulsion polymerization of silicone monomers in silicone polymer dispersions and physical methods) are also discussed. Prospects for further developments in the area of silicone-containing hybrid APD and related hybrid particles are presented. Copyright © 2015. Published by Elsevier B.V.

Effect of cationic monomer content on polyacrylamide copolymers by frit-inlet asymmetrical flow field-flow fractionation/multi-angle light scattering.

PubMed

Lee, Hyejin; Kim, Jin Yong; Choi, Woonjin; Moon, Myeong Hee

2017-06-23

In this study, ultrahigh-molecular-weight (MW) (>10 7 Da) cationic polyacrylamides (C-PAMs), which are water-soluble polymers used in waste water treatment, were characterized using frit-inlet asymmetrical flow field-flow fractionation coupled with multi-angle light scattering and differential refractive detection. C-PAMs copolymerized with acryloxyethyltrimethyl ammonium chloride (DAC) were prepared by varying the feed amount of cationic monomer, polymerization method (solution vs. emulsion), and degree of branching. The MW of the copolymers prepared using emulsion polymerization (10 7 -10 9 Da) was generally larger than that of copolymers prepared using solution polymerization (4×10 7 -10 8 Da). When the amount of cationic monomer was increased from 10 to 55mol% in solution polymerization, hydrophobic contraction of the core induced formation of more compact C-PAMs. The copolymers prepared using emulsion polymerization formed highly aggregated or supercoil structures owing to increased intermolecular hydrophobic interaction when less cationic monomer was used. However, the MW decreased with increased cationic group content. In addition, C-PAMs larger than ∼10 8 Da prepared using the emulsion method were separated by steric/hyperlayer elution mode while those in the 10 7 -10 8 Da range were analyzed in either normal or steric/hyperlayer mode depending on the decay patterns of field programming. Moreover, branched copolymers were found to be resolved with different elution modes under the same field decay pattern depending on the degree of branching: steric/hyperlayer for low-branching and normal for high-branching C-PAMs. Copyright © 2017 Elsevier B.V. All rights reserved.

Hollow latex particles: synthesis and applications.

PubMed

McDonald, Charles J; Devon, Michael J

2002-12-02

One of the major developments in emulsion polymerization over the last two decades has been the ability to make hollow latex particles. This has contributed many fundamental insights into the synthesis and the development of structure in particles. Hollow latex particles also enhance the performance of industrial coatings and potentially are useful in other technologies such as microencapsulation and controlled release. Ever since the publication of the initial process patents describing these particles, there has been a global R&D effort to extend the synthetic techniques and applications. One prominent synthetic approach to hollow particles is based on osmotic swelling. This dominates the literature, and usually starts with the synthesis of a structured latex particle containing an ionizable core that is subsequently expanded with the addition of base. Fundamental to this approach are a sophisticated control of transport phenomena, chemical reactivity within the particle, and the thermoplastic properties of the polymer shell. Hydrocarbon encapsulation technology has also been employed to make hollow latex particles. One approach involves a dispersed ternary system that balances transport, conversion kinetics, and phase separation variables to achieve the hollow morphology. Other techniques, including the use of blowing agents, are also present in the literature. The broad range of approaches that affords particles with a hollow structure demonstrates the unique flexibility of the emulsion polymerization process.

Asphaltene dispersants as demulsification aids

DOE Office of Scientific and Technical Information (OSTI.GOV)

Manek, M.B.

1995-11-01

Destabilization of petroleum asphaltenes may cause a multitude of problems in crude oil recovery and production. One major problem is their agglomeration at the water-oil interface of crude oil emulsions. Once agglomeration occurs, destabilized asphaltenes can form a thick pad in the dehydration equipment, which significantly reduces the demulsification rate. Certain polymeric dispersants increase asphaltene solubilization in hydrocarbon media, and when used in conjunction with emulsion breakers, facilitate the demulsification process. Two case studies are presented that demonstrate how asphaltene dispersants can efficiently inhibit pad formation and help reduce demulsifier dosage. Criteria for dispersant application and selection are discussed, whichmore » include the application of a novel laboratory technique to assess asphaltene stabilization in the crude oil. The technique monitors asphaltene agglomeration while undergoing titration with an incompatible solvent (precipitant). The method was used to evaluate stabilization of asphaltenes in the crude oil and to screen asphaltene dispersants.« less

Galantamine-loaded PLGA nanoparticles, from nano-emulsion templating, as novel advanced drug delivery systems to treat neurodegenerative diseases

NASA Astrophysics Data System (ADS)

Fornaguera, C.; Feiner-Gracia, N.; Calderó, G.; García-Celma, M. J.; Solans, C.

2015-07-01

Polymeric nanoparticles could be promising drug delivery systems to treat neurodegenerative diseases. Among the various methods of nanoparticle preparation, nano-emulsion templating was used in the present study to prepare galantamine-loaded nano-emulsions by a low-energy emulsification method followed by solvent evaporation to obtain galantamine-loaded polymeric nanoparticles. This approach was found to be suitable because biocompatible, biodegradable and safe nanoparticles with appropriate features (hydrodynamic radii around 20 nm, negative surface charge and stability higher than 3 months) for their intravenous administration were obtained. Encapsulation efficiencies higher than 90 wt% were obtained with a sustained drug release profile as compared to that from aqueous and micellar solutions. The enzymatic activity of the drug was maintained at 80% after its encapsulation into nanoparticles that were non-cytotoxic at the required therapeutic concentration. Therefore, novel galantamine-loaded polymeric nanoparticles have been designed for the first time using the nano-emulsification approach and showed the appropriate features to become advanced drug delivery systems to treat neurodegenerative diseases.Polymeric nanoparticles could be promising drug delivery systems to treat neurodegenerative diseases. Among the various methods of nanoparticle preparation, nano-emulsion templating was used in the present study to prepare galantamine-loaded nano-emulsions by a low-energy emulsification method followed by solvent evaporation to obtain galantamine-loaded polymeric nanoparticles. This approach was found to be suitable because biocompatible, biodegradable and safe nanoparticles with appropriate features (hydrodynamic radii around 20 nm, negative surface charge and stability higher than 3 months) for their intravenous administration were obtained. Encapsulation efficiencies higher than 90 wt% were obtained with a sustained drug release profile as compared to that from aqueous and micellar solutions. The enzymatic activity of the drug was maintained at 80% after its encapsulation into nanoparticles that were non-cytotoxic at the required therapeutic concentration. Therefore, novel galantamine-loaded polymeric nanoparticles have been designed for the first time using the nano-emulsification approach and showed the appropriate features to become advanced drug delivery systems to treat neurodegenerative diseases. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr03474d

Synthesis and Characterization of Graft Copolymers Poly(isoprene-g-styrene) of High Molecular Weight by a Combination of Anionic Polymerization and Emulsion Polymerization

DOE PAGES

Wang, Wenwen; Wang, Weiyu; Li, Hui; ...

2015-01-14

In this study, high molecular weight “comb-shaped” graft copolymers, poly(isoprene-g-styrene), with polyisoprene as the backbone and polystyrene as side chains, were synthesized via free radical emulsion polymerization by copolymerization of isoprene with a polystyrene macromonomer synthesized using anionic polymerization. A small amount of toluene was used in order to successfully disperse the macromonomer. Both a redox and thermal initiation system were used in the emulsion polymerization, and the latex particle size and distribution were investigated by dynamic light scattering. The structural characteristics of the macromonomer and comb graft copolymers were investigated through use of size exclusion chromatography, spectroscopy, microscopy, thermalmore » analysis, and rheology. While the macromonomer was successfully copolymerized to obtain the desired multigraft copolymers, small amounts of unreacted macromonomer remained in the products, reflecting its reduced reactivity due to steric effects. Nevertheless, the multigraft copolymers obtained were very high in molecular weight (5–12 × 10 5 g/mol) and up to 10 branches per chain, on average, could be incorporated. A material incorporating 29 wt% polystyrene exhibits a disordered microphase separated morphology and elastomeric properties. As a result, these materials show promise as new, highly tunable, and potentially low cost thermoplastic elastomers.« less

Investigation of in vitro Hydrophilic and Hydrophobic Dual Drug Release from Polymeric Films Produced by Sodium alginate-MaterBi® Drying Emulsions.

PubMed

Setti, Chiara; Suarato, Giulia; Perotto, Giovanni; Athanassiou, Athanassia; Bayer, Ilker S

2018-06-18

Emulsions are known to be effective carriers of hydrophobic drugs, and particularly injectable emulsions have been successfully implemented for in vivo controlled drug release. Recently, high internal phase emulsions have also been used to produce porous polymeric templates for pharmaceutical applications. However, emulsions containing dissolved biopolymers both in the oil and water phases are very scarce. In this study, we demonstrate such an emulsion, in which the oil phase contains a hydrophobic biodegradable polymer, MaterBi ® , and the water phase is aqueous sodium alginate dispersion. The two phases were emulsified simply by ultrasonic processing without any surfactants. The emulsions were stable for several days and were dried into composite solid films with varying MaterBi ® /alginate fractions. The films were loaded with two model drugs, a hydrophilic eosin-based cutaneous antiseptic and the hydrophobic curcumin. Drug release capacity of the films was investigated in detail, and controlled release of each model drug was achieved either by tuning the polymer fraction in the films during emulsification or by crosslinking sodium alginate fraction of the films by calcium salt solution immersion. The emulsions can be formulated to carry either a single model drug or both drugs depending on the desired application. Films demonstrate excellent cell biocompatibility against human dermal fibroblast, adult cells. Copyright © 2018. Published by Elsevier B.V.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Habercorn, Lasse; Merkl, Jan-Philip; Kloust, Hauke Christian

With the polymer encapsulation of quantum dots via seeded emulsion polymerization we present a powerful tool for the preparation of fluorescent nanoparticles with an extraordinary stability in aqueous solution. The method of the seeded emulsion polymerization allows a straightforward and simple in situ functionalization of the polymer shell under preserving the optical properties of the quantum dots. These requirements are inevitable for the application of semiconductor nanoparticles as markers for biomedical applications. Polymer encapsulated quantum dots have shown only a marginal loss of quantum yields when they were exposed to copper(II)-ions. Under normal conditions the quantum dots were totally quenchedmore » in presence of copper(II)-ions. Furthermore, a broad range of in situ functionalized polymer-coated quantum dots were obtained by addition of functional monomers or surfactants like fluorescent dye molecules, antibodies or specific DNA aptamers. Furthermore the emulsion polymerization can be used to prepare multifunctional hybrid systems, combining different nanoparticles within one construct without any adverse effect of the properties of the starting materials.{sup 1,2}.« less

Application of mercapto-silica polymerized high internal phase emulsions for the solid-phase extraction and preconcentration of trace lead(II).

PubMed

Su, Rihui; Ruan, Guihua; Chen, Zhengyi; Du, Fuyou; Li, Jianping

2015-12-01

A new class of solid-phase extraction column prepared with grafted mercapto-silica polymerized high internal phase emulsion particles was used for the preconcentration of trace lead. First, mercapto-silica polymerized high internal phase emulsion particles were synthesized by using high internal phase emulsion polymerization and carefully assembled in a polyethylene syringe column. The influences of various parameters including adsorption pH value, adsorption and desorption solvents, flow rate of the adsorption and desorption procedure were optimized, respectively, and the suitable uploading sample volumes, adsorption capacity, and reusability of solid phase extraction column were also investigated. Under the optimum conditions, Pb(2+) could be preconcentrated quantitatively over a wide pH range (2.0-5.0). In the presence of foreign ions, such as Na(+) , K(+) , Ca(2+) , Zn(2+) , Mg(2+) , Cu(2+) , Fe(2+) , Cd(2+) , Cl(-) and NO3 (-) , Pb(2+) could be recovered successfully. The prepared solid-phase extraction column performed with high stability and desirable durability, which allowed more than 100 replicate extractions without measurable changes of performance. The feasibility of the developed method was further validated by the extraction of Pb(2+) in rice samples. At three spiked levels of 40.0, 200 and 800 μg/kg, the average recoveries for Pb(2+) in rice samples ranged from 87.3 to 105.2%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Surfactant-free, cationic latices of poly(BMA-co-MMA) using AIBA initiator.

PubMed

Lee, Ki-Chang

2013-09-01

When polymer particles come into use, especially, for photonic crystal applications, their diameter, dispersivity, and refractive indices become very important. Poly(benzyl methacrylate) is known to be a kind of high refracive materials (n = 1.57) compared to poly(methyl methacrylate) (n = 1.49). Not many work was concerned for surfactant-free emulsion polymerization of benzyl methacrylate or its copolymerization using cationic initiators. Narrowly dispersed cationic poly(BMA-co-MMA) and PBMA latices were synthesized successfully by surfactant-free emulsion polymerization with AIBA. The influences of BMA/MMA ratio, BMA/MMA monomer and initiator concentrations, addition of DVB/EGDMA crosslink agent, and polymerization temperature on the kinetics and on the particle size and molecular weight were studied. Monodisperse cationic charged PBMA and poly(BMA-coMMA) latices with particle diameters varying between 160-494 nm and polymer molecular weights of the order 1.25 x 10(4) to 7.55 x 10(4) g/mol were prepared. The rate of polymerization increased with increasing MMA concentration in BMA/MMA ratio, AIBA concentration, DVB crosslink agent, and polymerization temperature. The particle diameter increased with BMA concentration in BMA/MMA ratio, AIBA concentration, and BMA/MMA monomer concentration. The molecular weight increased with BMA concentration in BMA/MMA ratio and BMA/MMA monomer concentration. The glass transition temperature of the latex copolymers decreased with increasing amount of BMA from 375 K for PMMA to 321 K for PBMA. It was, thus, found that the particle diameter and rate of polymerization as well as the polymer molecular weight for surfactant-free emulsion polymerization of BMA and MMA can be controlled easily by controlling the BMA/MMA ratio, BMA/MMA monomer concentration, AIBA concentration, and polymerization temperature.

Contribution of galloylation and polymerization to the antioxidant activity of polyphenols in fish lipid systems.

PubMed

Iglesias, Jacobo; Pazos, Manuel; Lois, Salomé; Medina, Isabel

2010-06-23

Polyphenolic fractions extracted from pine (Pinus pinaster) bark, grape (Vitis vinifera) pomace, and witch hazel (Hamamelis virginiana) bark were selected for investigating the influence of the number of phenolic units, polymerization, and the content of esterified galloyl residues (galloylation) on their efficacy for inhibiting lipid oxidation in fish lipid enriched foodstuffs. Experiments carried out with nongalloylated pine bark fractions with different polymerization degrees demonstrated that the number of catechin residues per molecule modulates their reducing and chelating properties in solution. In real food systems such as bulk fish oil and fish oil-in-water emulsions, the efficacy against lipid oxidation was highly dependent on the physical location of the antioxidant at the oxidative sensitive sites. The lowest polymerized fractions were the most efficient in bulk fish oil samples, whereas proanthocyanidins with an intermediate polymerization degree showed the highest activity in fish oil-in-water emulsions. Galloylation did not influence the antioxidant effectiveness of proanthocyanidins in bulk fish oils. The presence of galloyl groups favored the antioxidant activity of the polyphenols in emulsions, although results indicated that a high degree of galloylation did not improve significantly the activity found with medium galloylated proanthocyanidins. The results obtained in this research provide useful information about the relationship between structure and antioxidant activity in order to design antioxidant additives with application in fish oil-enriched functional foods.

Manufacture of poly(methyl methacrylate) microspheres using membrane emulsification

PubMed Central

Bux, Jaiyana; Manga, Mohamed S.; Hunter, Timothy N.

2016-01-01

Accurate control of particle size at relatively narrow polydispersity remains a key challenge in the production of synthetic polymer particles at scale. A cross-flow membrane emulsification (XME) technique was used here in the preparation of poly(methyl methacrylate) microspheres at a 1–10 l h−1 scale, to demonstrate its application for such a manufacturing challenge. XME technology has previously been shown to provide good control over emulsion droplet sizes with careful choice of the operating conditions. We demonstrate here that, for an appropriate formulation, equivalent control can be gained for a precursor emulsion in a batch suspension polymerization process. We report here the influence of key parameters on the emulsification process; we also demonstrate the close correlation in size between the precursor emulsion and the final polymer particles. Two types of polymer particle were produced in this work: a solid microsphere and an oil-filled matrix microcapsule. This article is part of the themed issue ‘Soft interfacial materials: from fundamentals to formulation’. PMID:27298430

Well-Defined High Molecular Weight Polystyrene with High Rates and High Livingness Synthesized via Two-Stage RAFT Emulsion Polymerization.

PubMed

Yan, Kun; Gao, Xiang; Luo, Yingwu

2015-07-01

A highly living polymer with over 100 kg mol(-1) molecular weight is very difficult to achieve by controlled radical polymerization since the unavoidable side reactions of irreversible radical termination and radical chain transfer to monomer reaction become significant. It is reported that over 500 kg mol(-1) polystyrene with high livingness and low dispersity could be synthesized by a facile two-stage reversible addition-fragmentation transfer emulsion polymerization. The monomer conversion reaches 90% within 10 h. High livingness of the product is ascribed to the extremely low initiator concentration and the chain transfer constant for monomer unexpectedly much lower than the well-accepted values in the conventional radical polymerization. The two-stage monomer feeding policy much decreases the dispersity of the product. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microchannel emulsification: A promising technique towards encapsulation of functional compounds.

PubMed

Khalid, Nauman; Kobayashi, Isao; Neves, Marcos A; Uemura, Kunihiko; Nakajima, Mitsutoshi

2017-06-13

This review provides an overview of microchannel emulsification (MCE) for production of functional monodispersed emulsion droplets. The main emphasis has been put on functional bioactives encapsulation using grooved-type and straight-through microchannel array plates. MCE successfully encapsulates the bioactives like β-carotene, oleuropein, γ-oryzanol, β-sitosterol, L-ascorbic acid and ascorbic acid derivatives, vitamin D and quercetin. These bioactives were encapsulated in a variety of delivery systems like simple and multiple emulsions, polymeric particles, microgels, solid lipid particles and functional vesicles. The droplet generation process in MCE is based upon spontaneous transformation of interfaces rather than high energy shear stress systems. The scale-up of MCE can increase the productivity of monodispersed droplets >100 L h -1 and makes it a promising tool at industrial level.

Preparation of l-phenylalanine-imprinted solid-phase extraction sorbent by Pickering emulsion polymerization and the selective enrichment of l-phenylalanine from human urine.

PubMed

Li, Ji; Hu, Xiaoling; Guan, Ping; Zhang, Xiaoyan; Qian, Liwei; Zhang, Nan; Du, Chunbao; Song, Renyuan

2016-05-01

A novel l-phenylalanine molecularly imprinted solid-phase extraction sorbent was synthesized by the combination of Pickering emulsion polymerization and ion-pair dummy template imprinting. Compared to other polymerization methods, the molecularly imprinted polymers thus prepared exhibit a high specific surface, large pore diameter, and appropriate particle size. The key parameters for solid-phase extraction were optimized, and the result indicated that the molecularly imprinted polymer thus prepared exhibits a good recovery of 98.9% for l-phenylalanine. Under the optimized conditions of the procedure, an analytical method for l-phenylalanine was well established. By comparing the performance of the molecularly imprinted polymer and a commercial reverse-phase silica gel, the obtained molecularly imprinted polymer as an solid-phase extraction sorbent is more suitable, exhibiting high precision (relative standard deviation 3.2%, n = 4) and a low limit of detection (60.0 ± 1.9 nmol·L(-1) ) for the isolation of l-phenylalanine. Based on these results, the combination of the Pickering emulsion polymerization and ion-pair dummy template imprinting is effective for preparing selective solid-phase extraction sorbents for the separation of amino acids and organic acids from complex biological samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

New hybrid latexes from a soybean oil-based waterborne polyurethane and acrylics via emulsion polymerization.

PubMed

Lu, Yongshang; Larock, Richard C

2007-10-01

A series of new waterborne polyurethane (PU)/acrylic hybrid latexes have been successfully synthesized by the emulsion polymerization of acrylic monomers (butyl acrylate and methyl methacrylate) in the presence of a soybean oil-based waterborne PU dispersion using potassium persulfate as an initiator. The waterborne PU dispersion has been synthesized by a polyaddition reaction of toluene 2,4-diisocyanate and a soybean oil-based polyol (SOL). The resulting hybrid latexes, containing 15-60 wt % SOL as a renewable resource, are very stable and exhibit uniform particle sizes of 125 +/- 20 nm as determined by transmittance electronic microscopy. The structure, thermal, and mechanical properties of the resulting hybrid latex films have been investigated by Fourier transform infrared spectroscopy, solid state 13C NMR spectroscopy, dynamic mechanical analysis, extraction, and mechanical testing. Grafting copolymerization of the acrylic monomers onto the PU network occurs during the emulsion polymerization, leading to a significant increase in the thermal and mechanical properties of the resulting hybrid latexes. This work provides a new way of utilizing renewable resources to prepare environmentally friendly hybrid latexes with high performance for coating applications.

Study and Optimization on graft polymerization under normal pressure and air atmospheric conditions, and its application to metal adsorbent

NASA Astrophysics Data System (ADS)

Ueki, Yuji; Chandra Dafader, Nirmal; Hoshina, Hiroyuki; Seko, Noriaki; Tamada, Masao

2012-07-01

Radiation-induced graft polymerization of glycidyl methacrylate (GMA) onto non-woven polyethylene (NWPE) fabric was achieved under normal pressure and air atmospheric conditions, without using unique apparatus such as glass ampoules or vacuum lines. To attain graft polymerization under normal pressure and air atmospheric conditions, the effects of the pre-irradiation dose, pre-irradiation atmosphere, pre-irradiation temperature, de-aeration of GMA-emulsion, grafting atmosphere in a reactor, and dissolved oxygen (DO) concentration in GMA-emulsion on the degree of grafting (Dg) were investigated in detail. It was found that the DO concentration had the strongest influence, the pre-irradiation dose, de-aeration of emulsion and grafting atmosphere had a relatively strong impact, and the pre-irradiation atmosphere and pre-irradiation temperature had the least effect on Dg. The optimum DO concentration before grafting was 2.0 mg/L or less. When a polyethylene bottle was used as a reactor instead of a glass ampoule, graft polymerization under normal pressure and air atmospheric conditions could be achieved under the following conditions; the pre-irradiation dose was more than 50 kGy, the volume ratio of GMA-emulsion to air was 50:1 or less, and the DO concentration in GMA-emulsion during grafting was below 2.0 mg/L. Under these grafting conditions, Dg was controlled within a range of up to 362%. The prepared GMA-grafted NWPE (GMA-g-NWPE) fabric was modified with a phosphoric acid to obtain an adsorbent for heavy metal ions. In the column-mode adsorption tests of Pb(II), the adsorption performance of the produced phosphorylated GMA-g-NWPE fabric (fibrous metal adsorbent) was not essentially dependent on the flow rate of the feed. The breakthrough points of 200, 500, and 1000 h-1 in space velocity were 483, 477 and 462 bed volumes, and the breakthrough capacities of the three flow rates were 1.16, 1.15 and 1.16 mmol-Pb(II)/g-adsorbent.

Non-coalescence of oppositely charged droplets in pH-sensitive emulsions

PubMed Central

Liu, Tingting; Seiffert, Sebastian; Thiele, Julian; Abate, Adam R.; Weitz, David A.; Richtering, Walter

2012-01-01

Like charges stabilize emulsions, whereas opposite charges break emulsions. This is the fundamental principle for many industrial and practical processes. Using micrometer-sized pH-sensitive polymeric hydrogel particles as emulsion stabilizers, we prepare emulsions that consist of oppositely charged droplets, which do not coalesce. We observe noncoalescence of oppositely charged droplets in bulk emulsification as well as in microfluidic devices, where oppositely charged droplets are forced to collide within channel junctions. The results demonstrate that electrostatic interactions between droplets do not determine their stability and reveal the unique pH-dependent properties of emulsions stabilized by soft microgel particles. The noncoalescence can be switched to coalescence by neutralizing the microgels, and the emulsion can be broken on demand. This unusual feature of the microgel-stabilized emulsions offers fascinating opportunities for future applications of these systems. PMID:22203968

Characterization of cinematographic films by Laser Induced Breakdown Spectroscopy

NASA Astrophysics Data System (ADS)

Gaspard, S.; Oujja, M.; Rebollar, E.; Abrusci, C.; Catalina, F.; Castillejo, M.

2007-12-01

The emulsion-coated transparent plastic-base film has been the main carrier for production and preservation of motion picture contents since the 19th century. The knowledge of the composition of black and white silver gelatine cinematographic films is of great importance for the characterization of the photographic process and for identifying the optimum conditions for conservation. A cinematographic film is a multi-component system that consists of a layer of photographic emulsion overcoating a polymeric support (plasticized cellulose triacetate) and a protective transparent cross-linked gelatine layer coating the emulsion. In the present work, Laser Induced Breakdown Spectroscopy (LIBS) is used to characterize the composition of the materials of cinematographic films. LIB spectra of film samples and of different individual film components, polymeric support and reference gelatines, were acquired in vacuum by excitation at 266 nm (Q-switched Nd:YAG laser, 6 ns, 10 Hz). In the cinematographic film, silver lines from the light-sensitive silver halide salts of the photographic emulsion are accompanied by iron, lead, chrome and phosphorus lines. Iron and lead are constituents of film developers, chrome is included in the composition of the hardening agents and phosphorus has its origin in the plasticizer used in the polymeric support. By applying successive pulses on the same spot of the film sample, it was possible to observe through stratigraphic analysis the different layers composition. Additionally, the results obtained reveal the analytical capacity of LIBS for the study and classification of the different gelatine types and qualities used for the protecting layer and the photographic emulsion.

Emulsifier-free emulsion polymerization produces highly charged, monodisperse particles for near infrared photonic crystals.

PubMed

Reese, Chad E; Asher, Sanford A

2002-04-01

We have developed emulsifier-free, emulsion polymerization recipes for the synthesis of highly charged, monodisperse latex particles of diameters between 500 and 1100 nm. These latexes consist of poly[styrene-(co-2-hydroxyethyl methacrylate)] spherical particles whose surfaces are functionalized with sulfate and carboxylic acid groups. These highly charged, monodisperse particles readily self-assemble into robust, three-dimensionally ordered crystalline colloidal array photonic crystals that Bragg diffract light in the near infrared spectral region. By altering the particle number density, the diffraction wavelength can be tuned from approximately 1000 to approximately 4000 nm.

Preparation, characterization, and in vitro gastrointestinal digestibility of oil-in-water emulsion-agar gels.

PubMed

Wang, Zheng; Neves, Marcos A; Kobayashi, Isao; Uemura, Kunihiko; Nakajima, Mitsutoshi

2013-01-01

Soybean oil-in-water (O/W) emulsion-agar gel samples were prepared and their digestibility evaluated by using an in vitro gastrointestinal digestion model. Emulsion-agar sols were obtained by mixing the prepared O/W emulsions with a 1.5 wt % agar solution at 60 °C, and their subsequent cooling at 5 °C for 1 h formed emulsion-agar gels. Their gel strength values increased with increasing degree of polymerization of the emulsifiers, and the relative gel strength increased in the case of droplets with an average diameter smaller than 700 nm. Flocculation and coalescence of the released emulsion droplets depended strongly on the emulsifier type; however, the emulsifier type hardly affected the ζ-potential of emulsion droplets released from the emulsion-agar gels during in vitro digestion. The total FFA content released from each emulsion towards the end of the digestion period was nearly twice that released from the emulsion-agar gel, indicating that gelation of the O/W emulsion may have delayed lipid hydrolysis.

Preparation of Pickering Double Emulsions Using Block Copolymer Worms

PubMed Central

2015-01-01

The rational formulation of Pickering double emulsions is described using a judicious combination of hydrophilic and hydrophobic block copolymer worms as highly anisotropic emulsifiers. More specifically, RAFT dispersion polymerization was utilized to prepare poly(lauryl methacrylate)–poly(benzyl methacrylate) worms at 20% w/w solids in n-dodecane and poly(glycerol monomethacrylate)–poly(2-hydroxypropyl methacrylate)–poly(benzyl methacrylate) worms at 13% w/w solids in water by polymerization-induced self-assembly (PISA). Water-in-oil-in-water (w/o/w) double emulsions can be readily prepared with mean droplet diameters ranging from 30 to 80 μm using a two-stage approach. First, a w/o precursor emulsion comprising 25 μm aqueous droplets is prepared using the hydrophobic worms, followed by encapsulation within oil droplets stabilized by the hydrophilic worms. The double emulsion droplet diameter and number of encapsulated water droplets can be readily varied by adjusting the stirring rate employed during the second stage. For each stage, the droplet volume fraction is relatively high at 0.50. The double emulsion nature of the final formulation was confirmed by optical and fluorescence microscopy studies. Such double emulsions are highly stable to coalescence, with little or no change in droplet diameter being detected over storage at 20 °C for 10 weeks as judged by laser diffraction. Preliminary experiments indicate that the complementary o/w/o emulsions can also be prepared using the same pair of worms by changing the order of homogenization, although somewhat lower droplet volume fractions were required in this case. Finally, we demonstrate that triple and even quadruple emulsions can be formulated using these new highly anisotropic Pickering emulsifiers. PMID:25834923

Investigation of Four Different Laponite Clays as Stabilizers in Pickering Emulsion Polymerization.

PubMed

Brunier, Barthélémy; Sheibat-Othman, Nida; Chniguir, Mehdi; Chevalier, Yves; Bourgeat-Lami, Elodie

2016-06-21

Clay-armored polymer particles were prepared by emulsion polymerization in the presence of Laponite platelets that adsorb at the surface of latex particles and act as stabilizers during the course of the polymerization. While Laponite RDS clay platelets are most often used, the choice of the type of clay still remains an open issue that is addressed in the present article. Four different grades of Laponite were investigated as stabilizers in the emulsion polymerization of styrene. First, the adsorption isotherms of the clays, on preformed polystyrene particles, were determined by ICP-AES analysis of the residual clay in the aqueous phase. Adsorption of clay depended on the type of clay at low concentrations corresponding to adsorption as a monolayer. Adsorption of clay particles as multilayers was observed for all the grades above a certain concentration under the considered ionic strength (mainly due to the initiator ionic species). The stabilization efficiency of these clays was investigated during the polymerization reaction (free of any other stabilizer). The clays did not have the same effect on stabilization, which was related to differences in their compositions and in their adsorption isotherms. The different grades led to different polymer particles sizes and therefore to different polymerization reaction rates. Laponite RDS and S482 gave similar results, ensuring the best stabilization efficiency and the fastest reaction rate; the number of particles increased as the clay concentration increased. Stabilization with Laponite XLS gave the same particles size and number as the latter two clays at low clay concentrations, but it reached an upper limit in the number of nucleated polymer particles at higher concentrations indicating a decrease of stabilization efficiency at high concentrations. Laponite JS did not ensure a sufficient stability of the polymer particles, as the polymerization results were comparable to a stabilizer-free polymerization system.

Production methodologies of polymeric and hydrogel particles for drug delivery applications.

PubMed

Lima, Ana Catarina; Sher, Praveen; Mano, João F

2012-02-01

Polymeric particles are ideal vehicles for controlled delivery applications due to their ability to encapsulate a variety of substances, namely low- and high-molecular mass therapeutics, antigens or DNA. Micro and nano scale spherical materials have been developed as carriers for therapies, using appropriated methodologies, in order to achieve a prolonged and controlled drug administration. This paper reviews the methodologies used for the production of polymeric micro/nanoparticles. Emulsions, phase separation, spray drying, ionic gelation, polyelectrolyte complexation and supercritical fluids precipitation are all widely used processes for polymeric micro/nanoencapsulation. This paper also discusses the recent developments and patents reported in this field. Other less conventional methodologies are also described, such as the use of superhydrophobic substrates to produce hydrogel and polymeric particulate biomaterials. Polymeric drug delivery systems have gained increased importance due to the need for improving the efficiency and versatility of existing therapies. This allows the development of innovative concepts that could create more efficient systems, which in turn may address many healthcare needs worldwide. The existing methods to produce polymeric release systems have some critical drawbacks, which compromise the efficiency of these techniques. Improvements and development of new methodologies could be achieved by using multidisciplinary approaches and tools taken from other subjects, including nanotechnologies, biomimetics, tissue engineering, polymer science or microfluidics.

Synthesis and characterization of functional acrylic copolymers via RAFT mini-emulsion polymerization

NASA Astrophysics Data System (ADS)

Yılmaz, Onur; Özkan, ćiǧdem Kılıçarislan; Yılmaz, Catalina N.; Yorgancıoǧlu, Ali; Özgünay, Hasan; Karavana, Hüseyin Ata

2017-12-01

Copolymers bearing reactive functional groups with controlled molecular weights are of importance since they can be used in many fields such as composites, coatings, membranes, catalysis, biology, optoelectronics, pharmaceuticals, etc. In the present study low molecular weight copolymers based on butyl acrylate (BA) and methyl methacrylate (MMA) in combination with reactive functional monomers of vinyl trietoxysilane (VTES), 3-trimetoxysilylpropyl methacrylate (TMSPMA) and glycidyl methacrylate (GMA) were synthesized via RAFT mini-emulsion technique using 2-cyano 2-propyldodecyldithiocarbonate as CTA agent. The results showed that the average molecular weights of copolymers were close to the theoretical values. On the other hand, PDI values were found to be higher than conventional RAFT polymers. The particle sizes of the latexes were small with very homogenous distributions and good stability. FTIR, H-NMR and TGA results verified the success of copolymer syntheses.

Differences in antioxidant activity between two rice protein concentrates in an oil-in-water emulsion

USDA-ARS?s Scientific Manuscript database

Two formulations of rice protein concentrates (RPC) derived from brown rice were evaluated for their antioxidant activity in bulk oil and in oil-in-water emulsions. Bulk oils were mixed with RPC and heated to 180°C, and total polar compounds and triacylglycerol polymerization were measured. Minimal ...

Annatto Polymeric Microparticles: Natural Product Encapsulation by the Emulsion-Solvent Evaporation Method

ERIC Educational Resources Information Center

Teixeira, Zaine; Duran, Nelson; Guterres, Silvia S.

2008-01-01

In this experiment, the extract from annatto seeds was encapsulated in poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) particles by the emulsion-solvent evaporation method. The particles were washed and centrifuged to remove excess stabilizer and then freeze-dried. The main compound of annatto seeds, bixin, has antioxidant properties as well…

Preparation of Fe 3O 4/poly(styrene-butyl acrylate-[2-(methacryloxy)ethyl]trimethylammonium chloride) by emulsifier-free emulsion polymerization and its interaction with DNA

NASA Astrophysics Data System (ADS)

Li, Xiaolong; Liu, Guoqiang; Yan, Wei; Chu, Paul K.; Yeung, Kelvin W. K.; Wu, Shuilin; Yi, Changfeng; Xu, Zushun

2012-04-01

Cationic magnetic polymer particles Fe3O4/poly(styrene-butyl acrylate-[2-(methacryloxy)ethyl]trimethylammonium chloride), a type of potential gene carrier, were prepared by emulsifier-free emulsion polymerization with oleic acid modified magnetite Fe3O4, styrene, butyl acrylate and [2-(methacryloxy)ethyl]trimethylammonium chloride) (METAC). The morphology of the particles was characterized by transmission electron microscopy and the composites of particles were characterized by FT-IR spectroscopy, X-ray diffraction. These results showed that magnetic particles were well dispersed in polymers with the content of about 15%(wt/wt). The composites exhibited superparamagnetism and possessed a certain level of magnetic response. The interactions between the particles with calf-thymus DNA (ct DNA) were confirmed by zeta potential measurement, UV-vis spectroscopy and fluorescence spectroscopy. The DNA-binding capacity determined by the agarose gel electrophoresis showed good binding capacity of the emulsion to DNA. These results suggested the potential of the cationic magnetic polymer emulsion as gene target delivery carrier.

Fabrication and evaluation of magnetic/hollow double-shelled imprinted sorbents formed by Pickering emulsion polymerization.

PubMed

Pan, Jianming; Li, Linzi; Hang, Hui; Wu, Runrun; Dai, Xiaohui; Shi, Weidong; Yan, Yongsheng

2013-06-25

Magnetic/hollow double-shelled imprinted polymers (MH-MIPs) were synthesized by Pickering emulsion polymerization. In this method, attapulgite (ATP) particles were used as stabilizers to establish a stable oil-in-water emulsion, and a few hydrophilic Fe3O4 nanoparticles were allowed to be magnetic separation carriers. The imprinting system was fabricated by radical polymerization in the presence of the functional and polymeric monomers in the oil phase. The results of characterization indicated that MH-MIPs exhibited magnetic sensitivity (Ms = 4.76 emu g(-1)), thermal stability (especially below 200 °C), and hollow structure and were composed of exterior ATP shells and interior imprinted polymers shells. Then MH-MIPs were evaluated as sorbents for the selective binding of λ-cyhalothrin as a result of their magnetism, enhanced mechanical strength, hydrophilic surface, and recognition ability. The kinetic properties of MH-MIPs were well described by the pseudo-second-order equation, indicating that the chemical process could be the rate-limiting step in the adsorption process for λ-cyhalothrin. The equilibrium adsorption capacity of MH-MIPs was 60.06 μmol g(-1) at 25 °C, and the Langmuir isotherm model gave a better fit to the experimental data, indicating the monolayer molecular adsorption for λ-cyhalothrin. The selective recognition experiments also demonstrated the high affinity and selectivity of MH-MIIPs toward λ-cyhalothrin over fenvalerate and diethyl phthalate.

Magnetic properties of the Fe{sup II} spin crossover complex in emulsion polymerization of trifluoroethylmethacrylate using poly(vinyl alcohol)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Suzuki, Atsushi, E-mail: suzuki@mat.usp.ac.j; Iguchi, Motoi; Oku, Takeo

2010-04-15

Influence of chemical substitution in the Fe{sup II} spin crossover complex on magnetic properties in emulsion polymerization of trifluoroethylmethacrylate using poly(vinyl alcohol) as a protective colloid was investigated near its high spin/low spin (HS/LS) phase transition. The obvious bi-stability of the HS/LS phase transition was considered by the identification of multiple spin states between the quintet (S=2) states to single state (S=0) across the excited triplet state (S=1). Magnetic parameters of gradual shifts of anisotropy g-tensor supported by the molecular distortion of the spin crossover complex would arise from a Jahn-Teller effect regarding ligand field theory on the basis ofmore » a B3LYP density functional theory using electron spin resonance (ESR) spectrum and X-ray powder diffraction. - Graphical abstract: AFM surface image of the emulsion particles with the spin crossover complex.« less

Fluorescent Labeling and Biodistribution of Latex Nanoparticles Formed by Surfactant-Free RAFT Emulsion Polymerization.

PubMed

Poon, Cheuk Ka; Tang, Owen; Chen, Xin-Ming; Kim, Byung; Hartlieb, Matthias; Pollock, Carol A; Hawkett, Brian S; Perrier, Sébastien

2017-10-01

The authors report the preparation of a novel range of functional polyacrylamide stabilized polystyrene nanoparticles, obtained by surfactant-free reversible addition-fragmentation chain transfer (RAFT) emulsion polymerization, their fluorescent tagging, cellular uptake, and biodistribution. The authors show the versatility of the RAFT emulsion process for the design of functional nanoparticles of well-defined size that can be used as drug delivery vectors. Functionalization with a fluorescent tag offers a useful visualization tool for tracing, localization, and clearance studies of these carriers in biological models. The studies are carried out by labeling the sterically stabilized latex particles chemically with rhodamine B. The fluorescent particles are incubated in a healthy human renal proximal tubular cell line model, and intravenously injected into a mouse model. Cellular localization and biodistribution of these particles on the biological models are explored. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparation of Paraffin@Poly(styrene-co-acrylic acid) Phase Change Nanocapsules via Combined Miniemulsion/Emulsion Polymerization.

PubMed

Zhang, Feng; Liu, Tian-Yu; Hou, Gui-Hua; Guan, Rong-Feng; Zhang, Jun-Hao

2018-06-01

The fast development of solid-liquid phase change materials calls for nanomaterials with large specific surface area for rapid heat transfer and encapsulation of phase change materials to prevent potential leakage. Here we report a combined miniemulsion/emulsion polymerization method to prepare poly(styrene-co-acrylic acid)-encapsulated paraffin (paraffin@P(St-co-AA)) nanocapsules. The method could suppress the shortcomings of common miniemulsion polymerization (such as evaporation of monomer and decomposition of initiator during ultrasonication). The paraffin@P(St-co-AA) nanocapsules are uniform in size and the polymer shell can be controlled by the weight ratio of St to paraffin. The phase change behavior of the nanocapsules is similar to that of pure paraffin. We believe our method can also be utilized to synthesize other core-shell phase change materials.

Methods for Generating Hydrogel Particles for Protein Delivery

PubMed Central

Liu, Allen L.; García, Andrés J.

2016-01-01

Proteins represent a major class of therapeutic molecules with vast potential for the treatment of acute and chronic diseases and regenerative medicine applications. Hydrogels have long been investigated for their potential in carrying and delivering proteins. As compared to bulk hydrogels, hydrogel microparticles (microgels) hold promise in improving aspects of delivery owing to their less traumatic route of entry into the body and improved versatility. This review discusses common methods of fabricating microgels, including emulsion polymerization, microfluidic techniques, and lithographic techniques. Microgels synthesized from both natural and synthetic polymers are discussed, as are a series of microgels fashioned from environment-responsive materials. PMID:27160672

Synthesis and Characterization of Novel Fluorine-Containing Water-Based Antirust Coating

NASA Astrophysics Data System (ADS)

Wang, Huiru; Wang, Xin; Zhao, Xiongyan

2018-01-01

A fluorine-containing polyacrylate copolymer emulsion was synthesized by a seed emulsion polymerization method, in which styrene(St) and butyl acrylate (BA) were used as main monomers and dodecafluoroheptyl methacrylate(DFMA) as fluorine-containing monomer. The structure and properties were characterized by Fourier transform infrared spectrum (FT-IR), scanning electron microscopy (SEM), particle size analysis, differential scanning calorimetry (DSC). The FTIR results showed that DFMA was effectively involved in the emulsion copolymerization, and the formed emulsion particles had a narrow particle size distribution. From the results salt spray test presented, it seems when the content of DFMA was 5wt% anti-rust performance of emulsion is relatively better. DSC and TGA also showed that their film exhibited higher thermal stability than that of fluorine-free emulsion.

An easily regenerable enzyme reactor prepared from polymerized high internal phase emulsions.

PubMed

Ruan, Guihua; Wu, Zhenwei; Huang, Yipeng; Wei, Meiping; Su, Rihui; Du, Fuyou

2016-04-22

A large-scale high-efficient enzyme reactor based on polymerized high internal phase emulsion monolith (polyHIPE) was prepared. First, a porous cross-linked polyHIPE monolith was prepared by in-situ thermal polymerization of a high internal phase emulsion containing styrene, divinylbenzene and polyglutaraldehyde. The enzyme of TPCK-Trypsin was then immobilized on the monolithic polyHIPE. The performance of the resultant enzyme reactor was assessed according to the conversion ability of Nα-benzoyl-l-arginine ethyl ester to Nα-benzoyl-l-arginine, and the protein digestibility of bovine serum albumin (BSA) and cytochrome (Cyt-C). The results showed that the prepared enzyme reactor exhibited high enzyme immobilization efficiency and fast and easy-control protein digestibility. BSA and Cyt-C could be digested in 10 min with sequence coverage of 59% and 78%, respectively. The peptides and residual protein could be easily rinsed out from reactor and the reactor could be regenerated easily with 4 M HCl without any structure destruction. Properties of multiple interconnected chambers with good permeability, fast digestion facility and easily reproducibility indicated that the polyHIPE enzyme reactor was a good selector potentially applied in proteomics and catalysis areas. Copyright © 2016 Elsevier Inc. All rights reserved.

Effect of Monomer Solubility on the Evolution of Copolymer Morphology during Polymerization-Induced Self-Assembly in Aqueous Solution

PubMed Central

2017-01-01

Polymerization-induced self-assembly (PISA) has become a widely used technique for the rational design of diblock copolymer nano-objects in concentrated aqueous solution. Depending on the specific PISA formulation, reversible addition–fragmentation chain transfer (RAFT) aqueous dispersion polymerization typically provides straightforward access to either spheres, worms, or vesicles. In contrast, RAFT aqueous emulsion polymerization formulations often lead to just kinetically-trapped spheres. This limitation is currently not understood, and only a few empirical exceptions have been reported in the literature. In the present work, the effect of monomer solubility on copolymer morphology is explored for an aqueous PISA formulation. Using 2-hydroxybutyl methacrylate (aqueous solubility = 20 g dm–3 at 70 °C) instead of benzyl methacrylate (0.40 g dm–3 at 70 °C) for the core-forming block allows access to an unusual “monkey nut” copolymer morphology over a relatively narrow range of target degrees of polymerization when using a poly(methacrylic acid) RAFT agent at pH 5. These new anisotropic nanoparticles have been characterized by transmission electron microscopy, dynamic light scattering, aqueous electrophoresis, shear-induced polarized light imaging (SIPLI), and small-angle X-ray scattering. PMID:28216792

Breaking of the Bancroft rule for multiple emulsions stabilized by a single stimulable polymer.

PubMed

Besnard, L; Protat, M; Malloggi, F; Daillant, J; Cousin, F; Pantoustier, N; Guenoun, P; Perrin, P

2014-09-28

We investigated emulsions of water and toluene stabilized by (co)polymers consisting of styrene (S) and 2-(dimethylamino)ethyl methacrylate (DMAEMA) monomer units with different compositions and structures such as a PDMAEMA homopolymer, a P(S-co-DMAEMA) random copolymer and various PS-b-PDMAEMA and PS-b-(S-co-DMAEMA) block copolymers. The model system is used to study the fundamental conditions under which the different kinds of polymer-stabilized emulsions (direct oil in water, inverse water in oil and multiple emulsions) are stabilized or destabilized by pH change (at constant temperature). Polymer properties like chain conformation at the toluene-water interface as probed by SANS and neutron reflectivity at the liquid-liquid interface, the oil-water partitioning of the polymer chains (Bancroft's rule of thumb) as determined by UV spectroscopy and interfacial tensions measured by the rising and spinning drop techniques are determined. Overall, results evidence that the curvature sign, as defined by positive and negative values as the chain segments occupy preferentially the water and toluene sides of the interface respectively, reliably predicts the emulsion kind. In contrast, the Bancroft rule failed at foreseeing the emulsion type. In the region of near zero curvature the crossover from direct to inverse emulsions occurs through the formation of either unstable coexisting direct and inverse emulsions (i) or multiple emulsions (ii). The high compact adsorption of the chains at the interface as shown by low interfacial tension values does not allow to discriminate between both cases. However, the toluene-water partitioning of the polymeric emulsifier is still a key factor driving the formation of (i) or (ii) emulsions. Interestingly, the stabilization of the multiple emulsions can be tuned to a large extent as the toluene-water polymer partitioning can be adjusted using quite a large number of physico-chemical parameters linked to polymer architecture like diblock length ratio or polymer total molar mass, for example. Moreover, we show that monitoring the oil-water partitioning aspect of the emulsion system can also be used to lower the interfacial tension at low pH to values slightly higher than 0.01 mN m(-1), irrespective of the curvature sign.

Structural micro-porous carbon anode for rechargeable lithium-ion batteries

DOEpatents

Delnick, Frank M.; Even, Jr., William R.; Sylwester, Alan P.; Wang, James C. F.; Zifer, Thomas

1995-01-01

A secondary battery having a rechargeable lithium-containing anode, a cathode and a separator positioned between the cathode and anode with an organic electrolyte solution absorbed therein is provided. The anode comprises three-dimensional microporous carbon structures synthesized from polymeric high internal phase emulsions or materials derived from this emulsion source, i.e., granules, powders, etc.

Effect of PLGA as a polymeric emulsifier on preparation of hydrophilic protein-loaded solid lipid nanoparticles.

PubMed

Xie, ShuYu; Wang, SiLiang; Zhao, BaoKai; Han, Chao; Wang, Ming; Zhou, WenZhong

2008-12-01

Most proteins are hydrophilic and poorly encapsulated into the hydrophobic matrix of solid lipid nanoparticles (SLN). To solve this problem, poly (lactic-co-glycolic acid) (PLGA) was utilized as a lipophilic polymeric emulsifier to prepare hydrophilic protein-loaded SLN by w/o/w double emulsion and solvent evaporation techniques. Hydrogenated castor oil (HCO) was used as a lipid matrix and bovine serum albumin (BSA), lysozyme and insulin were used as model proteins to investigate the effect of PLGA on the formulation of the SLN. The results showed that PLGA was essential for the primary w/o emulsification. In addition, the stability of the w/o emulsion, the encapsulation efficiency and loading capacity of the nanoparticles were enhanced with the increase of PLGA concentration. Furthermore, increasing PLGA concentration decreased zeta potential significantly but had no influence on particle size of the SLN. In vitro release study showed that PLGA significantly affected the initial burst release, i.e. the higher the content of PLGA, the lower the burst release. The released proteins maintained their integrity and bioactivity as confirmed by sodium dodecyl sulphate-polyacrylamide gel electrophoresis (SDS-PAGE) and biological assay. These results demonstrated that PLGA was an effective emulsifier for the preparation of hydrophilic protein-loaded SLN.

Nonequilibrium stabilization of an RNA/protein droplet emulsion by nuclear actin

NASA Astrophysics Data System (ADS)

Brangwynne, Clifford

2013-03-01

Actin plays a structural role in the cytoplasm. However, actin takes on new functions and structures in the nucleus that are poorly understood. The nuclei of the large oocytes of the frog X. laevisspecifically accumulate actin to reach high concentrations; however, it remains unclear if this actin polymerizes into a network, and what, if any, structural role such an actin network might play. Here, we use microrheological and confocal imaging techniques to probe the local architecture and mechanics of the nucleus. Our data show that actin forms a weak network that spatially organizes the nucleus by kinetically stabilizing embedded liquid-like RNA/protein bodies which are important for cell growth. In actin-disrupted nuclei this RNA/protein droplet emulsion is destabilized leading to homotypic coalescence into single large droplets. Our data provide intriguing new insights into why large cell nuclei require an actin-based structural scaffold.

Fluorescence correlation spectroscopy directly monitors coalescence during nanoparticle preparation.

PubMed

Schaeffel, David; Staff, Roland Hinrich; Butt, Hans-Juergen; Landfester, Katharina; Crespy, Daniel; Koynov, Kaloian

2012-11-14

Dual color fluorescence cross-correlation spectroscopy (DC FCCS) experiments were conducted to study the coalescence and aggregation during the formation of nanoparticles. To assess the generality of the method, three completely different processes were selected to prepare the nanoparticles. Polymeric nanoparticles were formed either by solvent evaporation from emulsion nanodroplets of polymer solutions or by miniemulsion polymerization. Inorganic nanocapsules were formed by polycondensation of alkoxysilanes at the interface of nanodroplets. In all cases, DC FCCS provided fast and unambiguous information about the occurrence of coalescence and thus a deeper insight into the mechanism of nanoparticle formation. In particular, it was found that coalescence played a minor role for the emulsion-solvent evaporation process and the miniemulsion polymerization, whereas substantial coalescence was detected during the formation of the inorganic nanocapsules. These findings demonstrate that DC FCCS is a powerful tool for monitoring nanoparticles genesis.

Synthesis of porous poly(styrene-co-acrylic acid) microspheres through one-step soap-free emulsion polymerization: whys and wherefores.

PubMed

Yan, Rui; Zhang, Yaoyao; Wang, Xiaohui; Xu, Jianxiong; Wang, Da; Zhang, Wangqing

2012-02-15

Synthesis of porous poly(styrene-co-acrylic acid) (PS-co-PAA) microspheres through one-step soap-free emulsion polymerization is reported. Various porous PS-co-PAA microspheres with the particle size ranging from 150 to 240 nm and with the pore size ranging from 4 to 25 nm are fabricated. The porous structure of the microspheres is confirmed by the transmission electron microscopy measurement and Brunauer-Emmett-Teller (BET) analysis. The reason for synthesis of the porous PS-co-PAA microspheres is discussed, and the phase separation between the encapsulated hydrophilic poly(acrylic acid) segment and the hydrophobic polystyrene domain within the PS-co-PAA microspheres is ascribed to the pore formation. The present synthesis of the porous PS-co-PAA microspheres is anticipated to be a new and convenient way to fabricate porous polymeric particles. Copyright © 2011 Elsevier Inc. All rights reserved.

Synthesis and characterization of magnetic and non-magnetic core-shell polyepoxide micrometer-sized particles of narrow size distribution.

PubMed

Omer-Mizrahi, Melany; Margel, Shlomo

2009-01-15

Core polystyrene microspheres of narrow size distribution were prepared by dispersion polymerization of styrene in a mixture of ethanol and 2-methoxy ethanol. Uniform polyglycidyl methacrylate/polystyrene core-shell micrometer-sized particles were prepared by emulsion polymerization at 73 degrees C of glycidyl methacrylate in the presence of the core polystyrene microspheres. Core-shell particles with different properties (size, surface morphology and composition) have been prepared by changing various parameters belonging to the above seeded emulsion polymerization process, e.g., volumes of the monomer glycidyl methacrylate and the crosslinker monomer ethylene glycol dimethacrylate. Magnetic Fe(3)O(4)/polyglycidyl methacrylate/polystyrene micrometer-sized particles were prepared by coating the former core-shell particles with magnetite nanoparticles via a nucleation and growth mechanism. Characterization of the various particles has been accomplished by routine methods such as light microscopy, SEM, FTIR, BET and magnetic measurements.

Penicillin-Bound Polyacrylate Nanoparticles: Restoring the Activity of β-Lactam Antibiotics Against MRSA

PubMed Central

Reddy, G. Suresh Kumar; Greenhalgh, Kerriann; Ramaraju, Praveen; Abeylath, Sampath C.; Jang, Seyoung; Dickey, Sonja; Lim, Daniel V.

2007-01-01

This report describes the preparation of antibacterially-active emulsified polyacrylate nanoparticles in which a penicillin antibiotic is covalently conjugated onto the polymeric framework. These nanoparticles were prepared in water by emulsion polymerization of an acrylated penicillin analogue pre-dissolved in a 7:3 (w:w) mixture of butyl acrylate and styrene in the presence of sodium dodecyl sulfate (surfactant) and potassium persulfate (radical initiator). Dynamic light scattering analysis and atomic force microscopy images show that the emulsions contain nanoparticles of approximately 40 nm in diameter. The nanoparticles have equipotent in vitro antibacterial properties against methicillin-susceptible and methicillin-resistant forms of Staphylococcus aureus and indefinite stability towards β-lactamase. PMID:17420125

Structural micro-porous carbon anode for rechargeable lithium-ion batteries

DOEpatents

Delnick, F.M.; Even, W.R. Jr.; Sylwester, A.P.; Wang, J.C.F.; Zifer, T.

1995-06-20

A secondary battery having a rechargeable lithium-containing anode, a cathode and a separator positioned between the cathode and anode with an organic electrolyte solution absorbed therein is provided. The anode comprises three-dimensional microporous carbon structures synthesized from polymeric high internal phase emulsions or materials derived from this emulsion source, i.e., granules, powders, etc. 6 figs.

An investigation into the characteristics and drug release properties of multiple W/O/W emulsion systems containing low concentration of lipophilic polymeric emulsifier.

PubMed

Vasiljevic, Dragana; Parojcic, Jelena; Primorac, Marija; Vuleta, Gordana

2006-02-17

Multiple W/O/W emulsions with high content of inner phase (Phi1=Phi2=0.8) were prepared using relatively low concentrations of lipophilic polymeric primary emulsifier, PEG 30-dipolyhydroxystearate, and diclofenac diethylamine (DDA) as a model drug. The investigated formulations were characterized and their stability over the time was evaluated by dynamic and oscillatory rheological measurements, microscopic analysis and in vitro drug release study. In vitro release profiles of the selected model drug were evaluated in terms of the effective diffusion coefficients and flux of the released drug. The multiple emulsion samples exhibited good stability during the ageing time. Concentration of the lipophilic primary emulsifier markedly affected rheological behaviour as well as the droplet size and in vitro drug release kinetics of the investigated systems. The multiple emulsion systems with highest concentration (2.4%, w/w) of the primary emulsifier had the lowest droplet size and the highest apparent viscosity and highest elastic characteristics. Drug release data indicated predominately diffusional drug release mechanism with sustained and prolonged drug release accomplished with 2.4% (w/w) of lipophilic emulsifier employed.

Radiation induced emulsion graft polymerization of 4-vinylpyridine onto PE/PP nonwoven fabric for As(V) adsorption

NASA Astrophysics Data System (ADS)

Akkaş Kavaklı, Pınar; Kavaklı, Cengiz; Seko, Noriaki; Tamada, Masao; Güven, Olgun

2016-10-01

A novel nonwoven fabric adsorbent having 4-vinylpyridine functional groups was prepared by using radiation-induced emulsion graft polymerization method and grafting 4-vinylpyridine monomer onto a polyethylene-coated polypropylene nonwoven fabric (NWF) in aqueous emulsion solution. The grafting conditions of the 4-vinylpyridine monomer onto the NWF were optimised and 150% Dg VP-g-NWF was prepared using 30 kGy pre-irradiation dose, 5% VP monomer concentration and 0.5% (w/w) Tween 20 in aqueous emulsion. Grafted 4-vinylpyridine chains on the NWF were then quaternized for the preparation of QVP-g-NWF adsorbent. All fabric structures were characterized by using Fourier-transform infrared spectrometer, x-ray photoelectron spectrometer and scanning electron microscope. QVP-g-NWF adsorbent was used in batch adsorption experiments for As(V) ions by studying the pH, contact time, and initial As(V) ion concentration parameters. Results showed that QVP-g-NWF adsorbent has significant As(V) adsorption and experimental As(V) adsorption capacity was 98.04 mg As(V)/g polymer from 500 mg/L initial As(V) concentration at pH 7.00.

ABC Triblock Copolymer Worms: Synthesis, Characterization, and Evaluation as Pickering Emulsifiers for Millimeter-Sized Droplets

PubMed Central

2016-01-01

Polymerization-induced self-assembly (PISA) is used to prepare linear poly(glycerol monomethacrylate)–poly(2-hydroxypropyl methacrylate)–poly(benzyl methacrylate) [PGMA–PHPMA–PBzMA] triblock copolymer nano-objects in the form of a concentrated aqueous dispersion via a three-step synthesis based on reversible addition–fragmentation chain transfer (RAFT) polymerization. First, GMA is polymerized via RAFT solution polymerization in ethanol, then HPMA is polymerized via RAFT aqueous solution polymerization, and finally BzMA is polymerized via “seeded” RAFT aqueous emulsion polymerization. For certain block compositions, highly anisotropic worm-like particles are obtained, which are characterized by small-angle X-ray scattering (SAXS) and transmission electron microscopy (TEM). The design rules for accessing higher order morphologies (i.e., worms or vesicles) are briefly explored. Surprisingly, vesicular morphologies cannot be accessed by targeting longer PBzMA blocks—instead, only spherical nanoparticles are formed. SAXS is used to rationalize these counterintuitive observations, which are best explained by considering subtle changes in the relative enthalpic incompatibilities between the three blocks during the growth of the PBzMA block. Finally, the PGMA–PHPMA–PBzMA worms are evaluated as Pickering emulsifiers for the stabilization of oil-in-water emulsions. Millimeter-sized oil droplets can be obtained using low-shear homogenization (hand-shaking) in the presence of 20 vol % n-dodecane. In contrast, control experiments performed using PGMA–PHPMA diblock copolymer worms indicate that these more delicate nanostructures do not survive even these mild conditions. PMID:27795581

USING ACID-RESISTANT PHOTOSENSITIVE EMULSIONS TO OBTAIN LOCAL INHOMOGENEITIES WITH A HIGH RESOLVING POWER ON MONOCRYSTALS AND FILMS OF GERMANIUM AND SILICON (PRIMENENIE KISLOTOSTOYKHIKH SVETOCHUVSTVITELNYKH EMULSII DLYA POLUCHENIYA LOKALNYKH NEODNORODNOSTEI S VYSOKIM RAZRESHENIEM NA MONOKRISTALLAKH I PLENKAKH GERMANIYA I KREMNIYA),

DTIC Science & Technology

It was found that the esters of polystyrene and cinnamic acid , polyvinyl alcohol, and cinnamic acid have high dielectric characteristics that change...Photosensitive acid -resisting emulsions for use in photoengraving of semiconductor parts and semiconductor surfaces were synthesized and tested...organosilicon compounds, cinnamic aldehyde, emulsions based on azo and diazo compounds and polymeric polyesters--were tested. The photoengraving method

Design of polymeric immunomicrospheres for cell labelling and cell separation

NASA Technical Reports Server (NTRS)

Rembaum, A.; Margel, S.

1978-01-01

Synthesis of several classes of hydrophylic microspheres applied to cell labeling and cell separation is described. Five classes of cross-linked microspheres with functional groups such as carboxyl, hydroxyl, amide and/or pyridine groups were synthesized. These functional groups were used to bind covalently antibodies and other proteins to the surface of the microspheres. To optimize the derivatisation technique, polyglutaraldehyde immunomicrospheres were prepared and utilized. Specific populations of human and murine lymphocytes were labelled with microspheres synthesized by the emulsion of the ionizing radiation technique. The labelling of the cells by means of microspheres containing an iron core produced successful separation of B from T lymphocytes by means of a magnetic field.

Antibiotic-conjugated polyacrylate nanoparticles: new opportunities for development of anti-MRSA agents.

PubMed

Turos, Edward; Shim, Jeung-Yeop; Wang, Yang; Greenhalgh, Kerriann; Reddy, G Suresh Kumar; Dickey, Sonja; Lim, Daniel V

2007-01-01

This report describes the preparation of polyacrylate nanoparticles in which an N-thiolated beta-lactam antibiotic is covalently conjugated onto the polymer framework. These nanoparticles are formed in water by emulsion polymerization of an acrylated antibiotic pre-dissolved in a liquid acrylate monomer (or mixture of co-monomers) in the presence of sodium dodecyl sulfate as a surfactant and potassium persulfate as a radical initiator. Dynamic light scattering analysis and electron microscopy images of these emulsions show that the nanoparticles are approximately 40 nm in diameter. The emulsions have potent in vitro antibacterial properties against methicillin-resistant Staphylococcus aureus and have improved bioactivity relative to the non-polymerized form of the antibiotic. A unique feature of this methodology is the ability to incorporate water-insoluble drugs directly into the nanoparticle framework without the need for post-synthetic modification. Additionally, the antibiotic properties of the nanoparticles can be modulated by changing the length or location of the acrylate linker on the drug monomer.

Structure- and oil type-based efficacy of emulsion adjuvants.

PubMed

Jansen, Theo; Hofmans, Marij P M; Theelen, Marc J G; Manders, Frans; Schijns, Virgil E J C

2006-06-29

Oil-based emulsions are well-known immunopotentiators for inactivated, "killed" vaccines. We addressed the relationship between emulsion structure and levels of in vivo antibody formation to inactivated New Castle Disease virus (NDV) and Infectious Bronchitis virus (IBV) as antigens in 3-week-old chickens. The use of a polymeric emulsifier allowed for direct comparison of three types of emulsions, water-in-oil (W/O), oil-in-water (O/W) and W/O-in-water (W/O/W), while maintaining an identical content of components for each vehicle. They were prepared with either non-metabolizable, mineral oil or metabolizable, Miglyol 840. In addition, we assessed the inherent release capacity of each emulsion variant in vitro. Remarkably, we noted that W/O-type emulsions induced the best immune responses, while they released no antigen during 3 weeks. In general, mineral oil vaccines showed superior efficacy compared to Miglyol 840-based vaccines.

Thiolated alkyl-modified carbomers: Novel excipients for mucoadhesive emulsions.

PubMed

Bonengel, Sonja; Hauptstein, Sabine; Leonaviciute, Gintare; Griessinger, Julia; Bernkop-Schnürch, Andreas

2015-07-30

The aim of this study was the design and evaluation of mucoadhesive emulsifying polymeric excipients. Three thiol bearing ligands with increasing pKa values of their sulfhydryl group, namely 4-aminothiophenol (pKa=6.86), l-cysteine (pKa=8.4) and d/l-homocysteine (pKa=10.0) were coupled to the polymeric backbone of alkyl-modified carbomer (PA1030). Resulting conjugates displayed 818.5μmol 4-aminothiophenol, 698.5μmol cysteine and 651.5μmol homocysteine per gram polymer and were evaluated regarding the reactivity of thiol groups, emulsifying and mucoadhesive properties. In general, the synthesized conjugates showed a pH dependent reactivity, whereby the fastest oxidation occurred in PA1030-cysteine, as almost no free thiol groups could be detected after 120min. Emulsification of medium chain triglycerides was feasible with all synthesized conjugates leading to oil-in-water-emulsions. Emulsions with PA1030-cysteine displayed the highest stability and the smallest droplet size among the tested formulations. Oxidation and consequently cross-linking of the thiomers prior to the emulsification process led to an overall decreased emulsion stability. Evaluating mucosal residence time of thiomer emulsions on porcine buccal mucosa, a 9.2-fold higher amount of formulation based on PA1030-cysteine remained on the mucosal tissue within 3h compared to the unmodified polymer. According to these results, the highest reactive ligand l-cysteine seems to be most promising in order to obtain thiolated polymers for the preparation of mucoadhesive o/w-emulsions. Copyright © 2015 Elsevier B.V. All rights reserved.

Effects of poly(lactic-co-glycolic acid) on preparation and characteristics of plasmid DNA-loaded solid lipid nanoparticles.

PubMed

Zhu, L; Xie, S; Dong, Z; Wang, X; Wang, Y; Zhou, W

2011-09-01

Poly(lactic-co-glycolic acid) (PLGA) was used as a polymeric emulsifier to encapsulate plasmid DNA into hydrogenated castor oil (HCO)-solid lipid nanoparticles (SLN) by w/o/w double emulsion and solvent evaporation techniques. The effects of PLGA on the preparation, characteristics and transfection efficiency of DNA-loaded SLN were studied. The results showed that PLGA was essential to form the primary w/o emulsion and the stability of the emulsion was enhanced with the increase of PLGA content. DNA-loaded SLN were spherical with smooth surfaces. The SLN had a negative charge in weak acid and alkaline environment but acquired a positive charge in acidic pH and the cationisation capacity of the SLN increased with the increase of PLGA/HCO ratio. Agarose gel electrophoresis demonstrated that the majority of the DNA maintained its structural integrity after preparation and being extracted or released from DNA-loaded SLN. When PLGA/HCO ratio increased from 5 to 15%, the encapsulation efficiency, loading capacity and transfection efficiency of the nanoparticles increased significantly, whereas the changes of particle size and polydispersity index were insignificant. Cytotoxicity study in cell culture demonstrated that the SLN was not toxic.

Preparation and characterization of a magneto-polymeric nanocomposite: Fe 3O 4 nanoparticles in a grafted, cross-linked and plasticized poly(vinyl chloride) matrix

NASA Astrophysics Data System (ADS)

Rodríguez-Fernández, Oliverio S.; Rodríguez-Calzadíaz, C. A.; Yáñez-Flores, Isaura G.; Montemayor, Sagrario M.

In this work two kind of materials: (1) grafted, cross-linked and plasticized poly(vinyl chloride) (PVC) "plastic films" and (2) magnetic plastic films "magneto-polymeric nanocomposites" were prepared. Precursor solutions or "plastisols" used to obtain the plastic films were obtained by mixing PVC (emulsion grade) as polymeric matrix, di(2-ethylhexyl)phthalate (DOP) as plasticizer, a thermal stabilizer based in Ca/Zn salts, and a cross-linking agent, 3-mercaptopropyltrimethoxysilane (MTMS) or 3-aminopropyltriethoxysilane (ATES), at several concentrations. Flexible films were obtained from the plastisols using static casting. The stress-strain behavior and the gel content (determined by Soxhlet extraction with boiling THF) of the flexible films were measured in order to evaluate the effect of the cross-linking agent and their content on the degree of cross-linking. The magneto-polymeric nanocomposites were obtained by mixing the optimum composition of the plastisols (analyzed previously) with magnetite (Fe 3O 4)-based ferrofluid and DOP. Later, flexible films were obtained by static casting of the plastisol/ferrofluid systems. The magnetic films were characterized by the above-mentioned techniques and X-ray diffraction, vibrating sample magnetometry and thermogravimetrical analysis.

Covalent bonding of polycations to small polymeric particles

NASA Technical Reports Server (NTRS)

Rembaum, A.

1975-01-01

Process produces small spherical polymeric particles which have polycations bound to them. In emulsion form, particles present large positively charged surface which is available to absorb polyanions. This properly can be used in removing heparin from blood or bile acids from the digestive tract. Other anions, such as DNA and RNA, can also be removed from aqueous solutions.

Protein specific polymeric immunomicrospheres

NASA Technical Reports Server (NTRS)

Yen, Shiao-Ping S. (Inventor); Dreyer, William J. (Inventor); Rembaum, Alan (Inventor)

1980-01-01

Small, round, bio-compatible microspheres capable of covalently bonding proteins and having a uniform diameter below about 3500 A are prepared by substantially instantaneously initiating polymerization of an aqueous emulsion containing no more than 35% total monomer including an acrylic monomer substituted with a covalently bondable group such as hydroxyl, amino or carboxyl and a minor amount of a cross-linking agent.

Highly temperature responsive core-shell magnetic particles: synthesis, characterization and colloidal properties.

PubMed

Rahman, Md Mahbubor; Chehimi, Mohamed M; Fessi, Hatem; Elaissari, Abdelhamid

2011-08-15

Temperature responsive magnetic polymer submicron particles were prepared by two step seed emulsion polymerization process. First, magnetic seed polymer particles were obtained by emulsion polymerization of styrene using potassium persulfate (KPS) as an initiator and divinylbenzne (DVB) as a cross-linker in the presence of oil-in-water magnetic emulsion (organic ferrofluid droplets). Thereafter, DVB cross-linked magnetic polymer particles were used as seed in the precipitation polymerization of N-isopropylacrylamide (NIPAM) to induce thermosensitive PNIPAM shell onto the hydrophobic polymer surface of the cross-linked magnetic polymer particles. To impart cationic functional groups in the thermosensitive PNIPAM backbone, the functional monomer aminoethylmethacrylate hydrochloride (AEMH) was used to polymerize with NIPAM while N,N'-methylenebisacrylamide (MBA) and 2, 2'-azobis (2-methylpropionamidine) dihydrochloride (V-50) were used as a cross-linker and as an initiator respectively. The effect of seed to monomer (w/w) ratio along with seed nature on the final particle morphology was investigated. Dynamic light scattering (DLS) results demonstrated particles swelling at below volume phase transition temperature (VPTT) and deswelling above the VPTT. The perfect core (magnetic) shell (polymer) structure of the particles prepared was confirmed by Transmission Electron Microscopy (TEM). The chemical composition of the particles were determined by thermogravimetric analysis (TGA). The effect of temperature, pH, ionic strength on the colloidal properties such as size and zeta potential of the micron sized thermo-sensitive magnetic particles were also studied. In addition, a short mechanistic discussion on the formation of core-shell morphology of magnetic polymer particles has also been discussed. Copyright © 2011 Elsevier Inc. All rights reserved.

A flexible, robust and antifouling asymmetric membrane based on ultra-long ceramic/polymeric fibers for high-efficiency separation of oil/water emulsions.

PubMed

Wang, Kui; Yiming, Wubulikasimu; Saththasivam, Jayaprakash; Liu, Zhaoyang

2017-07-06

Polymeric and ceramic asymmetric membranes have dominated commercial membranes for water treatment. However, polymeric membranes are prone to becoming fouled, while ceramic membranes are mechanically fragile. Here, we report a novel concept to develop asymmetric membranes based on ultra-long ceramic/polymeric fibers, with the combined merits of good mechanical stability, excellent fouling resistance and high oil/water selectivity, in order to meet the stringent requirements for practical oil/water separation. The ultra-long dimensions of ceramic nanofibers/polymeric microfibers endow this novel membrane with mechanical flexibility and robustness, due to the integrated and intertwined structure. This membrane is capable of separating oil/water emulsions with high oil-separation efficiency (99.9%), thanks to its nanoporous selective layer made of ceramic nanofibers. Further, this membrane also displays superior antifouling properties due to its underwater superoleophobicity and ultra-low oil adhesion of the ceramic-based selective layer. This membrane exhibits high water permeation flux (6.8 × 10 4 L m -2 h -1 bar -1 ) at low operation pressures, which is attributed to its 3-dimensional (3D) interconnected fiber-based structure throughout the membrane. In addition, the facile fabrication process and inexpensive materials required for this membrane suggest its significant potential for industrial applications.

Synthesis of High Molecular Weight Poly(glycerol monomethacrylate) via RAFT Emulsion Polymerization of Isopropylideneglycerol Methacrylate

PubMed Central

2018-01-01

High molecular weight water-soluble polymers are widely used as flocculants or thickeners. However, synthesis of such polymers via solution polymerization invariably results in highly viscous fluids, which makes subsequent processing somewhat problematic. Alternatively, such polymers can be prepared as colloidal dispersions; in principle, this is advantageous because the particulate nature of the polymer chains ensures a much lower fluid viscosity. Herein we exemplify the latter approach by reporting the convenient one-pot synthesis of high molecular weight poly(glycerol monomethacrylate) (PGMA) via the reversible addition–fragmentation chain transfer (RAFT) aqueous emulsion polymerization of a water-immiscible protected monomer precursor, isopropylideneglycerol methacrylate (IPGMA) at 70 °C, using a water-soluble poly(glycerol monomethacrylate) (PGMA) chain transfer agent as a steric stabilizer. This formulation produces a low-viscosity aqueous dispersion of PGMA–PIPGMA diblock copolymer nanoparticles at 20% solids. Subsequent acid deprotection of the hydrophobic core-forming PIPGMA block leads to particle dissolution and affords a viscous aqueous solution comprising high molecular weight PGMA homopolymer chains with a relatively narrow molecular weight distribution. Moreover, it is shown that this latex precursor route offers an important advantage compared to the RAFT aqueous solution polymerization of glycerol monomethacrylate since it provides a significantly faster rate of polymerization (and hence higher monomer conversion) under comparable conditions. PMID:29805184

Preparation of hybrid thiol-acrylate emulsion-templated porous polymers by interfacial copolymerization of high internal phase emulsions.

PubMed

Langford, Caitlin R; Johnson, David W; Cameron, Neil R

2015-05-01

Emulsion-templated highly porous polymers (polyHIPEs), containing distinct regions differing in composition, morphology, and/or properties, are prepared by the simultaneous polymerization of two high internal phase emulsions (HIPEs) contained within the same mould. The HIPEs are placed together in the mould and subjected to thiol-acrylate photopolymerization. The resulting polyHIPE material is found to contain two distinct semicircular regions, reflecting the composition of each HIPE. The original interface between the two emulsions becomes a copolymerized band between 100 and 300 μm wide, which is found to be mechanically robust. The separate polyHIPE layers are distinguished from one another by their differing average void diameter, chemical composition, and extent of contraction upon drying. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Methods for purifying and detoxifying sodium dodecyl sulfate-stabilized polyacrylate nanoparticles.

PubMed

Garay-Jimenez, Julio C; Young, Ashley; Gergeres, Danielle; Greenhalgh, Kerriann; Turos, Edward

2008-06-01

Recent research in our laboratory has centered on studies of polyacrylate and polyacrylamide nanoparticle emulsions for use in antibiotic delivery. Our goal is to develop these nanoparticle emulsions for treatment of life-threatening bacterial infections such as those caused by methicillin-resistant Staphylococcus aureus. For this intended application it is necessary to ensure that the biological activity of the emulsion is due only to the drug attached to the polymeric chain and not to any extraneous components. To investigate this we evaluated cytotoxicity and microbiological activity of the nanoparticle emulsions before and after purification by centrifugation, dialysis, and gel filtration. Depending on the amount of surfactant used, all or most of the microbial and cellular toxicity can be removed by a simple purification procedure.

Waterborne Polymeric Films.

DTIC Science & Technology

1979-12-01

resin types: 1) acrylic latex, 2) acrylic solution polymer, 3) epoxy emulsions, 4) polyurethane, 5) butadiene elastomeric latex, 6) polyester/ alkyd , 7...emulsions and the class of polyester/ alkyd resins were evaluated only as network, crosslinked films. -53- j z I, ACRYLIC SOLUTIONLATEX URE THANE ACRYLIC ...amount of "plasticizing" monomer such as ethyl acrylate . 2.3.1.3 Aqueous Polyester Alkyd Resins As indicated in section 2.2.7 of this report,

Synthesis of new solid polymer electrolyte and actuator based on PEDOT/NBR/ionic liquid

NASA Astrophysics Data System (ADS)

Cho, M. S.; Seo, H. J.; Nam, J. D.; Choi, H. R.; Koo, J. C.; Lee, Y.

2006-03-01

The conducting polymer actuator was presented. The solid polymer electrolyte based on nitrile rubber (NBR) activated with different ionic liquids was prepared. The three different grades of NBR films were synthesized by emulsion polymerization with different amount of acrylonitrile, 23, 35, and 40 mol. %, respectively. The effect of acrylonitrile content on the ionic conductivity and dielectric constant of solid polymer electrolytes was characterized. A conducting polymer, poly(3,4-ethylenedioxythiophene) (PEDOT), was synthesized on the surface of the NBR layer by using a chemical oxidation polymerization technique, and room temperature ionic liquids (RTIL) based on imidazolium salts, e.g. 1-butyl-3-methyl imidazolium X [where X= BF 4 -, PF 6 -, (CF 3SO II) IIN -], were absorbed into the composite film. The effects of the anion size of the ionic liquids on the displacement of the actuator were examined. The displacement increased with increasing the anion-size of the ionic liquids.

Ceramic microparticles and capsules via microfluidic processing of a preceramic polymer

PubMed Central

Ye, Congwang; Chen, Anthony; Colombo, Paolo; Martinez, Carlos

2010-01-01

We have developed a robust technique to fabricate monodispersed solid and porous ceramic particles and capsules from single and double emulsion drops composed of silsesquioxane preceramic polymer. A microcapillary microfluidic device was used to generate the monodispersed drops. In this device, two round capillaries are aligned facing each other inside a square capillary. Three fluids are needed to generate the double emulsions. The inner fluid, which flows through the input capillary, and the middle fluid, which flows through the void space between the square and inner fluid capillaries, form a coaxial co-flow in a direction that is opposite to the flow of the outer fluid. As the three fluids are forced through the exit capillary, the inner and middle fluids break into monodispersed double emulsion drops in a single-step process, at rates of up to 2000 drops s−1. Once the drops are generated, the silsesquioxane is cross-linked in solution and the cross-linked particles are dried and pyrolysed in an inert atmosphere to form oxycarbide glass particles. Particles with diameters ranging from 30 to 180 µm, shell thicknesses ranging from 10 to 50 µm and shell pore diameters ranging from 1 to 10 µm were easily prepared by changing fluid flow rates, device dimensions and fluid composition. The produced particles and capsules can be used in their polymeric state or pyrolysed to ceramic. This technique can be extended to other preceramic polymers and can be used to generate unique core–shell multimaterial particles. PMID:20484226

Ceramic microparticles and capsules via microfluidic processing of a preceramic polymer.

PubMed

Ye, Congwang; Chen, Anthony; Colombo, Paolo; Martinez, Carlos

2010-08-06

We have developed a robust technique to fabricate monodispersed solid and porous ceramic particles and capsules from single and double emulsion drops composed of silsesquioxane preceramic polymer. A microcapillary microfluidic device was used to generate the monodispersed drops. In this device, two round capillaries are aligned facing each other inside a square capillary. Three fluids are needed to generate the double emulsions. The inner fluid, which flows through the input capillary, and the middle fluid, which flows through the void space between the square and inner fluid capillaries, form a coaxial co-flow in a direction that is opposite to the flow of the outer fluid. As the three fluids are forced through the exit capillary, the inner and middle fluids break into monodispersed double emulsion drops in a single-step process, at rates of up to 2000 drops s(-1). Once the drops are generated, the silsesquioxane is cross-linked in solution and the cross-linked particles are dried and pyrolysed in an inert atmosphere to form oxycarbide glass particles. Particles with diameters ranging from 30 to 180 microm, shell thicknesses ranging from 10 to 50 microm and shell pore diameters ranging from 1 to 10 microm were easily prepared by changing fluid flow rates, device dimensions and fluid composition. The produced particles and capsules can be used in their polymeric state or pyrolysed to ceramic. This technique can be extended to other preceramic polymers and can be used to generate unique core-shell multimaterial particles.

Sulfonated amphiphilic block copolymers : synthesis, self-assembly in water, and application as stabilizer in emulsion polymerization

Treesearch

Jiguang Zhang; Matthew R. Dubay; Carl J. Houtman; Steven J. Severtson

2009-01-01

Described is the synthesis of diblock copolymers generated via sequential atom transfer radical polymerization (ATRP) of poly(n-butyl acrylate) (PnBA) followed by chain augmentation with either sulfonated poly(2-hydroxyethyl methacrylate) (PHEMA) or poly(2-hydroxyethyl acrylate) (PHEA) blocks. ATRP of PHEMA or PHEA from PnBA macroinitiator was conducted in acetone/...

Shear Driven Synthesis of Polymeric Micro- and Nanomaterials

NASA Astrophysics Data System (ADS)

Tian, Tian

Polymeric micro- and nanomaterials play a significant role in various current and emerging technologies. A liquid shear based method was developed to fabricate a wide range of polymeric materials, which include fibers, sheets, ribbons, rods and spheres in a scalable, cost-effective and simple way. During the process, droplet shearing, droplet deformation, droplet breaking up and polymer precipitation occur simultaneously. The size and morphology of the resultant structures are determined by the dominating process which is further controlled by the experimental parameters including polymer concentration, polymer molecular weight and antisolvent concentration. Among all of these structures, nanofibers have attracted the latest research interest due to the unique properties. Current leading fiber production approaches in the market possess certain drawbacks. For example, the throughput of electrospinning is limited to around 2.5 kg/hr and the diameter of fiber produced by wet spinning cannot be below micrometer while melt spinning is only applicable to melt-processable polymers. The breakthrough of our liquid shear driven technique for fiber synthesis is that it produces fibers with diameter from 200 nm to several micrometers from a wide range of liquid- processable polymers with high commercial yield (up to 12 kg/hr). Thus in Chapter 2, the optimum parameters range for fiber formation is established and the effects of those parameters on fiber size are investigated. In the original liquid shear method, medium with high viscosity is needed to exert strong shear stress on the droplet and to stretch the droplets to long strand. However, the viscous medium complicates the post sample washing procedure and introduces the potential slippery danger in the working area. Thus a non-viscous medium shearing method is developed in Chapter 3 and it is the first time proposed that the synthesis of PLA or PS nanofibers can be completed in the aqueous ethanol medium. Colloid science usually categorizes emulsion as oil in water (O/W) and water in oil (W/O) dispersions. Oil in oil emulsion can also be formulated from the immiscible organic liquid pairs. Using the phase separation in the PS-cyclohexane system, the emulsion are formed under continuous shearing while the continuous phase is solvent-rich and the disperse phase is polymer-rich. By shearing the emulsions, the fibers sizes are reduced around 10X due to the smaller initial polymer droplet size. The fiber sizes are further reduced to 100 nm which enhances the competitive advantages of liquid shear technique. Controlled drug release combines the advantages of increased therapeutic efficacy, reduced toxicity and lower administration frequency. By dispersing model drugs in the spinning polymer solution, these drugs are successfully encapsulated inside the biodegradable matrix and the encapsulation efficiency is modulated by polymer concentration and fiber size while the release profile of the drug is determined by the degradation rate of the polymer matrix.

Particulate Coacervation of Associative Polymer Brushes-Grafted Nanoparticles To Produce Structurally Stable Pickering Emulsions.

PubMed

Yang, Taeseung; Choi, Sang Koo; Park, Daehwan; Lee, Yea Ram; Chung, Chan Bok; Kim, Jin Woong

2016-12-20

This study introduces a new type of associative nanoparticle (ANP) that provides controlled chain-to-chain attraction with an associative polymer rheology modifier (APRM) to produce highly stable Pickering emulsions. The ANPs were synthesized by grafting hydrophobically modified hygroscopic zwitterionic poly(2-methacryloyloxyethyl phosphorylcholine-co-stearyl methacrylate) brushes onto 20 nm sized silica NPs via surface-mediated living radical polymerization. The ANP-stabilized Pickering emulsions show significant viscosity enhancement in the presence of the APRM. This indicates that the ANPs act as particulate concentration agents at the interface owing to their hydrophobic association with the APRM in the aqueous phase, which leads to the generation of an ANP-mediated complex colloidal film. Consequently, the described ANP-reinforced Pickering emulsion system exhibits improved resistance to pH and salinity changes. This coacervation approach is advantageous because the complex colloidal layer at the interface provides the emulsion drops with a mechanically robust barrier, thus guaranteeing the improved Pickering emulsion stability against harsh environmental factors.

Specially Treated Aramid Fiber Stabilized Gel-Emulsions: Preparation of Porous Polymeric Monoliths and Highly Efficient Removing of Airborne HCHO.

PubMed

Liu, Jianfei; Chen, Xiangli; Wang, Pei; Fu, Xuwei; Liu, Kaiqiang; Fang, Yu

2017-08-01

Porous polymeric monoliths with densities as low as ≈0.060 g cm -3 are prepared in a gel-emulsion template way, of which the stabilizer employed is a newly discovered acidified aramid fiber that is so efficient that 0.05% (w/v, accounts for continuous phase) is enough to gel the system. The porous monoliths as obtained can be dried at ambient conditions, avoiding energy-consuming processes. Importantly, the monoliths show selective adsorption to HCHO, and the corresponding adsorption capacity (M6) is ≈2700 mg g -1 , the best result that is reported until now. More importantly, the monoliths can be reused after drying. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Characterization of ultrahigh-molecular weight cationic polyacrylamide using frit-inlet asymmetrical flow field-flow fractionation and multi-angle light scattering.

PubMed

Woo, Sohee; Lee, Ju Yong; Choi, Woonjin; Moon, Myeong Hee

2016-01-15

In this study, frit inlet asymmetrical flow field-flow fractionation (FlFFF) with multi-angle light scattering (MALS) and differential refractive index (DRI) detection is utilized for size separation, determination of molecular weight (MW), and conformation of ultrahigh-MW (10(7)-10(9) g/mol) cationic polyacrylamides (C-PAMs), a class of water-soluble copolymers based on acrylamide and vinyl-type comonomers with quaternary ammonium cations that are widely used in wastewater treatment and in paper industries. Linear and branched C-PAM copolymers prepared in two different polymerization methods (solution and emulsion) from varying amounts of crosslinking agent and initiator were size fractionated by FlFFF with field-programming. It was found experimentally that the linear copolymers from both polymerization methods were less than 10(8) g/mol in MW with compact, nearly spherical structures, while the branched C-PAM copolymers from the emulsion polymerization showed a significant increase in average MW up to ∼ 10(9)g/mol, which was about 20-fold greater than those from the solution method, and the branched copolymers had more compact or shrunken conformations. While both linear and branched copolymers less than 10(8) g/mol MW were well resolved in an increasing order of MW (normal mode), it was noted that branched copolymers prepared through emulsion polymerization exhibited significantly larger MWs of 10(8-)10(9) g/mol and eluted in the steric/hyperlayer mode, in which the elution order is reversed in an extreme run condition (strong initial field strength followed by a fast field decay during programming). Copyright © 2015 Elsevier B.V. All rights reserved.

Preparation of poly(BMA-co-MMA) particles by soap-free emulsion polymerization and its optical properties as photonic crystals.

PubMed

Lee, Ki-Chang; Choo, Hun-Seung

2014-11-01

Narrowly dispersed poly(BMA-co-MMA) and PBMA latices with particle diameters ranging within 216-435 nm were synthesized successfully by surfactant-free emulsion polymerization with KPS and AIBA. The average particle diameter and particle size distribution, average molecular weight and its distribution, glass transition temperature, reflectance spectra in visible wavelength, and refractive indices for the respective poly(BMA-co-MMA) latices and their photonic crystals were systematically investigated in terms of BMA/MMA ratio, BMA content, polymerization temperature, and DVB effect. The rate of polymerization increased with increasing MMA concentration in BMA/MMA ratio. The particle diameter increased with BMA concentration in BMA/MMA ratio. The molecular weight increased with BMA concentration in BMA/MMA ratio and monomer concentration. The drying of the latices offered self-assembled shiny colloidal crystal films showing the characteristic structural colors in visible wavelength. All the poly(BMA-co-MMA) latices prepared in the study were fallen within the range of photonic grade microspheres. The reflectance measurement on the colloidal photonic crystals having different particle diameters clearly exhibited narrow stopbands. The reflection maxima (λ(max)) measured in this study were well close to the λ(max) calculated, derived from the Bragg's equation. The refractive indices of poly(BMA-co-MMA) photonic crystals were found to be almost same as the theoretical values and increased proportionally from 1.50 to 1.57 with BMA content in BMA/MMA ratios. It was, thus, found that the optical reflectance properties of the poly(BMA-co-MMA) colloidal photonic crystals can be controlled easily by adjusting the reaction conditions and BMA/MMA ratio in soap-free emulsion copolymerization of BMA and MMA.

Methods for Purifying and Detoxifying Sodium Dodecyl Sulfate-Stabilized Polyacrylate Nanoparticles

PubMed Central

Garay-Jimenez, Julio C.; Young, Ashley; Gergeres, Danielle; Greenhalgh, Kerriann; Turos, Edward

2008-01-01

Recent research in our laboratory has centered on studies of polyacrylate and polyacrylamide nanoparticle emulsions for use in antibiotic delivery. Our goal is to develop these nanoparticle emulsions for treatment of life-threatening bacterial infections such as those caused by methicillin-resistant Staphylococcus aureus (MRSA). For this intended application, it is necessary to ensure that the biological activity of the emulsion is due only to the drug attached to the polymeric chain, rather than to any extraneous components. To investigate this, we evaluated cytotoxicity and microbiological activity of the nanoparticle emulsions before and after purification by centrifugation, dialysis, and gel filtration. Depending on the amount of surfactant used, all or most of the microbial and cellular toxicity can be removed by a simple purification procedure. PMID:18472305

Superparamagnetic polymer emulsion particles from a soap-free seeded emulsion polymerization and their application for lipase immobilization.

PubMed

Cui, Yanjun; Chen, Xia; Li, Yanfeng; Liu, Xiao; Lei, Lin; Zhang, Yakui; Qian, Jiayu

2014-01-01

Using emulsion copolymer of styrene (St), glycidyl methacrylate (GMA) and 2-hydroxyethyl methacrylate (HEMA) as seed latexes, the superparamagnetic polymer emulsion particles were prepared by seeded emulsion copolymerization of butyl methacrylate (BMA), vinyl acetate (VAc) and ethylene glycol dimethacrylate in the presence of the seed latexes and superparamagnetic Fe3O4/SiOx nanoparticles (or Fe3O4-APTS nanoparticles) through a two-step process, without addition of any emulsifier. The magnetic emulsion particles named P(St-GMA-HEMA)/P(BMA-VAc) were characterized by transmission electron microscope and vibrating sample magnetometry. The results showed that the magnetic emulsion particles held a structure with a thinner shell (around 100 nm) and a bigger cavity (around 200 nm), and possessed a certain level of magnetic response. The resulting magnetic emulsion particles were employed in the immobilization of lipase by two strategies to immobilized lipase onto the resulting magnetic composites directly (S-1) or using glutaraldehyde as a coupling agent (S-2), thus, experimental data showed that the thermal stability and reusability of immobilized lipase based on S-2 were higher than that of S-1.

Synthesis and characterization of novel polyacid-stabilized latexes.

PubMed

Yang, Pengcheng; Armes, S P

2012-09-18

A series of novel polyacid macromonomers based on 2-hydroxypropyl methacrylate (HPMA) were prepared by atom transfer radical polymerization (ATRP) via a two-step route. First, a range of well-defined PHPMA homopolymer precursors were synthesized by ATRP using a tertiary amine-functionalized initiator, 2-(dimethylamino)ethyl-2-bromoisobutyrylamide, and a CuCl/2, 2'-bipyridine (bpy) catalyst in alcoholic media at 50 °C. ATRP polymerizations were relatively slow and poorly controlled in pure isopropanol (IPA), especially when targeting higher degrees of polymerization (DP > 30). Improved control was achieved by addition of water: low polydispersity (M(w)/M(n) < 1.25) PHPMA homopolymers of DP = 30, 40, 50, 60, or 70 were successfully prepared using a 9:1 w/w % IPA/water mixture at 50 °C. These PHPMA homopolymer precursors were then derivatized to produce the corresponding poly(2-(succinyloxy)propyl methacrylate) (PSPMA) macromonomers by quaternizing the tertiary amine end-group with excess 4-vinylbenzyl chloride, followed by esterification of the pendent hydroxyl groups using excess succinic anhydride at 20 °C. These polyacid macromonomers were evaluated as reactive steric stabilizers for polystyrene latex synthesis under either aqueous emulsion polymerization or alcoholic dispersion polymerization conditions. Near-monodisperse polystyrene latexes were obtained via aqueous emulsion polymerization using 10 wt % PSPMA macromonomer (with respect to styrene monomer) with various initiators as evidenced by scanning electron microscopy, disk centrifuge photosedimentometry and light scattering studies. PSPMA macromomer concentrations as low as 1.0 wt % also produced near-monodisperse latexes, suggesting that these PSPMA macromonomers are highly effective stabilizers. Alcoholic dispersion polymerization of styrene conducted in various ethanol/water mixtures with 10 wt % PSPMA(50) macromonomer produced relatively large near-monodisperse latexes. Increasing the water content in such formulations led to smaller latexes, as expected. Control experiments conducted with 10 wt % PSPMA(50) homopolymer produced relatively large polydisperse latexes via emulsion polymerization and only macroscopic precipitates via alcoholic dispersion polymerization. Thus the terminal styrene group on the macromonomer chains is essential for the formation of well-defined latexes. FT-IR spectroscopy indicated that these latexes contained PSPMA macromonomer, whereas (1)H NMR spectroscopy studies of dissolved latexes allowed stabilizer contents to be determined. Aqueous electrophoresis and X-ray photoelectron spectroscopy studies confirmed that the PSPMA macromonomer chains were located at the latex surface, as expected. Finally, these polyacid-stabilized polystyrene latexes exhibited excellent freeze-thaw stability and remained colloidally stable in the presence of electrolyte.

Physical Properties and Biological Activity of Poly(butyl acrylate–styrene) Nanoparticle Emulsions Prepared with Conventional and Polymerizable Surfactants

PubMed Central

Garay-Jimenez, Julio C.; Gergeres, Danielle; Young, Ashley; Dickey, Sonja; Lim, Daniel V.; Turos, Edward

2009-01-01

Recent efforts in our laboratory have explored the use of polyacrylate nanoparticles in aqueous media as stable emulsions for potential applications in treating drug-resistant bacterial infections. These emulsions are made by emulsion polymerization of acrylated antibiotic compounds in a mixture of butyl acrylate and styrene (7:3 w:w) using sodium dodecyl sulfate (SDS) as a surfactant. Prior work in our group established that the emulsions required purification to remove toxicity associated with extraneous surfactant present in the media. This paper summarizes our investigations of poly(butyl acrylate-styrene) emulsions made using anionic, cationic, zwitterionic, and non-charged (amphiphilic) surfactants, as well as attachable surfactant monomers (surfmers), comparing the cytotoxicity and microbiological activity levels of the emulsion both before and after purification. Our results show that the attachment of a polymerizable surfmer onto the matrix of the nanoparticle neither improves nor diminishes cytotoxic or antibacterial effects of the emulsion, regardless of whether the emulsions are purified or not, and that the optimal properties are associated with the use of the non-ionic surfactants versus those carrying anionic, cationic, or zwitterionic charge. Incorporation of an N-thiolated β-lactam antibacterial agent onto the nanoparticle matrix via covalent attachment endows the emulsion with antibiotic properties against pathogenic bacteria such as methicillin-resistant Staphylococcus aureus (MRSA), without changing the physical properties of the nanoparticles or their emulsions. PMID:19523413

The Morphology of Emulsion Polymerized Latex Particles

DOE R&D Accomplishments Database

Wignall, G. D.; Ramakrishnan, V. R.; Linne, M. A.; Klein, A.; Sperling, L. H.; Wai, M. P.; Gelman, R. A.; Fatica, M. G.; Hoerl, R. H.; Fisher, L. W.

1987-11-01

Under monomer starved feed conditions, emulsion polymerization of perdeuterated methyl methacrylate and styrene in the presence of preformed polymethylmethacrylate latexes resulted in particles with a core-shell morphology, as determined by small-angle neutron scattering (SANS) analysis for a hollow sphere. The locus of polymerization of the added deuterated monomer is therefore at the particle surface. In similar measurements a statistical copolymer of styrene and methyl methacrylate was used as seed particles for further polymerization of trideuteromethyl methacrylate. The resulting polymer latex was again shown to have a core-shell morphological structure as determined by SANS. SANS experiments were also undertaken on polystyrene latexes polymerized by equilibrium swelling methods, with deuterated polymer forming the first or second step. The experiments covered a molecular weight range of 6 x 10{sup 4} 10{sup 6} the molecular weights are consistent with the experimental errors, indicating that the deuterium labeled molecules are randomly distributed in the latex. These results led to the finding that the polymer chains were constrained in the latex particles by factors of 2 to 4 from the relaxed coil dimensions. For M < 10{sup 6} g/mol SANS gave zero angle scattering intensities much higher than expected on the basis of a random distribution of labeled molecules. Several models were examined, including the possible development of core-shell structures at lower molecular weights.

Lipid transfer in oil-in-water isasome emulsions: influence of arrested dynamics of the emulsion droplets entrapped in a hydrogel.

PubMed

Iglesias, Guillermo Ramón; Pirolt, Franz; Sadeghpour, Amin; Tomšič, Matija; Glatter, Otto

2013-12-17

The transfer kinetics of lipids between internally self-assembled droplets of O/W emulsions is studied. The droplets (isasomes) consist of various liquid-crystalline phases or W/O microemulsions stabilized by a polymeric stabilizer F127. The various internal phases were identified by the relative peak positions in the small-angle X-ray scattering (SAXS) curves. An arrested system composed of isasomes embedded in a gel matrix actually provides an additional possibility to control these systems in terms of the release of various host molecules. These experiments have been applied to examine the kinetics of the internal phase reorganization imposed by the lipids' release and uptake by the droplets embedded in a κ-carrageenan (KC) hydrogel network. Increasing the concentration of the gelling agent slows down the transfer from one droplet to the other through the aqueous phase. We examined the region where the free diffusion is stopped. i.e., the point where the system changes from the ergodic to the nonergodic state and the kinetics is essentially slowed down. This effect can be balanced by the addition of small amounts of free polymeric stabilizer, which speeds up the kinetics. This is even possible in the case of highly arrested dynamics of the emulsion droplets, as found for the highest KC hydrogel concentrations forming nonergodic systems.

Arrays of size and distance controlled platinum nanoparticles fabricated by a colloidal method

NASA Astrophysics Data System (ADS)

Manzke, Achim; Vogel, Nicolas; Weiss, Clemens K.; Ziener, Ulrich; Plettl, Alfred; Landfester, Katharina; Ziemann, Paul

2011-06-01

Based on emulsion polymerization in the presence of a Pt complex, polystyrene (PS) particles were prepared exhibiting a well defined average diameter with narrow size-distribution. Furthermore, the colloids contain a controlled concentration of the Pt precursor complex. Optimized coating of Si substrates with such colloids leads to extended areas of hexagonally ordered close-packed PS particles. Subsequent application of plasma etching and annealing steps allows complete removal of the PS carriers and in parallel nucleation and growth of Pt nanoparticles (NPs) which are located at the original center of the PS colloids. In this way, hexagonally arranged spherical Pt NPs are obtained with controlled size and interparticle distances demonstrating variability and precision with so far unknown parameter scalability. This control is demonstrated by the fabrication of Pt NP arrays at a fixed particle distance of 185 nm while systematically varying the diameters between 8 and 15 nm. Further progress could be achieved by seeded emulsion polymerization. Here, Pt loaded PS colloids of 130 nm were used as seeds for a subsequent additional emulsion polymerization, systematically enlarging the diameter of the PS particles. Applying the plasma and annealing steps as above, in this way hexagonally ordered arrays of 9 nm Pt NPs could be obtained at distances up to 260 nm. To demonstrate their stability, such Pt particles were used as etching masks during reactive ion etching thereby transferring their hexagonal pattern into the Si substrate resulting in corresponding arrays of nanopillars.Based on emulsion polymerization in the presence of a Pt complex, polystyrene (PS) particles were prepared exhibiting a well defined average diameter with narrow size-distribution. Furthermore, the colloids contain a controlled concentration of the Pt precursor complex. Optimized coating of Si substrates with such colloids leads to extended areas of hexagonally ordered close-packed PS particles. Subsequent application of plasma etching and annealing steps allows complete removal of the PS carriers and in parallel nucleation and growth of Pt nanoparticles (NPs) which are located at the original center of the PS colloids. In this way, hexagonally arranged spherical Pt NPs are obtained with controlled size and interparticle distances demonstrating variability and precision with so far unknown parameter scalability. This control is demonstrated by the fabrication of Pt NP arrays at a fixed particle distance of 185 nm while systematically varying the diameters between 8 and 15 nm. Further progress could be achieved by seeded emulsion polymerization. Here, Pt loaded PS colloids of 130 nm were used as seeds for a subsequent additional emulsion polymerization, systematically enlarging the diameter of the PS particles. Applying the plasma and annealing steps as above, in this way hexagonally ordered arrays of 9 nm Pt NPs could be obtained at distances up to 260 nm. To demonstrate their stability, such Pt particles were used as etching masks during reactive ion etching thereby transferring their hexagonal pattern into the Si substrate resulting in corresponding arrays of nanopillars. Electronic supplementary information (ESI) available: Detailed description of the experimental part (S1-S4) platinum concentration inside the polymer particles synthesized by a seeded polymerization from the same seed particles measured by ICP-OES (Fig. S1 and S5); SEM image of Pt complex containing PS particles after oxygen plasma treatment (Fig. S2 and S6); effect of hydrofluoric acid treatment on silicon oxide elevation under Pt NPs (Fig. S3 and S6); SEM images demonstrating the variability of Pt NP distance while keeping the diameter constant (Fig. S4 and S8); results of experimental determination of Pt content by ICP-OES (Tables S1 and S9); diameter of the particles at different fabrication states (Tables S2 and S10). See DOI: 10.1039/c1nr10169b

Preparation and characterization of Phase change material microcapsules by a core-shell-like emulsion polymerization method

NASA Astrophysics Data System (ADS)

Ding, Li-ming; Pei, Guang-ling

2015-07-01

Phase change material microcapsules (MicroPCMs) were synthesized by a coreshell-like emulsion polymerization method. Styrene and methylacrylic acid copolymer (PS- MAA) was used as a wall material, and paraffin was used as a core material in order to prepare spherical, high resistance and high enthalpy MicroPCMs. Scanning Electron Microscope (SEM), laser particle size analyzer, Fourier Transform Infrared Spectroscopy (FTIR), Thermogravimetry (TG) and Differential Scanning Calorimeter (DSC) were employed to characterize the MicroPCMs. The results indicated that the average particle size of MicroPCMs was 42.29 μm, and the content of paraffin within microcapsules was 57.6%. The melting temperature and crystallization temperature were 30.7°C and 25.2°C.The melting enthalpy and crystallization enthalpy were -84.1 J/g and 91.3 J/g, respectively.

Selective separation of lambdacyhalothrin by porous/magnetic molecularly imprinted polymers prepared by Pickering emulsion polymerization.

PubMed

Hang, Hui; Li, Chunxiang; Pan, Jianming; Li, Linzi; Dai, Jiangdong; Dai, Xiaohui; Yu, Ping; Feng, Yonghai

2013-10-01

Porous/magnetic molecularly imprinted polymers (PM-MIPs) were prepared by Pickering emulsion polymerization. The reaction was carried out in an oil/water emulsion using magnetic halloysite nanotubes as the stabilizer instead of a toxic surfactant. In the oil phase, the imprinting process was conducted by radical polymerization of functional and cross-linked monomers, and porogen chloroform generated steam under the high reaction temperature, which resulted in some pores decorated with easily accessible molecular binding sites within the as-made PM-MIPs. The characterization demonstrated that the PM-MIPs were porous and magnetic inorganic-polymer composite microparticles with magnetic sensitivity (M(s) = 0.7448 emu/g), thermal stability (below 473 K) and magnetic stability (over the pH range of 2.0-8.0). The PM-MIPs were used as a sorbent for the selective binding of lambdacyhalothrin (LC) and rapidly separated under an external magnetic field. The Freundlich isotherm model gave a good fit to the experimental data. The adsorption kinetics of the PM-MIPs was well described by pseudo-second-order kinetics, indicating that the chemical process could be the rate-limiting step in the adsorption of LC. The selective recognition experiments exhibited the outstanding selective adsorption effect of the PM-MIPs for target LC. Moreover, the PM-MIPs regeneration without significant loss in adsorption capacity was demonstrated by at least four repeated cycles. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Emulsion-Assisted Polymerization-Induced Hierarchical Self-Assembly of Giant Sea Urchin-like Aggregates in a Large Scale.

PubMed

Xu, Qingsong; Huang, Tong; Li, Shanlong; Li, Ke; Li, Chuanlong; Liu, Yannan; Wang, Yuling; Yu, Chunyang; Zhou, Yongfeng

2018-05-09

Hierarchical solution self-assembly has nowadays become an important biomimetic method to prepare highly complex and multifunctional supramolecular structures. However, despites the great progress, it is still highly challenging to prepare hierarchical self-assemblies in a large scale since the self-assembly processes are generally performed at high dilution. Herein, we report an emulsion-assisted polymerization-induced self-assembly (EAPISA) method with the advantages of in-situ self-assembly process, scalable preparation and facile functionalization to prepare hierarchical multiscale sea urchin-like aggregates (SUAs). It also extends horizons of PISA in monomers and in polymerization method. The obtained SUAs from amphiphilic alternating copolymers represent a novel self-assembled structure with micron-sized rattan ball-like capsule (RBC) acting as the hollow core body and radiating nanotubes tens of micrometers in length as the hollow spines. They can effectively capture model proteins at an ultra-low concentration (≈10 nM) after functionalized with amino groups through click copolymerization. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Tunable poly(methacrylic acid-co-acrylamide) nanoparticles through inverse emulsion polymerization.

PubMed

Zhong, Justin X; Clegg, John R; Ander, Eric W; Peppas, Nicholas A

2018-06-01

Environmentally responsive biomaterials have played key roles in the design of biosensors and drug delivery vehicles. Their physical response to external stimuli, such as temperature or pH, can transduce a signal or trigger the release of a drug. In this work, we designed a robust, highly tunable, pH-responsive nanoscale hydrogel system. We present the design and characterization of poly(methacrylic acid-co-acrylamide) hydrogel nanoparticles, crosslinked with methylenebisacrylamide, through inverse emulsion polymerization. The effects of polymerization parameters (i.e., identities and concentrations of monomer and surfactant) and polymer composition (i.e., weight fraction of ionic and crosslinking monomers) on the nanoparticles' bulk and environmentally responsive properties were determined. We generated uniform, spherical nanoparticles which, through modulation of crosslinking, exhibit a volume swelling of 1.77-4.07, relative to the collapsed state in an acidic environment. We believe our system has potential as a base platform for the targeted, injectable delivery of hydrophilic therapeutics. With equal importance, however, we hope that our systematic analysis of the individual impacts of polymerization and purification conditions on nanoparticle composition, morphology, and performance can be used to expedite the development of alternate hydrophilic nanomaterials for a range of biomedical applications. © 2018 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 106A: 1677-1686, 2018. © 2018 Wiley Periodicals, Inc.

Dispersion Polymerization of Polystyrene Particles Using Alcohol as Reaction Medium

NASA Astrophysics Data System (ADS)

Cho, Young-Sang; Shin, Cheol Hwan; Han, Sujin

2016-02-01

In this study, monodisperse polystyrene nanospheres were prepared by dispersion polymerization using alcohol as reaction medium to prepare colloidal clusters of the latex beads. Polyvinylpyrrolidone (PVP) and 2-(methacryloyloxy)ethyltrimethylammonium chloride (MTC) were used as dispersion stabilizer and comonomer, respectively. The particle size could be controlled by adjusting the reactant compositions such as the amount of stabilizer, comonomer, and water in the reactant mixture. The size and monodispersity of the polymeric particles could be also controlled by changing the reaction medium with different alcohols other than ethanol or adjusting the polymerization temperature. The synthesized particles could be self-organized inside water-in-oil emulsion droplets by evaporation-driven self-assembly to produce colloidal clusters of the polymeric nanospheres.

A convenient method to prepare emulsified polyacrylate nanoparticles from powders [corrected] for drug delivery applications.

PubMed

Garay-Jimenez, Julio C; Turos, Edward

2011-08-01

We describe a method to obtain purified, polyacrylate nanoparticles in a homogeneous powdered form that can be readily reconstituted in aqueous media for in vivo applications. Polyacrylate-based nanoparticles can be easily prepared by emulsion polymerization using a 7:3 mixture of butyl acrylate and styrene in water containing sodium dodecyl sulfate as a surfactant and potassium persulfate as a water-soluble radical initiator. The resulting emulsions contain nanoparticles measuring 40-50 nm in diameter with uniform morphology, and can be purified by centrifugation and dialysis to remove larger coagulants as well as residual surfactant and monomers associated with toxicity. These purified emulsions can be lyophilized in the presence of maltose (a non-toxic cryoprotectant) to provide a homogeneous dried powder, which can be reconstituted as an emulsion by addition of an aqueous diluent. Dynamic light scattering and microbiological experiments were carried out on the reconstituted nanoparticles. This procedure allows for ready preparation of nanoparticle emulsions for drug delivery applications. Copyright © 2011 Elsevier Ltd. All rights reserved.

Stability of lutein encapsulated whey protein nano-emulsion during storage

PubMed Central

Guo, Mingruo

2018-01-01

Lutein is a hydrophobic carotenoid that has multiple health functions. However, the application of lutein is limited due to its poor solubility in water and instability under certain conditions during storage. Hereby we generated lutein loaded nano-emulsions using whey protein isolate (WPI) or polymerized whey protein isolate (PWP) with assistance of high intensity ultrasound and evaluate their stability during storage at different conditions. We measured the particle size, zeta-potential, physical stability and lutein content change. Results showed that the PWP based nano-emulsion system was not stable in the tested Oil/Water/Ethanol system indicated by the appearance of stratification within only one week. The WPI based nano-emulsion system showed stable physiochemical stability during the storage at 4°C. The lutein content of the system was reduced by only 4% after four weeks storage at 4°C. In conclusion, our whey protein based nano-emulsion system provides a promising strategy for encapsulation of lutein or other hydrophobic bioactive molecules to expand their applications. PMID:29415071

A solid colloidal drug delivery system for the eye: encapsulation of pilocarpin in nanoparticles.

PubMed

Harmia, T; Speiser, P; Kreuter, J

1986-01-01

The present study was undertaken in order to encapsulate pilocarpin into nanoparticles. Two principally different methods for manufacturing these particles were investigated. Firstly, pilocarpin was dissolved in an aqueous medium in which the polymerization was carried out, and secondly, the polymerizing monomer was kept saturated with the drug solution under acidic conditions resulting in an incorporation into the nanoparticles in an aqueous environment. The amount of pilocarpin that could be incorporated into the nanoparticles was found to be largely influenced by the temperature at which the nanoparticles were produced and by the stabilizers used. At low temperatures, up to 60 per cent of pilocarpin nitrate could be encapsulated into butylcyanoacrylate nanoparticles using emulsion polymerization techniques. Larger amounts of pilocarpin could not be incorporated because of the hydrophilicity of the salts of this drug. The physico-chemical characteristics of the nanoparticles are reported: the particle size and morphology were determined by scanning and transmission electron microscopy and photon correlation spectrometry. The average particle size was about 100 nm. The results obtained in this study show that photon correlation spectrometry is a suitable method for the sizing of nanoparticles.

Combinatorial and high-throughput approaches in polymer science

NASA Astrophysics Data System (ADS)

Zhang, Huiqi; Hoogenboom, Richard; Meier, Michael A. R.; Schubert, Ulrich S.

2005-01-01

Combinatorial and high-throughput approaches have become topics of great interest in the last decade due to their potential ability to significantly increase research productivity. Recent years have witnessed a rapid extension of these approaches in many areas of the discovery of new materials including pharmaceuticals, inorganic materials, catalysts and polymers. This paper mainly highlights our progress in polymer research by using an automated parallel synthesizer, microwave synthesizer and ink-jet printer. The equipment and methodologies in our experiments, the high-throughput experimentation of different polymerizations (such as atom transfer radical polymerization, cationic ring-opening polymerization and emulsion polymerization) and the automated matrix-assisted laser desorption/ionization time-of-flight mass spectroscopy (MALDI-TOF MS) sample preparation are described.

Studies on the formation of polymeric nano-emulsions obtained via low-energy emulsification and their use as templates for drug delivery nanoparticle dispersions.

PubMed

Calderó, G; Montes, R; Llinàs, M; García-Celma, M J; Porras, M; Solans, C

2016-09-01

Ethylcellulose nanoparticles have been obtained from O/W nano-emulsions of the water/polyoxyethylene 10 oleyl ether/[ethyl acetate+4wt% ethylcellulose] system by low energy-energy emulsification at 25°C. Nano-emulsions with droplet sizes below 200nm and high kinetic stability were chosen for solubilising dexamethasone (DXM). Phase behaviour, conductivity and optical analysis studies of the system have evidenced for the first time that both, the polymer and the drug play a role on the structure of the aggregates formed along the emulsification path. Nano-emulsion formation may take place by both, phase inversion and self-emulsification. Spherical polymeric nanoparticles containing surfactant, showing sizes below 160nm have been obtained from the nano-emulsions by organic solvent evaporation. DXM loading in the nanoparticles was high (>90%). The release kinetics of nanoparticle dispersions with similar particle size and encapsulated DXM but different polymer to surfactant ratio were studied and compared to an aqueous DXM solution. Drug release from the nanoparticle dispersions was slower than from the aqueous solution. While the DXM solution showed a Fickian release pattern, the release behaviour from the nanoparticle dispersions was faster than that expected from a pure Fickian release. A coupled diffusion/relaxation model fitted the results very well, suggesting that polymer chains undergo conformational changes enhancing drug release. The contribution of diffusion and relaxation to drug transport in the nanoparticle dispersions depended on their composition and release time. Surfactant micelles present in the nanoparticle dispersion may exert a mild reservoir effect. The small particle size and the prolonged DXM release provided by the ethylcellulose nanoparticle dispersions make them suitable vehicles for controlled drug delivery applications. Copyright © 2016 Elsevier B.V. All rights reserved.

Porous and magnetic molecularly imprinted polymers via Pickering high internal phase emulsions polymerization for selective adsorption of λ-cyhalothrin

NASA Astrophysics Data System (ADS)

Wu, Yunlong; Ma, Yue; Pan, Jianming; Gu, Runxing; Luo, Jialu

2017-03-01

A novel macroporous magnetic molecularly imprinted polymer (MMIPs) of was prepared by W/O Pickering (high internal phase emulsions) HIPEs polymerization, and then it was adopted as adsorbent for selective adsorption of λ-cyhalothrin (LC). In static conditions, adsorption capacity of LC increased rapidly in the first 60 min and reached to equilibrium in approximately 2.0 h. Excellent conformity of the second-order model confirmed the chemical nature of the interaction between the LC and imprinted sites. The fitting adsorption isotherm was a Langmuir type, and the maximum monolayer adsorption capacity at 298 K was 404.4 µmol g-1. Thermodynamic parameters suggested the specific adsorption at 298 K was an exothermic, spontaneous, and entropy decreased process. Competitive recognition studies of the MMIPs were performed with diethyl phthalate (DEP) and the structurally similar compound fenvalerate (FL), and the MMIPs, which displayed high selectivity for LC.

Porous and Magnetic Molecularly Imprinted Polymers via Pickering High Internal Phase Emulsions Polymerization for Selective Adsorption of λ-Cyhalothrin.

PubMed

Wu, Yunlong; Ma, Yue; Pan, Jianming; Gu, Runxing; Luo, Jialu

2017-01-01

A novel macroporous magnetic molecularly imprinted polymer (MMIPs) of was prepared by W/O Pickering (high internal phase emulsions) HIPEs polymerization, and then it was adopted as adsorbent for selective adsorption of λ-cyhalothrin (LC). In static conditions, adsorption capacity of LC increased rapidly in the first 60 min and reached to equilibrium in ~2.0 h. Excellent conformity of the second-order model confirmed the chemical nature of the interaction between the LC and imprinted sites. The fitting adsorption isotherm was a Langmuir type, and the maximum monolayer adsorption capacity at 298 K was 404.4 μmol g -1 . Thermodynamic parameters suggested the specific adsorption at 298 K was an exothermic, spontaneous, and entropy decreased process. Competitive recognition studies of the MMIPs were performed with diethyl phthalate (DEP) and the structurally similar compound fenvalerate (FL), and the MMIPs, which displayed high selectivity for LC.

Porous and Magnetic Molecularly Imprinted Polymers via Pickering High Internal Phase Emulsions Polymerization for Selective Adsorption of λ-Cyhalothrin

PubMed Central

Wu, Yunlong; Ma, Yue; Pan, Jianming; Gu, Runxing; Luo, Jialu

2017-01-01

A novel macroporous magnetic molecularly imprinted polymer (MMIPs) of was prepared by W/O Pickering (high internal phase emulsions) HIPEs polymerization, and then it was adopted as adsorbent for selective adsorption of λ-cyhalothrin (LC). In static conditions, adsorption capacity of LC increased rapidly in the first 60 min and reached to equilibrium in ~2.0 h. Excellent conformity of the second-order model confirmed the chemical nature of the interaction between the LC and imprinted sites. The fitting adsorption isotherm was a Langmuir type, and the maximum monolayer adsorption capacity at 298 K was 404.4 μmol g−1. Thermodynamic parameters suggested the specific adsorption at 298 K was an exothermic, spontaneous, and entropy decreased process. Competitive recognition studies of the MMIPs were performed with diethyl phthalate (DEP) and the structurally similar compound fenvalerate (FL), and the MMIPs, which displayed high selectivity for LC. PMID:28401145

Sequence-controlled methacrylic multiblock copolymers via sulfur-free RAFT emulsion polymerization

NASA Astrophysics Data System (ADS)

Engelis, Nikolaos G.; Anastasaki, Athina; Nurumbetov, Gabit; Truong, Nghia P.; Nikolaou, Vasiliki; Shegiwal, Ataulla; Whittaker, Michael R.; Davis, Thomas P.; Haddleton, David M.

2017-02-01

Translating the precise monomer sequence control achieved in nature over macromolecular structure (for example, DNA) to whole synthetic systems has been limited due to the lack of efficient synthetic methodologies. So far, chemists have only been able to synthesize monomer sequence-controlled macromolecules by means of complex, time-consuming and iterative chemical strategies such as solid-state Merrifield-type approaches or molecularly dissolved solution-phase systems. Here, we report a rapid and quantitative synthesis of sequence-controlled multiblock polymers in discrete stable nanoscale compartments via an emulsion polymerization approach in which a vinyl-terminated macromolecule is used as an efficient chain-transfer agent. This approach is environmentally friendly, fully translatable to industry and thus represents a significant advance in the development of complex macromolecule synthesis, where a high level of molecular precision or monomer sequence control confers potential for molecular targeting, recognition and biocatalysis, as well as molecular information storage.

Estrone specific molecularly imprinted polymeric nanospheres: synthesis, characterization and applications for electrochemical sensor development.

PubMed

Congur, Gulsah; Senay, Hilal; Turkcan, Ceren; Canavar, Ece; Erdem, Arzum; Akgol, Sinan

2013-06-28

The aim of this study is (i) to prepare estrone-imprinted nanospheres (nano-EST-MIPs) and (ii) to integrate them into the electrochemical sensor as a recognition layer. N-methacryloyl-(l)-phenylalanine (MAPA) was chosen as the complexing monomer. Firstly, estrone (EST) was complexed with MAPA and the EST-imprinted poly(2-hyroxyethylmethacrylate-co-N-methacryloyl-(l)-phenylalanine) [EST-imprinted poly(HEMA-MAPA)] nanospheres were synthesized by surfactant- free emulsion polymerization method. The specific surface area of the EST-imprinted poly(HEMA-MAPA) nanospheres was found to be 1275 m2/g with a size of 163.2 nm in diameter. According to the elemental analysis results, the nanospheres contained 95.3 mmole MAPA/g nanosphere. The application of EST specific MIP nanospheres for the development of an electrochemical biosensor was introduced for the first time in our study by using electrochemical impedance spectroscopy (EIS) technique. This nano-MIP based sensor presented a great specificity and selectivity for EST.

Porous Polystyrene Monoliths and Microparticles Prepared from Core Cross-linked Star (CCS) Polymers-Stabilized Emulsions.

PubMed

Chen, Qijing; Shi, Ting; Han, Fei; Li, Zihan; Lin, Chao; Zhao, Peng

2017-08-17

A hydrophobic CCS polymer of poly(benzyl methacrylate) (PBzMA) was prepared in toluene by reversible addition-fragmentation chain transfer (RAFT)-mediated dispersion polymerization. The CCS polymer, with poly(benzyl methacrylate) as the arm and crosslinked N, N'-bis(acryloyl)cystamine (BAC) as the core, was confirmed by characterization with gel permeation chromatography (GPC) and nuclear magnetic resonance (NMR) spectroscopy. Three kinds of oils (toluene, anisole and styrene) were chosen to study the emulsification properties of PBzMA CCS polymer. The oils can be emulsified by CCS polymer to form water-in-oil (w/o) emulsions. Moreover, w/o high internal phase emulsions (HIPEs) can be obtained with the increase of toluene and styrene volume fractions from 75% to 80%. Porous polystyrene monolith and microparticles were prepared from the emulsion templates and characterized by the scanning electronic microscopy (SEM). With the internal phase volume fraction increased, open-pore porous monolith was obtained.

Pharmacokinetics of intramuscular microparticle depot of valdecoxib in an experimental model.

PubMed

Agnihotri, Sagar M; Vavia, Pradeep R

2009-09-01

We did a prospective study to investigate pharmacokinetics of a single intramuscularly (i.m.) administered Valdecoxib (VC) polymeric microparticles in New Zealand white rabbits. Poly[lac(glc-leu)] microparticles encapsulating a potent cyclooxygenase-2- selective inhibitor, VC, were prepared by emulsion and solvent evaporation technique and administered i.m. to rabbits for pharmacokinetic study. A single i.m. dose of drug-loaded poly[lac(glc-leu)] microparticles resulted in sustained therapeutic drug levels in the plasma for 49 days. The relative bioavailability was increased severalfold as compared with unencapsulated drug. Injectable poly[lac(glc-leu)] microparticles hold promise for increasing drug bioavailability and reducing dosing frequency for better management of rheumatoid arthritis.

Chitosan-g-lactide copolymers for fabrication of 3D scaffolds for tissue engineering

NASA Astrophysics Data System (ADS)

Demina, T. S.; Zaytseva-Zotova, D. S.; Timashev, P. S.; Bagratashvili, V. N.; Bardakova, K. N.; Sevrin, Ch; Svidchenko, E. A.; Surin, N. M.; Markvicheva, E. A.; Grandfils, Ch; Akopova, T. A.

2015-07-01

Chitosan-g-oligo (L, D-lactide) copolymers were synthesized and assessed to fabricate a number of 3D scaffolds using a variety of technologies such as oil/water emulsion evaporation technique, freeze-drying and two-photon photopolymerization. Solid-state copolymerization method allowed us to graft up to 160 wt-% of oligolactide onto chitosan backbone via chitosan amino group acetylation with substitution degree reaching up to 0.41. Grafting of hydrophobic oligolactide side chains with polymerization degree up to 10 results in chitosan amphiphilic properties. The synthesized chitosan-g-lactide copolymers were used to design 3D scaffolds for tissue engineering such as spherical microparticles and macroporous hydrogels.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Wenwen; Wang, Weiyu; Li, Hui

In this study, high molecular weight “comb-shaped” graft copolymers, poly(isoprene-g-styrene), with polyisoprene as the backbone and polystyrene as side chains, were synthesized via free radical emulsion polymerization by copolymerization of isoprene with a polystyrene macromonomer synthesized using anionic polymerization. A small amount of toluene was used in order to successfully disperse the macromonomer. Both a redox and thermal initiation system were used in the emulsion polymerization, and the latex particle size and distribution were investigated by dynamic light scattering. The structural characteristics of the macromonomer and comb graft copolymers were investigated through use of size exclusion chromatography, spectroscopy, microscopy, thermalmore » analysis, and rheology. While the macromonomer was successfully copolymerized to obtain the desired multigraft copolymers, small amounts of unreacted macromonomer remained in the products, reflecting its reduced reactivity due to steric effects. Nevertheless, the multigraft copolymers obtained were very high in molecular weight (5–12 × 10 5 g/mol) and up to 10 branches per chain, on average, could be incorporated. A material incorporating 29 wt% polystyrene exhibits a disordered microphase separated morphology and elastomeric properties. As a result, these materials show promise as new, highly tunable, and potentially low cost thermoplastic elastomers.« less

Influence of membrane material on the production of colloidal emulsions by premix membrane emulsification.

PubMed

Gehrmann, Sandra; Bunjes, Heike

2018-05-01

Premix membrane emulsification is a possibility to produce colloidal emulsions as carrier systems for poorly water soluble drugs. During the extrusion of a coarse pre-emulsion through a porous membrane, the emulsion droplets are disrupted into smaller droplets. The influence of the membrane material on the emulsification success was investigated in dependence on the emulsifier. Premixed medium chain triglyceride (MCT) emulsions stabilized with five different emulsifiers were extruded through seven different hydrophilic polymeric membrane materials with pore sizes of 200nm. The resulting emulsions differed strongly in particle size and particle size distribution with a range of median particle sizes between 0.08μm and 11μm. The particle size of the emulsions did not depend mainly on the structure or thickness of the membrane but on the combination of emulsifier and membrane material. Contact angle measurements indicated that the wetting of the membrane with the continuous phase of the emulsion was decisive for achieving emulsions with colloidal particle sizes. The type of dispersed phase was of minor importance as basically the same results were obtained with peanut oil instead of MCT. To prove the assumption that only sufficiently hydrophilic membrane materials led to emulsions with colloidal particle sizes, two membrane materials were hydrophilized by plasma treatment. After hydrophilization, the emulsifying process led to emulsions with smaller particle sizes. The use of an alumina membrane (Anodisc®) improved the process even more. With this type of membrane, emulsions with a median particle size below 250nm and a narrow particle size distribution could be obtained with all investigated emulsifiers. Copyright © 2016 Elsevier B.V. All rights reserved.

Oil encapsulation in core-shell alginate capsules by inverse gelation II: comparison between dripping techniques using W/O or O/W emulsions.

PubMed

Martins, Evandro; Poncelet, Denis; Rodrigues, Ramila Cristiane; Renard, Denis

2017-09-01

In the first part of this article, it was described an innovative method of oil encapsulation from dripping-inverse gelation using water-in-oil (W/O) emulsions. It was noticed that the method of oil encapsulation was quite different depending on the emulsion type (W/O or oil-in-water (O/W)) used and that the emulsion structure (W/O or O/W) had a high impact on the dripping technique and the capsules characteristics. The objective of this article was to elucidate the differences between the dripping techniques using both emulsions and compare the capsule properties (mechanical resistance and release of actives). The oil encapsulation using O/W emulsions was easier to perform and did not require the use of emulsion destabilisers. However, capsules produced from W/O emulsions were more resistant to compression and showed the slower release of actives over time. The findings detailed here widened the knowledge of the inverse gelation and gave opportunities to develop new techniques of oil encapsulation.

Double emulsion solvent evaporation techniques used for drug encapsulation.

PubMed

Iqbal, Muhammad; Zafar, Nadiah; Fessi, Hatem; Elaissari, Abdelhamid

2015-12-30

Double emulsions are complex systems, also called "emulsions of emulsions", in which the droplets of the dispersed phase contain one or more types of smaller dispersed droplets themselves. Double emulsions have the potential for encapsulation of both hydrophobic as well as hydrophilic drugs, cosmetics, foods and other high value products. Techniques based on double emulsions are commonly used for the encapsulation of hydrophilic molecules, which suffer from low encapsulation efficiency because of rapid drug partitioning into the external aqueous phase when using single emulsions. The main issue when using double emulsions is their production in a well-controlled manner, with homogeneous droplet size by optimizing different process variables. In this review special attention has been paid to the application of double emulsion techniques for the encapsulation of various hydrophilic and hydrophobic anticancer drugs, anti-inflammatory drugs, antibiotic drugs, proteins and amino acids and their applications in theranostics. Moreover, the optimized ratio of the different phases and other process parameters of double emulsions are discussed. Finally, the results published regarding various types of solvents, stabilizers and polymers used for the encapsulation of several active substances via double emulsion processes are reported. Copyright © 2015 Elsevier B.V. All rights reserved.

Under-oil superhydrophilic wetted PVDF electrospun modified membrane for continuous gravitational oil/water separation with outstanding flux.

PubMed

Obaid, M; Mohamed, Hend Omar; Yasin, Ahmed S; Yassin, Mohamed A; Fadali, Olfat A; Kim, HakYong; Barakat, Nasser A M

2017-10-15

Water in the world is becoming an increasingly scarce commodity and the membrane technology is a most effective strategy to address this issue. However, the fouling and low flux of the polymeric membrane remains the big challenges. Novel modified Polyvinylidene fluoride (PVDF) membrane was introduced, in this work, using a novel treatment technique for an electrospun polymeric PVDF membrane to be used in oil/water separation systems. The Characterizations of the modified and pristine membranes showed distinct changes in the phase and crystal structure of the membrane material as well as the wettability. The modification process altered the surface morphology and structure of the membrane by forming hydrophilic microspheres on the membrane surface. Therefore, the proposed treatment converts the membrane from highly hydrophobic to be a superhydrophilic under-oil when wetted with water. Accordingly, in the separation of oil/water mixtures, the modified membrane can achieve an outstanding flux of 20664 L/m 2 . hr under gravity, which is higher than the pristine membrane by infinite times. Moreover, in the separation of the emulsion, a high flux of 2727 L/m 2 . h was achieved. The results exhibited that the modified membrane can treat a huge amount of oily water with a minimal energy consumption. The corresponding separation efficiencies of both of oil/water mixtures and emulsion are more than 99%. The achieved characteristics for the modified and pristine membranes could be exploited to design a novel continuous system for oil/water separation with an excellent efficiency. Copyright © 2017 Elsevier Ltd. All rights reserved.

Hierarchical polymerized high internal phase emulsions synthesized from surfactant-stabilized emulsion templates.

PubMed

Wong, Ling L C; Villafranca, Pedro M Baiz; Menner, Angelika; Bismarck, Alexander

2013-05-21

In building construction, structural elements, such as lattice girders, are positioned specifically to support the mainframe of a building. This arrangement provides additional structural hierarchy, facilitating the transfer of load to its foundation while keeping the building weight down. We applied the same concept when synthesizing hierarchical open-celled macroporous polymers from high internal phase emulsion (HIPE) templates stabilized by varying concentrations of a polymeric non-ionic surfactant from 0.75 to 20 w/vol %. These hierarchical poly(merized)HIPEs have multimodally distributed pores, which are efficiently arranged to enhance the load transfer mechanism in the polymer foam. As a result, hierarchical polyHIPEs produced from HIPEs stabilized by 5 vol % surfactant showed a 93% improvement in Young's moduli compared to conventional polyHIPEs produced from HIPEs stabilized by 20 vol % of surfactant with the same porosity of 84%. The finite element method (FEM) was used to determine the effect of pore hierarchy on the mechanical performance of porous polymers under small periodic compressions. Results from the FEM showed a clear improvement in Young's moduli for simulated hierarchical porous geometries. This methodology could be further adapted as a predictive tool to determine the influence of hierarchy on the mechanical properties of a range of porous materials.

Selective removal of erythromycin by magnetic imprinted polymers synthesized from chitosan-stabilized Pickering emulsion.

PubMed

Ou, Hongxiang; Chen, Qunhui; Pan, Jianming; Zhang, Yunlei; Huang, Yong; Qi, Xueyong

2015-05-30

Magnetic imprinted polymers (MIPs) were synthesized by Pickering emulsion polymerization and used to adsorb erythromycin (ERY) from aqueous solution. The oil-in-water Pickering emulsion was stabilized by chitosan nanoparticles with hydrophobic Fe3O4 nanoparticles as magnetic carrier. The imprinting system was fabricated by radical polymerization with functional and crosslinked monomer in the oil phase. Batches of static and dynamic adsorption experiments were conducted to analyze the adsorption performance on ERY. Isotherm data of MIPs well fitted the Freundlich model (from 15 °C to 35 °C), which indicated heterogeneous adsorption for ERY. The ERY adsorption capacity of MIPs was about 52.32 μmol/g at 15 °C. The adsorption kinetics was well described by the pseudo-first-order model, which suggested that physical interactions were primarily responsible for ERY adsorption. The Thomas model used in the fixed-bed adsorption design provided a better fit to the experimental data. Meanwhile, ERY exhibited higher affinity during adsorption on the MIPs compared with the adsorption capacity of azithromycin and chloramphenicol. The MIPs also exhibited excellent regeneration capacity with only about 5.04% adsorption efficiency loss in at least three repeated adsorption-desorption cycles. Copyright © 2015 Elsevier B.V. All rights reserved.

Polymeric nanoparticles of siRNA prepared by a double-emulsion solvent-diffusion technique: Physicochemical properties, toxicity, biodistribution and efficacy in a mammary carcinoma mice model.

PubMed

Ben David-Naim, Meital; Grad, Etty; Aizik, Gil; Nordling-David, Mirjam M; Moshel, Ofra; Granot, Zvi; Golomb, Gershon

2017-11-01

siRNA-loaded nanoparticles (NPs) administered systemically can overcome the poor stability and rapid elimination of free double-stranded RNA in circulation, resulting in increased tumor accumulation and efficacy. siRNA against osteopontin (siOPN), a protein involved in breast cancer development, was encapsulated in poly(D,L-lactic-co-glycolic acid) NPs by a double emulsion solvent diffusion (DESD) technique. We also compared the effect of polyethylenimine (PEI) molecular weight (800 Da and 25 kDa), used as the counter-ion for siRNA complexation, on the physicochemical properties of the NPs, cytotoxicity, and cellular uptake. NPs prepared by the DESD technique were obtained at the desired size (∼170 nm) using both types of PEIs, and were characterized with a neutral surface charge, high encapsulation yield (up to ∼60%), siOPN concentration of 5.6-8.4 μg/mg, stability in physiologic conditions in vitro and in vivo, and long-term shelf-life stability (> 3 years). The NPs prepared using both PEIs exhibited no cytotoxicity in primary smooth muscle culture, and no detrimental effect on mice liver enzymes following their IV administration. Following cellular uptake and biodistribution studies, the therapeutic potential of the NPs was demonstrated by a significant decrease of tumor progression and size in an ectopic xenograft model of mammary carcinoma in mice. Copyright © 2017 Elsevier Ltd. All rights reserved.

Model Filled Polymers. 6. Determination of the Crosslink Density of Polymeric Beads by Swelling

DTIC Science & Technology

1990-08-22

7 References [1] M. Mooney , J. AppI. Phys., 11, 582 (1940). [2] R. S. Rivlin , and D. W. Sanders, Trans. Faraday Soc., 48, 200 (1952). [31 P. J. Flory...microbeads ranging in diameter from 0.2 to 1 p were prepared by emulsion polymerization in the absence of emulsifier [23]. Polytetrafluorethylene ( PTFE ...density of polymethyl methacrylate is 1.17 g/cm3 [201. Swelling A PTFE ultrafiltration membrane is weighed and inserted in a concave configuration

Ionene modified small polymeric beads

NASA Technical Reports Server (NTRS)

Rembaum, Alan (Inventor)

1977-01-01

Linear ionene polyquaternary cationic polymeric segments are bonded by means of the Menshutkin reaction (quaternization) to biocompatible, extremely small, porous particles containing halide or tertiary amine sites which are centers for attachment of the segments. The modified beads in the form of emulsions or suspensions offer a large, positively-charged surface area capable of irreversibly binding polyanions such as heparin, DNA, RNA or bile acids to remove them from solution or of reversibly binding monoanions such as penicillin, pesticides, sex attractants and the like for slow release from the suspension.

Creating nanoscale emulsions using condensation.

PubMed

Guha, Ingrid F; Anand, Sushant; Varanasi, Kripa K

2017-11-08

Nanoscale emulsions are essential components in numerous products, ranging from processed foods to novel drug delivery systems. Existing emulsification methods rely either on the breakup of larger droplets or solvent exchange/inversion. Here we report a simple, scalable method of creating nanoscale water-in-oil emulsions by condensing water vapor onto a subcooled oil-surfactant solution. Our technique enables a bottom-up approach to forming small-scale emulsions. Nanoscale water droplets nucleate at the oil/air interface and spontaneously disperse within the oil, due to the spreading dynamics of oil on water. Oil-soluble surfactants stabilize the resulting emulsions. We find that the oil-surfactant concentration controls the spreading behavior of oil on water, as well as the peak size, polydispersity, and stability of the resulting emulsions. Using condensation, we form emulsions with peak radii around 100 nm and polydispersities around 10%. This emulsion formation technique may open different routes to creating emulsions, colloidal systems, and emulsion-based materials.

An easily regenerable enzyme reactor prepared from polymerized high internal phase emulsions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ruan, Guihua, E-mail: guihuaruan@hotmail.com; Guangxi Collaborative Innovation Center for Water Pollution Control and Water Safety in Karst Area, Guilin University of Technology, Guilin 541004; Wu, Zhenwei

A large-scale high-efficient enzyme reactor based on polymerized high internal phase emulsion monolith (polyHIPE) was prepared. First, a porous cross-linked polyHIPE monolith was prepared by in-situ thermal polymerization of a high internal phase emulsion containing styrene, divinylbenzene and polyglutaraldehyde. The enzyme of TPCK-Trypsin was then immobilized on the monolithic polyHIPE. The performance of the resultant enzyme reactor was assessed according to the conversion ability of N{sub α}-benzoyl-L-arginine ethyl ester to N{sub α}-benzoyl-L-arginine, and the protein digestibility of bovine serum albumin (BSA) and cytochrome (Cyt-C). The results showed that the prepared enzyme reactor exhibited high enzyme immobilization efficiency and fast andmore » easy-control protein digestibility. BSA and Cyt-C could be digested in 10 min with sequence coverage of 59% and 78%, respectively. The peptides and residual protein could be easily rinsed out from reactor and the reactor could be regenerated easily with 4 M HCl without any structure destruction. Properties of multiple interconnected chambers with good permeability, fast digestion facility and easily reproducibility indicated that the polyHIPE enzyme reactor was a good selector potentially applied in proteomics and catalysis areas. - Graphical abstract: Schematic illustration of preparation of hypercrosslinking polyHIPE immobilized enzyme reactor for on-column protein digestion. - Highlights: • A reactor was prepared and used for enzyme immobilization and continuous on-column protein digestion. • The new polyHIPE IMER was quite suit for protein digestion with good properties. • On-column digestion revealed that the IMER was easy regenerated by HCl without any structure destruction.« less

Multiple emulsions: an overview.

PubMed

Khan, Azhar Yaqoob; Talegaonkar, Sushama; Iqbal, Zeenat; Ahmed, Farhan Jalees; Khar, Roop Krishan

2006-10-01

Multiple emulsions are complex polydispersed systems where both oil in water and water in oil emulsion exists simultaneously which are stabilized by lipophillic and hydrophilic surfactants respectively. The ratio of these surfactants is important in achieving stable multiple emulsions. Among water-in-oil-in-water (w/o/w) and oil-in-water-in-oil (o/w/o) type multiple emulsions, the former has wider areas of application and hence are studied in great detail. Formulation, preparation techniques and in vitro characterization methods for multiple emulsions are reviewed. Various factors affecting the stability of multiple emulsions and the stabilization approaches with specific reference to w/o/w type multiple emulsions are discussed in detail. Favorable drug release mechanisms and/or rate along with in vivo fate of multiple emulsions make them a versatile carrier. It finds wide range of applications in controlled or sustained drug delivery, targeted delivery, taste masking, bioavailability enhancement, enzyme immobilization, etc. Multiple emulsions have also been employed as intermediate step in the microencapsulation process and are the systems of increasing interest for the oral delivery of hydrophilic drugs, which are unstable in gastrointestinal tract like proteins and peptides. With the advancement in techniques for preparation, stabilization and rheological characterization of multiple emulsions, it will be able to provide a novel carrier system for drugs, cosmetics and pharmaceutical agents. In this review, emphasis is laid down on formulation, stabilization techniques and potential applications of multiple emulsion system.

Polyacrylates with High Biomass Contents for Pressure-Sensitive Adhesives Prepared via Mini-emulsion Polymerization

Treesearch

Gang Pu; Matthew R. Dubay; Jiguang Zhang; Steven J. Severtson; Carl J. Houtman

2012-01-01

n-Butyl acrylate and other acrylic monomers were copolymerized with an acrylated macromonomer to produce polymers for pressure-sensitive adhesive (PSA) applications. Macromonomers were generated through the ring-opening copolymerization of L-lactide and ε-caprolactone with 2-hydroxyethyl...

Reduced Graphene Oxide-Hybridized Polymeric High-Internal Phase Emulsions for Highly Efficient Removal of Polycyclic Aromatic Hydrocarbons from Water Matrix.

PubMed

Huang, Yipeng; Zhang, Wenjuan; Ruan, Guihua; Li, Xianxian; Cong, Yongzheng; Du, Fuyou; Li, Jianping

2018-03-27

Reduced graphene oxide (RGO)-hybridized polymeric high-internal phase emulsions (RGO/polyHIPEs) with an open-cell structure and hydrophobicity have been successfully prepared using 2-ethylhexyl acrylate and ethylene glycol dimethacrylate as the monomer and the cross-linker, respectively. The adsorption mechanism and performance of this RGO/polyHIPEs to polycyclic aromatic hydrocarbons (PAHs) were investigated. Adsorption isotherms of PAHs on RGO/polyHIPEs show that the saturated adsorption capacity is 47.5 mg/g and the equilibrium time is 8 h. Cycling tests show that the adsorption capacity of RGO/polyHIPEs remains stable in 10 adsorption-desorption cycles without observable structure change in RGO/polyHIPEs. Moreover, the PAH residues in water samples after being purified by RGO/polyHIPEs are lower than the limit values in drinking water set by the European Food Safety Authority. These results demonstrate that the RGO/polyHIPEs have great potentiality in PAH removal and water purification.

Carbon dioxide-in-oil emulsions stabilized with silicone-alkyl surfactants for waterless hydraulic fracturing.

PubMed

Alzobaidi, Shehab; Lee, Jason; Jiries, Summer; Da, Chang; Harris, Justin; Keene, Kaitlin; Rodriguez, Gianfranco; Beckman, Eric; Perry, Robert; Johnston, Keith P; Enick, Robert

2018-09-15

The design of surfactants for CO 2 /oil emulsions has been elusive given the low CO 2 -oil interfacial tension, and consequently, low driving force for surfactant adsorption. Our hypothesis is that waterless, high pressure CO 2 /oil emulsions can be stabilized by hydrophobic comb polymer surfactants that adsorb at the interface and sterically stabilize the CO 2 droplets. The emulsions were formed by mixing with an impeller or by co-injecting CO 2 and oil through a beadpack (CO 2 volume fractions (ϕ) of 0.50-0.90). Emulsions were generated with comb polymer surfactants with a polydimethylsiloxane (PDMS) backbone and pendant linear alkyl chains. The C 30 alkyl chains are CO 2 -insoluble but oil soluble (oleophilic), whereas PDMS with more than 50 repeat units is CO 2 -philic but only partially oleophilic. The adsorbed surfactants sterically stabilized CO 2 droplets against Ostwald ripening and coalescence. The optimum surfactant adsorption was obtained with a PDMS degree of polymerization of ∼88 and seven C 30 side chains. The emulsion apparent viscosity reached 18 cP at a ϕ of 0.70, several orders of magnitude higher than the viscosity of pure CO 2 , with CO 2 droplets in the 10-150 µm range. These environmentally benign waterless emulsions are of interest for hydraulic fracturing, especially in water-sensitive formations. Copyright © 2018 Elsevier Inc. All rights reserved.

Feasibility of the Simultaneous Determination of Monomer Concentrations and Particle Size in Emulsion Polymerization Using in Situ Raman Spectroscopy

PubMed Central

2015-01-01

An immersion Raman probe was used in emulsion copolymerization reactions to measure monomer concentrations and particle sizes. Quantitative determination of monomer concentrations is feasible in two-monomer copolymerizations, but only the overall conversion could be measured by Raman spectroscopy in a four-monomer copolymerization. The feasibility of measuring monomer conversion and particle size was established using partial least-squares (PLS) calibration models. A simplified theoretical framework for the measurement of particle sizes based on photon scattering is presented, based on the elastic-sphere-vibration and surface-tension models. PMID:26900256

Amphiphilic Soft Janus Particles as Interfacial Stabilizers

NASA Astrophysics Data System (ADS)

Wang, Wenda; Niu, Sunny; Sosa, Chris; Prud'Homme, Robert; Priestley, Rodney; Priestley Polymer Group Team; Prud'homme Research Group Team

Janus particles, which incorporate two or more ``faces'' with different chemical functionality, have attracted great attention in scientific research. Amphiphilic Janus particles have two faces with distinctly different hydrophobicity. This can be thought of as colloidal surfactants. Theoretical studies on the stabilization of emulsions using Janus particles have confirmed higher efficiency. Herein we synthesize the narrow distributed amphiphilic polymeric Janus particles via Precipitation-Induced Self-Assembly (PISA). The efficiency of the amphiphilic Janus particles are tested on different oil/water systems. Biocompatible polymers can also be used on this strategy and may potentially have wide application for food emulsion, cosmetics and personal products.

Histidine-functionalized carbon-based dot-Zinc(II) nanoparticles as a novel stabilizer for Pickering emulsion synthesis of polystyrene microspheres.

PubMed

Ruiyi, Li; Zaijun, Li; Junkang, Liu

2017-05-01

Carbon-based dots (CDs) are nanoparticles with size-dependent optical and electronic properties that have been widely applied in energy-efficient displays and lighting, photovoltaic devices and biological markers. However, conventional CDs are difficult to be used as ideal stabilizer for Pickering emulsion due to its irrational amphiphilic structure. The study designed and synthesized a new histidine-functionalized carbon dot-Zinc(II) nanoparticles, which is termed as His-CD-Zn. The His-CD was made via one-step hydrothermal treatment of histidine and maleic acid. The His-CD reacted with Zn 2+ to form His-CD-Zn. The as-prepared His-CD-Zn was used as a solid particle surfactant for stabilizing styrene-in-water emulsion. The Pickering emulsion exhibits high stability and sensitive pH-switching behaviour. The introduction of S 2 O 8 2- triggers the emulsion polymerization of styrene. The resulted polystyrene microsphere was well coated with His-CDs on the surface. It was successfully used as an ideal adsorbent for removal of heavy metallic ions from water with high adsorption capacity. The study also provides a prominent approach for fabrication of amphiphilic carbon-based nanoparticles for stabilizing Pickering emulsion. Copyright © 2017 Elsevier Inc. All rights reserved.

UV shielding with visible transparency based properties of poly (styrene-co-acrylonitrile)/Ag doped ZnO nanocomposite

NASA Astrophysics Data System (ADS)

Singh, Rajender; Verma, Karan; Singh, Tejbir; Barman, P. B.; Sharma, Dheeraj

2018-02-01

Development of ultraviolet (UV) shielding with visible transparency based thermoplastic polymer nanocomposite (PNs) presents an important requisite in terms of their efficiency and cost. Present study contributed for the same approach by dispersion of Ag doped ZnO nanoparticles upto 10 wt% in poly (styrene-co-acrylonitrile) matrix by insitu emulsion polymerization method. The crystal and chemical structure of PNs has been analyzed by x-ray diffraction (XRD) and fourier infrared spectrometer (FTIR) techniques. The morphological and elemental information of synthesized nanomaterial has been studied by field emission scanning electron microscope (FESEM) and energy dispersive spectroscopy (EDS) technique. The optical properties of PNs has been studied by UV-visible spectroscopy technique. The incorporation of nanoparticles in polymer matrix absorb the complete UV light with visible transparency. The present reported polymer nanocomposite (PNs) have tuned refractive index with UV blocking and visible transparency based properties which can serve as a viable alternative as compared to related conventional materials.

Surface Functionalization Methods to Enhance Bioconjugation in Metal-Labeled Polystyrene Particles

PubMed Central

Abdelrahman, Ahmed I.; Thickett, Stuart C.; Liang, Yi; Ornatsky, Olga; Baranov, Vladimir; Winnik, Mitchell A.

2011-01-01

Lanthanide-encoded polystyrene particles synthesized by dispersion polymerization are excellent candidates for mass cytometry based immunoassays, however they have previously lacked the ability to conjugate biomolecules to the particle surface. We present here three approaches to post-functionalize these particles, enabling the covalent attachment of proteins. Our first approach used partially hydrolyzed poly(N-vinylpyrrolidone) as a dispersion polymerization stabilizer to synthesize particles with high concentration of -COOH groups on the particle surface. In an alternative strategy to provide -COOH functionality to the lanthanide-encoded particles, we employed seeded emulsion polymerization to graft poly(methacrylic acid) (PMAA) chains onto the surface of these particles. However, these two approaches gave little to no improvement in the extent of bioconjugation. In our third approach, seeded emulsion polymerization was subsequently used as a method to grow a functional polymer shell (in this case, poly(glycidyl methacrylate) (PGMA)) onto the surface of these particles, which proved highly successful. The epoxide-rich PGMA shell permitted extensive surface bioconjugation of NeutrAvidin, as probed by an Lu-labeled biotin reporter (ca. 7 × 105 binding events per particle with a very low amount of non-specific binding) and analyzed by mass cytometry. It was shown that coupling agents such as EDC were not needed, such was the reactivity of the particle surface. These particles were stable and the addition of a polymeric shell was shown did not affect the narrow lanthanide ion distribution within the particle interior as analyzed by mass cytometry. These particles represent the most promising candidates for the development of a highly multiplexed bioassay based on lanthanide-labeled particles to date. PMID:21799543

Preparation and Characterization of Polymeric Nanoparticles: An Interdisciplinary Experiment

ERIC Educational Resources Information Center

Ramalho, Maria J.; Pereira, M. Carmo

2016-01-01

In this work, a laboratory experiment to introduce graduate students to nanotechnology is described. Students prepared poly(lactic-"co"-glycolic acid) (PLGA) nanoparticles using two different synthesis procedures, a single and a double emulsion-solvent evaporation method. The students also performed a physicochemical characterization of…

Sustained-releasing hollow microparticles with dual-anticancer drugs elicit greater shrinkage of tumor spheroids.

PubMed

Baek, Jong-Suep; Choo, Chee Chong; Tan, Nguan Soon; Loo, Say Chye Joachim

2017-10-06

Polymeric particulate delivery systems are vastly explored for the delivery of chemotherapeutic agents. However, the preparation of polymeric particulate systems with the capability of providing sustained release of two or more drugs is still a challenge. Herein, poly (D, L-lactic-co-glycolic acid, 50:50) hollow microparticles co-loaded with doxorubicin and paclitaxel were developed through double-emulsion solvent evaporation technique. Hollow microparticles were formed through the addition of an osmolyte into the fabrication process. The benefits of hollow over solid microparticles were found to be higher encapsulation efficiency and a more rapid drug release rate. Further modification of the hollow microparticles was accomplished through the introduction of methyl-β-cyclodextrin. With this, a higher encapsulation efficiency of both drugs and an enhanced cumulative release were achieved. Spheroid study further demonstrated that the controlled release of the drugs from the methyl-β-cyclodextrin -loaded hollow microparticles exhibited enhanced tumor regressions of MCF-7 tumor spheroids. Such hollow dual-drug-loaded hollow microparticles with sustained releasing capabilities may have a potential for future applications in cancer therapy.

Influence of pH and temperature of dip-coating solution on the properties of cellulose acetate-ceramic composite membrane for ultrafiltration.

PubMed

Kaur, Harjot; Bulasara, Vijaya Kumar; Gupta, Raj Kumar

2018-09-01

Polymer-ceramic composite membranes were prepared by dip coating technique using 5 wt.% cellulose acetate (CA) solution at different temperatures (15 °C, 25 °C and 40 °C). The effect of pH (2-12) of the polymeric solution on the properties of the membranes was studied using SEM, EDAX, FTIR, gas and liquid permeation. The thickness of the polymeric layer depended on the interaction of CA solution with the surface of ceramic support. Membrane permeability decreased with increase in pH because of decrease in pore size and porosity resulting from strong interaction of the polymer layer with the ceramic support. The porosity and mean pore size of the prepared membranes were found to be 28-60% and 30-47 nm (ultrafiltration range), respectively. The optimized membrane (pH 7) was used for ultrafiltration of oil in water emulsions (100 and 200 mg/L). Oil rejection of 99.61% was obtained for 100 mg/L of oil concentration in water. Copyright © 2018 Elsevier Ltd. All rights reserved.

Preparation of crosslinked amphiphilic silver nanogel as thin film corrosion protective layer for steel.

PubMed

Atta, Ayman M; El-Mahdy, Gamal A; Al-Lohedan, Hamad A; Ezzat, Abdelrahman O

2014-07-17

Monodisperse silver nanoparticles were synthesized by a new developed method via reaction of AgNO3 and oleic acid with the addition of a trace amount of Fe3+ ions. Emulsion polymerization at room temperature was employed to prepare a core-shell silver nanoparticle with controllable particle size. N,N'-methylenebisacrylamide (MBA) and potassium peroxydisulfate (KPS) were used as a crosslinker, and as redox initiator system, respectively for crosslinking polymerization. The structure and morphology of the silver nanogels were characterized by Fourier transform infrared spectroscopy (FTIR), transmission and scanning electron microscopy (TEM and SEM). The effectiveness of the synthesized compounds as corrosion inhibitors for steel in 1 M HCl was investigated by various electrochemical techniques such as potentiodynamic polarization and electrochemical impedance spectroscopy (EIS). Monolayers of silver nanoparticle were self-assembled on the fresh active surface of the steel electrode and have been tested as a corrosion inhibitor for steel in 1 M HCl solution. The results of polarization measurements showed that nanogel particles act as a mixed type inhibitor.

Glyconanobiotics: Novel carbohydrated nanoparticle antibiotics for MRSA and Bacillus anthracis.

PubMed

Abeylath, Sampath C; Turos, Edward; Dickey, Sonja; Lim, Daniel V

2008-03-01

This report describes the synthesis and evaluation of glycosylated polyacrylate nanoparticles that have covalently-bound antibiotics within their framework. The requisite glycosylated drug monomers were prepared from one of three known antibiotics, an N-sec-butylthio beta-lactam, ciprofloxacin, and a penicillin, by acylation with 3-O-acryloyl-1,2-O-isopropylidene-5,6 bis((chlorosuccinyl)oxy)-d-glucofuranose (7) or 6-O-acetyl-3-O-acryloyl-1,2-O-isopropylidene-5-(chlorosuccinyl)oxy-alpha-d-glucofuranose (10). These acrylated monomers were subjected to emulsion polymerization in a 7:3 (w:w) mixture of butyl acrylate-styrene in the presence of sodium dodecyl sulfate as surfactant (3 weight %) and potassium persulfate as a radical initiator (1 weight %). The resulting nanoparticle emulsions were characterized by dynamic light scattering and found to have similar diameters ( approximately 40 nm) and size distributions to those of our previously studied systems. Microbiological testing showed that the N-sec-butylthio beta-lactam and ciprofloxacin nanoparticles both have powerful in vitro activities against methicillin-resistant Staphylococcus aureus and Bacillus anthracis, while the penicillin-bound nanoparticles have no antimicrobial activity. This indicates the need for matching a suitable antibiotic with the nanoparticle carrier. Overall, the study shows that even relatively large, polar acrylate monomers (MW>1000 amu) can be efficiently incorporated into the nanoparticle matrix by emulsion polymerization, providing opportunities for further advances in nanomedicine.

Glyconanobiotics: Novel carbohydrated nanoparticle antibiotics for MRSA and Bacillus anthracis

PubMed Central

Abeylath, Sampath C.; Turos, Edward; Dickey, Sonja; Limb, Daniel V.

2008-01-01

This report describes the synthesis and evaluation of glycosylated polyacrylate nanoparticles that have covalently-bound antibiotics within their framework. The requisite glycosylated drug monomers were prepared from one of three known antibiotics, an N-sec-butylthio β-lactam, ciprofloxacin, and a penicillin, by acylation with 3-O-acryloyl-1,2-O-isopropylidene-5,6 bis((chlorosuccinyl)oxy)-D-glucofuranose (7) or 6-O-acetyl-3-O-acryloyl-1,2-O-isopropylidene-5-(chlorosuccinyl)oxy-α-D-glucofuranose (10). These acrylated monomers were subjected to emulsion polymerization in a 7:3 (w:w) mixture of butyl acrylate-styrene in the presence of sodium dodecyl sulfate as surfactant (3 weight %) and potassium persulfate as a radical initiator (1 weight %). The resulting nanoparticle emulsions were characterized by dynamic light scattering and found to have similar diameters (~40 nm) and size distributions to those of our previously studied systems. Microbiological testing showed that the N-sec-butylthio β-lactam and ciprofloxacin nanoparticles both have powerful in vitro activities against methicillin-resistant Staphylococcus aureus and Bacillus anthracis, while the penicillin-bound nanoparticles have no antimicrobial activity. This indicates the need for matching a suitable antibiotic with the nanoparticle carrier. Overall, the study shows that even relatively large, polar acrylate monomers (MW>1000 amu) can be efficiently incorporated into the nanoparticle matrix by emulsion polymerization, providing opportunities for further advances in nanomedicine. PMID:18063370

General route for the assembly of functional inorganic capsules.

PubMed

Akartuna, Ilke; Tervoort, Elena; Studart, André R; Gauckler, Ludwig J

2009-11-03

Semipermeable, hollow capsules are attractive materials for the encapsulation and delivery of active agents in food processing, pharmaceutical and agricultural industries, and biomedicine. These capsules can be produced by forming a solid shell of close packed colloidal particles, typically polymeric particles, at the surface of emulsion droplets. However, current methods to prepare such capsules may involve multistep chemical procedures to tailor the surface chemistry of particles or are limited to particles that exhibit inherently the right hydrophobic-hydrophilic balance to adsorb around emulsion droplets. In this work, we describe a general and simple method to fabricate semipermeable, inorganic capsules from emulsion droplets stabilized by a wide variety of colloidal metal oxide particles. The assembly of particles at the oil-water interface is induced by the in situ hydrophobization of the particle surface through the adsorption of short amphiphilic molecules. The adsorption of particles at the interface leads to stable capsules comprising a single layer of particles in the outer shell. Such capsules can be used in the wet state or can be further processed into dry capsules. The permeability of the capsules can be modified by filling the interstices between the shell particles with polymeric or inorganic species. Functional capsules with biocompatible, bioresorbable, heat-resistant, chemical-resistant, and magnetic properties were prepared using alumina, silica, iron oxide, or tricalcium phosphate as particles in the shell.

Enhancement of thermal and mechanical properties of poly(MMA-co-BA)/Cloisite 30B nanocomposites by ultrasound-assisted in-situ emulsion polymerization.

PubMed

Sharma, Sachin; Kumar Poddar, Maneesh; Moholkar, Vijayanand S

2017-05-01

This study reports synthesis and characterization of poly(MMA-co-BA)/Cloisite 30B (organo-modified montmorillonite clay) nanocomposites by ultrasound-assisted in-situ emulsion polymerization. Copolymers have been synthesized with MMA:BA monomer ratio of 4:1, and varying clay loading (1-5wt% monomer). The poly(MMA-co-BA)/Cloisite 30B nanocomposites have been characterized for their thermal and mechanical properties. Ultrasonically synthesized nanocomposites have been revealed to possess higher thermal degradation resistance and mechanical strength than the nanocomposites synthesized using conventional techniques. These properties, however, show an optimum (or maxima) with clay loading. The maximum values of thermal and mechanical properties of the nanocomposites with optimum clay loading are as follows. Thermal degradation temperatures: T 10% =320°C (4wt%), T 50 =373°C (4wt%), maximum degradation temperature=384°C (4wt%); glass transition temperature=64.8°C (4wt%); tensile strength=20MPa (2wt%), Young's modulus=1.31GPa (2wt%), Percentage elongation=17.5% (1wt%). Enhanced properties of poly(MMA-co-BA)/Cloisite 30B nanocomposites are attributed to effective exfoliation and dispersion of clay nanoparticles in copolymer matrix due to intense micro-convection induced by ultrasound and cavitation. Clay platelets help in effective heat absorption with maximum surface interaction/adhesion that results in increased thermal resistivity of nanocomposites. Hindered motion of the copolymer chains due to clay platelets results in enhancement of tensile strength and Young's modulus of nanocomposite. Rheological (liquid) study of the nanocomposites reveals that nanocomposites have higher yield stress and infinite shear viscosity than neat copolymer. Nonetheless, nanocomposites still display shear thinning behavior - which is typical of the neat copolymer. Copyright © 2016 Elsevier B.V. All rights reserved.

Long-term biobarriers to plant and animal intrusions of uranium tailings. [24% trifluralin, 18% carbon black, and 58% polymer

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cline, J.F.; Burton, F.G.; Cataldo, D.A.

1982-09-01

The objective of this project was to develop and evaluate the effectiveness of physical and chemical barriers designed to prevent plant and animal breachment of uranium mill tailings containment systems for an extended period of time. A polymeric carrier/biocide delivery system was developed and tested in the laboratory, greenhouse and field. A continuous flow technique was established to determine the release rates of the biocides from the PCD systems; polymeric carrier specifications were established. Studies were conducted to determine effective biocide concentrations required to produce a phytotoxic response and the relative rates of phytotoxin degradation resulting from chemical and biologicalmore » breakdown in soils. The final PCD system developed was a pelletized system containing 24% trifluralin, 18% carbon black and 58% polymer. Pellets were placed in the soil at the Grand Junction U-tailings site at one in. and two in. intervals. Data obtained in the field determined that the pellets released enough herbicide to the soil layer to stop root elongation past the barrier. Physical barriers to subsurface movement of burrowing animals were investigated. Small crushed stone (1 to 1 1/2 in. diameter) placed over asphalt emulsion and multilayer soil seals proved effective as barriers to a small mammal (ground squirrels) but were not of sufficient size to stop a larger animal (the prairie dog). No penetrations were made through the asphalt emulsion or the clay layer of the multilayer soil seals by either of the two mammals tested. A literature survey was prepared and published on the burrowing habits of the animals that may be found at U-tailings sites.« less

The development of self-emulsifying oil-in-water emulsion adjuvant and an evaluation of the impact of droplet size on performance.

PubMed

Shah, Ruchi R; Dodd, Stephanie; Schaefer, Mary; Ugozzoli, Mildred; Singh, Manmohan; Otten, Gillis R; Amiji, Mansoor M; O'Hagan, Derek T; Brito, Luis A

2015-04-01

Microfluidization is an established technique for preparing emulsion adjuvant formulations for use in vaccines. Although this technique reproducibly yields high-quality stable emulsions, it is complex, expensive, and requires proprietary equipment. For this study, we developed a novel and simple low shear process to prepare stable reproducible emulsions without the use of any proprietary equipment. We found this process can produce a wide range of differently sized emulsions based on the modification of ratios of oil and surfactants. Using this process, we prepared a novel 20-nm-sized emulsion that was stable, reproducible, and showed adjuvant effects. During evaluation of this emulsion, we studied a range of emulsions with the same composition all sized below 200; 20, 90, and 160 nm in vivo and established a correlation between adjuvant size and immune responses. Our studies indicate that 160-nm-sized emulsions generate the strongest immune responses. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

Prospects of pharmaceuticals and biopharmaceuticals loaded microparticles prepared by double emulsion technique for controlled delivery

PubMed Central

Giri, Tapan Kumar; Choudhary, Chhatrapal; Ajazuddin; Alexander, Amit; Badwaik, Hemant; Tripathi, Dulal Krishna

2012-01-01

Several methods and techniques are potentially useful for the preparation of microparticles in the field of controlled drug delivery. The type and the size of the microparticles, the entrapment, release characteristics and stability of drug in microparticles in the formulations are dependent on the method used. One of the most common methods of preparing microparticles is the single emulsion technique. Poorly soluble, lipophilic drugs are successfully retained within the microparticles prepared by this method. However, the encapsulation of highly water soluble compounds including protein and peptides presents formidable challenges to the researchers. The successful encapsulation of such compounds requires high drug loading in the microparticles, prevention of protein and peptide degradation by the encapsulation method involved and predictable release, both rate and extent, of the drug compound from the microparticles. The above mentioned problems can be overcome by using the double emulsion technique, alternatively called as multiple emulsion technique. Aiming to achieve this various techniques have been examined to prepare stable formulations utilizing w/o/w, s/o/w, w/o/o, and s/o/o type double emulsion methods. This article reviews the current state of the art in double emulsion based technologies for the preparation of microparticles including the investigation of various classes of substances that are pharmaceutically and biopharmaceutically active. PMID:23960828

Synthesis, characterization, and morphology study of poly(acrylamide-co-acrylic acid)-grafted-poly(styrene-co-methyl methacrylate) "raspberry"-shape like structure microgels by pre-emulsified semi-batch emulsion polymerization.

PubMed

Ramli, Ros Azlinawati; Hashim, Shahrir; Laftah, Waham Ashaier

2013-02-01

A novel microgels were polymerized using styrene (St), methyl methacrylate (MMA), acrylamide (AAm), and acrylic acid (AAc) monomers in the presence of N,N'-methylenebisacrylamide (MBA) cross-linker. Pre-emulsified monomer was first prepared followed by polymerizing monomers using semi-batch emulsion polymerization. Fourier Transform Infrared Spectroscopy (FTIR) and (1)H Nuclear Magnetic Resonance (NMR) were used to determine the chemical structure and to indentify the related functional group. Grafting and cross-linking of poly(acrylamide-co-acrilic acid)-grafted-poly(styrene-co-methyl methacrylate) [poly(AAm-co-AAc)-g-poly(St-co-MMA)] microgels are approved by the disappearance of band at 1300 cm(-1), 1200 cm(-1) and 1163 cm(-1) of FTIR spectrum and the appearance of CH peaks at 5.5-5.7 ppm in (1)H NMR spectrum. Scanning Electron Microscope (SEM) images indicated that poly(St-co-MMA) particle was lobed morphology coated by cross-linked poly(AAm-co-AAc) shell. Furthermore, SEM results revealed that poly(AAm-co-AAc)-g-poly(St-co-MMA) is composite particle that consist of "raspberry"-shape like structure core. Internal structures of the microgels showed homogeneous network of pores, an extensive interconnection among pores, thicker pore walls, and open network structures. Water absorbency test indicated that the sample with particle size 0.43 μm had lower equilibrium water content, % than the sample with particle size 7.39 μm. Copyright © 2012 Elsevier Inc. All rights reserved.

Water-in-oil Pickering emulsions stabilized by stearoylated microcrystalline cellulose.

PubMed

Pang, Bo; Liu, Huan; Liu, Peiwen; Peng, Xinwen; Zhang, Kai

2018-03-01

Hydrophobic particles with static water contact angles larger than 90° are more like to stabilize W/O Pickering emulsions. In particular, high internal phase Pickering emulsions (HIPEs) are of great interest for diverse applications. However, W/O HIPEs have rarely been realized using sustainable biopolymers. Herein, we used stearoylated microcrystalline cellulose (SMCC) to stabilize W/O Pickering emulsions and especially, W/O HIPEs. Moreover, these W/O HIPEs can be further used as platforms for the preparation of porous materials, such as porous foams. Stearoylated microcrystalline cellulose (SMCC) was prepared by modifying MCC with stearoyl chloride under heterogeneous conditions. Using SMCC as emulsifiers, W/O medium and high internal phase Pickering emulsions (MIPEs and HIPEs) with various organic solvents as continuous phases were prepared using one-step and two-step methods, respectively. Polystyrene (PS) foams were prepared after polymerization of oil phase using HIPEs as templates and their oil/water separation capacity were studied. SMCC could efficiently stabilize W/O Pickering emulsions and HIPEs could only be prepared via the two-step method. The internal phase volume fraction of the SMCC-stabilized HIPEs reached as high as 89%. Diverse internal phase volume fractions led to distinct inner structures of foams with closed or open cells. These macroporous polystyrene (PS) foams demonstrated great potential for the effective absorption of organic solvents from underwater. Copyright © 2017 Elsevier Inc. All rights reserved.

A Study of Functional Polymer Colloids Prepared Using Thiol-Ene/Yne Click Chemistry

NASA Astrophysics Data System (ADS)

Durham, Olivia Z.

This project demonstrates the first instance of thiol-ene chemistry as the polymerization method for the production of polymer colloids in two-phase heterogeneous suspensions, miniemulsions, and emulsions. This work was also expanded to thiol-yne chemistry for the production of polymer particles containing increased crosslinking density. The utility of thiol-ene and thiol-yne chemistries for polymerization and polymer modification is well established in bulk systems. These reactions are considered 'click' reactions, which can be defined as processes that are both facile and simple, offering high yields with nearly 100% conversion, no side products, easy product separation, compatibility with a diverse variety of commercially available starting materials, and orthogonality with other chemistries. In addition, thiol-ene and thiol-yne chemistry follow a step-growth mechanism for the development of highly uniform polymer networks, where polymer growth is dependent on the coupling of functional groups. These step-growth polymerization systems are in stark contrast to the chain-growth mechanisms of acrylic and styrenic monomers that have dominated the field of conventional heterogeneous polymerizations. Preliminary studies evaluated the mechanism of particle production in suspension and miniemulsion systems. Monomer droplets were compared to the final polymer particles to confirm that particle growth occurred through the polymerization of monomer droplets. Additional parameters examined include homogenization energy (mechanical mixing), diluent species and concentration, and monomer content. These reactions were conducted using photoinitiation to yield particles in a matter of minutes with diameters in the size range of several microns to hundreds of microns in suspensions or submicron particles in miniemulsions. Improved control over the particle size and size distribution was examined through variation of reaction parameters. In addition, a method of seeded suspension polymerization was attempted. This project was further expanded through an extensive evaluation of stabilizers in thiol-ene suspension polymerizations. The scope of stabilizers used included synthetic surfactants (ionic and nonionic), natural gums, and colloidal silica (Pickering stabilization). Suspension polymerizations were further expanded to include thiol-yne chemistry for the evaluation of polymer composition and thermal properties. In addition, polymer particles with excess ene, yne, or thiol functionality were successfully developed to demonstrate the potential for further functionalization. The self-limiting behavior of thiol-ene/yne reactions allows for successful synthesis of functional polymer colloids using off-stoichiometric amounts of monomers. This capacity to control functionality is illustrated through the creation of fluorescent polymer particles using both an in situ thiol-ene polymerization reaction with a vinyl chromophore as well as through post-polymerization modification of thiol-ene and thiol-yne polymers with excess thiol functionality via thiol-isocyanate chemistry. To produce smaller polymer particles without the need for intense homogenization energy or high stabilizer concentrations, an emulsion polymerization system was implemented using a water soluble-thermal initiator. It was found that unlike thiol-ene suspensions, which are limited to crosslinked systems, thiol-ene emulsion polymerizations allowed for the production of polymer particles comprised of either crosslinked or linear polymer networks. For the crosslinked systems, various anionic SDS surfactant concentrations were examined to observe the influence on particle size. In linear polymer systems, variations in polymer composition were examined. Preliminary studies performed with a monomer with an ethylene glycol-like structure indicated that the synthesis of polymer particles with narrower size distributions compared to any of the other emulsion compositions was possible. Finally, thiol-ene chemistry was also employed toward the synthesis of degradable polyanhydride polymer particles. Unlike the aforementioned studies, the approach to particle synthesis was conducted by using a premade thiol-ene polymer. Various linear thiol-ene polyanhydrides were emulsified in water or buffered solutions via sonication. Polymer latex was obtained upon solvent evaporation of the dichloromethane (DCM) solvent used to solubilize the polymer. In this work, variation of polymer composition as well as degradation was examined. Additional experiments included a study of the release of Rhodamine B dye, functionalization of the linear polymers, and studies involving the delay of degradation through the incorporation of crosslinking in the polymer particles. The projects presented herein provide an innovative approach to the synthesis of polymer colloids using thiol-ene and thiol-yne 'click' chemistry in both heterogeneous polymerizations as well as through solvent evaporation of premade polymer solutions. Polymer colloids prove to be an area of great interest for numerous applications that encompass various areas involving biomedical and industrial technologies including paints and coatings, cosmetics, diagnostics, and drug delivery. Improvements in methods of chemical synthesis as well as advances in the tailoring of material properties are of utmost importance for the ever increasing demands of new technologies and educational enlightenment.

Fabrication and Properties of polyacrylic acid by ionic surfactant disturbance method

NASA Astrophysics Data System (ADS)

Lawan, S.; Osotchan, T.; Chuajiw, W.; Subannajui, K.

2017-09-01

The formation of polymeric materials can be achieved by several methods such as melting and casting, screw extrusion, cross-linking of resin or rubber in a mold, and so on. In this work, the polyacrylic acid is formed by using the emulsion disturbance method. Despite extensively used in the colour painting and coating industries, acrylic emulsion can be processed into a foam and powder configuration by a reaction between acrylic emulsion and salt. The solidification hardly changes the volume between liquid emulsion and solidified polymer which means the final structure of polyacrylic acid is filled with opened air cells. The opened air cell structure is confirmed by the result from scanning electron microscopy. The chemical analysis and crystallography of acrylic powder and foam are examined by Fourier-transform infrared spectroscopy and X-ray diffraction respectively. The phase transformation and Thermal stability are studied by differential scanning calorimetry and thermo gravimetric analysis. Moreover, the mechanical properties of acrylic foam were observed by tensile, compressive and hardness test. In addition to the basic property analysis, acrylic foam was also used in the particle filtration application.

Polymerization model for hydrogen peroxide initiated synthesis of polypyrrole nanoparticles.

PubMed

Leonavicius, Karolis; Ramanaviciene, Almira; Ramanavicius, Arunas

2011-09-06

A very simple, environmentally friendly, one-step oxidative polymerization route to fabricate polypyrrole (Ppy) nanoparticles of fixed size and morphology was developed and investigated. The herein proposed method is based on the application of sodium dodecyl sulfate and hydrogen peroxide, both easily degradable and cheap materials. The polymerization reaction is performed on 24 h time scale under standard conditions. We monitored a polaronic peak at 465 nm and estimated nanoparticle concentration during various stages of the reaction. Using this data we proposed a mechanism for Ppy nanoparticle formation in accordance with earlier emulsion polymerization mechanisms. Rates of various steps in the polymerization mechanism were accounted for and the resulting particles identified using atomic force microscopy. Application of Ppy nanoparticles prepared by the route presented here seems very promising for biomedical applications where biocompatibility is paramount. In addition, this kind of synthesis could be suitable for the development of solar cells, where very pure and low-cost conducting polymers are required. © 2011 American Chemical Society

Surface Enrichment by Conventional and Polymerizable Sulfated Nonylphenol Ethoxylate Emulsifiers in Water-Based Pressure-Sensitive Adhesive

Treesearch

Jilin Zhang; Yuxi Zhao; Matthew R. Dubay; Steven J. Severtson; Larry E. Gwin; Carl J. Houtman

2013-01-01

Comparisons of properties are made for pressure-sensitive adhesives (PSAs) generated via emulsion polymerization using both conventional and reactive emulsifiers. The emulsifiers are ammonium salts of sulfated nonylphenol ethoxylates with similar chemical structures and hydrophilic−lipophilic balances. The polymerizable surfactant possesses a reactive double...

Hg(II) adsorption using amidoximated porous acrylonitrile/itaconic copolymers prepared by suspended emulsion polymerization.

PubMed

Ji, Chunnuan; Qu, Rongjun; Chen, Hou; Liu, Xiguang; Sun, Changmei; Ma, Caixia

2016-01-01

Initially, porous acrylonitrile/itaconic acid copolymers (AN/IA) were prepared by suspended emulsion polymerization. Successively, the cyano groups in AN/IA copolymers were converted to amidoxime (AO) groups by the reaction with hydroxylamine hydrochloride. The structures of the AN/IA and amidoximated AN/IA (AO AN/IA) were characterized by infrared spectroscopy, scanning electron microscopy, and porous structural analysis. The adsorption properties of AO AN/IA for Hg(II) were investigated. The results show that AO AN/IA has mesopores and macropores, and surface area of 11.71 m(2) g(-1). It was found that AO AN/IA has higher affinity for Hg(II), with the maximum adsorption capacity of 84.25 mg g(-1). The AO AN/IA also can effectively remove Hg(II) from different binary metal ion mixture systems. Furthermore, the adsorption kinetics and thermodynamics were studied in detail. The adsorption equilibrium can quickly be achieved in 4 h determined by an adsorption kinetics study. The adsorption process is found to belong to the second-order model, and can be described by the Freundlich model.

Super-enhanced particle nucleation in styrene emulsion polymerization in the presence of sodium styrene sulfonate.

PubMed

Farias-Cepeda, Lorena; Herrera-Ordonez, Jorge; Hernandez-Martinez, Angel R; Estevez, Miriam; Rosales-Marines, Lucero

2017-08-15

The styrene (St) emulsion polymerization using Aerosol MA80 as surfactant and in the presence of sodium styrene sulfonate (NaSS) was studied. The effect of NaSS content was assessed using MA80 concentrations below and at the critical micellar concentration. It was found that at the higher NaSS and MA80 contents, the number of particles (N) reaches a maximum of the order of 10 17 particles/cm 3 water, a huge value that has never been reported. In this work an explanation for this super-enhanced particle nucleation phenomenon is proposed. Such hypothesis is based on the role of St-NaSS oligomers formed in the aqueous phase and their synergy with MA80 molecules to provide colloidal stability to the system. The proposal seems to be consistent with the experimental data obtained for the evolution of monomer conversion, N, particles size distribution and the wideness of this latter as well as with a theoretical estimation of the N. Copyright © 2017 Elsevier Inc. All rights reserved.

Facile and low energy consumption synthesis of microencapsulated phase change materials with hybrid shell for thermal energy storage

NASA Astrophysics Data System (ADS)

Wang, Hao; Zhao, Liang; Chen, Lijie; Song, Guolin; Tang, Guoyi

2017-12-01

We designed a photocurable pickering emulsion polymerization to create microencapsulated phase change materials (MicroPCM) with polymer-silica hybrid shell. The emulsion was stabilized by modified SiO2 particles without any surfactant or dispersant. The polymerization process can be carried out at ambient temperature only for 5 min ultraviolet radiation, which is a low-energy procedure. The resultant capsules were shown a good core-shell structure and uniform in size. The surface of the microcapsules was covered by SiO2 particles. According to the DSC and TGA examinations, the microcapsules has good thermal energy storage-release performance, enhanced thermal reliability and thermal stability. When ratio of MMA/n-octadecane was 1.5/1.5. The encapsulation efficiency of the microcapsules reached 62.55%, accompanied with 122.31 J/g melting enthalpy. The work is virtually applicable to the construction of a wide variety of organic-inorganic hybrid shell MicroPCM. Furthermore, with the application of this method, exciting opportunities may arise for realizing rapid, continuous and large-scale industrial preparation of MicroPCM.

Structure-activity relationships of polyphenols to prevent lipid oxidation in pelagic fish muscle.

PubMed

Pazos, Manuel; Iglesias, Jacobo; Maestre, Rodrigo; Medina, Isabel

2010-10-27

The influence of polymerization (number of monomers) and galloylation (content of esterified gallates) of oligomeric catechins (proanthocyanidins) on their effectiveness to prevent lipid oxidation in pelagic fish muscle was evaluated. Non-galloylated oligomers of catechin with diverse mean polymerization (1.9-3.4 monomeric units) were extracted from pine (Pinus pinaster) bark. Homologous fractions with galloylation ranging from 0.25 to <1 gallate group per molecule were obtained from grape (Vitis vinifera) and witch hazel (Hamamelis virginiana). The results showed the convenience of proanthocyanidins with medium size (2-3 monomeric units) and low galloylation degree (0.15-0.25 gallate group/molecule) to inhibit lipid oxidation in pelagic fish muscle. These optimal structural characteristics of proanthocyanidins were similar to those lately reported in fish oil-in-water emulsions using phosphatidylcholine as emulsifier. This finding suggests that the antioxidant behavior of polyphenols in muscle-based foods can be mimicked in emulsions prepared with phospholipids as emulsifier agents. The present data give relevant information to achieve an optimum use of polyphenols in pelagic fish muscle.

Monodispersepoly[BMA-co-(COPS-I)] Particles by Soap-Free Emulsion Copolymerization and Its Optical Properties as Photonic Crystals.

PubMed

Lee, Ki Chang; Choo, Hun Seung

2015-10-01

In order to study the surfactant-free emulsion copolymerization of benzyl methacrylate (BMA) with sodium 1-allyloxy-2-hydroxypropane sulfonate (COPS-I) and the resulting optical properties, a series of experiments was carried out at various reaction conditions such as the changes of BMA concentration, COPS-I concentration, BMA concentration under a fixed COPS-I amount, initiator and divinyl benzene (DVB) concentration. All the latices showed highly monodispersed spherical particles in the size range of 144~435 nm and the respective shiny structural colors from their colloidal photonic crystals. It is found that the changes in such polymerization factors greatly affect the number of particles and particle diameter, polymerization rate, molecular weight, zeta-potential, and refractive indices. The increase of number of particles led to the increased rate of polymerization and zeta-potential of the latices, on the other hand, to the decreased molecular weight. Refractive indices and the reflectivity increased with COPS-I concentration, on the other hand, and decreased with DVB concentration. Especially, refractive indices of the resulting poly[BMA-co-(COPS-I)] colloidal photonic crystals showed much higher values of 1.65~2.21 than that of polystyrene, due to the formation of core-shell shaped morphology. Monodisperse and high refractive index of poly[BMA-co-(COPS-I)] particles prepared in this work could be used for the study in photonic crystals and electrophoretic display.

Invert emulsion: Method of preparation and application as proper formulation of entomopathogenic fungi.

PubMed

Batta, Yacoub A

2016-01-01

The present article describes the technique used for preparing the invert emulsion (water-in-oil type) then, selecting the most proper formulation of invert emulsion for being used as a carrier formulation of entomopathogenic fungi. It also describes the method used for testing the efficacy of the formulated fungi as biocontrol agents of targeted insects. Detailed examples demonstrating the efficacy of formulated strains of entomopathogenic fungi against certain species of insect pests were included in the present article. The techniques and methods described in this article are reproducible and helpful in enhancing the effectiveness of formulated fungi against wide range of targeted insects in comparison with the unformulated form of these fungi. Also, these techniques and methods can be used effectively in crop protection and in the integrated pest management programs. Finally, it is important to indicate that the ingredients used for preparation of the invert emulsion have no environmental side-effects or health risks since these ingredients are safe to use and can be used in manufacturing of cosmetics or as food additives.•Description of method used for preparation of invert emulsion (water-in-oil type) and selecting the most stable and non-viscous emulsion.•Description of technique used for introducing the entomopathogenic fungi into the selected stable and non-viscous invert emulsion.•Description of method for testing the efficacy of introduced entomopathogenic fungus into the selected invert emulsion against targeted insects with detailed examples on the efficacy testing.

Impact of Lipid and Protein Co-oxidation on Digestibility of Dairy Proteins in Oil-in-Water (O/W) Emulsions.

PubMed

Obando, Mónica; Papastergiadis, Antonios; Li, Shanshan; De Meulenaer, Bruno

2015-11-11

Enrichment of polyunsaturated fatty acids (PUFAs) is a growing trend in the food industry. However, PUFAs are known to be susceptible to lipid oxidation. It has been shown that oxidizing lipids react with proteins present in the food and that as a result polymeric protein complexes are produced. Therefore, the aim of this work was to investigate the impact of lipid and protein co-oxidation on protein digestibility. Casein and whey protein (6 mg/mL) based emulsions with 1% oil with different levels of PUFAs were subjected to respectively autoxidation and photo-oxidation. Upon autoxidation at 70 °C, protein digestibility of whey protein based emulsions containing fish oil decreased to 47.7 ± 0.8% after 48 h, whereas in the controls without oil 67.8 ± 0.7% was observed. Upon photo-oxidation at 4 °C during 30 days, mainly casein-based emulsions containing fish oil were affected: the digestibility amounted to 43.9 ± 1.2%, whereas in the control casein solutions without oil, 72.6 ± 0.2% of the proteins were digestible. Emulsions containing oils with high PUFA levels were more prone to lipid oxidation and thus upon progressive oxidation showed a higher impact on protein digestibility.

Acetalated Dextran Microparticulate Vaccine Formulated via Coaxial Electrospray Preserves Toxin Neutralization and Enhances Murine Survival Following Inhalational Bacillus Anthracis Exposure.

PubMed

Gallovic, Matthew D; Schully, Kevin L; Bell, Matthew G; Elberson, Margaret A; Palmer, John R; Darko, Christian A; Bachelder, Eric M; Wyslouzil, Barbara E; Keane-Myers, Andrea M; Ainslie, Kristy M

2016-10-01

Subunit formulations are regarded as the safest type of vaccine, but they often contain a protein-based antigen that can result in significant challenges, such as preserving antigenicity during formulation and administration. Many studies have demonstrated that encapsulation of protein antigens in polymeric microparticles (MPs) via emulsion techniques results in total IgG antibody titers comparable to alum formulations, however, the antibodies themselves are non-neutralizing. To address this issue, a coaxial electrohydrodynamic spraying (electrospray) technique is used to formulate a microparticulate-based subunit anthrax vaccine under conditions that minimize recombinant protective antigen (rPA) exposure to harsh solvents and high shear stress. rPA and the adjuvant resiquimod are encapsulated either in separate or the same acetalated dextran MPs. Using a murine model, the electrospray formulations lead to higher IgG2a subtype titers as well as comparable total IgG antibody titers and toxin neutralization relative to the FDA-approved vaccine (BioThrax). BioThrax provides no protection against a lethal inhalational challenge of the highly virulent Ames Bacillus anthracis anthrax strain, whereas 50% of the mice vaccinated with separately encapsulated electrospray MPs survive. Overall, this study demonstrates the potential use of electrospray for encapsulating protein antigens in polymeric MPs. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Thick phase holographic gratings recorded on BB-640 and PFG-01 silver halide materials

NASA Astrophysics Data System (ADS)

Neipp, Cristian; Márquez, Andrés; Pascual, Inmaculada; Beléndez, Augusto

2003-09-01

Photographic emulsions are still widely used to record holographic optical elements. In particular, if high diffraction efficiencies are needed, phase volume holograms are preferably recorded on these emulsions. Two particular techniques producing high-quality volume phase holograms are fixation-free rehalogenating bleaching and the use of silver-halide-sensitized gelatin. In this work we compare these two particular techniques applied to three different red-sensitive emulsions: Agfa 8E75 HD, BB-640, and Slavich PFG-01 emulsions. The differences between these emulsions determine the particular experimental conditions needed to record high-quality volume holograms on them. In this work these differences are analysed, and also their influence on the experimental procedure.

Hybrid self-healing matrix using core-shell nanofibers and capsuleless microdroplets.

PubMed

Lee, Min Wook; An, Seongpil; Lee, Changmin; Liou, Minho; Yarin, Alexander L; Yoon, Sam S

2014-07-09

In this work, we developed novel self-healing anticorrosive hierarchical coatings that consist of several components. Namely, as a skeleton we prepared a core-shell nanofiber mat electrospun from emulsions of cure material (dimethyl methylhydrogen siloxane) in a poly(acrylonitrile) (PAN) solution in dimethylformamide. In these nanofibers, cure is in the core, while PAN is in the shell. The skeleton deposited on a protected surface is encased in an epoxy-based matrix, which contains emulsified liquid droplets of dimethylvinyl-terminated dimethylsiloxane resin monomer. When such hierarchical coatings are damaged, cure is released from the nanofiber cores and the resin monomer, released from the damaged matrix, is polymerized in the presence of cure. This polymerization and solidification process takes about 1-2 days and eventually heals the damaged material when solid poly(dimethylsiloxane) resin is formed. The self-healing effect was demonstrated using an electrochemical analogue of the scanning vibrating electrode technique. Damaged samples were left for 2 days. After that, the electric current through a damaged coating was found to be negligibly small for the samples with self-healing properties. On the other hand, for the samples without self-healing properties, the electric current was significant.

Formation of 2D and 3D superlattices of silver nanoparticles inside an emulsion droplet

NASA Astrophysics Data System (ADS)

Hussain Shaik, Aabid; Srinivasa Reddy, D.

2017-03-01

This work is aimed at the formation of 2D and 3D superlattices (SL) of silver nanoparticles inside an emulsion droplet. The monodisperse nanoparticles required for SL formation were prepared by a digestive ripening technique. Digestive ripening is a post processing technique where polydisperse colloids are refluxed with excess surface-active ligands to prepare a monodisperse colloid. More uniform silver nanoparticles (~3.6  ±  0.5 nm) were formed by slow evaporation of organosols on a carbon-coated copper grid. The best 3D silver superlattices have been formed using an oil in water (o/w) emulsion method by aging the monodisperse particles in a confined environment like o/w emulsion at different temperatures ranging from 5 °C-4 °C. The kinetics of the formation of superlattices inside an emulsion droplet were investigated by controlling various parameters. The kinetics were found to be dependent on the emulsion aging period (30 d) and storage temperature of the emulsion (-4 °C).

Controlled assembly of nanoparticle structures: spherical and toroidal superlattices and nanoparticle-coated polymeric beads.

PubMed

Isojima, Tatsushi; Suh, Su Kyung; Vander Sande, John B; Hatton, T Alan

2009-07-21

The emulsion droplet solvent evaporation method has been used to prepare nanoclusters of monodisperse magnetite nanoparticles of varying morphologies depending on the temperature and rate of solvent evaporation and on the composition (solvent, presence of polymer, nanoparticle concentration, etc.) of the emulsion droplets. In the absence of a polymer, and with increasing solvent evaporation temperatures, the nanoparticles formed single- or multidomain crystalline superlattices, amorphous spherical aggregates, or toroidal clusters, as determined by the energetics and dynamics of the solvent evaporation process. When polymers that are incompatible with the nanoparticle coatings were included in the emulsion formulation, monolayer- and multilayer-coated polymer beads and partially coated Janus beads were prepared; the nanoparticles were expelled by the polymer as its concentration increased on evaporation of the solvent and accumulated on the surfaces of the beads in a well-ordered structure. The precise number of nanoparticle layers depended on the polymer/magnetic nanoparticle ratio in the oil droplet phase parent emulsion. The magnetic nanoparticle superstructures responded to the application of a modest magnetic field by forming regular chains with alignment of nonuniform structures (e.g., toroids and Janus beads) that are in accord with theoretical predictions and with observations in other systems.

Molecularly Imprinted Polymers: Novel Discovery for Drug Delivery.

PubMed

Dhanashree, Surve; Priyanka, Mohite; Manisha, Karpe; Vilasrao, Kadam

2016-01-01

Molecularly imprinted polymers (MIP) are novel carriers synthesized by imprinting of a template over a polymer. This paper presents the recent application of MIP for diagnostic and therapeutic drug delivery. MIP owing to their 3D polymeric structures and due to bond formation with the template serves as a reservoir of active causing stimuli sensitive, enantioselective, targetted and/or controlled release. The review elaborates about key factors for optimization of MIP, controlled release by MIP for various administration routes various forms like patches, contact lenses, nanowires along with illustrations. To overcome the limitation of organic solvent usage causing increased cost, water compatible MIP and use of supercritical fluid technology for molecular imprinting were developed. Novel methods for developing water compatible MIP like pickering emulsion polymerization, co-precipitation method, cyclodextrin imprinting, surface grafting, controlled/living radical chain polymerization methods are described with illustration in this review. Various protein imprinting methods like bulk, epitope and surface imprinting are described along with illustrations. Further, application of MIP in microdevices as biomimetic sensing element for personalized therapy is elaborated. Although development and application of MIP in drug delivery is still at its infancy, constant efforts of researchers will lead to a novel intelligent drug delivery with commercial value. Efforts should be directed in developing solid oral dosage forms consisting of MIP for therapeutic protein and peptide delivery and targeted release of potent drugs addressing life threatening disease like cancer. Amalgamation of bio-engineering and pharmaceutical techniques can make these future prospects into reality.

Naltrexone-loaded poly[La-(Glc-Leu)] polymeric microspheres for the treatment of alcohol dependence: in vitro characterization and in vivo biocompatibility assessment.

PubMed

Pagar, Kunal P; Vavia, Pradeep R

2014-06-01

The poly[La-(Glc-Leu)] copolymer was applied in the present investigation as polymeric carrier to fabricate naltrexone (NTX)-loaded poly[La-(Glc-Leu)] microspheres in the single emulsion solvent evaporation technique for the long-term treatment of alcohol dependence. Newly synthesized poly[La-(Glc-Leu)] copolymer exhibited diminished crystallanity, good biocompatibility and favorable biodegradability to be explored for drug delivery application. Scanning Electron Microscopy study revealed smooth and spherical-shaped NTX-loaded polymeric microspheres with a mean size of 10-90 µm. Influence of various decisive formulation variables such as amount of polymer, stabilizer concentration, homogenization speed, homogenization time, drug loading and organic-to-aqueous phase ratio on particle size, and entrapment efficiency was studied. Differential scanning calorimeter and X-ray diffractometry study confirmed the drug entrapment within polymer matrix into the microsphere environment. In vitro drug release showed the sustained drug release of formulation for the period of 28 d giving biphasic release pattern. Histological examination of NTX-loaded poly[La-(Glc-Leu)] microspheres injected intramuscularly into the thigh muscle of Wistar rats showed minimal inflammatory reaction, demonstrating that NTX-loaded microspheres were biocompatible. Insignificant increase in the serum creatine phosphokinase level (p < 0.05) as compared with the normal value revealed good muscle compatibility of the poly[La-(Glc-Leu)] microsphere system. Biocompatible nature and sustained drug-release action of poly[La-(Glc-Leu)] microspheres may have potential application in depot therapy.

Preparation of small bio-compatible microspheres

NASA Technical Reports Server (NTRS)

Rembaum, Alan (Inventor); Yen, Shiao-Ping S. (Inventor); Dreyer, William J. (Inventor)

1979-01-01

Small, round, bio-compatible microspheres capable of covalently bonding proteins and having a uniform diameter below about 3500 A are prepared by substantially instantaneously initiating polymerization of an aqueous emulsion containing no more than 35% total monomer including an acrylic monomer substituted with a covalently bondable group such a hydroxyl, amino or carboxyl and a minor amount of a cross-linking agent.

Preparation of silica-coated poly(styrene-co-4-vinylpyridine) particles and hollow particles.

PubMed

Zou, Hua; Wu, Shishan; Shen, Jian

2008-09-16

This paper presents a novel method for preparation of polymer-silica colloidal nanocomposites based on emulsion polymerization and subsequent sol-gel nanocoating process. The polystyrene latex particles bearing basic groups on their surfaces were successfully synthesized through emulsion polymerization using 4-vinylpyridine (4VP) as a functional comonomer and polyvinylpyrrolidone (PVP) as a surfactant. A series of poly(styrene-co-4-vinylpyridine)/SiO2 nanocomposite particles with smooth or rough core-shell morphology were obtained through the coating process. The poly(styrene-co-4-vinylpyridine) particles could be dissolved subsequently or simultaneously during the sol-gel coating process to form hollow particles. The effects of the amount of 4VP, PVP, NH(4)OH, and tetraethoxysilane (TEOS) on both the nanocomposite particles and hollow particles were investigated. Transmission electron microscopy showed that the morphology of the nanocomposite particles and hollow particles was strongly influenced by the initial feed of the comonomer 4VP and the coupling agent PVP. The conditions to obtain all hollow particles were also studied. Thermogravimetric analysis and energy dispersive X-ray spectroscopy analyses indicated that the interiors of hollow particles were not really "hollow".

Ultrasound assisted synthesis of PANI/ZnMoO4 nanocomposite for simultaneous improvement in anticorrosion, physico-chemical properties and its application in gas sensing.

PubMed

Bhanvase, B A; Darda, N S; Veerkar, N C; Shende, A S; Satpute, S R; Sonawane, S H

2015-05-01

Ultrasound assisted in-situ semi-batch emulsion polymerization has been used for the preparation of polyaniline (PANI) and PANI/ZnMoO4 nanocomposite with different loading of ZnMoO4 (ZM) nanoparticles. ZM nanoparticles were functionalized using Myristic acid (MA) for better compatibility with PANI. The cavitational effects induced due to ultrasonic irradiations have been shown significant enhancement in the dispersion of functionalized ZM nanoparticles into the PANI during ultrasound assisted in-situ emulsion polymerization process. TEM images of PANI/ZM nanocomposite particles give the direct evidence of fine dispersion and encapsulation of MA treated ZM nanoparticles in PANI matrix. The presence of ZM nanoparticles in PANI/ZM nanocomposite shows significant improvement in the mechanical (cross-cut adhesion), thermal, anticorrosion and sensing properties of PANI/ZM nanocomposite/alkyd coatings over PANI/alkyd and neat alkyd resin coating. Fine and uniform dispersion of ZM nanoparticles in PANI matrix using this novel synthesis method (PANI (p-type)/ZM (n-type) hetero-junction) improves LPG sensing ability and minimizes response time to sense LPG significantly compared with neat PANI. Copyright © 2014 Elsevier B.V. All rights reserved.

Interconnected Porous Polymers with Tunable Pore Throat Size Prepared via Pickering High Internal Phase Emulsions.

PubMed

Xu, Hongyun; Zheng, Xianhua; Huang, Yifei; Wang, Haitao; Du, Qiangguo

2016-01-12

Interconnected macroporous polymers were prepared by copolymerizing methyl acrylate (MA) via Pickering high internal phase emulsion (HIPE) templates with modified silica particles. The pore structure of the obtained polymer foams was observed by field-emission scanning electron microscopy (FE-SEM). Gas permeability was characterized to evaluate the interconnectivity of macroporous polymers. The polymerization shrinkage of continuous phase tends to form open pores while the solid particles surrounding the droplets act as barriers to produce closed pores. These two conflicting factors are crucial in determining the interconnectivity of macroporous polymers. Thus, poly-Pickering HIPEs with high permeability and well-defined pore structure can be achieved by tuning the MA content, the internal phase fraction, and the content of modified silica particles.

Closed-Loop Multitarget Optimization for Discovery of New Emulsion Polymerization Recipes

PubMed Central

2015-01-01

Self-optimization of chemical reactions enables faster optimization of reaction conditions or discovery of molecules with required target properties. The technology of self-optimization has been expanded to discovery of new process recipes for manufacture of complex functional products. A new machine-learning algorithm, specifically designed for multiobjective target optimization with an explicit aim to minimize the number of “expensive” experiments, guides the discovery process. This “black-box” approach assumes no a priori knowledge of chemical system and hence particularly suited to rapid development of processes to manufacture specialist low-volume, high-value products. The approach was demonstrated in discovery of process recipes for a semibatch emulsion copolymerization, targeting a specific particle size and full conversion. PMID:26435638

A microscopy method for scanning transmission electron microscopy imaging of the antibacterial activity of polymeric nanoparticles on a biofilm with an ionic liquid.

PubMed

Takahashi, Chisato; Muto, Shunsuke; Yamamoto, Hiromitsu

2017-08-01

In this study, we developed a scanning transmission electron microscopy (STEM) method for imaging the antibacterial activity of organic polymeric nanoparticles (NPs) toward biofilms formed by Staphylococcus epidermidis bacterial cells, for optimizing NPs to treat biofilm infections. The combination of sample preparation method using a hydrophilic ionic liquid (IL) and STEM observation using the cooling holder eliminates the need for specialized equipment and techniques for biological sample preparation. The annular dark-field STEM results indicated that the two types of biodegradable poly-(DL-lactide-co-glycolide) (PLGA) NPs: PLGA modified with chitosan (CS), and clarithromycin (CAM)-loaded + CS-modified PLGA, prepared by emulsion solvent diffusion exhibited different antibacterial activities in nanoscale. To confirm damage to the sample during STEM observation, we observed the PLGA NPs and the biofilm treated with PLGA NPs by both the conventional method and the newly developed method. The optimized method allows microstructure of the biofilm treated with PLGA NPs to be maintained for 25 min at a current flow of 40 pA. The developed simple sample preparation method would be helpful to understand the interaction of drugs with target materials. In addition, this technique could contribute to the visualization of other deformable composite materials at the nanoscale level. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 105B: 1432-1437, 2017. © 2016 Wiley Periodicals, Inc.

Development of a water purifier for radioactive cesium removal from contaminated natural water by radiation-induced graft polymerization

NASA Astrophysics Data System (ADS)

Seko, Noriaki; Hoshina, Hiroyuki; Kasai, Noboru; Shibata, Takuya; Saiki, Seiichi; Ueki, Yuji

2018-02-01

Six years after the Fukushima-nuclear accident, the dissolved radioactive cesium (Cs) is now hardly detected in environmental natural waters. These natural waters are directly used as source of drinking and domestic waters in disaster-stricken areas in Fukushima. However, the possibility that some radioactive Cs adsorbed on soil or leaves will contaminate these natural waters during heavy rains or typhoon is always present. In order for the returning residents to live with peace of mind, it is important to demonstrate the safety of the domestic waters that they will use for their daily life. For this purpose, we have synthesized a material for selective removal of radioactive Cs by introducing ammonium 12-molybdophosphate (AMP) onto polyethylene nonwoven fabric through radiation-induced emulsion graft polymerization technique. Water purifiers filled with the grafted Cs adsorbent were installed in selected houses in Fukushima. The capability of the grafted adsorbent to remove Cs from domestic waters was evaluated for a whole year. The results showed that the tap water filtered through the developed water purifier contained no radioactive Cs, signifying the very effective adsorption performance of the developed grafted adsorbent. From several demonstrations, we have commercialized the water purifier named "KranCsair®". Furthermore, we have also developed a method for the mass production of the grafted nonwoven fabric. Using a 30 L grafting reactor, it was possible to produce the grafted nonwoven fabric with a suitable range of degree of grafting. When an irradiated roll of nonwoven trunk fabric with a length of 10 m and a width of 30 cm was set in the reactor filled with glycidyl methacrylate (GMA), AMP, Tween 80 monomer emulsion solution at 40 °C for 1 h, the difference of Dgs in the length and the width on roll of fabrics was negligible.

pH Sensitive Microcapsules for Delivery of Corrosion Inhibitors

NASA Technical Reports Server (NTRS)

Li, Wenyan; Calle, Luz M.

2006-01-01

A considerable number of corrosion problems can be solved by coatings. However, even the best protective coatings can fail by allowing the slow diffusion of oxygen and moisture to the metal surface. Corrosion accelerates when a coating delaminates. Often, the problems start when microscopic nicks or pits on the surface develop during manufacturing or through wear and tear. This problem can be solved by the incorporation of a self-healing function into the coating. Several new concepts are currently under development to incorporate this function into a coating. Conductive polymers, nanoparticles, and microcapsules are used to release corrosion-inhibiting ions at a defect site. The objective of this investigation is to develop a smart coating for the early detection and inhibition of corrosion. The dual function of this new smart coating system is performed by pH-triggered release microcapsules. The microcapsules can be used to deliver healing agents to terminate the corrosion process at its early stage or as corrosion indicators by releasing dyes at the localized corrosion sites. The dyes can be color dyes or fluorescent dyes, with or without pH sensitivity. Microcapsules were formed through the interfacial polymerization process. The average size of the microcapsules can be adjusted from 1 to 100 micron by adjusting the emulsion formula and the microcapsule forming conditions. A typical microcapsule size is around 10 microns with a narrow size distribution. The pH sensitivity of the microcapsule can also be controlled by adjusting the emulsion formula and the polymerization reaction time. Both corrosion indicator (pH indicator) and corrosion inhibitor containing microcapsules were formed and incorporated into paint systems. Test panels of selected steels and aluminum alloys were painted using these paints. Testing of compatibility between the microcapsule system and different paint systems are in progress. Initial experiments with the microcapsule containing paint show visible color changes at induced corrosion sites and improvement of corrosion protection. Further investigation of the performance of the coating using electrochemical techniques and long term exposure are currently underway.

Non-destructive monitoring of creaming of oil-in-water emulsion-based formulations using magnetic resonance imaging.

PubMed

Onuki, Yoshinori; Horita, Akihiro; Kuribayashi, Hideto; Okuno, Yoshihide; Obata, Yasuko; Takayama, Kozo

2014-07-01

A non-destructive method for monitoring creaming of emulsion-based formulations is in great demand because it allows us to understand fully their instability mechanisms. This study was aimed at demonstrating the usefulness of magnetic resonance (MR) techniques, including MR imaging (MRI) and MR spectroscopy (MRS), for evaluating the physicochemical stability of emulsion-based formulations. Emulsions that are applicable as the base of practical skin creams were used as test samples. Substantial creaming was developed by centrifugation, which was then monitored by MRI. The creaming oil droplet layer and aqueous phase were clearly distinguished by quantitative MRI by measuring T1 and the apparent diffusion coefficient. Components in a selected volume in the emulsions could be analyzed using MRS. Then, model emulsions having different hydrophilic-lipophilic balance (HLB) values were tested, and the optimal HLB value for a stable dispersion was determined. In addition, the MRI examination enables the detection of creaming occurring in a polyethylene tube, which is commonly used for commercial products, without losing any image quality. These findings strongly indicate that MR techniques are powerful tools to evaluate the physicochemical stability of emulsion-based formulations. This study will make a great contribution to the development and quality control of emulsion-based formulations.

An Investigation of a Photographic Technique of Measuring High Surface Temperatures

NASA Technical Reports Server (NTRS)

Siviter, James H., Jr.; Strass, H. Kurt

1960-01-01

A photographic method of temperature determination has been developed to measure elevated temperatures of surfaces. The technique presented herein minimizes calibration procedures and permits wide variation in emulsion developing techniques. The present work indicates that the lower limit of applicability is approximately 1,400 F when conventional cameras, emulsions, and moderate exposures are used. The upper limit is determined by the calibration technique and the accuracy required.

Superhydrophilic poly (styrene co acrylonitrile)-ZnO nanocomposite surfaces for UV shielding and self-cleaning applications

NASA Astrophysics Data System (ADS)

Singh, Rajender; Sharma, Ramesh; Barman, P. B.; Sharma, Dheeraj

2017-11-01

UV shielding based super hydrophilic material is developed in the present formulation by in situ emulsion polymerization of poly (styrene-acrylonitrile) with ZnO nanoparticles. The ESI-MS technique confirms the structure of polymer nanocomposite by their mass fragments. The XRD study confirms the presence of ZnO phase in polymer matrix. PSAN/ZnO nanocomposite leads to give effective UV shielding (upto 375 nm) and visible luminescence with ZnO content in polymer matrix. The FESEM and TEM studies confirm the symmetrical, controlled growth of PNs. The incorporation of ZnO nanofillers into PSAN matrix lead to restructuring the PNs surfaces into superhydrophilic surfaces in water contact angle (WCA) from 70° to 10°. We believe our synthesized PSAN/ZnO nanocomposite could be potential as UV shielding, luminescent and super hydrophilic nature based materials in related commercial applications.

Electrokinetic properties of PMAA functionalized NiFe2O4 nanoparticles synthesized by thermal plasma route

NASA Astrophysics Data System (ADS)

Bhosale, Shivaji V.; Mhaske, Pravin; Kanhe, N.; Navale, A. B.; Bhoraskar, S. V.; Mathe, V. L.; Bhatt, S. K.

2014-04-01

The magnetic nickel ferrite (NiFe2O4) nanoparticles with an average size of 30nm were synthesised by Transferred arc DC Thermal Plasma route. The synthesized nickel ferrite nanoparticles were characterized by TEM and FTIR techniques. The synthesized nickel ferrite nanoparticles were further functionalized with PMAA (polymethacrylic acid) by self emulsion polymerization method and subsequently were characterized by FTIR and Zeta Analyzer. The variation of zeta potential with pH was systematically studied for both PMAA functionalized (PNFO) and uncoated nickel ferrite nanoparticles (NFO). The IEP (isoelectric points) for PNFO and NFO was determined from the graph of zeta potential vs pH. It was observed that the IEP for NFO was at 7.20 and for PNFO it was 2.52. The decrease in IEP of PNFO was attributed to the COOH functional group of PMAA.

Synthesis and self-assembly of amphiphilic polymeric microparticles.

PubMed

Dendukuri, Dhananjay; Hatton, T Alan; Doyle, Patrick S

2007-04-10

We report the synthesis and self-assembly of amphiphilic, nonspherical, polymeric microparticles. Wedge-shaped particles bearing segregated hydrophilic and hydrophobic sections were synthesized in a microfludic channel by polymerizing across laminar coflowing streams of hydrophilic and hydrophobic polymers using continuous flow lithography (CFL). Particle monodispersity was characterized by measuring both the size of the particles formed and the extent of amphiphilicity. The coefficient of variation (COV) was found to be less than 2.5% in all measured dimensions. Particle structure was further characterized by measuring the curvature of the interface between the sections and the extent of cross-linking using FTIR spectroscopy. The amphiphilic particles were allowed to self-assemble in water or at water-oil interfaces. In water, the geometry of the particles enabled the formation of micelle-like structures, while in emulsions, the particles migrated to the oil-water interface and oriented themselves to minimize their surface energy.

Formation of random and regular relief-phase structures on silver halide photographic emulsions by holographic methods

NASA Astrophysics Data System (ADS)

Ganzherli, N. M.; Gulyaev, S. N.; Gurin, A. S.; Kramushchenko, D. D.; Maurer, I. A.; Chernykh, D. F.

2009-07-01

The formation of diffusers and microlens rasters on silver halide emulsions by holographic methods is considered. Two techniques for converting amplitude holographic recording to relief-phase recording, selective curing and irradiation of the emulsion gelatin by short-wavelength UV radiation, are compared.

Radiation induced graft copolymerization of methyl methacrylate onto chrome-tanned pig skins

NASA Astrophysics Data System (ADS)

Pietrucha, K.; Pȩkala, W.; Kroh, J.

Graft copolymerization of methyl methacrylate (MMA) onto chrome-tanned pig skins was carried out by the irradiation with 60Co ?-rays. The grafted polymethyl methacrylate (PMMA) chains were isolated by acid hydrolysis of the collagen backbone in order to characterize the graft copolymers. Proof of grafting was obtained through the detection of amino acid endgroups in the isolated grafts by reaction with ninhydrin. The grafting yield of MMA in aqueous emulsion was found to be higher than that for pure MMA and MMA in acetone. The degree of grafting increases with increasing monomer concentration in emulsion and reaches maximum at radiation dose ca 15 kGy. The yield of grafting is very high - ca 90% of monomer converts into copolymer and only 10% is converted into homopolymer. The present paper reports the physical properties of chrome-tanned pig skins after graft polymerization with MMA in emulsion. Modified leathers are more resistant against water absorption and abrasion in comparison with unmodified ones. They have more uniform structure over the whole surface, greater thickness and stiffness. The results reported seem to indicate that MMA may be used in the production of shoe upper and sole leathers. The mechanism of some of the processes occuring during radiation grafting of MMA in water emulsion on tanned leathers has been also suggested and discussed.

Direct technique for monitoring lipid oxidation in water-in-oil emulsions based on micro-calorimetry.

PubMed

Dridi, Wafa; Toutain, Jean; Sommier, Alain; Essafi, Wafa; Leal-Calderon, Fernando; Cansell, Maud

2017-09-01

An experimental device based on the measurement of the heat flux dissipated during chemical reactions, previously validated for monitoring lipid oxidation in plant oils, was extended to follow lipid oxidation in water-in-oil emulsions. Firstly, validation of the approach was performed by correlating conjugated diene concentrations measured by spectrophotometry and the heat flux dissipated by oxidation reactions and measured directly in water-in-oil emulsions, in isothermal conditions at 60°C. Secondly, several emulsions based on plant oils differing in their n-3 fatty acid content were compared. The oxidability parameter derived from the enthalpy curves reflected the α-linolenic acid proportion in the oils. On the whole, the micro-calorimetry technique provides a sensitive method to assess lipid oxidation in water-in-oil emulsions without requiring any phase extraction. Copyright © 2017 Elsevier Ltd. All rights reserved.

Molecularly imprinted polymer microspheres prepared by Pickering emulsion polymerization for selective solid-phase extraction of eight bisphenols from human urine samples.

PubMed

Yang, Jiajia; Li, Yun; Wang, Jincheng; Sun, Xiaoli; Cao, Rong; Sun, Hao; Huang, Chaonan; Chen, Jiping

2015-05-04

The bisphenol A (BPA) imprinted polymer microspheres were prepared by simple Pickering emulsion polymerization. Compared to traditional bulk polymerization, both high yields of polymer and good control of particle sizes were achieved. The characterization results of scanning electron microscopy and nitrogen adsorption-desorption measurements showed that the obtained molecularly imprinted polymer microsphere (MIPMS) particles possessed regular spherical shape, narrow diameter distribution (30-60 μm), a specific surface area (S(BET)) of 281.26 m(2) g(-1) and a total pore volume (V(t)) of 0.459 cm(3) g(-1). Good specific adsorption capacity for BPA was obtained in the sorption experiment and good class selectivity for BPA and its seven structural analogs (bisphenol F, bisphenol B, bisphenol E, bisphenol AF, bisphenol S, bisphenol AP and bisphenol Z) was demonstrated by the chromatographic evaluation experiment. The MIPMS as solid-phase extraction (SPE) packing material was then evaluated for extraction and clean-up of these bisphenols (BPs) from human urine samples. An accurate and sensitive analytical method based on the MIPMS-SPE coupled with HPLC-DAD has been successfully established for simultaneous determination of eight BPs from human urine samples with detection limits of 1.2-2.2 ng mL(-1). The recoveries of BPs for urine samples at two spiking levels (100 and 500 ng mL(-1) for each BP) were in the range of 81.3-106.7% with RSD values below 8.3%. Copyright © 2015 Elsevier B.V. All rights reserved.

Improved insulin loading in poly(lactic-co-glycolic) acid (PLGA) nanoparticles upon self-assembly with lipids.

PubMed

García-Díaz, María; Foged, Camilla; Nielsen, Hanne Mørck

2015-03-30

Polymeric nanoparticles are widely investigated as drug delivery systems for oral administration. However, the hydrophobic nature of many polymers hampers effective loading of the particles with hydrophilic macromolecules such as insulin. Thus, the aim of this work was to improve the loading of insulin into poly(lactic-co-glycolic) acid (PLGA) nanoparticles by pre-assembly with amphiphilic lipids. Insulin was complexed with soybean phosphatidylcholine or sodium caprate by self-assembly and subsequently loaded into PLGA nanoparticles by using the double emulsion-solvent evaporation technique. The nanoparticles were characterized in terms of size, zeta potential, insulin encapsulation efficiency and loading capacity. Upon pre-assembly with lipids, there was an increased distribution of insulin into the organic phase of the emulsion, eventually resulting in significantly enhanced encapsulation efficiencies (90% as compared to 24% in the absence of lipids). Importantly, the insulin loading capacity was increased up to 20% by using the lipid-insulin complexes. The results further showed that a main fraction of the lipid was incorporated into the nanoparticles and remained associated to the polymer during release studies in buffers, whereas insulin was released in a non-complexed form as a burst of approximately 80% of the loaded insulin. In conclusion, the protein load in PLGA nanoparticles can be significantly increased by employing self-assembled protein-lipid complexes. Copyright © 2014 Elsevier B.V. All rights reserved.

Polymeric nanoparticles containing diazepam: preparation, optimization, characterization, in-vitro drug release and release kinetic study

NASA Astrophysics Data System (ADS)

Bohrey, Sarvesh; Chourasiya, Vibha; Pandey, Archna

2016-03-01

Nanoparticles formulated from biodegradable polymers like poly(lactic-co-glycolic acid) (PLGA) are being extensively investigated as drug delivery systems due to their two important properties such as biocompatibility and controlled drug release characteristics. The aim of this work to formulated diazepam loaded PLGA nanoparticles by using emulsion solvent evaporation technique. Polyvinyl alcohol (PVA) is used as stabilizing agent. Diazepam is a benzodiazepine derivative drug, and widely used as an anticonvulsant in the treatment of various types of epilepsy, insomnia and anxiety. This work investigates the effects of some preparation variables on the size and shape of nanoparticles prepared by emulsion solvent evaporation method. These nanoparticles were characterized by photon correlation spectroscopy (PCS), transmission electron microscopy (TEM). Zeta potential study was also performed to understand the surface charge of nanoparticles. The drug release from drug loaded nanoparticles was studied by dialysis bag method and the in vitro drug release data was also studied by various kinetic models. The results show that sonication time, polymer content, surfactant concentration, ratio of organic to aqueous phase volume, and the amount of drug have an important effect on the size of nanoparticles. Hopefully we produced spherical shape Diazepam loaded PLGA nanoparticles with a size range under 250 nm with zeta potential -23.3 mV. The in vitro drug release analysis shows sustained release of drug from nanoparticles and follow Korsmeyer-Peppas model.

Convection-enhanced delivery and in vivo imaging of polymeric nanoparticles for the treatment of malignant glioma.

PubMed

Bernal, Giovanna M; LaRiviere, Michael J; Mansour, Nassir; Pytel, Peter; Cahill, Kirk E; Voce, David J; Kang, Shijun; Spretz, Ruben; Welp, Ulrich; Noriega, Sandra E; Nunez, Luis; Larsen, Gustavo F; Weichselbaum, Ralph R; Yamini, Bakhtiar

2014-01-01

A major obstacle to the management of malignant glioma is the inability to effectively deliver therapeutic agent to the tumor. In this study, we describe a polymeric nanoparticle vector that not only delivers viable therapeutic, but can also be tracked in vivo using MRI. Nanoparticles, produced by a non-emulsion technique, were fabricated to carry iron oxide within the shell and the chemotherapeutic agent, temozolomide (TMZ), as the payload. Nanoparticle properties were characterized and subsequently their endocytosis-mediated uptake by glioma cells was demonstrated. Convection-enhanced delivery (CED) can disperse nanoparticles through the rodent brain and their distribution is accurately visualized by MRI. Infusion of nanoparticles does not result in observable animal toxicity relative to control. CED of TMZ-bearing nanoparticles prolongs the survival of animals with intracranial xenografts compared to control. In conclusion, the described nanoparticle vector represents a unique multifunctional platform that can be used for image-guided treatment of malignant glioma. GBM remains one of the most notoriously treatment-unresponsive cancer types. In this study, a multifunctional nanoparticle-based temozolomide delivery system was demonstrated to possess enhanced treatment efficacy in a rodent xenograft GBM model, with the added benefit of MRI-based tracking via the incorporation of iron oxide as a T2* contrast material in the nanoparticles. © 2014.

Synthesis of highly monodisperse particles composed of a magnetic core and fluorescent shell.

PubMed

Nagao, Daisuke; Yokoyama, Mikio; Yamauchi, Noriko; Matsumoto, Hideki; Kobayashi, Yoshio; Konno, Mikio

2008-09-02

Highly monodisperse particles composed of a magnetic silica core and fluorescent polymer shell were synthesized with a combined technique of heterocoagulation and soap-free emulsion polymerization. Prior to heterocoagulation, monodisperse, submicrometer-sized silica particles were prepared with the Stober method, and magnetic nanoparticles were prepared with a modified Massart method in which a cationic silane coupling agent of N-trimethoxysilylpropyl- N, N, N-trimethylammonium chloride was added just after coprecipitation of Fe (2+) and Fe (3+). The silica particles with negative surface potential were heterocoagulated with the magnetic nanoparticles with positive surface potential. The magnetic silica particles obtained with the heterocoagulation were treated with sodium silicate to modify their surfaces with silica. In the formation of a fluorescent polymer shell onto the silica-coated magnetic silica cores, an amphoteric initiator of 2,2'-azobis[ N-(2-carboxyethyl)-2-2-methylpropionamidine] (VA-057) was used to control the colloidal stability of the magnetic cores during the polymer coating. The polymerization of St in the presence of a hydrophobic fluorophore of pyrene could coat the cores with fluorescent polymer shells, resulting in monodisperse particles with a magnetic silica core and fluorescent polymer shell. Measurements of zeta potential for the composite particles in different pH values indicated that the composite particles had an amphoteric property originating from VA-057 initiator.

Nucleation of polystyrene latex particles in the presence of gamma-methacryloxypropyltrimethoxysilane: functionalized silica particles.

PubMed

Bourgeat-Lami, Elodie; Insulaire, Mickaelle; Reculusa, Stéphane; Perro, Adeline; Ravaine, Serge; Duguet, Etienne

2006-02-01

Silica/polystyrene nanocomposite particles with different morphologies were synthesized through emulsion polymerization of styrene in the presence of silica particles previously modified by gamma-methacryloxypropyltrimethoxysilane (MPS). Grafting of the silane molecule was performed by direct addition of MPS to the aqueous silica suspension in the presence of an anionic surfactant under basic conditions. The MPS grafting density on the silica surface was determined using the depletion method and plotted against the initial MPS concentration. The influence of the MPS grafting density, the silica particles size and concentration and the nature of the surfactant on the polymerization kinetics and the particles morphology was investigated. When the polymerization was performed in the presence of an anionic surfactant, transmission electron microscopy images showed the formation of polymer spheres around silica for MPS grafting densities lower than typically 1 micromole x m(-2) while the conversion versus time curves indicated a strong acceleration effect under such conditions. In contrast, polymerizations performed in the presence of a larger amount of MPS moieties or in the presence of a non ionic emulsifier resulted in the formation of "excentered" core-shell morphologies and lower polymerization rates. The paper identifies the parameters that allow to control particles morphology and polymerization kinetics and describes the mechanism of formation of the nanocomposite colloids.

Charge Identification of Highly Ionizing Particles in Desensitized Nuclear Emulsion Using High Speed Read-Out System

DOE Office of Scientific and Technical Information (OSTI.GOV)

Toshito, T.; Kodama, K.; Yusa, K.

2006-05-10

We performed an experimental study of charge identification of heavy ions from helium to carbon having energy of about 290 MeV/u using an emulsion chamber. Emulsion was desensitized by means of forced fading (refreshing) to expand a dynamic range of response to highly charged particles. For the track reconstruction and charge identification, the fully automated high speed emulsion read-out system, which was originally developed for identifying minimum ionizing particles, was used without any modification. Clear track by track charge identification up to Z=6 was demonstrated. The refreshing technique has proved to be a powerful technique to expand response of emulsionmore » film to highly ionizing particles.« less

Surface shear inviscidity of soluble surfactants

PubMed Central

Zell, Zachary A.; Nowbahar, Arash; Mansard, Vincent; Leal, L. Gary; Deshmukh, Suraj S.; Mecca, Jodi M.; Tucker, Christopher J.; Squires, Todd M.

2014-01-01

Foam and emulsion stability has long been believed to correlate with the surface shear viscosity of the surfactant used to stabilize them. Many subtleties arise in interpreting surface shear viscosity measurements, however, and correlations do not necessarily indicate causation. Using a sensitive technique designed to excite purely surface shear deformations, we make the most sensitive and precise measurements to date of the surface shear viscosity of a variety of soluble surfactants, focusing on SDS in particular. Our measurements reveal the surface shear viscosity of SDS to be below the sensitivity limit of our technique, giving an upper bound of order 0.01 μN·s/m. This conflicts directly with almost all previous studies, which reported values up to 103–104 times higher. Multiple control and complementary measurements confirm this result, including direct visualization of monolayer deformation, for SDS and a wide variety of soluble polymeric, ionic, and nonionic surfactants of high- and low-foaming character. No soluble, small-molecule surfactant was found to have a measurable surface shear viscosity, which seriously undermines most support for any correlation between foam stability and surface shear rheology of soluble surfactants. PMID:24563383

PLGA nanoparticles from nano-emulsion templating as imaging agents: Versatile technology to obtain nanoparticles loaded with fluorescent dyes.

PubMed

Fornaguera, C; Feiner-Gracia, N; Calderó, G; García-Celma, M J; Solans, C

2016-11-01

The interest in polymeric nanoparticles as imaging systems for biomedical applications has increased notably in the last decades. In this work, PLGA nanoparticles, prepared from nano-emulsion templating, have been used to prepare novel fluorescent imaging agents. Two model fluorescent dyes were chosen and dissolved in the oil phase of the nano-emulsions together with PLGA. Nano-emulsions were prepared by the phase inversion composition (PIC) low-energy method. Fluorescent dye-loaded nanoparticles were obtained by solvent evaporation of nano-emulsion templates. PLGA nanoparticles loaded with the fluorescent dyes showed hydrodynamic radii lower than 40nm; markedly lower than those reported in previous studies. The small nanoparticle size was attributed to the nano-emulsification strategy used. PLGA nanoparticles showed negative surface charge and enough stability to be used for biomedical imaging purposes. Encapsulation efficiencies were higher than 99%, which was also attributed to the nano-emulsification approach as well as to the low solubility of the dyes in the aqueous component. Release kinetics of both fluorescent dyes from the nanoparticle dispersions was pH-independent and sustained. These results indicate that the dyes could remain encapsulated enough time to reach any organ and that the decrease of the pH produced during cell internalization by the endocytic route would not affect their release. Therefore, it can be assumed that these nanoparticles are appropriate as systemic imaging agents. In addition, in vitro toxicity tests showed that nanoparticles are non-cytotoxic. Consequently, it can be concluded that the preparation of PLGA nanoparticles from nano-emulsion templating represents a very versatile technology that enables obtaining biocompatible, biodegradable and safe imaging agents suitable for biomedical purposes. Copyright © 2016 Elsevier B.V. All rights reserved.

Single-cell Genomics using Droplet-based Microfluidics

NASA Astrophysics Data System (ADS)

Basu, Anindita; Macosko, Evan; Shalek, Alex; McCarroll, Steven; Regev, Aviv; Weitz, Dave

2014-03-01

We develop a system to profile the transcriptome of mammalian cells in isolation using reverse emulsion droplet-based microfluidic techniques. This is accomplished by (a) encapsulating and lysing one cell per emulsion droplet, and (b) uniquely barcoding the RNA contents from each cell using unique DNA-barcoded microgel beads. This enables us to study the transcriptional behavior of a large number of cells at single-cell resolution. We then use these techniques to study transcriptional responses of isolated immune cells to precisely controlled chemical and pathological stimuli provided in the emulsion droplet.

Use of hydrophobically modified inulin for the preparation of polymethyl methacrylate/polybutyl acrylate latex particles using a semicontinuous reactor.

PubMed

Obiols-Rabasa, M; Ramos, J; Forcada, J; Esquena, J; Solans, C; Levecke, B; Booten, K; Tadros, Tharwat F

2010-06-01

The seeded semicontinuous emulsion copolymerization of methyl methacrylate (MMA) and butyl acrylate (BuA) stabilized with a graft polymeric surfactant based on inulin, INUTEC SP1, as well as its mixture with sodium lauryl sulfate (SLS) is described. The mixture of SLS and Brij58 (alcohol ethoxylated) and the mixture of SLS and Pluronic P85 (block copolymer PEO-PPO-PEO) are also used as surfactant systems. The addition of methacrylic acid (MAA) or acrylic acid (AA) as comonomers is also studied. Previous results proved this inulin-derivative surfactant, INUTEC SP1, to be very effective on synthesizing latexes using a very low surfactant concentration. The kinetic features of the emulsion polymerization (instantaneous conversion and total conversion) were gravimetrically determined along the reactions. Latex dispersions were characterized by photon correlation spectroscopy (PCS) and transmission electron microscopy (TEM) to obtain the average particle size, the particle size distributions (PSDs) as well as the polydispersity index (PdI). The stability was determined by turbidimetry measurements and expressed in terms of critical coagulation concentration. The results showed that the use of the graft polymeric surfactant allowed obtaining highly stable nanoparticles, at low surfactant concentrations and high solid contents (up to 37 wt %). This is an improvement with respect to previous works, in which a mixture of the graft polymeric surfactant with another surfactant was required to obtain stable nanoparticles with low polydispersity, at high solid content. In the present work, low polydispersity was achieved using INUTEC as the only emulsifier, which was related to the absence of secondary nucleations. When a mixture of INUTEC SP1 and SLS is used, a wider PSD is obtained due to secondary nucleations. Replacing INUTEC SP1 by other nonionic surfactants such as Brij58 or Pluronic P85 leads to an increase of average particle size and wider PSD.

Design of polystyrene latex particles covered with polyoxometalate clusters via multiple covalent bonding

DOE PAGES

Chen, Xinyue; Li, Hui; Yin, Panchao; ...

2015-02-27

In this study, polyoxometalates (POMs) covalently functionalized with methyl methacrylate groups were applied as surfactants in the emulsion polymerization reaction of styrene. Due to the copolymerization of the methyl methacrylate groups and the styrene monomers, the polyoxometalate clusters are covalently grafted onto the surface of polystyrene latex nanoparticles. Finally, such latex particles are fully covered with catalytic POM clusters and might serve as quasi-homogeneous catalysts.

Kinetics of successive seeding of monodisperse polystyrene latexes. I - Initiation via potassium persulfate. II - Azo initiators with and without inhibitors

NASA Technical Reports Server (NTRS)

Sudol, E. D.; El-Aasser, M. S.; Vanderhoff, J. W.

1986-01-01

The polymerization kinetics of monodisperse polystyrene latexes with diameters of 1 micron are studied. The monodisperse latexes were prepared by the successive seeding method using 1 mM K2S2O8 with an 8 percent emulsifier surface coverage and 0.5 mM K2S2O8 with a 4 percent emulsifier surface coverage, and the kinetics were measured in a piston/cylinder dialometer. The data reveal that the polymerization rate decreases with increasing particle size; and the surface charge decreases with increasing particle size. The effects of initiators (AIBN and AMBN) and inhibitors (NH24SCN, NaNO2, and hydroquinone) on the product monodispersity and polymerization kinetics of latexes with diameters greater than 1 micron are investigated in a second experiment. It is observed that hydroquinone combined with AMBN are most effective in reducing nucleation without causing flocculation. It is noted that the kinetic transition from emulsion to bulk is complete for a particle size exceeding 1 micron in which the polymerization rate is independent of the particle size.

Preparation of uniform-sized multiple emulsions and micro/nano particulates for drug delivery by membrane emulsification.

PubMed

Liu, Wei; Yang, Xiang-Liang; Ho, W S Winston

2011-01-01

Much attention has in recent years been paid to fine applications of drug delivery systems, such as multiple emulsions, micro/nano solid lipid and polymer particles (spheres or capsules). Precise control of particle size and size distribution is especially important in such fine applications. Membrane emulsification can be used to prepare uniform-sized multiple emulsions and micro/nano particulates for drug delivery. It is a promising technique because of the better control of size and size distribution, the mildness of the process, the low energy consumption, easy operation and simple equipment, and amendable for large scale production. This review describes the state of the art of membrane emulsification in the preparation of monodisperse multiple emulsions and micro/nano particulates for drug delivery in recent years. The principles, influence of process parameters, advantages and disadvantages, and applications in preparing different types of drug delivery systems are reviewed. It can be concluded that the membrane emulsification technique in preparing emulsion/particulate products for drug delivery will further expand in the near future in conjunction with more basic investigations on this technique. Copyright © 2010 Wiley-Liss, Inc. and the American Pharmacists Association

Tricosane (C23H48) and Octacosane (C28H58) mixture phase transition insight via Light scattering techniques

NASA Astrophysics Data System (ADS)

Kuryakov, V. N.; De Sanctis Lucentini, P. G.; Ivanova, D. D.

2018-04-01

In this study we analyse several emulsion samples of pure Tricosane (C23H48) and Octacosane (C28H58) paraffins as well as their mixtures with different component concentrations, prepared by means of ultrasonic dispersion without the addition of surfactants. We show that from the measurements of Static Light Scattering temperature dependences it is possible to determine the phase transition temperatures of the paraffins emulsion during the heating and cooling cycles (melting, crystallization and rotator phases). The results for the pure paraffin are in good agreement with the literature data. We produce the outcomes of the Dynamic Light Scattering technique to determine the cluster size of the obtained emulsions (radius 70-120 nm). Those emulsions proved to remain stable during several months.

Actinide bioimaging in tissues: Comparison of emulsion and solid track autoradiography techniques with the iQID camera

PubMed Central

Miller, Brian W.; Van der Meeren, Anne; Tazrart, Anissa; Angulo, Jaime F.; Griffiths, Nina M.

2017-01-01

This work presents a comparison of three autoradiography techniques for imaging biological samples contaminated with actinides: emulsion-based, plastic-based autoradiography and a quantitative digital technique, the iQID camera, based on the numerical analysis of light from a scintillator screen. In radiation toxicology it has been important to develop means of imaging actinide distribution in tissues as these radionuclides may be heterogeneously distributed within and between tissues after internal contamination. Actinide distribution determines which cells are exposed to alpha radiation and is thus potentially critical for assessing absorbed dose. The comparison was carried out by generating autoradiographs of the same biological samples contaminated with actinides with the three autoradiography techniques. These samples were cell preparations or tissue sections collected from animals contaminated with different physico-chemical forms of actinides. The autoradiograph characteristics and the performances of the techniques were evaluated and discussed mainly in terms of acquisition process, activity distribution patterns, spatial resolution and feasibility of activity quantification. The obtained autoradiographs presented similar actinide distribution at low magnification. Out of the three techniques, emulsion autoradiography is the only one to provide a highly-resolved image of the actinide distribution inherently superimposed on the biological sample. Emulsion autoradiography is hence best interpreted at higher magnifications. However, this technique is destructive for the biological sample. Both emulsion- and plastic-based autoradiography record alpha tracks and thus enabled the differentiation between ionized forms of actinides and oxide particles. This feature can help in the evaluation of decorporation therapy efficacy. The most recent technique, the iQID camera, presents several additional features: real-time imaging, separate imaging of alpha particles and gamma rays, and alpha activity quantification. The comparison of these three autoradiography techniques showed that they are complementary and the choice of the technique depends on the purpose of the imaging experiment. PMID:29023595

Powdery Emulsion Explosive: A New Excellent Industrial Explosive

NASA Astrophysics Data System (ADS)

Ni, Ouqi; Zhang, Kaiming; Yu, Zhengquan; Tang, Shujuan

2012-07-01

Powdery emulsion explosive (PEE), a new powdery industrial explosive with perfect properties, has been made using an emulsification-spray drying technique. PEE is composed of 91-92.5 wt% ammonium nitrate (AN), 4.5-6 wt% organic fuels, and 1.5-1.8 wt% water. Due to its microstructure as a water-in-oil (W/O) emulsion and low water content, it has excellent detonation performance, outstanding water resistance, reliable safety, and good application compared with other industrial explosives, such as ammonite, emulsion explosives, and ANFO.

Thermal tuning the reversible optical band gap of self-assembled polystyrene photonic crystals

NASA Astrophysics Data System (ADS)

Vakili Tahami, S. H.; Pourmahdian, S.; Shirkavand Hadavand, B.; Azizi, Z. S.; Tehranchi, M. M.

2016-11-01

Nano-sized polymeric colloidal particles could undergo self-organization into three-dimensional structures to produce desired optical properties. In this research, a facile emulsifier-free emulsion polymerization method was employed to synthesize highly mono-disperse sub-micron polystyrene colloids. A high quality photonic crystal (PhC) structure was prepared by colloidal polystyrene. The reversible thermal tuning effect on photonic band gap position as well as the attenuation of the band gap was investigated in detail. The position of PBG can be tuned from 420 nm to 400 nm by varying the temperature of the PhC structure, reversibly. This reversible effect provides a reconfigurable PhC structure which could be used as thermo-responsive shape memory polymers.

Incorporation of iodine in polymeric microparticles and emulsions

NASA Astrophysics Data System (ADS)

Kolontaeva, Olga A.; Khokhlova, Anastasia R.; Markina, Natalia E.; Markin, Alexey V.; Burmistrova, Natalia A.

2016-04-01

Application of different methods for formation of microcontainers containing iodine is proposed in this paper. Two types of microcontainers: microemulsions and microparticles have been investigated, conditions and methods for obtaining microcontainers were optimized. Microparticles were formed by layer-by-layer method with cores of calcium carbonate (CaCO3) as templates. Incorporation of complexes of iodine with polymers (chitosan, starch, polyvinyl alcohol) into core, shell and hollow capsules was investigated and loadings of microparticles with iodine were estimated. It was found that the complex of iodine with chitosan adsorbed at CaCO3 core is the most stable under physiological conditions and its value of loading can be 450 μg of I2 per 1 g of CaCO3. Moreover, chitosan was chosen as a ligand because of its biocompatibility and biodegradability as well as very low toxicity while its complex with iodine is very stable. A small amount of microparticles containing a iodine-chitosan complex can be used for prolonged release of iodine in the human body since iodine daily intake for adults is around 100 μg. "Oil-in-water" emulsions were prepared by ultrasonication of iodinated oils (sunflower and linseed) with sodium laurilsulfate (SLS) as surfactant solution. At optimal conditions, the homogenous emulsions remained stable for weeks, with total content of iodine in such emulsion being up to 1% (w/w). The oil:SLS ratio was equal to 1:10 (w/w), optimal duration and power of ultrasound exposure were 1.5 min and 7 W, correspondingly. Favorable application of iodized linseed oil for emulsion preparation with suitable oil microdroplets size was proved.

Organic Thin Films Deposited by Emulsion-Based, Resonant Infrared, Matrix-Assisted Pulsed Laser Evaporation: Fundamentals and Applications

NASA Astrophysics Data System (ADS)

Ge, Wangyao

Thin film deposition techniques are indispensable to the development of modern technologies as thin film based optical coatings, optoelectronic devices, sensors, and biological implants are the building blocks of many complicated technologies, and their performance heavily depends on the applied deposition technique. Particularly, the emergence of novel solution-processed materials, such as soft organic molecules, inorganic compounds and colloidal nanoparticles, facilitates the development of flexible and printed electronics that are inexpensive, light weight, green and smart, and these thin film devices represent future trends for new technologies. One appealing feature of solution-processed materials is that they can be deposited into thin films using solution-processed deposition techniques that are straightforward, inexpensive, high throughput and advantageous to industrialize thin film based devices. However, solution-processed techniques rely on wet deposition, which has limitations in certain applications, such as multi-layered film deposition of similar materials and blended film deposition of dissimilar materials. These limitations cannot be addressed by traditional, vacuum-based deposition techniques because these dry approaches are often too energetic and can degrade soft materials, such as polymers, such that the performance of resulting thin film based devices is compromised. The work presented in this dissertation explores a novel thin film deposition technique, namely emulsion-based, resonant infrared, matrix-assisted pulsed laser evaporation (RIR-MAPLE), which combines characteristics of wet and dry deposition techniques for solution-processed materials. Previous studies have demonstrated the feasibility of emulsion-based RIR-MAPLE to deposit uniform and continuous organic, nanoparticle and blended films, as well as hetero-structures that otherwise are difficult to achieve. However, fundamental understanding of the growth mechanisms that govern emulsion-based RIR-MAPLE is still missing, which increases the difficulty of using rational design to improve the performance of initial RIR-MAPLE devices that have been demonstrated. As a result, it is important to study the fundamentals of emulsion-based RIR-MAPLE in order to provide insight into the long-term prospects for this thin film deposition technique. This dissertation explores the fundamental deposition mechanisms of emulsion-based RIR-MAPLE by considering the effects of the emulsion target composition (namely, the primary solvent, secondary solvent, and surfactant) on the properties of deposited polymer films. The study of primary solvent effects on hydrophobic polymer deposition helps identify the unique method of film formation for emulsion-based RIR-MAPLE, which can be described as cluster-by-cluster deposition of emulsified particles that yields two levels of ordering (i.e., within the clusters and among the clusters). The generality of this film formation mechanism is tested by applying the lessons learned to hydrophilic polymer deposition. Based on these studies, the deposition design rules to achieve smooth polymer films, which are important for different device applications, are identified according to the properties of the polymer. After discussion of the fundamental deposition mechanisms, three applications of emulsion-based RIR-MAPLE, namely thin film deposition of organic solar cells, polymer/nanoparticle hybrid solar cells, and antimicrobial/fouling-release multifunctional films, are studied. The work on organic solar cells identifies the ideal deposition mode for blended films with nanoscale domain sizes, as well as demonstrates the relationships among emulsion target composition, film properties, and corresponding device performance. The studies of polymer/nanoparticle hybrid solar cells demonstrate precise control of colloidal nanoparticle deposition, in which the integrity of nanoparticles is maintained and a distinct film morphology is achieved when co-deposited with polymers. Finally, the application of antimicrobial and fouling-release multifunctional films demonstrates the importance of blended film deposition with nanoscale phase separation, a key feature to achieving reusable bio-films that can kill bacteria when illuminated with ultraviolet light. Thus, this dissertation provides great insight to the fundamentals of emulsion-based RIR-MAPLE, serves as a valuable reference for future development, and paves the pathway for wider adoption of this unique thin film deposition technique, especially for organic solar cells.

The application of novel nano-thermal and imaging techniques for monitoring drug microstructure and distribution within PLGA microspheres.

PubMed

Yang, Fan; Chen, De; Guo, Zhe-Fei; Zhang, Yong-Ming; Liu, Yi; Askin, Sean; Craig, Duncan Q M; Zhao, Min

2017-04-30

Poly (d,l-lactic-co-glycolic) acid (PLGA) based microspheres have been extensively used as controlled drug release systems. However, the burst effect has been a persistent issue associated with such systems, especially for those prepared by the double emulsion technique. An effective approach to preventing the burst effect and achieving a more ideal drug release profile is to improve the drug distribution within the polymeric matrix. Therefore, it is of great importance to establish a rapid and robust tool for screening and optimizing the drug distribution during pre-formulation. Transition Temperature Microscopy (TTM), a novel nano-thermal and imaging technique, is an extension of nano-thermal analysis (nano-TA) whereby a transition temperature is detected at a localized region of a sample and then designated a color based on a particular temperature/color palette, finally resulting in a coded map based on transition temperatures detected by carrying out a series of nanoTA measurements across the surface of the sample. In this study, we investigate the feasibility of applying the aforementioned technique combined with other thermal, imaging and structural techniques for monitoring the drug microstructure and spatial distribution within bovine serum albumin (BSA) loaded and nimodipine loaded PLGA microspheres, with a view to better predicting the in vitro drug release performance. Copyright © 2017 Elsevier B.V. All rights reserved.

Computed tomography-guided screening of surfactant effect on blood circulation time of emulsions: application to the design of an emulsion formulation for paclitaxel.

PubMed

Lee, Eun-Hye; Hong, Soon-Seok; Kim, So Hee; Lee, Mi-Kyung; Lim, Joon Seok; Lim, Soo-Jeong

2014-08-01

In an effort to apply the imaging techniques currently used in disease diagnosis for monitoring the pharmacokinetics and biodisposition of particulate drug carriers, we sought to use computed tomography (CT) scanning methodology to investigate the impact of surfactant on the blood residence time of emulsions. We prepared the iodinated oil Lipiodol emulsions with different compositions of surfactants and investigated the impact of surfactant on the blood residence time of emulsions by CT scanning. The blood circulation time of emulsions was prolonged by including Tween 80 or DSPE-PEG (polyethylene glycol 2000) in emulsions. Tween 80 was less effective than DSPE-PEG in terms of prolongation effect, but the blood circulating time of emulsions was prolonged in a Tween 80 content-dependent manner. As a proof-of-concept demonstration of the usefulness of CT-guided screening in the process of formulating drugs that need to be loaded in emulsions, paclitaxel was loaded in emulsions prepared with 87 or 65% Tween 80-containing surfactant mixtures. A pharmacokinetics study showed that paclitaxel loaded in 87% Tween 80 emulsions circulated longer in the bloodstream compared to those in 65% Tween 80 emulsions, as predicted by CT imaging. CT-visible, Lipiodol emulsions enabled the simple evaluation of surfactant composition effects on the biodisposition of emulsions.

Automated Track Recognition and Event Reconstruction in Nuclear Emulsion

NASA Technical Reports Server (NTRS)

Deines-Jones, P.; Cherry, M. L.; Dabrowska, A.; Holynski, R.; Jones, W. V.; Kolganova, E. D.; Kudzia, D.; Nilsen, B. S.; Olszewski, A.; Pozharova, E. A.;

Control of lipid oxidation by nonmigratory active packaging films prepared by photoinitiated graft polymerization.

PubMed

Tian, Fang; Decker, Eric A; Goddard, Julie M

2012-08-08

Transition metal-promoted oxidation impacts the quality, shelf life, and nutrition of many packaged foods. Metal-chelating active packaging therefore offers a means to protect foods against oxidation. Herein, we report the development and characterization of nonmigratory metal-chelating active packaging. To prepare the films, carboxylic acids were grafted onto the surfaces of polypropylene films by photoinitiated graft polymerization of acrylic acid. Attenuated total reflectance/Fourier transform infrared spectroscopy, contact angle, scanning electron microscopy, and iron-chelating assay were used to characterize film properties. Graft polymerization yielded a carboxylic acid density of 68.67 ± 9.99 nmol per cm(2) film, with ferrous iron-chelating activity of 71.07 ± 12.95 nmol per cm(2). The functionalized films extended the lag phase of lipid oxidation in a soybean oil-in-water emulsion system from 2 to 9 days. The application of such nonmigratory active packaging films represents a promising approach to reduce additive use while maintaining food quality.

Pore Structure and Fluoride Ion Adsorption Characteristics of Zr (IV) Surface-Immobilized Resin Prepared Using Polystyrene as a Porogen

NASA Astrophysics Data System (ADS)

Mizuki, Hidenobu; Ito, Yudai; Harada, Hisashi; Uezu, Kazuya

Zr(IV) surface-immobilized resins for removal of fluoride ion were prepared by surface template polymerization using polystyrene as a porogen. At polymerization, polystyrene was added in order to increase mesopores (2-50 nm) and macropore (>50 nm) with large macropores (around 300 nm) formed with internal aqueous phase of W⁄O emulsion. The pore structure of Zr(IV) surface-immobilized resins was evaluated by measuring specific surface area, pore volume, and pore size distribution with volumetric adsorption measurement instrument and mercury porosimeter. The adsorption isotherms were well fitted by Langmuir equation. The removal of fluoride was also carried out with column method. Zr(IV) surface-immobilized resins, using 10 g⁄L polystyrene in toluene at polymerization, possessed higher volume of not only mesopores and macropores but also large macropores. Furethermore, by adding the polystyrene with smaller molecular size, the pore volume of mesopores, macropores and large macropores was significantly increased, and the fluoride ion adsorption capacity and the column utilization also increased.

Synthesis of berberine loaded polymeric nanoparticles by central composite design

NASA Astrophysics Data System (ADS)

Mehra, Meenakshi; Sheorain, Jyoti; Kumari, Santosh

2016-04-01

Berberine is an isoquinoline alkaloid which is extracted from bark and roots of Berberis vulgaris plant. It has been used in ayurvedic medicine as it possess antimicrobial, antidiabetic, anticancer, antioxidant properties etc. But poor solubility of berberine leads to poor stability and bioavailability in medical formulations decreasing its efficacy. Hence nanoformulations of berberine can help in removing the limiting factors of alkaloid enhancing its utilization in pharmaceutical industry. Sodium alginate polymer was used to encapsulate berberine within nanoparticles by emulsion solvent evaporation method using tween 80 as a surfactant. Two factors and three level in central composite design was used to study the formulation. The optimized formulation (1% v/v of Tween 80 and 0.01% w/v of sodium alginate) of polymeric nanoparticles was taken for further evaluations. The size of synthesized nanoparticles was found to be 71.18 nm by particle size analysis (PSA). The berberine loaded polymeric nanoparticles showed better antibacterial activity compared to aqueous solution of berberine by well diffusion assay.

The development of a super-fine-grained nuclear emulsion

NASA Astrophysics Data System (ADS)

Asada, Takashi; Naka, Tatsuhiro; Kuwabara, Ken-ichi; Yoshimoto, Masahiro

2017-06-01

A nuclear emulsion with micronized crystals is required for the tracking detection of submicron ionizing particles, which are one of the targets of dark-matter detection and other techniques. We found that a new production method, called the PVA—gelatin mixing method (PGMM), could effectively control crystal size from 20 nm to 50 nm. We called the two types of emulsion produced with the new method the nano imaging tracker and the ultra-nano imaging tracker. Their composition and spatial resolution were measured, and the results indicate that these emulsions detect extremely short tracks.

Development of novel zein-sodium caseinate nanoparticle (ZP)-stabilized emulsion films for improved water barrier properties via emulsion/solvent evaporation.

PubMed

Wang, Li-Juan; Yin, Ye-Chong; Yin, Shou-Wei; Yang, Xiao-Quan; Shi, Wei-Jian; Tang, Chuan-He; Wang, Jin-Mei

2013-11-20

This work attempted to develop novel high barrier zein/SC nanoparticle (ZP)-stabilized emulsion films through microfluidic emulsification (ZPE films) or in combination with solvent (ethyl acetate) evaporation techniques (ZPE-EA films). Some physical properties, including tensile and optical properties, water vapor permeability (WVP), and surface hydrophobicity, as well as the microstructure of ZP-stabilized emulsion films were evaluated and compared with SC emulsion (SCE) films. The emulsion/solvent evaporation approach reduced lipid droplets of ZP-stabilized emulsions, and lipid droplets of ZP-stabilized emulsions were similar to or slightly lower than that of SC emulsions. However, ZP- and SC-stabilized emulsion films exhibited a completely different microstructure, nanoscalar lipid droplets were homogeneously distributed in the ZPE film matrix and interpenetrating protein-oil complex networks occurred within ZPE-EA films, whereas SCE films presented a heterogeneous microstructure. The different stabilization mechanisms against creaming or coalescence during film formation accounted for the preceding discrepancy of the microstructures between ZP-and SC-stabilized emulsion films. Interestingly, ZP-stabilized emulsion films exhibited a better water barrier efficiency, and the WVP values were only 40-50% of SCE films. A schematic representation for the formation of ZP-stabilized emulsion films was proposed to relate the physical performance of the films with their microstructure and to elucidate the possible forming mechanism of the films.

Rational design and evaluation of HBsAg polymeric nanoparticles as antigen delivery carriers.

PubMed

Dewangan, Hitesh Kumar; Pandey, Tarun; Maurya, Lakshmi; Singh, Sanjay

2018-05-01

The present work is focused on the development and evaluation of single dose sustained-release Hepatitis B surface antigen (HBsAg) loaded nanovaccine for Hepatitis B. The conventional treatment suffers from repeated administration and hence requires a booster dose. Therefore, polymeric nanovaccine of HBsAg was developed by double emulsion solvent evaporation technique, utilizing central composite design for formulation optimization. The effects of independent variables (like polymer amount, stabilizer concentration, aqueous/organic phase ratio and homogenizer speed) were also studied on critical quality attributes like particle size and entrapment efficiency. Nanovaccine was characterized in terms of physicochemical parameters, release, internalization and in vivo immunological evaluation in BALB/c mice after administration by different routes such as oral, sub-cutaneous, nasal and intramuscular. The designed nanovaccine demonstrated nanometric size with smooth surface, negative zeta potential, maximum entrapment, sustained release and better internalization in macrophage and MRC-5 cell line. The immune-stimulating activity of nanovaccine administered by different routes was evaluated by measuring anti-HBsAg titre like specific immunoglobulin IgG and IgA response and cytokine level (interleukin-2, interferon-Y) measurement. The results indicated that the nanovaccine administered by intramuscular route produced better humoral as well as cellular responses and potential carriers for antigen delivery at single dose administration via intramuscular route. Copyright © 2018 Elsevier B.V. All rights reserved.

Preparation and in vitro evaluation of poly(D,L-lactide-co-glycolide) air-filled nanocapsules as a contrast agent for ultrasound imaging.

PubMed

Néstor, Mendoza-Muñoz; Kei, Noriega-Peláez Eddy; Guadalupe, Nava-Arzaluz María; Elisa, Mendoza-Elvira Susana; Adriana, Ganem-Quintanar; David, Quintanar-Guerrero

2011-10-01

The aim of this study was to prepare air-filled nanocapsules intended ultrasound contrast agents (UCAs) with a biodegradable polymeric shell composed of poly(d,l-lactide-co-glycolide) (PLGA). Because of their size, current commercial UCAs are not capable of penetrating the irregular vasculature that feeds growing tumors. The new generation of UCAs should be designed on the nanoscale to enhance tumor detection, in addition, the polymeric shell in contrast with monomolecular stabilized UCAs improves the mechanical properties against ultrasound pressure and lack of stability. The preparation method of air-filled nanocapsules was based on a modification of the double-emulsion solvent evaporation technique. Air-filled nanocapsules with a mean diameter of 370±96nm were obtained. Electronic microscopies revealed spherical-shaped particles with smooth surfaces and a capsular morphology, with a shell thickness of ∼50nm. Air-filled nanocapsules showed echogenic power in vitro, providing an enhancement of up to 15dB at a concentration of 0.045mg/mL at a frequency of 10MHz. Loss of signal for air-filled nanocapsules was 2dB after 30min, suggesting high stability. The prepared contrast agent in this work has the potential to be used in ultrasound imaging. Copyright © 2011 Elsevier B.V. All rights reserved.

Morphological study of polymethyl methacrylate microcapsules filled with self-healing agents

NASA Astrophysics Data System (ADS)

Ahangaran, Fatemeh; Hayaty, Mehran; Navarchian, Amir H.

2017-03-01

Polymethyl methacrylate (PMMA) microcapsules filled with epoxy prepolymer, 3-aminomethyl-3,5,5-trimethylcyclohexylamine, and pentaerythritol tetrakis (3-mercaptopropionate) as healing agents have been prepared separately through internal phase separation method for self-healing purposes. PMMA with two different molecular weights (M bar1 = 36,000 g/mol and M bar2 = 550,000 g/mol) were used with two types of different emulsifiers (ionic and polymeric) to prepare microcapsules. The morphology of healing agent microcapsules was investigated using field emission scanning electron microscopy (FESEM). It was found that PMMA microcapsules separately filled with epoxy and amine had core-shell morphologies with smooth surfaces. The mercaptan/PMMA particles exhibited core-shell and acorn-shape morphologies. The surface morphology of mercaptan microcapsules changed from holed to plain in different emulsion systems. The spreading coefficient (S) of phases in the prepared emulsion systems were calculated from interfacial tension (σ) and contact angle (θ) measurements. The theoretical equilibrium morphology of PMMA microcapsules was predicted according to spreading coefficient values of phases in emulsion systems. It was also found that the surface morphology of PMMA microcapsules depended strongly on the nature of the core, molecular weight of PMMA, type and concentration of emulsifier.

NEW DEVELOPMENTS AND APPLICATIONS OF SUPERHEATED EMULSIONS: WARHEAD VERIFICATION AND SPECIAL NUCLEAR MATERIAL INTERDICTION.

PubMed

d'Errico, F; Chierici, A; Gattas-Sethi, M; Philippe, S; Goldston, R; Glaser, A

2018-04-25

In recent years, neutron detection with superheated emulsions has received renewed attention thanks to improved detector manufacturing and read-out techniques, and thanks to successful applications in warhead verification and special nuclear material (SNM) interdiction. Detectors are currently manufactured with methods allowing high uniformity of the drop sizes, which in turn allows the use of optical read-out techniques based on dynamic light scattering. Small detector cartridges arranged in 2D matrices are developed for the verification of a declared warhead without revealing its design. For this application, the enabling features of the emulsions are that bubbles formed at different times cannot be distinguished from each other, while the passive nature of the detectors avoids the susceptibility to electronic snooping and tampering. Large modules of emulsions are developed to detect the presence of shielded special nuclear materials hidden in cargo containers 'interrogated' with high energy X-rays. In this case, the enabling features of the emulsions are photon discrimination, a neutron detection threshold close to 3 MeV and a rate-insensitive read-out.

Co-polymerization of methyl methacrylate and styrene via surfactant-free emulsion polymerization, as a potential material for photonic crystal application

NASA Astrophysics Data System (ADS)

Kassim, Syara; Zahari, Siti Balqis; Tahrin, Rabiatul Addawiyah Azwa; Harun, Noor Aniza

2017-09-01

Photonic crystals are being the great interest of researcher to studies due to a variety of potential application for the interaction of light including the solar cells, optical sensors and paints. In order to evaluate the fabrication of photonic crystals thin film, a free-emulsifier emulsion copolymerization of styrene and methyl methacrylate was carried out. By using the self -assembly approach, this method offers the opportunity to produce crystalline polymer sphere in more ease operation, low cost and environmental friendly. The influences of the mixing ratio of monomer and amount of initiators were studied. In advance, the presence of styrene as co-monomer had improved the thermal degradation of polymer methyl methacrylate. While in changing the mixing ratio of styrene and methyl methacrylate resulted in particle size of the sphere. The size of polymer particles slightly increased on increasing volume of styrene monomer ratio. This occurred because the properties of styrene in water where it sparingly soluble and lead to coagulation of particles. This simple, yet effective method for preparing functional complex 3D structures has the potential to be used generically to fabricate a variety of functional porous 3D structures that could find application not only in new or improved photonic crystal (PC) devices but also in areas such as catalysis, solar cell, separation, fuel cells technology, microelectronics and optoelectronics.

Pharmacological aspects of release from microcapsules - from polymeric multilayers to lipid membranes.

PubMed

Wuytens, Pieter; Parakhonskiy, Bogdan; Yashchenok, Alexey; Winterhalter, Mathias; Skirtach, Andre

2014-10-01

This review is devoted to pharmacological applications of principles of release from capsules to overcome the membrane barrier. Many of these principles were developed in the context of polymeric multilayer capsule membrane modulation, but they are also pertinent to liposomes, polymersomes, capsosomes, particles, emulsion-based carriers and other carriers. We look at these methods from the physical, chemical or biological driving mechanisms point of view. In addition to applicability for carriers in drug delivery, these release methods are significant for another area directly related to pharmacology - modulation of the permeability of the membranes and thus promoting the action of drugs. Emerging technologies, including ionic current monitoring through a lipid membrane on a nanopore, are also highlighted. Copyright © 2014 Elsevier Ltd. All rights reserved.

Preparation of an Adhesive in Emulsion for Maxillofacial Prosthetic

PubMed Central

Sánchez-García, Judith A.; Ortega, Alejandra; Barceló-Santana, Federico H.; Palacios-Alquisira, Joaquín

2010-01-01

Maxillofacial prostheses is a dental medicine specialty aimed at restoring anatomical facial defects caused by cancer, trauma or congenital malformations through an artificial device, which is commonly attached to the skin with the help of an adhesive. The purpose of our research was to develop a pressure-sensitive adhesive (PSA) based on acrylic monomers, characterizing and determining its drying kinetics, that is to say the time it takes to lose 50 to 90% of its moisture. The adhesive synthesis was realized by means of emulsion polymerization; the composition of formulations was: (AA-MMA-EA) and (AA-MMA-2EHA) with different molar ratios. The formulation based on (AA-MMA-2EHA) with 50 w% of solids, presented good adhesive properties such as tack, bond strength, and short drying time. We propose this formulation as a PSA, because it offers an alternative for systemically compromised patients, by less irritation compared to organic solvent-based adhesives. PMID:21152308

Molecular Design of Squalene/Squalane Countertypes via the Controlled Oligomerization of Isoprene and Evaluation of Vaccine Adjuvant Applications.

PubMed

Adlington, Kevin; El Harfi, Jaouad; Li, Jianing; Carmichael, Kim; Guderian, Jeffrey A; Fox, Christopher B; Irvine, Derek J

2016-01-11

The potential to replace shark-derived squalene in vaccine adjuvant applications with synthetic squalene/poly(isoprene) oligomers, synthesized by the controlled oligomerization of isoprene is demonstrated. Following on from our previous work regarding the synthesis of poly(isoprene) oligomers, we demonstrate the ability to tune the molecular weight of the synthetic poly(isoprene) material beyond that of natural squalene, while retaining a final backbone structure that contained a minimum of 75% of 1,4 addition product and an acceptable polydispersity. The synthesis was successfully scaled from the 2 g to the 40 g scale both in the bulk (i.e., solvent free) and with the aid of additional solvent by utilizing catalytic chain transfer polymerization (CCTP) as the control method, such that the target molecular weight, acceptable dispersity levels, and the desired level of 1,4 addition in the backbone structure and an acceptable yield (∼60%) are achieved. Moreover, the stability and in vitro bioactivity of nanoemulsion adjuvant formulations manufactured with the synthetic poly(isoprene) material are evaluated in comparison to emulsions made with shark-derived squalene. Emulsions containing the synthetic poly(isoprene) achieved smaller particle size and equivalent or enhanced bioactivity (stimulation of cytokine production in human whole blood) compared to corresponding shark squalene emulsions. However, as opposed to the shark squalene-based emulsions, the poly(isoprene) emulsions demonstrated reduced long-term size stability and induced hemolysis at high concentrations. Finally, we demonstrate that the synthetic oligomeric poly(isoprene) material could successfully be hydrogenated such that >95% of the double bonds were successfully removed to give a representative poly(isoprene)-derived squalane mimic.

[Preparation and in vitro release characteristics of vincristine sulphate loaded poly (butylcyanoacrylate) nanoparticles].

PubMed

Tan, Rong; Liu, Ying; Feng, Nianping; Zhao, Jihui

2011-06-01

To prepare vincristine sulphate loaded poly (butylcyanoacrylate) nanoparticles (VCR-PBCA-NPs) and to investigate the in vitro release charactersitics. VCR-PBCA-NPs were prepared by emulsion polymerization method, and characterized for morphology, particle size, drug encapsulation efficiency and loading efficiency. The formulation was optimized using central composite design and response surface methodology. In vitro release study of VCR-PBCA-NPs was performed by dialysis technique. Model fitting was used to determine the kinetics and to discuss the mechanism. The nanoparticles were spherical and uniform with a mean diameter of (98.9 +/- 3.05) nm. The drug encapsulation efficiency and loading efficiency were (55.23 +/- 0.96)% and (7.87 +/- 0.11)%, respectively. In vitro release results showed that 63.66% of VCR was released from VCR-PBCA-NPs in 4 h, and the Weibull model fitted VCR release pattern best. The VCR-PBCA-NPs prepared in this study showed sustained release compared with VCR solution.

Preparation and characterization of solid lipid nanoparticles-a review.

PubMed

Parhi, Rabinarayan; Suresh, Padilama

2012-03-01

In the present scenario, most of the developed and new discovered drugs are posing real challenge to the formulation scientists due to their poor aqueous solubility which in turn is responsible for poor bioavailability. One of the approach to overcome above problem is the packaging of the drug in to particulate carrier system. Among various carriers, lipid emerged as very attractive candidate because of its unique property of enhancing the bioavailability of poorly water soluble drugs. Solid lipid, one of the physical forms of lipid, is used to formulate nanoparticles, popularly known as Solid lipid nanoparticles (SLNs), as an alternative carrier system to emulsions, liposomes and polymeric micro- and nano-particles. SLNs combine advantages of the traditional systems but avoid some of their major disadvantages. This paper reviews numerous production techniques for SLNs along with their advantages and disadvantages. Special attention is paid to the characterization of the SLNs by using various analytical tools. It also emphasizes on physical state of lipid (supercooled melts, different lipid modifications).

Development and characterisation of polymeric microparticle of poly(d,l-lactic acid) loaded with holmium acetylacetonate.

PubMed

de Azevedo, Mariangela de Burgos M; de Melo, Vitor H S; Soares, Carlos Roberto J; Miyamoto, Douglas M; Katayama, Ricardo A; Squair, Peterson L; Barros, Caio H N; Tasic, Ljubica

2018-06-14

Biodegradable polymers containing radioactive isotopes such as Holmium 166 ( 166 Ho) have potential applications as beta particle emitters in tumour tissues. It is also a gamma ray emitter, allowing nuclear imaging of any tissue to be acquired. It is frequently used in the form of complexes such as holmium acetylacetonate (HoAcAc), which may cause damages in tissues next to the targets cancer cells, as it is difficult to control its linkage or healthy tissues radiotherapy effects. Poly(d,l-lactic acid), PDLLA, was used to encapsulate holmium acetylacetonate (HoAcAc) using an emulsion solvent extraction/evaporation technique. Microspheres with sizes between 20-53 µm were extensively characterised. HoAcAc release from the microspheres was assessed through studies using Inductively Coupled Plasma - Optical Emission Spectroscopy, and the microspheres showed no holmium leakage after a period of 10 half-lives and following gamma irradiation. Thus, HoAcAc loaded microspheres are here presented as a potential system for brachytherapy and imaging purposes.

Three-dimensional molecular mapping of a multiple emulsion by means of CARS microscopy.

PubMed

Meyer, Tobias; Akimov, Denis; Tarcea, Nicolae; Chatzipapadopoulos, Susana; Muschiolik, Gerald; Kobow, Jens; Schmitt, Michael; Popp, Jürgen

2008-02-07

Multiple emulsions consisting of water droplets dispersed in an oil phase containing emulsifier which is emulsified in an outer water phase (W/O/W) are of great interest in pharmacology for developing new drugs, in the nutrition sciences for designing functional food, and in biology as model systems for cell organelles such as liposomes. In the food industry multiple emulsions with high sugar content in the aqueous phase can be used for the production of sweets, because the high sugar content prevents deterioration. However, for these emulsions the refractive indexes of oil and aqueous phase are very similar. This seriously impedes the analysis of these emulsions, e.g., for process monitoring, because microscopic techniques based on transmission or reflection do not provide sufficient contrast. We have characterized the inner dispersed phase of concentrated W/O/W emulsions with the same refractive index of the three phases by micro Raman spectroscopy and investigated the composition and molecular distribution in water-oil-water emulsions by means of three-dimensional laser scanning CARS (coherent anti-Stokes Raman scattering) microscopy. CARS microscopy has been used to study water droplets dispersed in oil droplets at different Raman resonances to visualize different molecular species. Water droplets with a diameter of about 700 nm could clearly be visualized. The advantages of CARS microscopy for studying this particular system are emphasized by comparing this microscopic technique with conventional confocal reflection and transmission microscopies.

Muon radiography in Russia with emulsion technique. First experiments future perspectives

DOE Office of Scientific and Technical Information (OSTI.GOV)

Aleksandrov, A. B.; Bagulya, A. V.; Chernyavsky, M. M.

Cosmic ray muon radiography is a novel technique for imaging the internal structures of massive objects. It exploits the capability of high energy muons from cosmic-rays in order to obtain a density map of investigated object and trying to guess information on the variation in the density distribution. Nuclear emulsions are tracking detectors well suited to be employed in this context since they have an excellent angular resolution (few mrad), they are cheap, compact and robust, easily transportable, able to work in harsh environments, and do not require power supply. This work presents the first successful results in the fieldmore » of muon radiography in Russia with nuclear emulsions.« less

Phase recording for formation of holographic optical elements on silver-halide photographic emulsions

NASA Astrophysics Data System (ADS)

Ganzherli, Nina M.; Gulyaev, Sergey N.; Maurer, Irina A.; Chernykh, Dmitrii F.

2009-05-01

Holographic fabrication methods of regular and nonregular relief-phase structures on silver-halide photographic emulsions are considered. Methods of gelatin photodestruction under short-wave ultra-violet radiation and chemical hardening with the help of dichromated solutions were used as a technique for surface relief formation. The developed techniques permitted us to study specimens of holographic diffusers and microlens rasters with small absorption and high light efficiency.

Rapid crystallization and morphological adjustment of zeolite ZSM-5 in nonionic emulsions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang Ying, E-mail: yingzh1977@163.co; Jin Chao; Research Institute of Petroleum Processing, Beijing 100083

2011-01-15

Zeolite ZSM-5 was synthesized for the first time in a nonionic emulsion composed of polyoxyethylated alkylphenol, butanol, cyclohexane and tetraethylammonium hydroxide (TEAOH)-containing zeolite synthesis mixture. The crystallization kinetics in the emulsion was investigated and the ZSM-5 product was characterized in detail by XRD, SEM, FT-IR, TG, N{sub 2} adsorption and CHN analysis techniques. Compared with the conventionally hydrothermal synthesis with the same structure directing agent TEAOH, the emulsion system allows rapid crystallization of ZSM-5. The ZSM-5 product exhibits unusual agglomerated structure and possesses larger specific surface area. The FT-IR, TG results plus CHN analysis show the encapsulation of a tracemore » of emulsion components in the emulsion ZSM-5. Control experiments show the emulsion system exerts the crystallization induction and morphological adjustment effects mainly during the aging period. The effects are tentatively attributed to the confined space domains, surfactant-water interaction as well as surfactant-growing crystals interaction existing in the emulsion. -- Graphical abstract: The nonionic emulsion synthesis allows rapid crystallization and morphological adjustment of zeolite ZSM-5 compared with the conventional hydrothermal synthesis. Display Omitted« less

Water-in-Water Emulsion Based Synthesis of Hydrogel Nanospheres with Tunable Release Kinetics

NASA Astrophysics Data System (ADS)

Aydın, Derya; Kızılel, Seda

2017-07-01

Poly(ethylene glycol) (PEG) micro/nanospheres have several unique advantages as polymer based drug delivery systems (DDS) such as tunable size, large surface area to volume ratio, and colloidal stability. Emulsification is one of the widely used methods for facile synthesis of micro/nanospheres. Two-phase aqueous system based on polymer-polymer immiscibility is a novel approach for preparation of water-in-water (w/w) emulsions. This method is promising for the synthesis of PEG micro/nanospheres for biological systems, since the emulsion is aqueous and do not require organic solvents or surfactants. Here, we report the synthesis of nano-scale PEG hydrogel particles using w/w emulsions using phase separation of dextran and PEG prepolymer. Dynamic light scattering (DLS) and scaning electron microscopy (SEM) results demonstrated that nano-scale hydrogel spheres could be obtained with this approach. We investigated the release kinetics of a model drug, pregabalin (PGB) from PEG nanospheres and demonstrated the influence of polymerization conditions on loading and release of the drug as well as the morphology and size distribution of PEG nanospheres. The experimental drug release data was fitted to a stretched exponential function which suggested high correlation with experimental results to predict half-time and drug release rates from the model equation. The biocompatibility of nanospheres on human dermal fibroblasts using cell-survival assay suggested that PEG nanospheres with altered concentrations are non-toxic, and can be considered for controlled drug/molecule delivery.

3D confocal Raman imaging of oil-rich emulsion from enzyme-assisted aqueous extraction of extruded soybean powder.

PubMed

Wu, Longkun; Wang, Limin; Qi, Baokun; Zhang, Xiaonan; Chen, Fusheng; Li, Yang; Sui, Xiaonan; Jiang, Lianzhou

2018-05-30

The understanding of the structure morphology of oil-rich emulsion from enzyme-assisted extraction processing (EAEP) was a critical step to break the oil-rich emulsion structure in order to recover oil. Albeit EAEP method has been applied as an alternative way to conventional solvent extraction method, the structure morphology of oil-rich emulsion was still unclear. The current study aimed to investigate the structure morphology of oil-rich emulsion from EAEP using 3D confocal Raman imaging technique. With increasing the enzymatic hydrolysis duration from 1 to 3 h, the stability of oil-rich emulsion was decreased as visualized in the 3D confocal Raman images that the protein and oil were mixed together. The subsequent Raman spectrum analysis further revealed that the decreased stability of oil-rich emulsion was due to the protein aggregations via SS bonds or protein-lipid interactions. The conformational transfer in protein indicated the formation of a compact structure. Copyright © 2017 Elsevier Ltd. All rights reserved.

Rejuvenation of Spent Media via Supported Emulsion Liquid Membranes

NASA Technical Reports Server (NTRS)

Wiencek, John M.

2002-01-01

The overall goal of this project was to maximize the reuseability of spent fermentation media. Supported emulsion liquid membrane separation, a highly efficient extraction technique, was used to remove inhibitory byproducts during fermentation; thus, improve the yield while reducing the need for fresh water. The key objectives of this study were: (1) Develop an emulsion liquid membrane system targeting low molecular weight organic acids which has minimal toxicity on a variety of microbial systems. (2) Conduct mass transfer studies to allow proper modeling and design of a supported emulsion liquid membrane system. (3) Investigate the effect of gravity on emulsion coalescence within the membrane unit. (4) Access the effect of water re-use on fermentation yields in a model microbial system. and (5) Develop a perfusion-type fermentor utilizing a supported emulsion liquid membrane system to control inhibitory fermentation byproducts (not completed due to lack of funds)

Dynamically reconfigurable complex emulsions via tunable interfacial tensions

PubMed Central

Zarzar, Lauren D.; Sresht, Vishnu; Sletten, Ellen M.; Kalow, Julia A.; Blankschtein, Daniel; Swager, Timothy M.

2015-01-01

Emulsification is a powerful, well-known technique for mixing and dispersing immiscible components within a continuous liquid phase. Consequently, emulsions are central components of medicine, food and performance materials. Complex emulsions, including multiple emulsions and Janus droplets which contain hemispheres of differing material, are of increasing importance1 in pharmaceuticals and medical diagnostics2, in the fabrication of microparticles and capsules3–5 for food6, in chemical separations7, in cosmetics8, and in dynamic optics9. Because complex emulsion properties and functions are related to the droplet geometry and composition, the development of rapid, simple fabrication approaches allowing precise control over the droplets’ physical and chemical characteristics is critical. Significant advances in the fabrication of complex emulsions have been made using a number of procedures, ranging from large-scale, less precise techniques that give compositional heterogeneity using high-shear mixers and membranes10, to small-volume but more precise microfluidic methods11,12. However, such approaches have yet to create droplet morphologies that can be controllably altered after emulsification. Reconfigurable complex liquids potentially have greatly increased utility as dynamically tunable materials. Here we describe an approach to the one-step fabrication of three- and four-phase complex emulsions with highly controllable and reconfigurable morphologies. The fabrication makes use of the temperature-sensitive miscibility of hydrocarbon, silicone and fluorocarbon liquids, and is applied to both the microfluidic and the scalable batch production of complex droplets. We demonstrate that droplet geometries can be alternated between encapsulated and Janus configurations by varying the interfacial tensions using hydrocarbon and fluorinated surfactants including stimuli-responsive and cleavable surfactants. This yields a generalizable strategy for the fabrication of multiphase emulsions with controllably reconfigurable morphologies and the potential to create a wide range of responsive materials. PMID:25719669

Dynamically reconfigurable complex emulsions via tunable interfacial tensions.

PubMed

Zarzar, Lauren D; Sresht, Vishnu; Sletten, Ellen M; Kalow, Julia A; Blankschtein, Daniel; Swager, Timothy M

2015-02-26

Emulsification is a powerful, well-known technique for mixing and dispersing immiscible components within a continuous liquid phase. Consequently, emulsions are central components of medicine, food and performance materials. Complex emulsions, including Janus droplets (that is, droplets with faces of differing chemistries) and multiple emulsions, are of increasing importance in pharmaceuticals and medical diagnostics, in the fabrication of microparticles and capsules for food, in chemical separations, in cosmetics, and in dynamic optics. Because complex emulsion properties and functions are related to the droplet geometry and composition, the development of rapid, simple fabrication approaches allowing precise control over the droplets' physical and chemical characteristics is critical. Significant advances in the fabrication of complex emulsions have been made using a number of procedures, ranging from large-scale, less precise techniques that give compositional heterogeneity using high-shear mixers and membranes, to small-volume but more precise microfluidic methods. However, such approaches have yet to create droplet morphologies that can be controllably altered after emulsification. Reconfigurable complex liquids potentially have great utility as dynamically tunable materials. Here we describe an approach to the one-step fabrication of three- and four-phase complex emulsions with highly controllable and reconfigurable morphologies. The fabrication makes use of the temperature-sensitive miscibility of hydrocarbon, silicone and fluorocarbon liquids, and is applied to both the microfluidic and the scalable batch production of complex droplets. We demonstrate that droplet geometries can be alternated between encapsulated and Janus configurations by varying the interfacial tensions using hydrocarbon and fluorinated surfactants including stimuli-responsive and cleavable surfactants. This yields a generalizable strategy for the fabrication of multiphase emulsions with controllably reconfigurable morphologies and the potential to create a wide range of responsive materials.

Dynamically reconfigurable complex emulsions via tunable interfacial tensions

NASA Astrophysics Data System (ADS)

Zarzar, Lauren D.; Sresht, Vishnu; Sletten, Ellen M.; Kalow, Julia A.; Blankschtein, Daniel; Swager, Timothy M.

2015-02-01

Emulsification is a powerful, well-known technique for mixing and dispersing immiscible components within a continuous liquid phase. Consequently, emulsions are central components of medicine, food and performance materials. Complex emulsions, including Janus droplets (that is, droplets with faces of differing chemistries) and multiple emulsions, are of increasing importance in pharmaceuticals and medical diagnostics, in the fabrication of microparticles and capsules for food, in chemical separations, in cosmetics, and in dynamic optics. Because complex emulsion properties and functions are related to the droplet geometry and composition, the development of rapid, simple fabrication approaches allowing precise control over the droplets' physical and chemical characteristics is critical. Significant advances in the fabrication of complex emulsions have been made using a number of procedures, ranging from large-scale, less precise techniques that give compositional heterogeneity using high-shear mixers and membranes, to small-volume but more precise microfluidic methods. However, such approaches have yet to create droplet morphologies that can be controllably altered after emulsification. Reconfigurable complex liquids potentially have great utility as dynamically tunable materials. Here we describe an approach to the one-step fabrication of three- and four-phase complex emulsions with highly controllable and reconfigurable morphologies. The fabrication makes use of the temperature-sensitive miscibility of hydrocarbon, silicone and fluorocarbon liquids, and is applied to both the microfluidic and the scalable batch production of complex droplets. We demonstrate that droplet geometries can be alternated between encapsulated and Janus configurations by varying the interfacial tensions using hydrocarbon and fluorinated surfactants including stimuli-responsive and cleavable surfactants. This yields a generalizable strategy for the fabrication of multiphase emulsions with controllably reconfigurable morphologies and the potential to create a wide range of responsive materials.

Development of Large Area Emulsion Chamber Methods with a Super Conducting Magnet for Observation of Cosmic Ray Nuclei from 1 GeV to 1,000 TeV (Emulsion Techniques)

NASA Technical Reports Server (NTRS)

Takahashi, Yoshiyuki; Gregory, John C.; Tominaga, Taka; Dong, Bei Lei

1997-01-01

The research developed the fundamental techniques of the emulsion chamber methods that permit measurements of the composition and energy spectra of cosmic rays at energies ranging from 1 GeV/n to over 1,000 TeV/n. The research program consisted of exploring new principles and techniques in measuring very high energy cosmic nuclei with large-area emulsion chambers for high statistics experiments. These tasks have been accomplished and their use was essential in successful analysis of the balloon-borne emulsion chamber experiments up to 10(exp 14) eV. It also provided the fundamental technologies for designing large-area detectors that are aimed at measuring the composition at above 1015 eV region. The latter is now partially succeeded by a NASA Mission Concept, Advanced Cosmic Composition Experiments on the Space Station (ACCESS). The cosmic ray group at the University of Alabama in Huntsville has performed technological R & D as well as contributing to the Japanese-American-Emulsion-Chamber-Experiments (JACEE) Collaboration with the regular data analysis. While primary research support for other institutions' efforts in the JACEE experiments came from NSF and DOE, primary support for the University of Alabama in Huntsville was this contract. Supplemental tasks to standardize the data base and hardware upgrades (automatized microscope) had this institutions cooperation. Investigation of new techniques in this program consisted of development of a fast calorimetry, magnetic/scattering selection of high momentum tracks for a pairmeter, and high statistics momentum measurements for low energy nuclei (E < 1 TeV/n). The highest energy calorimetry and a pairmeter have been considered as strawman instruments by the GOAL (Galactic Origin and Acceleration Limit) proposal of the NASA Cosmic Ray Working Group for long- duration balloon flights. We accomplished the objectives of the GOAL program with three circumpolar, Antarctic JACEE balloon flights during 1992 - 1994.

Study on preparation and formation mechanism of n-alkanol/water emulsion using alpha-cyclodextrin.

PubMed

Hashizaki, Kaname; Kageyama, Takashi; Inoue, Motoki; Taguchi, Hiroyuki; Ueda, Haruhisa; Saito, Yoshihiro

2007-11-01

Surfactants are usually used for the preparation of emulsions; however, some have an adverse effect on the human body such as skin irritation, hemolysis, and protein denaturation, etc. In this study, we examined the preparation and formation mechanism of n-alkanol/water emulsions using alpha-cyclodextrin (alpha-CD) as an emulsifier. Emulsions were prepared by mixing oil and water phases for 4 min at 2500 rpm using a vortex mixer. The mechanism of emulsification was investigated with some physico-chemical techniques. From phase diagrams of n-alkanol/alpha-CD/water systems, the emulsion phase extended as the chain length of n-alkanols and the amount of alpha-CD added increased. Furthermore, the emulsion was not formed in the region where the n-alkanol/alpha-CD complex didn't precipitate; however, the emulsion was formed in the region where the complex precipitated. In addition, it was clear that the emulsions have a yield stress value and correspond to the Maxwell model from rheological measurement. Our experiments clearly showed that the stable emulsions are formed because the precipitated complexes form a dense film at the oil-water interface and prevent aggregation among dispersed phases. Furthermore, it is suggested that the creation of a three-dimensional network structure formed by precipitated complexes in the continuous phase contributes to the stabilization of the emulsion. Thus, we concluded that the n-alkanol/water emulsions using alpha-cyclodextrin were a kind of the Pickering emulsion.

Asymmetric flow field flow fractionation for the characterization of globule size distribution in complex formulations: A cyclosporine ophthalmic emulsion case.

PubMed

Qu, Haiou; Wang, Jiang; Wu, Yong; Zheng, Jiwen; Krishnaiah, Yellela S R; Absar, Mohammad; Choi, Stephanie; Ashraf, Muhammad; Cruz, Celia N; Xu, Xiaoming

2018-03-01

Commonly used characterization techniques such as cryogenic-transmission electron microscopy (cryo-TEM) and batch-mode dynamic light scattering (DLS) are either time consuming or unable to offer high resolution to discern the poly-dispersity of complex drug products like cyclosporine ophthalmic emulsions. Here, a size-based separation and characterization method for globule size distribution using an asymmetric flow field flow fractionation (AF4) is reported for comparative assessment of cyclosporine ophthalmic emulsion drug products (model formulation) with a wide size span and poly-dispersity. Cyclosporine emulsion formulations that are qualitatively (Q1) and quantitatively (Q2) the same as Restasis® were prepared in house with varying manufacturing processes and analyzed using the optimized AF4 method. Based on our results, the commercially available cyclosporine ophthalmic emulsion has a globule size span from 30 nm to a few hundred nanometers with majority smaller than 100 nm. The results with in-house formulations demonstrated the sensitivity of AF4 in determining the differences in the globule size distribution caused by the changes to the manufacturing process. It is concluded that the optimized AF4 is a potential analytical technique for comprehensive understanding of the microstructure and assessment of complex emulsion drug products with high poly-dispersity. Published by Elsevier B.V.

Generation of colloidal granules and capsules from double emulsion drops

NASA Astrophysics Data System (ADS)

Hess, Kathryn S.

Assemblies of colloidal particles are extensively used in ceramic processing, pharmaceuticals, inks and coatings. In this project, the aim was to develop a new technique to fabricate monodispersed colloidal assemblies. The use of microfluidic devices and emulsion processing allows for the fabrication of complex materials that can be used in a variety of applications. A microfluidic device is used to create monodispersed water/oil/water (w/o/w) double emulsions with interior droplets of colloidal silica suspension ranging in size from tens to hundreds of microns. By tailoring the osmotic pressure using glycerol as a solute in the continuous and inner phases of the emulsion, we can control the final volume size of the monodispersed silica colloidal crystals that form in the inner droplets of the double emulsion. Modifying the ionic strength in the colloidal dispersion can be used to affect the particle-particle interactions and crystal formation of the final colloidal particle. This w/o/w technique has been used with other systems of metal oxide colloids and cellulose nanocrystals. Encapsulation of the colloidal suspension in a polymer shell for the generation of ceramic-polymer core-shell particles has also been developed. These core-shell particles have spawned new research in the field of locally resonant acoustic metamaterials. Systems and chemistries for creating cellulose hydrogels within the double emulsions have also been researched. Water in oil single emulsions and double emulsions have been used to create cellulose hydrogel spheres in the sub-100 micron diameter range. Oil/water/oil double emulsions allow us to create stable cellulose capsules. The addition of a second hydrogel polymer, such as acrylate or alginate, further strengthens the cellulose gel network and can also be processed into capsules and particles using the microfluidic device. This work could have promising applications in acoustic metamaterials, personal care products, pharmaceuticals, and agricultural applications, among others.

[Effect of techniques of composite resin insertion and polymerization on microleakage and microhardness].

PubMed

Amaral, Cristiane Mariote; Castro, Ana Karina Barbieri Bedran de; Pimenta, Luiz André Freire; Ambrosano, Glaucia Maria Boni

2002-01-01

The aim of this study was to evaluate the influence of techniques of composite resin polymerization and insertion on microleakage and microhardness. One hundred and eighty class II cavities were prepared in bovine teeth and assigned to six groups: G1 - bulk filling + conventional polymerization; G2 - bucco-lingual increments + conventional polymerization; G3 - bulk filling + soft-start polymerization; G4 - bucco-lingual increments + soft-start polymerization; G5 - bulk filling + progressive polymerization; G6 - bucco-lingual increments + progressive polymerization. All cavities were restored with the Z100/Single Bond system (3M). After thermocycling, the samples were immersed in 2% methylene blue dye solution for 4 hours. Half of the samples were embedded in polystyrene resin, and Knoop microhardness was measured. The Kruskal-Wallis test did not reveal statistical differences (p > 0.05) between the polymerization and insertion techniques as to microleakage. Regarding microhardness, the two-way ANOVA and the Tukey test did not reveal statistical differences between the restorative techniques (p > 0.05), but progressive polymerization (G5 and G6) was associated with smaller Knoop microhardness values (p < 0.05): G = 144.11; G2 = 143.89; G3 = 141.14; G4 = 142.79; G5 = 132.15; G6 = 131.67. It was concluded that the evaluated polymerization and insertion techniques did not affect marginal microleakage, but a decrease in microhardness occurred when progressive polymerization was carried out.

OPERA experiment and its releted emulsion techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ariga, Akitaka

2008-02-21

The OPERA experiment is designed to clarify neutrino oscillation by detecting appearance of {nu}{sub {tau}} in pure {nu}{sub {mu}} beam through a long baseline method (CNGS beam from cern to the Gran Sasso laboratory). The key technique is the use of emulsion films and their scanning. We developed a new high speed scanning system with speed of 50 cm{sup 2}/h and it was successfully demonstrated in 2006 CNGS commissioning. The new scanning system is not only meant for the OPERA experiment, but it has large potential of applications. For example, measurement of {nu}{sub e} with strong separation power against {pi}{supmore » 0}. Or a compact emulsion spectrometer for future neutrino experiments.« less

One-dimensional, two-dimensional, and three-dimensional photonic crystals fabricated with interferometric techniques on ultrafine-grain silver halide emulsions

NASA Astrophysics Data System (ADS)

Ulibarrena, Manuel; Carretero, Luis; Acebal, Pablo; Madrigal, Roque; Blaya, Salvador; Fimia, Antonio

2004-09-01

Holographic techniques have been used for manufacturing multiple band one-dimensional, two-dimensional, and three-dimensional photonic crystals with different configurations, by multiplexing reflection and transmission setups on a single layer of holographic material. The recording material used for storage is an ultra fine grain silver halide emulsion, with an average grain size around 20 nm. The results are a set of photonic crystals with the one-dimensional, two-dimensional, and three-dimensional index modulation structure consisting of silver halide particles embedded in the gelatin layer of the emulsion. The characterisation of the fabricated photonic crystals by measuring their transmission band structures has been done and compared with theoretical calculations.

Effect of high hydrostatic pressure and high dynamic pressure on stability and rheological properties of model oil-in-water emulsions

NASA Astrophysics Data System (ADS)

Bigikocin, Erman; Mert, Behic; Alpas, Hami

2011-09-01

Both static and dynamic high pressure applications provide interesting modifications in food structures which lead to new product formulations. In this study, the effects of two different treatments, high hydrostatic pressure (HHP) and high dynamic pressure (HDP), on oil-in-water emulsions were identified and compared. Microfluidization was selected from among the HDP homogenization techniques. The performance of each process was analyzed in terms of rheological modifications and emulsion stability improvements compared with the coarse emulsions. The stability of the emulsions was determined comparatively by using an analytical photo-centrifuge device employing novel analysis technology. Whey protein isolate (WPI) in combination with a food polysaccharide (xanthan gum, guar gum or locust bean gum) were used as emulsifying and stabilizing ingredients. The effective disruption of oil droplets and the degradation of polysaccharides by the shear forces under high pressure in HDP microfluidization yielded finer emulsions with lower viscosities, leading to distinctive improvements in emulsion stability. On the other hand, improvements in stability obtained with HHP treatment were due to the thickening of the emulsions mainly induced by protein unfolding. The corresponding increases in viscosity were intensified in emulsion formulations containing higher oil content. Apart from these, HHP treatment was found to be relatively more contributive to the enhancements in viscoelastic properties.

Nanoscale and Microscale Iron Emulsions for Treating DNAPL

NASA Technical Reports Server (NTRS)

Geiger, Cherie L.

2002-01-01

This study demonstrated the feasibility of using emulsified nanoscale and microscale iron particles to enhance dehalogenation of (Dense Non-Aqueous Phase Liquid) DNAPL free-phase. The emulsified system consisted of a surfactant-stabilized, biodegradable oil-in-water emulsion with nanoscale or microscale iron particles contained within the emulsion droplets. It was demonstrated that DNAPLs, such as trichloroethene (TCE), diffuse through the oil membrane of the emulsion particle whereupon they reach an aqueous interior and the surface of an iron particle where dehalogenation takes place. The hydrocarbon reaction by-products of the dehalogenation reaction, primarily ethene (no chlorinated products detected), diffuse out of the emulsion droplet. This study also demonstrated that an iron-emulsion system could be delivered in-situ to the DNAPL pool in a soil matrix by using a simulated push well technique. Iron emulsions degraded pure TCE at a rate comparable to the degradation of dissolved phase TCE by iron particles, while pure iron had a very low degradation rate for free-phase TCE. The iron-emulsion systems can be injected into a sand matrix where they become immobilized and are not moved by flowing water. It has been documented that surfactant micelles possess the ability to pull pooled TCE into emulsion droplets where degradation of TCE takes place.

Thermal stability and mechanism of decomposition of emulsion explosives in the presence of pyrite.

PubMed

Xu, Zhi-Xiang; Wang, Qian; Fu, Xiao-Qi

2015-12-30

The reaction of emulsion explosives (ammonium nitrate) with pyrite was studied using techniques of TG-DTG-DTA. TG-DSC-MS was also used to analyze samples thermal decomposition process. When a mixture of pyrite and emulsion explosives was heated at a constant heating rate of 10K/min from room temperature to 350°C, exothermic reactions occurred at about 200°C. The essence of reaction between emulsion explosives and pyrite is the reaction between ammonium nitrate and pyrite. Emulsion explosives have excellent thermal stability but it does not mean it showed the same excellent thermal stability when pyrite was added. Package emulsion explosives were more suitable to use in pyrite shale than bulk emulsion explosives. The exothermic reaction was considered to take place between ammonium nitrate and pyrite where NO, NO2, NH3, SO2 and N2O gases were produced. Based on the analysis of the gaseous, a new overall reaction was proposed, which was thermodynamically favorable. The results have significant implication in the understanding of stability of emulsion explosives in reactive mining grounds containing pyrite minerals. Copyright © 2015 Elsevier B.V. All rights reserved.

Formulation and evaluation of carrot seed oil-based cosmetic emulsions.

PubMed

Singh, Shalini; Lohani, Alka; Mishra, Arun Kumar; Verma, Anurag

2018-05-08

The present study deals with the evaluation of antiaging potential of carrot seed oil-based cosmetic emulsions. Briefly, cosmetic emulsions composed of carrot seed oil in varying proportions (2, 4, and 6% w/v) were prepared using the hydrophile-lipophile balance (HLB) technique. Coconut oil, nonionic surfactants (Tween 80 and Span 80), and xanthan gum were used as the oil phase, emulgent, and emulsion stabilizer, respectively. The formed emulsions were evaluated for various physical, chemical, and biochemical parameters such as the zeta potential, globule size measurement, antioxidant activity, sun protection factor (SPF), skin irritation, and biochemical studies. The zeta potential values ranged from -43.2 to -48.3, indicating good stability. The polydispersity index (PDI) of various emulsion formulations ranged from 0.353 to 0.816. 1,1-Diphenyl-2-picrylhydrazyl- (DPPH) and nitric oxide-free radical scavenging activity showed the antioxidant potential of the prepared carrot seed oil emulsions. The highest SPF value (6.92) was shown by F3 having 6%w/v carrot seed oil. Histopathological data and biochemical analysis (ascorbic acid (ASC) and total protein content) suggest that these cosmetic emulsions have sufficient potential to be used as potential skin rejuvenating preparations.

Efficiency of emulsifier-free emulsions and emulsions containing rapeseed lecithin as delivery systems for vectorization and release of coenzyme Q10: physico-chemical properties and in vitro evaluation.

PubMed

Kaci, M; Arab-Tehrany, E; Dostert, G; Desjardins, I; Velot, E; Desobry, S

2016-11-01

To improve the encapsulation and release of coenzyme Q10 (CoQ10), emulsifier-free-emulsions were developed with a new emulsification process using high-frequency ultrasound (HFU) at 1.7MHz. Nano-emulsions containing CoQ10 were prepared with or without rapeseed lecithin as an emulsifier. The emulsions prepared with HFU were compared with an emulsion of CoQ10 containing emulsifier prepared with the same emulsification technique as well as with emulsions prepared with low-frequency ultrasound coupled with high-pressure homogenization (LFU+HPH). The physico-chemical properties of the emulsions were determined by average droplet size measurement with nano-droplet tracking analysis, droplet surface charge with ζ potential measurement, surface tension and rheological behaviour. Emulsions made by LFU+HPH with an emulsifier showed lower droplet sizes due to cavitation generated by the HFU process. Surface tension results showed that there was no significant difference between emulsions containing lecithin emulsifier regardless of the preparation process or the inclusion of CoQ10. In vitro biocompatibility tests were performed on human mesenchymal stem cells in order to show the cytotoxicity of various formulations and the efficiency of CoQ10-loaded emulsions. In vitro tests proved that the vectors were not toxic. Furthermore, CoQ10 facilitated a high rate of cell proliferation and metabolic activity especially when in an emulsifier-free formulation. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis and Characterization of Graphene Oxide-Polystyrene Composite Capsules with Aqueous Cargo via a Water-Oil-Water Multiple Emulsion Templating Route.

PubMed

Ali, Muthana; McCoy, Thomas M; McKinnon, Ian R; Majumder, Mainak; Tabor, Rico F

2017-05-31

Graphene oxide/polystyrene (GO/PS) nanocomposite capsules containing a two-compartment cargo have been successfully fabricated using a Pickering emulsion strategy. Highly purified GO sheets with typically micrometer-scale lateral dimensions and amphiphilic characteristics were prepared from the oxidation reaction of graphite with concomitant exfoliation of the graphite structure. These GO sheets were employed as a stabilizer for oil-in-water emulsions where the oil phase comprised toluene or olive oil. The stability and morphology of the emulsions were extensively studied as a function of different parameters including GO concentration, aqueous phase pH, ultrasonication time, effects of added electrolytes and stability to dilution. In selected conditions, the olive oil emulsions showed spontaneous formation of multiple w/o/w emulsions with high stability, whereas toluene formed simple o/w emulsions of lower overall stability. Olive oil emulsions were therefore used to prepare capsules templated from emulsion droplets by surrounding the oil phase with a GO/PS shell. The GO sheets, emulsions and composite capsules were characterized using a variety of physical and spectroscopic techniques in order to unravel the interactions responsible for capsule formation. The ability of the capsules to control the release of a model active agent in the form of a hydrophilic dye was explored, and release kinetics were monitored using UV-visible spectroscopy to obtain rate parameters. The composite capsules showed promising sustained release properties, with release rates 11× lower than the precursor GO-stabilized multiple emulsion droplets.

Fabricating core (Au)-shell (different stimuli-responsive polymers) nanoparticles via inverse emulsion polymerization: Comparing DOX release behavior in dark room and under NIR lighting.

PubMed

Mazloomi-Rezvani, Mahsa; Salami-Kalajahi, Mehdi; Roghani-Mamaqani, Hossein

2018-06-01

Different core-shell nanoparticles with Au as core and stimuli-responsive polymers such as poly(acrylic acid) (PAA), poly(methacrylic acid) (PMAA), poly(N-isopropylacrylamide) (PNIPAAm), poly(N,N'-methylenebis(acrylamide)) (PMBA), poly(2-hydroxyethyl methacrylate) (PHEMA) and poly((2-dimethylamino)ethyl methacrylate) (PDMAEMA) as shells were fabricated via inverse emulsion polymerization. Dynamic light scattering (DLS) was used to investigate particles sizes and particle size distributions and transmission electron microscopy (TEM) was applied to observe the core-shell structure of Au-polymer nanoparticles. Also, surface charge of all samples was studied by measurement of zeta potentials. Synthesized core-shell nanoparticles were utilized as nanocarriers of DOX as anti-cancer drug and drug release behaviors were investigated in dark room and under irradiation of near-infrared (NIR) light. Results showed that all core-shell samples have particle sizes less than 100 nm with narrow particle size distributions. Moreover, amount of drug loading decreased by increasing zeta potential. In dark room, lower pH resulted in higher cumulative drug release due to better solubility of DOX in acidic media. Also, NIR lighting on DOX-loaded samples led to increasing cumulative drug release significantly. However, DOX-loaded Au-PAA and Au-PMAA showed higher drug release at pH = 7.4 compared to 5.3 under NIR lighting. Copyright © 2018 Elsevier B.V. All rights reserved.

Production of exopolysaccharide from rhizobia with potential biotechnological and bioremediation applications.

PubMed

Castellane, Tereza Cristina Luque; Persona, Michelli Romanoli; Campanharo, João Carlos; de Macedo Lemos, Eliana Gertrudes

2015-03-01

The potential use of rhizobia under controlled fermentation conditions may result in the production of new extracellular polymeric substances (EPS) having novel and superior properties that will open up new areas of industrial applications and thus increase their demand. The production of EPS and the stability of emulsions formed with soybean oil, diesel oil and toluene using different concentrations of purified EPS derived from wild-type and mutant strains of Rhizobium tropici SEMIA 4077 was investigated. The EPS was defined as a heteropolysaccharide composed of six constituent monosaccharides that displayed higher intrinsic viscosity and pseudoplastic non-Newtonian fluid behavior in an aqueous solution. The ratio between the total EPS production and the cellular biomass was 76.70 for the 4077::Z04 mutant strain and only 8.10 for the wild-type strain. The EPS produced by the wild-type R. tropici SEMIA 4077 resulted in more stable emulsions with the tested toluene than xanthan gum, and the emulsification indexes with hydrocarbons and soybean oil were higher than 50%, indicating strong emulsion-stabilizing capacity. These results demonstrate that the EPS of R. tropici strains could be attractive for use in industrial and environmental applications, as it had higher intrinsic viscosity and good emulsification activity. Copyright © 2015 Elsevier B.V. All rights reserved.

Biomimetic Multilayer Nanofibrous Membranes with Elaborated Superwettability for Effective Purification of Emulsified Oily Wastewater.

PubMed

Ge, Jianlong; Jin, Qing; Zong, Dingding; Yu, Jianyong; Ding, Bin

2018-05-09

Creating a porous membrane to effectively separate the emulsified oil-in-water emulsions with energy-saving property is highly desired but remains a challenge. Herein, a multilayer nanofibrous membrane was developed with the inspiration of the natural architectures of earth for gravity-driven water purification. As a result, the obtained biomimetic multilayer nanofibrous membranes exhibited three individual layers with designed functions; they were the inorganic nanofibrous layer to block the serious intrusion of oil to prevent the destructive fouling of the polymeric matrix; the submicron porous layer with designed honeycomb-like cavities to catch the smaller oil droplets and ensures a satisfactory water permeability; and the high porous fibrous substrate with larger pore size provided a template support and allows water to pass through quickly. Consequently, with the cooperation of these three functional layers, the resultant composite membrane possessed superior anti-oil-fouling property and robust oil-in-water emulsion separation performance with good separation efficiency and competitive permeation flux solely under the drive of gravity. The permeation flux of the membrane for the emulsion was up to 5163 L m -2 h -1 with a separation efficiency of 99.5%. We anticipate that our strategy could provide a facile route for developing a new generation of specific membranes for oily wastewater remediation.

Fabrication of advanced particles and particle-based materials assisted by droplet-based microfluidics.

PubMed

Wang, Jing-Tao; Wang, Juan; Han, Jun-Jie

2011-07-04

Recent advances in the fabrication of complex particles and particle-based materials assisted by droplet-based microfluidics are reviewed. Monodisperse particles with expected internal structures, morphologies, and sizes in the range of nanometers to hundreds of micrometers have received a good deal of attention in recent years. Due to the capability of generating monodisperse emulsions and of executing precise control and operations on the suspended droplets inside the microchannels, droplet-based microfluidic devices have become powerful tools for fabricating complex particles with desired properties. Emulsions and multiple-emulsions generated in the microfluidic devices can be composed of a variety of materials including aqueous solutions, gels, polymers and solutions containing functional nanoparticles. They are ideal microreactors or fine templates for synthesizing advanced particles, such as polymer particles, microcapsules, nanocrystals, and photonic crystal clusters or beads by further chemical or physical operations. These particles are promising materials that may be applicable for many fields, such as photonic materials, drug delivery systems, and bio-analysis. From simple to complex, from spherical to nonspherical, from polymerization and reaction crystallization to self-assembly, this review aims to help readers be aware of the many aspects of this field. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Demulsification of crude oil-in-water emulsions by means of fungal spores.

PubMed

Vallejo-Cardona, Alba Adriana; Martínez-Palou, Rafael; Chávez-Gómez, Benjamín; García-Caloca, Graciela; Guerra-Camacho, Jairo; Cerón-Camacho, Ricardo; Reyes-Ávila, Jesús; Karamath, James Robert; Aburto, Jorge

2017-01-01

The present feature describes for the first time the application of spores from Aspergillus sp. IMPMS7 to break out crude oil-in-water emulsions (O/W). The fungal spores were isolated from marine sediments polluted with petroleum hydrocarbons. The spores exhibited the ability to destabilize different O/W emulsions prepared with medium, heavy or extra-heavy Mexican crude oils with specific gravities between 10.1 and 21.2°API. The isolated fungal spores showed a high hydrophobic power of 89.3 ± 1.9% and with 2 g of spores per liter of emulsion, the half-life for emulsion destabilization was roughly 3.5 and 0.7 h for extra-heavy and medium crude oil, respectively. Then, the kinetics of water separation and the breaking of the O/W emulsion prepared with heavy oil through a spectrofluorometric technique were studied. A decrease in the fluorescence ratio at 339 and 326 nm (I339/I326) was observed in emulsions treated with spores, which is similar to previously reported results using chemical demulsifiers.

Study the effect of polymers on the stability and rheological properties of oil-in-water (O/W) Pickering emulsion muds

NASA Astrophysics Data System (ADS)

Jha, Praveen Kumar; Mahto, Vikas; Saxena, Vinod Kumar

2018-05-01

A new type of oil-in-water (O/W) Pickering emulsion systems, which were prepared by polymers such as xanthan gum, carboxymethyl cellulose (CMC), and sodium lignosulfonate have been investigated for their properties as multifunctional emulsion muds with respect to rheological control and filtration control properties. Diesel oil was used as dispersed phase and KCl-brine as continuous phase in the developed emulsions. Initially, rheological parameters like apparent viscosity, plastic viscosity, gel strength, and filtration control properties were measured using recommended practices. Emulsion stability was analyzed using steady state shear stress-shear rate and oscillatory (dynamic) rheological measurement techniques. The emulsions were found to exhibit shear-thinning (pseudoplastic) behavior. Experiments conducted for oscillatory rheological measurements have shown that emulsions are stable as per the stability criteria G' (elastic modulus) > G'' (loss modulus) and both are independent of changing ω (Frequency). These fluids have shown stable properties upto 70°C which shows that they can be used as drilling muds for drilling oil and gas wells.

Demulsification of crude oil-in-water emulsions by means of fungal spores

PubMed Central

Vallejo-Cardona, Alba Adriana; Martínez-Palou, Rafael; Chávez-Gómez, Benjamín; García-Caloca, Graciela; Guerra-Camacho, Jairo; Cerón-Camacho, Ricardo; Reyes-Ávila, Jesús; Karamath, James Robert

2017-01-01

The present feature describes for the first time the application of spores from Aspergillus sp. IMPMS7 to break out crude oil-in-water emulsions (O/W). The fungal spores were isolated from marine sediments polluted with petroleum hydrocarbons. The spores exhibited the ability to destabilize different O/W emulsions prepared with medium, heavy or extra-heavy Mexican crude oils with specific gravities between 10.1 and 21.2°API. The isolated fungal spores showed a high hydrophobic power of 89.3 ± 1.9% and with 2 g of spores per liter of emulsion, the half-life for emulsion destabilization was roughly 3.5 and 0.7 h for extra-heavy and medium crude oil, respectively. Then, the kinetics of water separation and the breaking of the O/W emulsion prepared with heavy oil through a spectrofluorometric technique were studied. A decrease in the fluorescence ratio at 339 and 326 nm (I339/I326) was observed in emulsions treated with spores, which is similar to previously reported results using chemical demulsifiers. PMID:28234917

Influence of interfacial and bulk properties of cellulose ethers on lipolysis of oil-in-water emulsions.

PubMed

Torcello-Gómez, Amelia; Foster, Timothy J

2016-06-25

Cellulose ethers are usually used as secondary emulsifiers. Different types of commercial hydroxypropylmethylcellulose (HPMC) have been used here as the main emulsifier of oil-in-water emulsions to probe their impact on the lipid digestibility under simulated intestinal conditions. The droplet size distribution and ζ-potential of the emulsions subjected to in-vitro lipolysis have been compared with that of control samples (non-digested). The lipolysis has been quantified over time by means of the pH-stat method. The displacement of HPMC from the oil-water interface by bile salts has been assessed by interfacial tension technique. Results show that HPMC delays the lipid digestion of emulsions regardless of the Mw and methoxyl content. The destabilisation of emulsions under intestinal conditions as well as the resistance of HPMC to be displaced from the emulsion interface by bile salts may contribute to this feature. This provides new insights into the mechanisms whereby dietary fibre reduces fat absorption. Copyright © 2016 Elsevier Ltd. All rights reserved.

Particle Identification in Nuclear Emulsion by Measuring Multiple Coulomb Scattering

NASA Astrophysics Data System (ADS)

Than Tint, Khin; Nakazawa, Kazuma; Yoshida, Junya; Kyaw Soe, Myint; Mishina, Akihiro; Kinbara, Shinji; Itoh, Hiroki; Endo, Yoko; Kobayashi, Hidetaka; E07 Collaboration

2014-09-01

We are developing particle identification techniques for single charged particles such as Xi, proton, K and π by measuring multiple Coulomb scattering in nuclear emulsion. Nuclear emulsion is the best three dimensional detector for double strangeness (S = -2) nuclear system. We expect to accumulate about 10000 Xi-minus stop events which produce double lambda hypernucleus in J-PARC E07 emulsion counter hybrid experiment. The purpose of this particle identification (PID) in nuclear emulsion is to purify Xi-minus stop events which gives information about production probability of double hypernucleus and branching ratio of decay mode. Amount of scattering parameterized as angular distribution and second difference is inversely proportional to the momentum of particle. We produced several thousands of various charged particle tracks in nuclear emulsion stack via Geant4 simulation. In this talk, PID with some measuring methods for multiple scattering will be discussed by comparing with simulation data and real Xi-minus stop events in KEK-E373 experiment.

Tri-fuel (diesel-biodiesel-ethanol) emulsion characterization, stability and the corrosion effect

NASA Astrophysics Data System (ADS)

Low, M. H.; Mukhtar, N. A. M.; Yohaness Hagos, Ftwi; Noor, M. M.

2017-10-01

This paper presents the result of experimenting emulsified tri-fuel in term of stability, physico-chemical properties and corrosion effect on three common metals. The results were interpreted in terms of the impact of five minutes emulsification approach. Tri-fuel emulsions were varied in proportion ratio consist of biodiesel; 0%, 5%, 10%, and ethanol; 5%, 10%, 15%. Fuel characterization includes density, calorific value, flash point, and kinematic viscosity. Flash point of tri-fuel emulsion came with range catalog. Calorific value of tri-fuel emulsion appeared in declining pattern as more ethanol and biodiesel were added. Biodiesel promoted flow resistance while ethanol with opposite effect. 15% ethanol content in tri-fuel emulsion separated faster than 10% ethanol content but ethanol content with 5% yield no phase separation at all. Close cap under static immersion with various ratio of tri-fuel emulsions for over a month, corrosiveness attack was detected via weight loss technique on aluminum, stainless steel and mild steel.

Rejuvenation of Spent Media via Supported Emulsion Liquid Membranes

NASA Technical Reports Server (NTRS)

Wiencek, John M.

2002-01-01

The overall goal of this project is to maximize the reuseability of spent fermentation media. Supported emulsion liquid membrane separation, a highly efficient extraction technique, is used to remove inhibitory byproducts during fermentation; thus, improving the yield while reducing the need for fresh water. The key objectives of this study are: Develop an emulsion liquid membrane system targeting low molecular weight organic acids which has minimal toxicity on a variety of microbial systems; Conduct mass transfer studies to allow proper modeling and design of a supported emulsion liquid membrane system; Investigate the effect of gravity on emulsion coalescence within the membrane unit; Access the effect of water re-use on fermentation yields in a model microbial system; Develop a perfusion-type fermentor utilizing a supported emulsion liquid membrane system to control inhibitory fermentation byproducts; Work for the coming year will focus on the determination of toxicity of various solvents, selection of the emulsifying agents, as well as characterizing the mass transfer of hollow-fiber contactors.

New oil-in-water magnetic emulsion as contrast agent for in vivo magnetic resonance imaging (MRI).

PubMed

Ahmed, Naveed; Jaafar-Maalej, Chiraz; Eissa, Mohamed Mahmoud; Fessi, Hatem; Elaissari, Abdelhamid

2013-09-01

Nowadays, bio-imaging techniques are widely applied for the diagnosis of various diseased/tumoral tissues in the body using different contrast agents. Accordingly, the advancement in bionanotechnology research is enhanced in this regard. Among contrast agents used, superparamagnetic iron oxide nanoparticles were developed by many researchers and applied for in vive magnetic resonance imaging (MRI). In this study, a new oil-in-water magnetic emulsion was used as contrast agent in MRI, after being characterized in terms of particle size, iron oxide content, magnetic properties and colloidal stability using dynamic light scattering (DLS), thermal gravimetric analysis (TGA), vibrating sample magnetometer (VSM) and zeta potential measurement techniques, respectively. The hydrodynamic size and magnetic content of the magnetic colloidal particles were found to be 250 nm and 75 wt%, respectively. In addition, the used magnetic emulsion possesses superparamagentic properties and high colloidal stability in aqueous medium. Then, the magnetic emulsion was highly diluted and administered intravenously to the Sprague dawley rats to be tested as contrast agent for in vivo MRI. In this preliminary study, MRI images showed significant enhancement in contrast, especially for T2 (relaxation time) contrast enhancement, indicating the distribution of magnetic colloidal nanoparticles within organs, like liver, spleen and kidneys of the Sprague dawley rats. In addition, it was found that 500 microL of the highly diluted magnetic emulsion (0.05 wt%) was found adequate for MRI analysis. This seems to be useful for further investigations especially in theranostic applications of magnetic emulsion.

Synthesis, characterisation and physicochemical properties of hydrophobically modified inulin using long-chain fatty acyl chlorides.

PubMed

Han, Lingyu; Ratcliffe, I; Williams, P A

2017-12-15

A series of inulin derivatives were synthesized in aqueous solution using acyl chlorides with varying alkyl chain length (C10-C16). They were characterised using a number of techniques including MALDI TOF-MS, 1 H NMR and FTIR and their degree of substitution determined. The solution properties of the hydrophobically modified inulins were investigated using dye solubilisation and surface tension and it was confirmed that the molecules aggregated in solution above a critical concentration (critical aggregation concentration, CAC). The value of the CAC was found to be reasonably consistent between the different techniques and was shown to decrease with increasing hydrophobe chain length. It was found that the C10, C12 and C14 derivatives formed stable oil-in-water emulsions and the emulsion droplet size decreased with increasing alkyl chain length. The C16 derivative was not able to produce stable oil-in-water emulsions; however, it was able to form stable water-in-oil emulsions. The fact that the derivatives are able to form micellar-like aggregates and stabilise emulsions makes them suitable candidates for the encapsulation and delivery of active compounds with potential application in food, cosmetic, personal care and pharmaceutical formulations. Copyright © 2017 Elsevier Ltd. All rights reserved.

A lyophilized etoposide submicron emulsion with a high drug loading for intravenous injection: preparation, evaluation, and pharmacokinetics in rats.

PubMed

Chen, Hao; Shi, Shuai; Zhao, Mingming; Zhang, Ling; He, Haibing; Tang, Xing

2010-12-01

To develop a submicron emulsion for etoposide with a high drug loading capacity using a drug-phospholipid complex combined with drug freeze-drying techniques. An etoposide-phospholipid complex (EPC) was prepared and its structure was confirmed by X-ray diffraction and differential scanning calorimetry analysis. A freeze-drying technique was used to produce lyophilized etoposide emulsions (LEPE), and LEPE was investigated with regard to their appearance, particle size, and zeta potential. The pharmacokinetic study in vivo was determined by the UPLC/MS/MS system. It showed that EPC significantly improved the liposolubility of etoposide, indicating a high drug loading intravenous emulsion could be easily prepared by EPC. Moreover, the obtained loading of etoposide in the submicron emulsion was 3.0 mg/mL, which was three times higher than that of the previous liquid emulsions. The optimum cryoprotectant was trehalose (15%) in freeze-drying test. The median diameter, polydispersity index, and zeta potential of the optimum formulation of LEPE were 226.1 ± 5.1 nm, 0.107 ± 0.011, and -36.20 ± 1.13 mV, respectively. In addition, these parameters had no significant change during 6 months storage at 4 ± 2°C. The main pharmacokinetic parameters exhibited no significant differences between LEPE and etoposide commercial solution except for area under the concentration-time curve and clearance. The stable etoposide emulsion with a high drug loading was successfully prepared, indicating the amount of excipients such as the oil phase and emulsifiers significantly decreased following administration of the same dose of drug, effectively reducing the metabolism by patients while increasing their compliance. Therefore, LEPE has a great potential for clinical applications.

Stability of cosmetic emulsion containing different amount of hemp oil.

PubMed

Kowalska, M; Ziomek, M; Żbikowska, A

2015-08-01

The aim of the study was to determine the optimal conditions, that is the content of hemp oil and time of homogenization to obtain stable dispersion systems. For this purpose, six emulsions were prepared, their stability was examined empirically and the most correctly formulated emulsion composition was determined using a computer simulation. Variable parameters (oil content and homogenization time) were indicated by the optimization software based on Kleeman's method. Physical properties of the synthesized emulsions were studied by numerous techniques involving particle size analysis, optical microscopy, Turbiscan test and viscosity of emulsions. The emulsion containing 50 g of oil and being homogenized for 6 min had the highest stability. Empirically determined parameters proved to be consistent with the results obtained using the computer software. The computer simulation showed that the most stable emulsion should contain from 30 to 50 g of oil and should be homogenized for 2.5-6 min. The computer software based on Kleeman's method proved to be useful for quick optimization of the composition and production parameters of stable emulsion systems. Moreover, obtaining an emulsion system with proper stability justifies further research extended with sensory analysis, which will allow the application of such systems (containing hemp oil, beneficial for skin) in the cosmetic industry. © 2015 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

Drug delivery properties of macroporous polystyrene solid foams.

PubMed

Canal, Cristina; Aparicio, Rosa Maria; Vilchez, Alejandro; Esquena, Jordi; García-Celma, Maria José

2012-01-01

Polymeric porous foams have been evaluated as possible new pharmaceutical dosage forms. These materials were obtained by polymerization in the continuous phase of highly concentrated emulsions prepared by the phase inversion temperature method. Their porosity, specific surface and surface topography were characterized, and the incorporation and release of active principles was studied using ketoprofen as model lipophilic molecule. Solid foams with very high pore volume, mainly inside macropores, were obtained by this method. The pore morphology of the materials was characterized, and very rough topography was observed, which contributed to their nearly superhydrophobic properties. These solid foams could be used as delivery systems for active principles with pharmaceutical interest, and in the present work ketoprofen was used as a model lipophilic molecule. Drug incorporation and release was studied from solid foam disks, using different concentrations of the loading solutions, achieving a delayed release with short lag-time.

Biodegradable gelatin-based nanospheres as pH-responsive drug delivery systems

NASA Astrophysics Data System (ADS)

Curcio, Manuela; Altimari, Ilaria; Spizzirri, Umile Gianfranco; Cirillo, Giuseppe; Vittorio, Orazio; Puoci, Francesco; Picci, Nevio; Iemma, Francesca

2013-04-01

Native gelatin, N, N'-ethylenebisacrylamide, and sodium methacrylate were inserted into a spherical crosslinked structure by a solvent-free emulsion polymerization method, in which sunflower seed oil containing different amounts of lecithin was selected as continuous phase. Nanogels were characterized by morphological analysis, particle size distribution, and determination of swelling degree. Different dimensional distributions (100-500 nm) and water affinities were obtained by varying the amount of surfactant in the polymerization feed. Nanogels were non-toxic on human bone marrow mesenchymal stromal cells and enzymatically stable in the gastric tract, with weight losses ranging from 58 to 20 % in pancreatin solution. Release profiles of diclofenac sodium salt from the nanogels were evaluated at different pH and found to depend on crosslinking degree and drug-polymer interactions; while in pancreatin solution, a complete release of the drug was observed. The release mechanism and the diffusional contribution were evaluated by semiempirical equations.

Facile synthesis of hollow Sn-Co@PMMA nanospheres as high performance anodes for lithium-ion batteries via galvanic replacement reaction and in situ polymerization

NASA Astrophysics Data System (ADS)

Yu, Xiaohui; Jiang, Anni; Yang, Hongyan; Meng, Haowen; Dou, Peng; Ma, Daqian; Xu, Xinhua

2015-08-01

Polymethyl methacrylate (PMMA)-coated hollow Sn-Co nanospheres (Sn-Co@PMMA) with superior electrochemical performance had been synthesized via a facile galvanic replacement method followed by an in situ emulsion polymerization route. The properties were investigated in detail and results show that the hollow Sn-Co nanospheres were evenly coated with PMMA. Benefiting from the protection of the PMMA layers, the hollow Sn-Co@PMMA nanocomposite is capable of retaining a high capacity of 590 mAh g-1 after 100 cycles with a coulomb efficiency above 98%, revealing better electrochemical properties compared with hollow Sn-Co anodes. The PMMA coating could help accommodate the mechanical strain caused by volume expansion and stabilize the solid electrolyte interphase (SEI) film formed on the electrode. Such a facile process could be further extended to other anode materials for lithium-ion batteries.

Preparation and properties of PMMA nanoparticles as 3 dimensional photonic crystals and its thin film via surfactant-free emulsion polymerization

NASA Astrophysics Data System (ADS)

Tahrin, Rabiatul Addawiyah Azwa; Azma, Nur Syafiqa; Kassim, Syara; Harun, Noor Aniza

2017-09-01

3-dimensional (3D) photonic crystals have been extended use in wide research and application from material to sensor. Nanoparticles of poly (methyl methacrylate) (PMMA) latex beads have been successfully prepared by green-chemistry approach where no surfactant, linking agent and solvent were involved. Regardless of the effect of initiator in polymerization reaction, this study presents the effect of temperature, monomer concentration, stirring speed and reaction period in order to tune the particle size. Its morphology of uniformity sized-tuned was confirming by using particle size analyzer (PSA) and scanning electron microscopy (SEM). The fabrication of 3D photonic crystals film by using self-assembly method to pattern the desired PMMA layers which is the most feasible, low cost method are also presented. The detailed properties of PMMA nanoparticles from this experimental study will be discussed and its potential used in photonic application will be explained.

Process for preparation of large-particle-size monodisperse latexes

NASA Technical Reports Server (NTRS)

Vanderhoff, J. W.; Micale, F. J.; El-Aasser, M. S.; Kornfeld, D. M. (Inventor)

1981-01-01

Monodisperse latexes having a particle size in the range of 2 to 40 microns are prepared by seeded emulsion polymerization in microgravity. A reaction mixture containing smaller monodisperse latex seed particles, predetermined amounts of monomer, emulsifier, initiator, inhibitor and water is placed in a microgravity environment, and polymerization is initiated by heating. The reaction is allowed to continue until the seed particles grow to a predetermined size, and the resulting enlarged particles are then recovered. A plurality of particle-growing steps can be used to reach larger sizes within the stated range, with enlarge particles from the previous steps being used as seed particles for the succeeding steps. Microgravity enables preparation of particles in the stated size range by avoiding gravity related problems of creaming and settling, and flocculation induced by mechanical shear that have precluded their preparation in a normal gravity environment.

Polyethylenimine-immobilized core-shell nanoparticles: synthesis, characterization, and biocompatibility test.

PubMed

Ratanajanchai, Montri; Soodvilai, Sunhapas; Pimpha, Nuttaporn; Sunintaboon, Panya

2014-01-01

Herein, we prepared PEI-immobilized core-shell particles possessing various types of polymer cores via a visible light-induced surfactant-free emulsion polymerization (SFEP) of three vinyl monomers: styrene (St), methyl methacrylate (MMA), and 2-hydroxyethyl methacrylate (HEMA). An effect of monomers on the polymerization and characteristics of resulting products was investigated. Monomers with high polarity can provide high monomer conversion, high percentage of grafted PEI, stable particles with uniform size distribution but less amino groups per particles. All prepared nanoparticles exhibited a core-shell nanostructure, containing PEI on the shell with hydrodynamic size around 140-230nm. For in-vitro study in Caco-2 cells, we found that the incorporation of PEI into these core-shell nanoparticles can significantly reduce its cytotoxic effect and also be able to internalized within the cells. Accordingly, these biocompatible particles would be useful for various biomedical applications, including gene transfection and intracellular drug delivery. © 2013.

3-Dimensional Colloidal Crystals From Hollow Spheres

NASA Astrophysics Data System (ADS)

Zhang, Jian; Work, William J.; Sanyal, Subrata; Lin, Keng-Hui; Yodh, A. G.

2000-03-01

We have succeeded in synthesizing submicron-sized, hollow PMMA spheres and self-assembling them into colloidal crystalline structures using the depletion force. The resulting structures can be used as templates to make high refractive-index contrast, porous, inorganic structures without the need to use calcination or chemical-etching. With the method of emulsion polymerization, we managed to coat a thin PMMA shell around a swellable P(MMA/MAA/EGDMA) core. After neutralization and heating above the glass transition temperature of PMMA, we obtained water-swollen hydrogel particles encapsulated in PMMA shells. These composite particles become hollow spheres after drying. We characterized the particles with both transmission electron microscopy (TEM) and dynamic light scattering (DLS). The TEM results confirmed that each sphere has a hollow core. The DLS results showed that our hollow spheres are submicron-sized, with a swelling ratio of at least 25%, and with a polydispersity less than 5%. We anticipate using this method in the near-future to encapsulate ferrofluid emulsion droplets and liquid crystal droplets.

A Facile Method for Preparation of Polymer Particles Having a "Cylindrical" Shape.

PubMed

Li, Wei; Suzuki, Toyoko; Minami, Hideto

2018-06-16

A facile and novel approach to prepare monodisperse polystyrene (PS) particles having a "cylindrical" shape was discovered. The proposed synthetic method involved dispersion polymerization of the spherical PS particles stirred in a polyvinylpyrrolidone (PVP) aqueous solution for several hours using a magnetic stirrer at room temperature. In the presence of PVP, the spherical PS particles deformed into cylindrical shapes following stirring; however, the particles did not deform in the absence of PVP. The deformation rate of the particles was affected by the molecular weight of the dissolved PVP. This stirring method is not only highly efficient and provides high yield, but is also applicable to other materials such as polymethyl methacrylate. Moreover, the cylindrical particles were successfully applied as particulate surfactants in a Pickering emulsion system, which exhibited excellent stability as comparison with the system using spherical particles as a surfactant. In the latter case, the emulsion was left standing for more than 4 months. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Photo-triggered release in polyamide nanosized capsules

DOE Office of Scientific and Technical Information (OSTI.GOV)

Marturano, V.; Ambrogi, V.; Cerruti, P.

2014-05-15

In this work, nanosized capsules based on a lightly cross-linked polyamide containing azobenzene moieties in the main chain were synthesized by miniemulsion interfacial polymerization. The obtained nanocapsules were loaded either with toluene or with the fluorescent probe coumarin-6 as a core. Diameters of the nanocapsules were in the 100-900 nm range, depending on the selected emulsion conditions. The morphology and shape of the samples were observed by TEM and SEM while the emulsion droplets and nanocapsules size was measured by DLS. Under continuous UV irradiation the polymer underwent E-Z photoisomerization allowing the release of the encapsulated material. Variation in diametermore » of the nanocapsules with the time of UV irradiation was detected through DLS analysis. 10-30% growth was observed, depending on the sample. The kinetics of release of coumarin-6 was followed by spectrofluorimetry in ethanol. In absence of irradiation, the fluorescence intensity appeared to be constant over time, while it increased when the sample was irradiated with 360 nm UV light.« less

Retaining Oxidative Stability of Emulsified Foods by Novel Nonmigratory Polyphenol Coated Active Packaging.

PubMed

Roman, Maxine J; Decker, Eric A; Goddard, Julie M

2016-07-13

Oxidation causes lipid rancidity, discoloration, and nutrient degradation that decrease shelf life of packaged foods. Synthetic additives are effective oxidation inhibitors, but are undesirable to consumers who prefer "clean" label products. The aim of this study was to improve oxidative stability of emulsified foods by a novel nonmigratory polyphenol coated active packaging. Polyphenol coatings were applied to chitosan functionalized polypropylene (PP) by laccase assisted polymerization of catechol and catechin. Polyphenol coated PP exhibited both metal chelating (39.3 ± 2.5 nmol Fe(3+) cm(-2), pH 4.0) and radical scavenging (up to 52.9 ± 1.8 nmol Trolox eq cm(-2)) capacity, resulting in dual antioxidant functionality to inhibit lipid oxidation and lycopene degradation in emulsions. Nonmigratory polyphenol coated PP inhibited ferric iron promoted degradation better than soluble chelators, potentially by partitioning iron from the emulsion droplet interface. This work demonstrates that polyphenol coatings can be designed for advanced material chemistry solutions in active food packaging.

Synthesis and Evaluation of a Molecularly Imprinted Polymer for the Determination of Metronidazole in Water Samples.

PubMed

de León-Martínez, L Díaz; Rodríguez-Aguilar, M; Ocampo-Pérez, R; Gutiérrez-Hernández, J M; Díaz-Barriga, F; Batres-Esquivel, L; Flores-Ramírez, R

2018-03-01

A molecularly imprinted polymer was developed and evaluated for selective determination of metronidazole (MNZ) in wastewater. This was achieved by using sodium methacrylate as monomer, toluene as porogen, ethylene glycol dimethacrylate as crosslinker, azobisisobutyronitrile as initiator and metronidazole as template molecule to generate the selectivity of the polymer for the compound, as well as non-imprinted polymers were synthesized. Two different polymerization approaches were used, bulk and emulsion and the polymers obtained by emulsion presented higher retention percentages the MIP 2-M presented the higher retention (83%). The performed method, was validated in fortified water, showing linearity from 10 up to 1000 ng/mL; limit of detection and quantification for compound were between 3 and 10 ng/mL, respectively. Finally, the method was applied in samples of a wastewater treatment plant in the city of San Luis Potosí, México, and the concentrations of MNZ in these samples were 84.1-114 ng/mL.

In vitro evaluation of suspoemulsions for in situ-forming polymeric microspheres and controlled release of progesterone.

PubMed

Turino, Ludmila N; Mariano, Rodolfo N; Mengatto, Luciano N; Luna, Julio A

2015-01-01

One possibility to obtain a higher dose of drug in a lower formulation volume can be by using of saturated quantity of drug in one of the phases of an emulsion. These formulations are called suspoemulsions (S/O/W). When a hydrophobic polymer is added to the organic phase of suspoemulsions, these formulations can be used to entrap the drug inside microspheres after in situ precipitation of the polymer-drug-excipients mix. In this work, performance and stability of progesterone suspensions in triacetin as organic phase of suspoemulsions were evaluated. These formulations were compared with O/W emulsions. Mathematical models were used to study in vitro release profiles. The results confirmed that S/O/W systems could be an attractive alternative to O/W formulations for the entrapment of progesterone inside poly(d,l-lactide-co-glycolide) microspheres. Diffusive-based models fit the in vitro release of progesterone from in situ-formed microspheres. For longer release periods, a time-dependent diffusion coefficient was successfully estimated.

Microcapsule and methods of making and using microcapsules

DOEpatents

Okawa, David C.; Pastine, Stefan J.; Zettl, Alexander K.; Frechet, Jean M.J.

2014-09-02

An embodiment of a microcapsule includes a shell surrounding a space, a liquid within the shell, and a light absorbing material within the liquid. An embodiment of a method of making microcapsules includes forming a mixture of a light absorbing material and an organic solution. An emulsion of the mixture and an aqueous solution is then formed. A polymerization agent is added to the emulsion, which causes microcapsules to be formed. Each microcapsule includes a shell surrounding a space, a liquid within the shell, and light absorbing material within the liquid. An embodiment of a method of using microcapsules includes providing phototriggerable microcapsules within a bulk material. Each of the phototriggerable microcapsules includes a shell surrounding a space, a chemically reactive material within the shell, and a light absorbing material within the shell. At least some of the phototriggerable microcapsules are exposed to light, which causes the chemically reactive material to release from the shell and to come into contact with bulk material.

A New Adjuvant Combined with Inactivated Influenza Enhances Specific CD8 T Cell Response in Mice and Decreases Symptoms in Swine Upon Challenge.

PubMed

Bouguyon, Edwige; Goncalves, Elodie; Shevtsov, Alexander; Maisonnasse, Pauline; Remyga, Stepan; Goryushev, Oleg; Deville, Sebastien; Bertho, Nicolas; Ben Arous, Juliette

2015-11-01

Vaccination is the most effective way to control swine influenza virus (SIV) in the field. Classical vaccines are based on inactivated antigens formulated with an oil emulsion or a polymeric adjuvant. Standard adjuvants enhance the humoral response and orient the immune response toward a Th2 response. An important issue is that current vaccines do not protect against new strains. One approach to improve cross-protection is to enhance Th1 and cytotoxic responses. The development of adjuvants orienting the immune response of inactivated vaccines toward Th1/Cytotoxic responses would be highly beneficial. This study shows that the water in oil in water emulsion adjuvant Montanide™ ISA 201 VG allows the induction of anti-influenza CD8 T cell in mice and induces homologous protection against an H1N1 challenge in swine. Such adjuvants that induce both humoral and cell-mediated immunity could improve the protection conferred by SIV vaccines in the field.

Comparative study of DNA encapsulation into PLGA microparticles using modified double emulsion methods and spray drying techniques.

PubMed

Oster, C G; Kissel, T

2005-05-01

Recently, several research groups have shown the potential of microencapsulated DNA as adjuvant for DNA immunization and in tissue engineering approaches. Among techniques generally used for microencapsulation of hydrophilic drug substances into hydrophobic polymers, modified WOW double emulsion method and spray drying of water-in-oil dispersions take a prominent position. The key parameters for optimized microspheres are particle size, encapsulation efficiency, continuous DNA release and stabilization of DNA against enzymatic and mechanical degradation. This study investigates the possibility to encapsulate DNA avoiding shear forces which readily degrade DNA during this microencapsulation. DNA microparticles were prepared with polyethylenimine (PEI) as a complexation agent for DNA. Polycations are capable of stabilizing DNA against enzymatic, as well as mechanical degradation. Further, complexation was hypothesized to facilitate the encapsulation by reducing the size of the macromolecule. This study additionally evaluated the possibility of encapsulating lyophilized DNA and lyophilized DNA/PEI complexes. For this purpose, the spray drying and double emulsion techniques were compared. The size of the microparticles was characterized by laser diffractometry and the particles were visualized by scanning electron microscopy (SEM). DNA encapsulation efficiencies were investigated photometrically after complete hydrolysis of the particles. Finally, the DNA release characteristics from the particles were studied. Particles with a size of <10 microm which represent the threshold for phagocytic uptake could be prepared with these techniques. The encapsulation efficiency ranged from 100-35% for low theoretical DNA loadings. DNA complexation with PEI 25?kDa prior to the encapsulation process reduced the initial burst release of DNA for all techniques used. Spray-dried particles without PEI exhibited high burst releases, whereas double emulsion techniques showed continuous release rates.

Preparation and Characterization of Mesoporous Zirconia Made by Using a Poly (methyl methacrylate) Template

NASA Astrophysics Data System (ADS)

Duan, Guorong; Zhang, Chunxiang; Li, Aimei; Yang, Xujie; Lu, Lude; Wang, Xin

2008-03-01

Superfine powders of poly (methyl methacrylate) (PMMA) have been prepared by means of an emulsion polymerization method. These have been used as templates in the synthesis of tetragonal phase mesoporous zirconia by the sol gel method, using zirconium oxychloride and oxalic acid as raw materials. The products have been characterized by infrared spectroscopy, X-ray diffraction analysis, transmission electron microscopy, N2 adsorption-desorption isotherms, and pore size distribution. The results indicate that the average pore size was found to be 3.7 nm.

Synthesis of Size-Tunable CO2-Philic Imprinted Polymeric Particles (MIPs) for Low-Pressure CO2 Capture Using Oil-in-Oil Suspension Polymerization.

PubMed

Nabavi, Seyed Ali; Vladisavljević, Goran T; Zhu, Yidi; Manović, Vasilije

2017-10-03

Highly selective molecularly imprinted poly[acrylamide-co-(ethylene glycol dimethacrylate)] polymer particles (MIPs) for CO 2 capture were synthesized by suspension polymerization via oil-in-oil emulsion. Creation of CO 2 -philic, amide-decorated cavities in the polymer matrix led to a high affinity to CO 2 . At 0.15 bar CO 2 partial pressure, the CO 2 /N 2 selectivity was 49 (corresponding to 91% purity of the gas stream after regeneration), and reached 97 at ultralow CO 2 partial pressures. The imprinted polymers showed considerably higher CO 2 uptakes compared to their nonimprinted counterparts, and the maximum equilibrium CO 2 capture capacity of 1.1 mmol g -1 was achieved at 273 K. The heat of adsorption was below 32 kJ mol -1 and the temperature of onset of intense thermal degradation was 351-376 °C. An increase in monomer-to-cross-linker molar ratio in the dispersed phase up to 1:2.5 led to a higher affinity toward CO 2 due to higher density of selective amide groups in the polymer network. MIPs are a promising option for industrial packed and fluidized bed CO 2 capture systems due to large particles with a diameter up to 1200 μm and irregular oblong shapes formed due to arrested coalescence during polymerization, occurring as a result of internal elasticity of the partially polymerized semisolid drops.

Discovery of naked charm particles and lifetime differences among charm species using nuclear emulsion techniques innovated in Japan

PubMed Central

NIU, Kiyoshi

2008-01-01

This is a historical review of the discovery of naked charm particles and lifetime differences among charm species. These discoveries in the field of cosmic-ray physics were made by the innovation of nuclear emulsion techniques in Japan. A pair of naked charm particles was discovered in 1971 in a cosmic-ray interaction, three years prior to the discovery of the hidden charm particle, J/Ψ, in western countries. Lifetime differences between charged and neutral charm particles were pointed out in 1975, which were later re-confirmed by the collaborative Experiment E531 at Fermilab. Japanese physicists led by K.Niu made essential contributions to it with improved emulsion techniques, complemented by electronic detectors. This review also discusses the discovery of artificially produced naked charm particles by us in an accelerator experiment at Fermilab in 1975 and of multiple-pair productions of charm particles in a single interaction in 1987 by the collaborative Experiment WA75 at CERN. PMID:18941283

Monitoring Interfacial Lipid Oxidation in Oil-in-Water Emulsions Using Spatially Resolved Optical Techniques.

PubMed

Banerjee, Chiranjib; Westberg, Michael; Breitenbach, Thomas; Bregnhøj, Mikkel; Ogilby, Peter R

2017-06-06

The oxidation of lipids is an important phenomenon with ramifications for disciplines that range from food science to cell biology. The development and characterization of tools and techniques to monitor lipid oxidation are thus relevant. Of particular significance in this regard are tools that facilitate the study of oxidations at interfaces in heterogeneous samples (e.g., oil-in-water emulsions, cell membranes). In this article, we establish a proof-of-principle for methods to initiate and then monitor such oxidations with high spatial resolution. The experiments were performed using oil-in-water emulsions of polyunsaturated fatty acids (PUFAs) prepared from cod liver oil. We produced singlet oxygen at a point near the oil-water interface of a given PUFA droplet in a spatially localized two-photon photosensitized process. We then followed the oxidation reactions initiated by this process with the fluorescence-based imaging technique of structured illumination microscopy (SIM). We conclude that the approach reported herein has attributes well-suited to the study of lipid oxidation in heterogeneous samples.

Ionic Liquid Microemullsions, Templates for Directing Morphology of Cellulose Biopolymer Nanoparticles (Briefing Charts)

DTIC Science & Technology

2015-08-19

Morphologies Emulsion Directed Cellulose Morphology (NOT nanocellulose) T. Suzuki et al. / Journal of Colloid and Interface Science 418 (2014) 126–131...Ternary phase diagram constructed with BmimCl/Span80/Tween20/Sunflower Oil. Warm emulsion technique adapted at 50 °C, for reduced viscosity. Cellulose

RIR-MAPLE deposition of conjugated polymers and hybrid nanocomposites for application to optoelectronic devices

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stiff-Roberts, Adrienne D.; Pate, Ryan; McCormick, Ryan

2012-07-30

Resonant infrared matrix-assisted pulsed laser evaporation (RIR-MAPLE) is a variation of pulsed laser deposition that is useful for organic-based thin films because it reduces material degradation by selective absorption of infrared radiation in the host matrix. A unique emulsion-based RIR-MAPLE approach has been developed that reduces substrate exposure to solvents and provides controlled and repeatable organic thin film deposition. In order to establish emulsion-based RIR-MAPLE as a preferred deposition technique for conjugated polymer or hybrid nanocomposite optoelectronic devices, studies have been conducted to demonstrate the value added by the approach in comparison to traditional solution-based deposition techniques, and this workmore » will be reviewed. The control of hybrid nanocomposite thin film deposition, and the photoconductivity in such materials deposited using emulsion-based RIR-MAPLE, will also be reviewed. The overall result of these studies is the demonstration of emulsion-based RIR-MAPLE as a viable option for the fabrication of conjugated polymer and hybrid nanocomposite optoelectronic devices that could yield improved device performance.« less

Intra-lymph node injection of biodegradable polymer particles.

PubMed

Andorko, James I; Tostanoski, Lisa H; Solano, Eduardo; Mukhamedova, Maryam; Jewell, Christopher M

2014-01-02

Generation of adaptive immune response relies on efficient drainage or trafficking of antigen to lymph nodes for processing and presentation of these foreign molecules to T and B lymphocytes. Lymph nodes have thus become critical targets for new vaccines and immunotherapies. A recent strategy for targeting these tissues is direct lymph node injection of soluble vaccine components, and clinical trials involving this technique have been promising. Several biomaterial strategies have also been investigated to improve lymph node targeting, for example, tuning particle size for optimal drainage of biomaterial vaccine particles. In this paper we present a new method that combines direct lymph node injection with biodegradable polymer particles that can be laden with antigen, adjuvant, or other vaccine components. In this method polymeric microparticles or nanoparticles are synthesized by a modified double emulsion protocol incorporating lipid stabilizers. Particle properties (e.g. size, cargo loading) are confirmed by laser diffraction and fluorescent microscopy, respectively. Mouse lymph nodes are then identified by peripheral injection of a nontoxic tracer dye that allows visualization of the target injection site and subsequent deposition of polymer particles in lymph nodes. This technique allows direct control over the doses and combinations of biomaterials and vaccine components delivered to lymph nodes and could be harnessed in the development of new biomaterial-based vaccines.

Investigation on Electrochemical Properties of Polythiophene Nanocomposite with Graphite Derivatives as Supercapacitor Material on Breath Figure-Decorated PMMA Electrode

NASA Astrophysics Data System (ADS)

Azimi, Mona; Abbaspour, Mohsen; Fazli, Ali; Setoodeh, Hamideh; Pourabbas, Behzad

2018-03-01

Breath figures have been formed by the direct breath figure method on polymethyl methacrylate electrode sand hexagonal oriented holes with 0.5- to 10- μm2 surface area have been created. Deposition of materials on the electrodes has been performed by the spray-coating method. polythiophene (PTh) nanoparticles, polythiophene-graphene oxide (PTh-GO) and polythiophene-reduced graphene oxide (PTh-G) nanocomposites were synthesized by emulsion polymerization, while characterization of synthetic materials have been carried out by Fourier transform infrared, Χ-ray diffraction, transmission electron microscopy, UV-Vis spectroscopy and field emission scanning electron microscopy techniques. Also, the electrochemical properties of the designed electrodes were investigated by cyclic voltammetry, galvanostatic charge-discharge and electrochemical impedance spectroscopy techniques. Specific capacitance of porous electrodes coated by PTh nanoparticles, PTh-GO and PTh-G nanocomposites were calculated from cyclic voltammetry curves at 5 mV/s scan rate, andthe values are 3.5 F/g, 16.39 F/g, and 28.68 F/g, respectively. Also, the energy density of each electrode at 5 mV/s scan rate has been calculated and the results show that incorporation of GO and G nanolayers with PTh nanoparticles enhances the electrochemical properties of electrodes.

Preparation of solid lipid nanoparticles from W/O/W emulsions: preliminary studies on insulin encapsulation.

PubMed

Gallarate, Marina; Trotta, Michele; Battaglia, Luigi; Chirio, Daniela

2009-08-01

A method to produce solid lipid nanoparticles (SLN) from W/O/W multiple emulsions was developed applying the solvent-in-water emulsion-diffusion technique. Insulin was chosen as hydrophilic peptide drug to be dissolved in the acidic inner aqueous phase of multiple emulsions and to be consequently carried in SLN. Several partially water-miscible solvents with low toxicity were screened in order to optimize emulsions and SLN composition, after assessing that insulin did not undergo any chemical modification in the presence of the different solvents and under the production process conditions. SLN of spherical shape and with mean diameters in the 600-1200 nm range were obtained by simple water dilution of the W/O/W emulsion. Best results, in terms of SLN mean diameter and encapsulation efficiencies, were obtained using glyceryl monostearate as lipid matrix, butyl lactate as a solvent, and soy lecithin and Pluronic F68 as surfactants. Encapsulation efficiencies up to 40% of the loaded amount were obtained, owing to the actual multiplicity of the system; the use of multiple emulsion-derived SLN can be considered a useful strategy to encapsulate a hydrophilic drug in a lipid matrix.

Chemical Polymerization and Langmuir-Blodgett Techniques. 2. The Polymerization of Monolayers of 3-Substituted Pyrroles

DTIC Science & Technology

1993-09-12

the liquid -air interface could be monitored by changes in the surface area. Deposition of monolayers by Langmuir - Blodgett technique is possible and...polymerization product from the LB trough in chloroform solution. Figure 10 Langmuir - Blodgett transfer of poly (3-hexadecyl pyrrole) onto hydrophobized glass... Langmuir - Blodgett Techniques, 2: The Polymerization of Monolayers of 3-Substituted Pyrroles by W.M. Sigmund, C. Marestin, S. Keil, H. Zhou and R.S

Investigation of non-isocyanate urethane functional latexes and carbon nanofiller/epoxy coatings

NASA Astrophysics Data System (ADS)

Meng, Lei

This dissertation consists of two parts. In the first part, a new class of non-isocyanate urethane methacrylates was synthesized and the effect of the new monomers on the urethane functional latex was investigated. The second part focused on a comparison of carbon nanofillers in inorganic/organic epoxy coating system for anticorrosive applications. A new class of non-isocyanate urethane methacrylates (UMAs) monomers was synthesized through an environmentally friendly non-isocyanate pathway. The kinetics of seeded semibatch emulsion polymerization of UMAs with methyl methacrylate (MMA) and butyl acrylate (BA) was monitored. The particle size and morphology were investigated by dynamic light scattering (DLS), ultrasound acoustic attenuation spectroscopy (UAAS) and transmission electron microscopy (TEM). The minimum film formation temperature (MFFT), mechanical and viscoelastic properties were studied. It was found that the emulsion polymerization processes all proceeded via Smith-Ewart control, leading to the uniform morphology and particle size. The glass transition temperature (Tg) and the mechanical properties of poly(MMA/BA/UMA) decreased with the increasing chain length of urethane methacrylate monomers due to the increasing flexibility of side chains. Without the effect of Tg, lower MFFT and improved mechanical properties were observed from urethane functional latexes. The improved mechanical properties were due to the increasing particle interaction by forming hydrogen bonding. Furthermore, the effect of urethane functionality in terms of the polymer composition, the location and the concentration was investigated by the batch, single-stage and two-stage semibatch polymerization of 2-[(butylcarbamoyl)oxy]ethyl methacrylate (BEM) with MMA and BA. The core-shell and homogeneous structures were evaluated by TEM, differential scanning calorimetry (DSC), and solid state nuclear magnetic resonance (SS-NMR). The compositional drift was observed from the batch polymerization. The mechanical properties were improved with increasing urethane and the best was from the urethane in the shell due to higher concentration of urethane in the continuous phase. The inorganic/organic alkoxysilane modified epoxy coating system was formulated with carbon nanofillers, i.e. carbon black, mixture of carbon black and nanotubes, unpurified and purified non-fullerene carbon nanotubes and fullerene carbon nanotubes. Mechanical, thermal, electrical and anticorrosive properties of cured films were evaluated by tensile tests, DMTA, DSC, four-point probe method and electrochemical impedance spectroscopy (EIS), respectively. It was found that the most efficient material to enhance the electrical conductivity and anticorrosive properties of nanocomposite coating systems was fullerene CNTs.

Nanobeads-based assays. The case of gluten detection

NASA Astrophysics Data System (ADS)

Venditti, Iole; Fratoddi, Ilaria; Vittoria Russo, Maria; Bellucci, Stefano; Crescenzo, Roberta; Iozzino, Luisa; Staiano, Maria; Aurilia, Vincenzo; Varriale, Antonio; Rossi, Mosè; D'Auria, Sabato

2008-11-01

In order to verify if the use of nanobeads of poly[phenylacetylene-(co-acrylic acid)] (PPA/AA) in the ELISA test would affect the immune-activity of the antibodies (Ab) and/or the activity of the enzymes used to label the Ab anti-rabbit IGg, in this work we immobilized the horse liver peroxidase labelled Ab anti-rabbit IGg onto PPA/AA nanobeads. The gluten test was chosen as the model to demonstrate the usefulness of these nanobeads in immunoassays. The synthesis of PPA/AA nanobeads was performed by a modified emulsion polymerization. Self-assembly of nanospheres with mean diameter equal to 200 nm was achieved by casting aqueous suspensions. The materials were characterized by traditional spectroscopic techniques, while the size and dispersion of the particles were analysed by scanning electron microscopy (SEM) measurements. The obtained results show that the immobilization process of the Abs onto PPA/AA did not affect either the immune-response of the Abs or the functional activity of the peroxidase suggesting the usefulness of PPA/AA for the design of advanced nanobeads-based assays for the simultaneous screening of several analytes in complex media.

Recent advances in engineering microparticles and their nascent utilization in biomedical delivery and diagnostic applications.

PubMed

Choi, Andrew; Seo, Kyoung Duck; Kim, Do Wan; Kim, Bum Chang; Kim, Dong Sung

2017-02-14

Complex microparticles (MPs) bearing unique characteristics such as well-tailored sizes, various morphologies, and multi-compartments have been attempted to be produced by many researchers in the past decades. However, a conventionally used method of fabricating MPs, emulsion polymerization, has a limitation in achieving the aforementioned characteristics and several approaches such as the microfluidics-assisted (droplet-based microfluidics and flow lithography-based microfluidics), electrohydrodynamics (EHD)-based, centrifugation-based, and template-based methods have been recently suggested to overcome this limitation. The outstanding features of complex MPs engineered through these suggested methods have provided new opportunities for MPs to be applied in a wider range of applications including cell carriers, drug delivery agents, active pigments for display, microsensors, interface stabilizers, and catalyst substrates. Overall, the engineered MPs expose their potential particularly in the field of biomedical engineering as the increased complexity in the engineered MPs fulfills well the requirements of the high-end applications. This review outlines the current trends of newly developed techniques used for engineered MPs fabrication and focuses on the current state of engineered MPs in biomedical applications.

Poly methacrylic acid modified CDHA nanocomposites as potential pH responsive drug delivery vehicles.

PubMed

Victor, Sunita Prem; Sharma, Chandra P

2013-08-01

The objective of this study was to prepare pH sensitive polymethacrylic acid-calcium deficient hydroxyapatite (CDHA) nanocomposites. The CDHA nanoparticles were prepared by coprecipitation method. The modification of CDHA by methacrylic acid (MA) was achieved by AIBN initiated free radical polymerization with sodium bisulphite as catalyst followed by emulsion technique. These nanocomposites with a half life of 8h consisted of high aspect ratio, needle like particles and exhibited an increase in swelling behaviour with pH. The in vivo potential of the nanocomposites was evaluated in vitro by the results of cell aggregation, protein adsorption, MTT assay and haemolytic activity. The invitro loading and release studies using albumin as a model drug indicate that the nanocomposites gave better loading when compared to the CDHA nanoparticles and altered the drug release rates. The nanocomposites also exhibited good uptake on C6 glioma cells as studied by fluorescence microscopy. The results obtained suggest that these nanocomposites have great potential for oral controlled protein delivery and can be extended further for intracellular drug delivery applications. Copyright © 2013 Elsevier B.V. All rights reserved.

Preparation of diclofenac-imprinted polymer beads for selective molecular separation in water.

PubMed

Zhou, Tongchang; Kamra, Tripta; Ye, Lei

2018-03-01

Molecular imprinting technique is an attractive strategy to prepare materials for target recognition and rapid separation. In this work, a new type of diclofenac (DFC)-imprinted polymer beads was synthesized by Pickering emulsion polymerization using 2-(dimethylamino)ethyl methacrylate as the functional monomer. The selectivity and capacity of the molecularly imprinted polymers (MIPs) were investigated in aqueous solution. Equilibrium binding results show that the MIPs have a high selectivity to bind DFC in a wide range of pH values. Moreover, in liquid chromatography experiment, the imprinted polymer beads were packed into column to investigate the binding selectivity under nonequilibrium conditions. The retention time of DFC on the MIP column is significantly longer than its structural analogues. Also, retention of DFC on the MIP column was significantly longer than on the nonimprinted polymer column under aqueous condition. As the new MIP beads can be used to achieve direct separation of DFC from water, the synthetic method and the affinity beads developed in this work opened new possibilities for removing toxic chemicals from environmental and drinking water. Copyright © 2017 John Wiley & Sons, Ltd.

Parameters for Stable Water-in-Oil Lipiodol Emulsion for Liver Trans-Arterial Chemo-Eembolization.

PubMed

Deschamps, F; Moine, L; Isoardo, T; Tselikas, L; Paci, A; Mir, L M; Huang, N; Fattal, E; de Baère, T

2017-12-01

Water-in-oil type and stability are important properties for Lipiodol emulsions during conventional trans-arterial chemo-embolization. Our purpose is to evaluate the influence of 3 technical parameters on those properties. The Lipiodol emulsions have been formulated by repetitive back-and-forth pumping of two 10-ml syringes through a 3-way stopcock. Three parameters were compared: Lipiodol/doxorubicin ratio (2/1 vs. 3/1), doxorubicin concentration (10 vs. 20 mg/ml) and speed of incorporation of doxorubicin in Lipiodol (bolus vs. incremental vs. continuous). The percentage of water-in-oil emulsion obtained and the duration until complete coalescence (stability) for water-in-oil emulsions were, respectively, evaluated with the drop-test and static light scattering technique (Turbiscan). Among the 48 emulsions formulated, 32 emulsions (67%) were water-in-oil. The percentage of water-in-oil emulsions obtained was significantly higher for incremental (94%) and for continuous (100%) injections compared to bolus injection (6%) of doxorubicin. Emulsion type was neither influenced by Lipiodol/doxorubicin ratio nor by doxorubicin concentration. The mean stability of water-in-oil emulsions was 215 ± 257 min. The emulsions stability was significantly longer when formulated using continuous compared to incremental injection (326 ± 309 vs. 96 ± 101 min, p = 0.018) and using 3/1 compared to 2/1 ratio of Lipiodol/doxorubicin (372 ± 276 vs. 47 ± 43 min, p = <0.0001). Stability was not influenced by the doxorubicin concentration. The continuous and incremental injections of doxorubicin in the Lipiodol result in highly predictable water-in-oil emulsion type. It also demonstrates a significant increase in stability compared to bolus injection. Higher ratio of Lipiodol/doxorubicin is a critical parameter for emulsion stability too.

Whey protein/polysaccharide-stabilized emulsions: Effect of polymer type and pH on release and topical delivery of salicylic acid.

PubMed

Combrinck, Johann; Otto, Anja; du Plessis, Jeanetta

2014-06-01

Emulsions are widely used as topical formulations in the pharmaceutical and cosmetic industries. They are thermodynamically unstable and require emulsifiers for stabilization. Studies have indicated that emulsifiers could affect topical delivery of actives, and this study was therefore designed to investigate the effects of different polymers, applied as emulsifiers, as well as the effects of pH on the release and topical delivery of the active. O/w emulsions were prepared by the layer-by-layer technique, with whey protein forming the first layer around the oil droplets, while either chitosan or carrageenan was subsequently adsorbed to the protein at the interface. Additionally, the emulsions were prepared at three different pH values to introduce different charges to the polymers. The active ingredient, salicylic acid, was incorporated into the oil phase of the emulsions. Physical characterization of the resulting formulations, i.e., droplet size, zeta potential, stability, and turbidity in the water phase, was performed. Release studies were conducted, after which skin absorption studies were performed on the five most stable emulsions, by using Franz type diffusion cells and utilizing human, abdominal skin membranes. It was found that an increase in emulsion droplet charge could negatively affect the release of salicylic acid from these formulations. Contrary, positively charged emulsion droplets were found to enhance dermal and transdermal delivery of salicylic acid from emulsions. It was hypothesized that electrostatic complex formation between the emulsifier and salicylic acid could affect its release, whereas electrostatic interaction between the emulsion droplets and skin could influence dermal/transdermal delivery of the active.

Treatment of local-anesthetic toxicity with lipid emulsion therapy.

PubMed

Burch, Melissa S; McAllister, Russell K; Meyer, Tricia A

2011-01-15

The use of lipid emulsion to treat local-anesthetic toxicity is discussed. Systemic toxicity from local anesthetics is a rare but potentially fatal complication of regional anesthesia. There is increasing evidence that lipid emulsion may be an effective treatment to reverse the cardiac and neurologic effects of local-anesthetic toxicity. A literature search identified seven case reports of local-anesthetic toxicity in which lipid emulsion was used. Lipid emulsion was found to be successful in the treatment of local-anesthetic toxicity associated with various regional anesthetic techniques and multiple local anesthetics. The majority of patients in the case reports reviewed were unresponsive to initial management of local-anesthetic toxicity with standard resuscitative measures, but all recovered completely after receiving lipid emulsion therapy. The initial dose of lipid emulsion administered varied among the case reports, as well as whether a lipid emulsion infusion was started and at what point during resuscitation. Based on the case reports reviewed, an initial bolus dose of 1.5 mL/kg followed by an infusion of 10 mL/min as soon as local-anesthetic toxicity is suspected seems most beneficial. The pharmacokinetics of lipid emulsion therapy in the treatment of local-anesthetic toxicity has not been fully elucidated but likely involves increasing metabolism, distribution, or partitioning of the local anesthetic away from receptors into lipid within tissues. Lipid emulsion has been reported useful in the treatment of systemic toxicity caused by local anesthetics. The mechanism of effect is unclear, and evidence for the benefit of lipid therapy in humans is from case reports only.

Transformation of eutectic emulsion to nanosuspension fabricating with solvent evaporation and ultrasonication technique

PubMed Central

Phaechamud, Thawatchai; Tuntarawongsa, Sarun

2016-01-01

Eutectic solvent can solubilize high amount of some therapeutic compounds. Volatile eutectic solvent is interesting to be used as solvent in the preparation of nanosuspension with emulsion solvent evaporation technique. The mechanism of transformation from the eutectic emulsion to nanosuspension was investigated in this study. The 30% w/w ibuprofen eutectic solution was used as the internal phase, and the external phase is composed of Tween 80 as emulsifier. Ibuprofen nanosuspension was prepared by eutectic emulsion solvent evaporating method followed with ultrasonication. During evaporation process, the ibuprofen concentration in emulsion droplets was increased leading to a drug supersaturation but did not immediately recrystallize because of low glass transition temperature (Tg) of ibuprofen. The contact angle of the internal phase on ibuprofen was apparently lower than that of the external phase at all times of evaporation, indicating that the ibuprofen crystals were preferentially wetted by the internal phase than the external phase. From calculated dewetting value ibuprofen crystallization occurred in the droplet. Crystallization of the drug was initiated with external mechanical force, and the particle size of the drug was larger due to Ostwald ripening. Cavitation force from ultrasonication minimized the ibuprofen crystals to the nanoscale. Particle size and zeta potential of formulated ibuprofen nanosuspension were 330.87±51.49 nm and −31.1±1.6 mV, respectively, and exhibited a fast dissolution. Therefore, the combination of eutectic emulsion solvent evaporation method with ultrasonication was favorable for fabricating an ibuprofen nanosuspension, and the transformation mechanism was attained successfully. PMID:27366064

Transformation of eutectic emulsion to nanosuspension fabricating with solvent evaporation and ultrasonication technique.

PubMed

Phaechamud, Thawatchai; Tuntarawongsa, Sarun

2016-01-01

Eutectic solvent can solubilize high amount of some therapeutic compounds. Volatile eutectic solvent is interesting to be used as solvent in the preparation of nanosuspension with emulsion solvent evaporation technique. The mechanism of transformation from the eutectic emulsion to nanosuspension was investigated in this study. The 30% w/w ibuprofen eutectic solution was used as the internal phase, and the external phase is composed of Tween 80 as emulsifier. Ibuprofen nanosuspension was prepared by eutectic emulsion solvent evaporating method followed with ultrasonication. During evaporation process, the ibuprofen concentration in emulsion droplets was increased leading to a drug supersaturation but did not immediately recrystallize because of low glass transition temperature (T g) of ibuprofen. The contact angle of the internal phase on ibuprofen was apparently lower than that of the external phase at all times of evaporation, indicating that the ibuprofen crystals were preferentially wetted by the internal phase than the external phase. From calculated dewetting value ibuprofen crystallization occurred in the droplet. Crystallization of the drug was initiated with external mechanical force, and the particle size of the drug was larger due to Ostwald ripening. Cavitation force from ultrasonication minimized the ibuprofen crystals to the nanoscale. Particle size and zeta potential of formulated ibuprofen nanosuspension were 330.87±51.49 nm and -31.1±1.6 mV, respectively, and exhibited a fast dissolution. Therefore, the combination of eutectic emulsion solvent evaporation method with ultrasonication was favorable for fabricating an ibuprofen nanosuspension, and the transformation mechanism was attained successfully.

Solid-stabilized emulsion formation using stearoyl lactylate coated iron oxide nanoparticles

NASA Astrophysics Data System (ADS)

Vengsarkar, Pranav S.; Roberts, Christopher B.

2014-10-01

Iron oxide nanoparticles can exhibit highly tunable physicochemical properties that are extremely important in applications such as catalysis, biomedicine and environmental remediation. The small size of iron oxide nanoparticles can be used to stabilize oil-in-water Pickering emulsions due to their high energy of adsorption at the interface of oil droplets in water. The objective of this work is to investigate the effect of the primary particle characteristics and stabilizing agent chemistry on the stability of oil-in-water Pickering emulsions. Iron oxide nanoparticles were synthesized by the co-precipitation method using stoichiometric amounts of Fe2+ and Fe3+ salts. Sodium stearoyl lactylate (SSL), a Food and Drug Administration approved food additive, was used to functionalize the iron oxide nanoparticles. SSL is useful in the generation of fat-in-water emulsions due to its high hydrophilic-lipophilic balance and its bilayer-forming capacity. Generation of a monolayer or a bilayer coating on the nanoparticles was controlled through systematic changes in reagent concentrations. The coated particles were then characterized using various analytical techniques to determine their size, their crystal structure and surface functionalization. The capacity of these bilayer coated nanoparticles to stabilize oil-in-water emulsions under various salt concentrations and pH values was also systematically determined using various characterization techniques. This study successfully demonstrated the ability to synthesize iron oxide nanoparticles (20-40 nm) coated with SSL in order to generate stable Pickering emulsions that were pH-responsive and resistant to significant destabilization in a saline environment, thereby lending themselves to applications in advanced oil spill recovery and remediation.

Multiwalled Carbon Nanotubes at the Interface of Pickering Emulsions.

PubMed

Briggs, Nicholas M; Weston, Javen S; Li, Brian; Venkataramani, Deepika; Aichele, Clint P; Harwell, Jeffrey H; Crossley, Steven P

2015-12-08

Carbon nanotubes exhibit very unique properties in biphasic systems. Their interparticle attraction leads to reduced droplet coalescence rates and corresponding improvements in emulsion stability. Here we use covalent and noncovalent techniques to modify the hydrophilicity of multiwalled carbon nanotubes (MWCNTs) and study their resulting behavior at an oil-water interface. By using both paraffin wax/water and dodecane/water systems, the thickness of the layer of MWNTs at the interface and resulting emulsion stability are shown to vary significantly with the approach used to modify the MWNTs. Increased hydrophilicity of the MWNTs shifts the emulsions from water-in-oil to oil-in-water. The stability of the emulsion is found to correlate with the thickness of nanotubes populating the oil-water interface and relative strength of the carbon nanotube network. The addition of a surfactant decreases the thickness of nanotubes at the interface and enhances the overall interfacial area stabilized at the expense of increased droplet coalescence rates. To the best of our knowledge, this is the first time the interfacial thickness of modified carbon nanotubes has been quantified and correlated to emulsion stability.

Molecular and functional assessment of multicellular cancer spheroids produced in double emulsions enabled by efficient airway resistance based selective surface treatment

NASA Astrophysics Data System (ADS)

Ma, Xiao; Leth Jepsen, Morten; Ivarsen, Anne Kathrine R.; Knudsen, Birgitta R.; Ho, Yi-Ping

2017-09-01

Multicellular spheroids have garnered significant attention as an in vitro three-dimensional cancer model which can mimick the in vivo microenvironmental features. While microfluidics generated double emulsions have become a potential method to generate spheroids, challenges remain on the tedious procedures. Enabled by a novel ‘airway resistance’ based selective surface treatment, this study presents an easy and facile generation of double emulsions for the initiation and cultivation of multicellular spheroids in a scaffold-free format. Combining with our previously developed DNA nanosensors, intestinal spheroids produced in the double emulsions have shown an elevated activities of an essential DNA modifying enzyme, the topoisomerase I. The observed molecular and functional characteristics of spheroids produced in double emulsions are similar to the counterparts produced by the commercially available ultra-low attachment plates. However, the double emulsions excel for their improved uniformity, and the consistency of the results obtained by subsequent analysis of the spheroids. The presented technique is expected to ease the burden of producing spheroids and to promote the spheroids model for cancer or stem cell study.

Detection of Vegetable Oil Variance Using Surface Plasmon Resonance (SPR) Technique

NASA Astrophysics Data System (ADS)

Supardianningsih; Panggabean, R. D.; Romadhon, I. A.; Laksono, F. D.; Nofianti, U.; Abraha, K.

2018-05-01

The difference between coconut oil, corn oil, olive oil, and palm oil has been detected using surface plasmon resonance (SPR) technique. This is a new method in material characterization that can be used to identify vegetable oil variance. The SPR curve was measured by SPR system consisting of optical instruments, mechanical instruments, Main UNIT, and user interface (computer). He-Ne laser beam of wavelength 633 nm was used as light source, while gold (Au) thin film evaporated on half cylinder prism was used as the base so that surface plasmon polariton (SPP) waves propagate at the interface. Tween-80 and PEG-400 are used as surfactant and co-surfactant to make water-oil emulsion from each sample. The sample was prepared with the ratio of oil: surfactant: co-surfactant as 1:2:1 and then stirred on the water to make emulsions. The angle shift was measured by the change of SPR angle from prism/Au/air system to prism/Au/water-oil emulsion. The different SPR angle of each sample has been detected in the various number of spray, a method that was used for depositing the emulsion. From this work, we conclude that the saturated fatty acid component was the most significant component that changes the refractive index in the vegetable oil in water emulsion that can be used to characterize the vegetable oil variance.

Exploring the Dynamics and Structure of Soft Colloids at Oil-water Interfaces

NASA Astrophysics Data System (ADS)

Kwok, Man Hin

The ability of solid colloidal particles to physically stabilize emulsions, also referred to as Pickering emulsions, has been studied for a long time since their activity at the interface was discovered one hundred years ago. Pickering emulsions display various interesting phenomena because of it high desorption energy at the interface compared with conventional surfactant stabilizers. In addition, Pickering emulsions are considered to be 'surfactant free' emulsion and the adverse effects of using surfactants could be eliminated. In the past few years, the use of submicrometer, poly(N-isopropylacrylamide) (PNIPAM)-based mcirogel particles for stabilizing emulsions has captured the interest of many scientists. Being soft, the microgels, which are spherical in solution, become deformed at the oil-water interface. This deformability leads to the special dynamic properties of interfacial layers and packing structures, which in turn alters the interfacial tension and the rheological properties of the interface. In addition, being responsiveness, PNIPAM microgels enable emulsions to be prepared and broken on demand. Despite all of the practical advantages and unique properties that have already been demonstrated, the mechanisms that govern emulsion stabilization and destabilization using microgels are far from completely understood. The study of soft colloids at the interface thus is of great academic interest and the fundamental understanding of them is the key to achieve the application potential of such novel materials. This thesis focuses on the dynamics and structure of soft colloidal particles at the oil-water interfaces. First, in order to prepare tailored colloids for the study, the syntheses of multi-responsive PNIPAM microgels with different size, co-monomers, deformability and morphologies were thoroughly investigated. The combination of semi-batch synthesis and temperature-programmed technique resulted in a novel preparation of micron-sized PNIPAM microgels. Various experimental parameters were tested and modified in order to give microgels with optimized quality. The thermo- and pH- responsiveness of these microgels were characterized by laser diffraction and dynamic light scattering (DLS). Next, a novel labeling technique of the soft PNIPAM microgel particles was developed. This technique was based on the physical adsorption of small fluorescent molecules. Instead of chemically bonded dye molecules, these adsorbed fluorescent dyes could move freely inside the polymer network of the microgel particle. It was also found that the fluorescent dye interacted with different parts of the microgel differently. Therefore, the internal structure and morphology of microgels could be directly visualized by confocal laser scanning microscopy (CLSM) in aqueous environment. The improvement of imaging techniques of microgel particles is essential for studying their behavior at the oil-water interface. It is because conventional scanning electron microscopy (SEM) requires dried sample, which might not reflects the actual states of microgels in aqueous environment. With the improved labeling method under CLSM mentioned above, the conformation of micron-sized PNIPAM microgel particles was captured at the oil-water interface. Particularly, anisotropic deformation of soft pH-responsive microgels was observed at the oil-water interface. Nevertheless, it was found that microgels were not likely to deform significantly unless they were extremely swollen. We also use Langmuir trough to study the dynamics of microgel at an interface with changing area. Forced desorption-spontaneous adsorption cycles of microgel particles at the oil-water interface were successfully demonstrated. More interestingly, it was discovered that the microgel particles would be desorbed before having a significant deformation in Langmuir trough compression. Finally, the emulsion stability of the microgel stabilized Pickering emulsion was characterized by centrifugation. By comparing the stability of different microgels in different conditions, the correlation between the microgel properties and the corresponding Pickering emulsion stability was found. The emulsion stability and the interfacial behaviors of PNIPAM based microgels can now be better controlled and predicted, which gives great advantages for future applications using soft colloids as stabilizers.

Folic acid conjugated cross-linked acrylic polymer (FA-CLAP) hydrogel for site specific delivery of hydrophobic drugs to cancer cells.

PubMed

Pillai, Jisha Jayadevan; Thulasidasan, Arun Kumar Theralikattu; Anto, Ruby John; Chithralekha, Devika Nandan; Narayanan, Ashwanikumar; Kumar, Gopalakrishnapillai Sankaramangalam Vinod

2014-07-15

The hydrogel based system is found to be rarely reported for the delivery of hydrophobic drug due to the incompatibility of hydrophilicity of the polymer network and the hydrophobicity of drug. This problem can be solved by preparing semi-interpenetrating network of cross-linked polymer for tuning the hydrophilicity so as to entrap the hydrophobic drugs. The current study is to develop a folic acid conjugated cross-linked pH sensitive, biocompatible polymeric hydrogel to achieve a site specific drug delivery. For that, we have synthesized a folic acid conjugated PEG cross-linked acrylic polymer (FA-CLAP) hydrogel and investigated its loading and release of curcumin. The formed polymer hydrogel was then conjugated with folic acid for the site specific delivery of curcumin to cancer cells and then further characterized and conducted the cell uptake and cytotoxicity studies on human cervical cancer cell lines (HeLa). In this study, we synthesized folic acid conjugated cross-linked acrylic hydrogel for the delivery of hydrophobic drugs to the cancer site. Poly (ethyleneglycol) (PEG) diacrylate cross-linked acrylic polymer (PAA) was prepared via inverse emulsion polymerization technique and later conjugated it with folic acid (FA-CLAP). Hydrophobic drug curcumin is entrapped into it and investigated the entrapment efficiency. Characterization of synthesized hydogel was done by using Fourier Transform-Infrared spectroscopy (FT-IR), Transmission Electron Microscopy (TEM), Differential Scanning Calorimetry (DSC). Polymerization and folate conjugation was confirmed by FT-IR spectroscopy. The release kinetics of drug from the entrapped form was studied which showed initial burst release followed by sustained release due to swelling and increased cross-linking. In vitro cytotoxicity and cell uptake studies were conducted in human cervical cancer (HeLa) cell lines. Results showed that curcumin entrapped folate conjugated cross-linked acrylic polymer (FA-CLAP) hydrogel showed higher cellular uptake than the non folate conjugated form. So this can be suggested as a better delivery system for site specific release of hydrophobic cancer drugs.

Antimicrobial efficacy of an innovative emulsion of medium chain triglycerides against canine and feline periodontopathogens.

PubMed

Laverty, G; Gilmore, B F; Jones, D S; Coyle, L; Folan, M; Breathnach, R

2015-04-01

To test the in vitro antimicrobial efficacy of a non-toxic emulsion of free fatty acids against clinically relevant canine and feline periodontopathogens Antimicrobial kill kinetics were established utilising an alamarBlue(®) viability assay against 10 species of canine and feline periodontopathogens in the biofilm mode of growth at a concentration of 0·125% v/v medium chain triglyceride (ML:8) emulsion. The results were compared with 0·12% v/v chlorhexidine digluconate and a xylitol-containing dental formulation. Mammalian cellular cytotoxicity was also investigated for both the ML:8 emulsion and chlorhexidine digluconate (0·25 to 0·0625% v/v) using in vitro tissue culture techniques. No statistically significant difference was observed in the antimicrobial activity of the ML:8 emulsion and chlorhexidine digluconate; a high percentage kill rate (>70%) was achieved within 5 minutes of exposure and was maintained at subsequent time points. A statistically significant improvement in antibiofilm activity was observed with the ML:8 emulsion compared with the xylitol-containing formulation. The ML:8 emulsion possessed a significantly lower (P < 0·001) toxicity profile compared with the chlorhexidine digluconate in mammalian cellular cytotoxicity assays. The ML:8 emulsion exhibited significant potential as a putative effective antimicrobial alternative to chlorhexidine- and xylitol- based products for the reduction of canine and feline periodontopathogens. © 2015 British Small Animal Veterinary Association.

Emulsion-Based RIR-MAPLE Deposition of Conjugated Polymers: Primary Solvent Effect and Its Implications on Organic Solar Cell Performance.

PubMed

Ge, Wangyao; Li, Nan K; McCormick, Ryan D; Lichtenberg, Eli; Yingling, Yaroslava G; Stiff-Roberts, Adrienne D

2016-08-03

Emulsion-based, resonant infrared matrix-assisted pulsed laser evaporation (RIR-MAPLE) has been demonstrated as an alternative technique to deposit conjugated polymer films for photovoltaic applications; yet, a fundamental understanding of how the emulsion target characteristics translate into film properties and solar cell performance is unclear. Such understanding is crucial to enable the rational improvement of organic solar cell (OSC) efficiency and to realize the expected advantages of emulsion-based RIR-MAPLE for OSC fabrication. In this paper, the effect of the primary solvent used in the emulsion target is studied, both experimentally and theoretically, and it is found to determine the conjugated polymer cluster size in the emulsion as well as surface roughness and internal morphology of resulting polymer films. By using a primary solvent with low solubility-in-water and low vapor pressure, the surface roughness of deposited P3HT and PCPDTBT polymer films was reduced to 10 nm, and the efficiency of P3HT:PC61BM OSCs was increased to 3.2% (∼100 times higher compared to the first MAPLE OSC demonstration [ Caricato , A. P. ; Appl. Phys. Lett. 2012 , 100 , 073306 ]). This work unveils the mechanism of polymer film formation using emulsion-based RIR-MAPLE and provides insight and direction to determine the best ways to take advantage of the emulsion target approach to control film properties for different applications.

How to fabricate robust microfluidic systems for a dollar

NASA Astrophysics Data System (ADS)

Lapierre, Florian; Cameron, Neil R.; Oakeshott, John; Peat, Thomas; Zhu, Yonggang

2013-12-01

Since the past decade, the interest towards microfluidic devices has sensibly grown due to the wide variety of multidisciplinary applications. One branch of the microfluidic domain consists in the synthesis of various types of emulsions requested by cosmetic, food and biotechnological industries In particular, monodisperse water-in-oil microemulsion synthetised in microfluidic devices are quickly becoming the new generation of emulsions for precise bead control and high surface area. These microemulsions are generally aqueous bioreactors in the form of droplets from 500 nm to 10 μm in diameter, enclosed in an oil environment. An increasing demand for bigger emulsions has led us to investigate new techniques for fabricating fluidic devices allowing a better control over the final size of the droplets. An easy, cheap, reproducible and fast technology for generating emulsions in the range of 100s μm with high throughout (up to mL/h) is reported. Simply using pipette tips and tubing, an innovative microfluidic device was fabricated, able to synthetise water-in-oil emulsions within the range 50 - 500 _μm and double emulsions. These new emulsions are currently used for the synthesis of highly porous polymers beads from High Internal Phase Emulsion (HIPE). These beads will find high potential in 3D cell culture due to their high porosity (up to 90%) and pore size (from 5 to 30μm).

Preparation of stimulus responsive multiple emulsions by membrane emulsification using con a as biochemical sensor.

PubMed

Piacentini, Emma; Drioli, Enrico; Giorno, Lidietta

2011-04-01

In this work, a novel strategy for the controlled fabrication of biomolecular stimulus responsive water-in-oil-in-water (W/O/W) multiple emulsion using the membrane emulsification process was investigated. The emulsions interface was functionalized with a biomolecule able to function as a receptor for a target compound. The interaction between the biomolecular receptor and target stimulus activated the release of bioactive molecules contained within the structured emulsion. A glucose sensitive emulsion was investigated as a model study case. Concanavalin A (Con A) was used as the biomolecular glucose sensor. Various physicochemical strategies for stimulus responsive materials formulation are available in literature, but the preparation of biomolecule-responsive emulsions has been explored for the first time in this paper. The development of novel drug delivery systems requires advanced and highly precise techniques to obtain their particular properties and targeting requirements. The present study has proven the flexibility and suitability of membrane emulsification for the preparation of stable and functional multiple emulsions containing Con A as interfacial biomolecular receptor able to activate the release of a bioactive molecule as a consequence of interaction with the glucose target molecule. The influence of emulsion interfacial composition and membrane emulsification operating conditions on droplets stability and functional properties have been investigated. The release of the bioactive molecule as a function of glucose stimulus and its concentration has been demonstrated. Copyright © 2010 Wiley Periodicals, Inc.

Emulsion Solvent Evaporation-Induced Self-Assembly of Block Copolymers Containing pH-Sensitive Block.

PubMed

Wu, Yuqing; Wang, Ke; Tan, Haiying; Xu, Jiangping; Zhu, Jintao

2017-09-26

A simple yet efficient method is developed to manipulate the self-assembly of pH-sensitive block copolymers (BCPs) confined in emulsion droplets. Addition of acid induces significant variation in morphological transition (e.g., structure and surface composition changes) of the polystyrene-block-poly(4-vinylpyridine) (PS-b-P4VP) assemblies, due to the hydrophobic-hydrophilic transition of the pH-sensitive P4VP block via protonation. In the case of pH > pKa (P4VP) (pKa (P4VP) = 4.8), the BCPs can self-assemble into pupa-like particles because of the nearly neutral wetting of PS and P4VP blocks at the oil/water interface. As expected, onion-like particles obtained when pH is slightly lower than pKa (P4VP) (e.g., pH = 3.00), due to the interfacial affinity to the weakly hydrophilic P4VP block. Interestingly, when pH was further decreased to ∼2.5, interfacial instability of the emulsion droplets was observed, and each emulsion droplet generated nanoscale assemblies including vesicles, worm-like and/or spherical micelles rather than a nanostructured microparticle. Furthermore, homopolymer with different molecular weights and addition ratio are employed to adjust the interactions among copolymer blocks. By this means, particles with hierarchical structures can be obtained. Moreover, owing to the kinetically controlled processing, we found that temperature and stirring speed, which can significantly affect the kinetics of the evaporation of organic solvent and the formation of particles, played a key role in the morphology of the assemblies. We believe that manipulation of the property for the aqueous phase is a promising strategy to rationally design and fabricate polymeric assemblies with desirable shapes and internal structures.

Biodegradable metal adsorbent synthesized by graft polymerization onto nonwoven cotton fabric

NASA Astrophysics Data System (ADS)

Sekine, Ayako; Seko, Noriaki; Tamada, Masao; Suzuki, Yoshio

2010-01-01

A fibrous adsorbent for Hg ions was synthesized by radiation-induced emulsion graft polymerization of glycidyl methacrylate (GMA) onto a nonwoven cotton fabric and subsequent chemical modification. The optimal pre-irradiation dose for initiation of the graft polymerization of GMA, which minimized the effects of radiation damage on the mechanical strength of the nonwoven cotton fabric, was found to be 10 kGy. The GMA-grafted nonwoven cotton fabric was subsequently modified with ethylenediamine (EDA) or diethylenetriamine (DETA) to obtain a Hg adsorbent. The resulting amine-type adsorbents were evaluated for batch and continuous adsorption of Hg. In batch adsorption, the distribution coefficients of Hg reached 1.9×10 5 and 1.0×10 5 for EDA- and DETA-type adsorbents, respectively. A column packed with EDA-type adsorbent removed Hg from 1.8 ppm Hg solution at a space velocity of 100 h -1, which corresponds to 16,000 times the volume of the packed adsorbent. The adsorbed Hg on the EDA-type adsorbent could be completely eluted by 1 M HCl solution. A microbial oxidative degradation test revealed that the EDA-type adsorbent is biodegradable.

A technique for improved maxillary record base adaptation through controlled polymerization of light-activated dental resins.

PubMed

Hopkins, D S; Phoenix, R D; Abrahamsen, T C

1997-09-01

A technique for the fabrication of light-activated maxillary record bases is described. The use of a segmental polymerization process provides improved palatal adaptation by minimizing the effects of polymerization shrinkage. Utilization of this technique results in record bases that are well adapted to the corresponding master casts.

Micellar emulsions composed of mPEG-PCL/MCT as novel nanocarriers for systemic delivery of genistein: a comparative study with micelles

PubMed Central

Zhang, Tianpeng; Wang, Huan; Ye, Yanghuan; Zhang, Xingwang; Wu, Baojian

2015-01-01

Polymeric micelles receive considerable attention as drug delivery vehicles, depending on the versatility in drug solubilization and targeting therapy. However, their use invariably suffers with poor stability both in in vitro and in vivo conditions. Here, we aimed to develop a novel nanocarrier (micellar emulsions, MEs) for a systemic delivery of genistein (Gen), a poorly soluble anticancer agent. Gen-loaded MEs (Gen-MEs) were prepared from methoxy poly(ethylene glycol)-block-(ε-caprolactone) and medium-chain triglycerides (MCT) by solvent-diffusion technique. Nanocarriers were characterized by dynamic light scattering, transmission electron microscopy, and in vitro release. The resulting Gen-MEs were approximately 46 nm in particle size with a narrow distribution. Gen-MEs produced a different in vitro release profile from the counterpart of Gen-ME. The incorporation of MCT significantly enhanced the stability of nanoparticles against dilution with simulated body fluid. Pharmacokinetic study revealed that MEs could notably extend the mean retention time of Gen, 1.57- and 7.38-fold as long as that of micelles and solution formulation, respectively, following intravenous injection. Furthermore, MEs markedly increased the elimination half-life (t1/2β) of Gen, which was 2.63-fold larger than that of Gen solution. Interestingly, Gen distribution in the liver and kidney for MEs group was significantly low relative to the micelle group in the first 2 hours, indicating less perfusion in such two tissues, which well accorded with the elongated mean retention time. Our findings suggested that MEs may be promising carriers as an alternative of micelles to systemically deliver poorly soluble drugs. PMID:26491290

Humid Heat Autoclaving of Hybrid Nanoparticles Achieved by Decreased Nanoparticle Concentration and Improved Nanoparticle Stability Using Medium Chain Triglycerides as a Modifier.

PubMed

Gou, Jingxin; Chao, Yanhui; Liang, Yuheng; Zhang, Ning; He, Haibing; Yin, Tian; Zhang, Yu; Xu, Hui; Tang, Xing

2016-09-01

Humid heat autoclaving is a facile technique widely used in the sterilization of injections, but the high temperature employed would destroy nanoparticles composed of biodegradable polymers. The aim of this study was to investigate whether incorporation of medium chain triglycerides (MCT) could stabilize nanoparticles composed of poly (ethylene glycol)-b-polycaprolactone (PEG-b-PCL) during autoclaving (121°C, 10 min). Polymeric nanoparticles with different MCT contents were prepared by dialysis. Block copolymer degradation was studied by GPC. The critical aggregation concentrations of nanoparticles at different temperatures were determined using pyrene fluorescence. The size, morphology and weight averaged molecular weight of pristine/autoclaved nanoparticles were studied using DLS, TEM and SLS, respectively. Drug loading content and release profile were determined using RP-HPLC. The protecting effect of MCT on nanoparticles was dependent on the amount of MCT incorporated. Nanoparticles with high MCT contents, which assumed an emulsion-like morphology, showed reduced block copolymer degradation and particle disassociation after incubation at 100°C for 24 h. Nanoparticles with high MCT content showed the lowest critical aggregation concentration (CAC) under either room temperature or 60°C and the lowest particle concentration among all samples. And the particle size, drug loading content, physical stability and release profile of nanoparticles with high MCT contents remained nearly unchanged after autoclaving. Incorporation of high amount of MCT changed the morphology of PEG-b-PCL based nanoparticles to an emulsion-like structure and the nanoparticles prepared could withstand autoclaving due to improved particle stability and decreased particle concentration caused by MCT incorporation.

Indinavir-loaded pH-sensitive microparticles for taste masking: toward extemporaneous pediatric anti-HIV/AIDS liquid formulations with improved patient compliance.

PubMed

Chiappetta, Diego A; Carcaboso, Angel M; Bregni, Carlos; Rubio, Modesto; Bramuglia, Guillermo; Sosnik, Alejandro

2009-01-01

The aim of this work was to develop indinavir pediatric anti-HIV/AIDS formulations enabling convenient dose adjustment, ease of oral administration, and improved organoleptic properties by means of the generation of drug-loaded microparticles made of a polymer that is insoluble under intake conditions and dissolves fast in the stomach in order to completely release the active agent. Indinavir-loaded microparticles made of a pH-dependent polymeric excipient soluble at pH < 5, Eudragit E100, were prepared using a double emulsion solvent diffusion technique and the in vitro release profiles characterized. Finally, taste masking properties were evaluated in blind randomized sensory experiments by ten healthy human volunteers. The use of a w/o/o emulsion system resulted in indinavir loads around 90%. Thermal analysis of the microparticles by differential scanning calorimetry revealed that indinavir appeared mainly dispersed at the molecular level. Concentrations of residual organic solvents as determined by gas chromatography were below the upper limits specified by the European Pharmacopeia for pharmaceutical oral formulations. Then, the behavior of drug-containing microparticles in aqueous media at different pH values was assessed. While they selectively dissolved in gastric-like medium, in tap water (intake conditions), the matrix remained almost unchanged and efficiently prevented drug dissolution. Finally, sensoring taste tests performed by volunteers indicated that systems with indinavir loads approximately 15% displayed acceptable taste. This work explored the production of indinavir-containing microparticles based on a common pharmaceutical excipient as a means for the improvement of medicines of drugs involved in the treatment of HIV/AIDS. For systems containing about 15% drug, taste studies confirmed the acceptability of the formulation. In pediatric regimes, this composition would require an acceptable amount of formulation (0.7-1.5 g).

Retention of denture bases fabricated by three different processing techniques – An in vivo study

PubMed Central

Chalapathi Kumar, V. H.; Surapaneni, Hemchand; Ravikiran, V.; Chandra, B. Sarat; Balusu, Srilatha; Reddy, V. Naveen

2016-01-01

Aim: Distortion due to Polymerization shrinkage compromises the retention. To evaluate the amount of retention of denture bases fabricated by conventional, anchorized, and injection molding polymerization techniques. Materials and Methods: Ten completely edentulous patients were selected, impressions were made, and master cast obtained was duplicated to fabricate denture bases by three polymerization techniques. Loop was attached to the finished denture bases to estimate the force required to dislodge them by retention apparatus. Readings were subjected to nonparametric Friedman two-way analysis of variance followed by Bonferroni correction methods and Wilcoxon matched-pairs signed-ranks test. Results: Denture bases fabricated by injection molding (3740 g), anchorized techniques (2913 g) recorded greater retention values than conventional technique (2468 g). Significant difference was seen between these techniques. Conclusions: Denture bases obtained by injection molding polymerization technique exhibited maximum retention, followed by anchorized technique, and least retention was seen in conventional molding technique. PMID:27382542

Making Polymeric Microspheres

NASA Technical Reports Server (NTRS)

Rhim, Won-Kyu; Hyson, Michael T.; Chung, Sang-Kun; Colvin, Michael S.; Chang, Manchium

1989-01-01

Combination of advanced techniques yields uniform particles for biomedical applications. Process combines ink-jet and irradiation/freeze-polymerization techniques to make polymeric microspheres of uniform size in diameters from 100 to 400 micrometer. Microspheres used in chromatography, cell sorting, cell labeling, and manufacture of pharmaceutical materials.

Precise measurements of droplet-droplet contact forces in quasi-2D emulsions

NASA Astrophysics Data System (ADS)

Lowensohn, Janna; Orellana, Carlos; Weeks, Eric

2015-03-01

We use microscopy to visualize a quasi-2D oil-in-water emulsion confined between two parallel slides. We then use the droplet shapes to infer the forces they exert on each other. To calibrate our force law, we set up an emulsion in a tilted sample chamber so that the droplets feel a known buoyant force. By correlating radius of the droplet and length of contacts with the buoyant forces, we validate our empirical force law. We improve upon prior work in our lab by using a high-resolution camera to image each droplet multiple times, thus providing sub-pixel resolution and reducing the noise. Our new technique identifies contact forces with only a 1% uncertainty, five times better than prior work. We demonstrate the utility of our technique by examining the normal modes of the droplet contact network in our samples.

Treatment of a waste oil-in-water emulsion from a copper-rolling process by ultrafiltration and vacuum evaporation.

PubMed

Gutiérrez, Gemma; Lobo, Alberto; Benito, José M; Coca, José; Pazos, Carmen

2011-01-30

A process is proposed for the treatment of a waste oil-in-water (O/W) emulsion generated in an industrial copper-rolling operation. The use of demulsifier agents improves the subsequent treatment by techniques such as ultrafiltration (UF) or evaporation. The effluent COD is reduced up to 50% when the O/W emulsion is treated by UF using a flat 30 nm TiO(2) ceramic membrane (ΔP = 0.1 MPa) and up to 70% when it is treated by vacuum evaporation, after an emulsion destabilization pretreatment in both cases. Increases in the UF permeate flux and in the evaporation rate are observed when a chemical demulsifier is used in the pretreatment step. A combined process consisting of destabilization/settling, UF, and vacuum evaporation can yield a very high-quality aqueous effluent that could be used for process cooling or emulsion reformulation. Copyright © 2010 Elsevier B.V. All rights reserved.

Industrywide studies report of an in-depth survey at Copolymer Rubber and Chemical Corporation, Baton Rouge, Louisiana

DOE Office of Scientific and Technical Information (OSTI.GOV)

Krishnan, E.R.; Fajen, J.M.

1987-05-08

An in depth industrial hygiene survey was conducted at the Copolymer Rubber and Chemical Corporation located in Baton Rouge, Louisiana. The facility produced styrene-butadiene rubber and nitrile-butadiene rubber by continuous emulsion polymerization. The ultimate use of this product was for the manufacture of tire and rubber products. The authors recommend that leaking pumps which can present a potential for 1,3-butadiene exposure in the tank farm and recovery areas should be controlled through the use of dual mechanical seals. Employees assigned to maintenance tasks should use respirators with organic vapor cartridges.

Colloidal crystal beads composed of core-shell particles for multiplex bioassay.

PubMed

Xu, Hua; Zhu, Cun; Zhao, Yuanjin; Zhao, Xiangwei; Hu, Jing; Gu, Zhongze

2009-04-01

A convenient method was developed to fabricate colloidal crystal beads (CCBs) with tough mechanical strength, which was used as encoded carriers for multiplex bioassay. The latex particles used for the construction of the CCBs were designed with a rigid core PS and a elastomeric shell poly(MMA/EA/MAA), and were prepared via one-step soap-free emulsion polymerization. The as-above-prepared CCBs were thermo-treated to drive the elastomeric shells of adjacent latex particles joining together. It was found that the coalescence of latex particles can greatly improve the mechanical strength of the CCBs for multiplex bioassay.

WE-AB-BRA-03: Non-Invasive Controlled Release from Implantable Hydrogel Scaffolds Using Ultrasound

DOE Office of Scientific and Technical Information (OSTI.GOV)

Moncion, A; Kripfgans, O.D; Putnam, A.J

Purpose: To control release of a model payload in acoustically responsive scaffolds (ARSs) using focused ultrasound (FUS). Methods: Fluorescently-labeled dextran (10 kDa) was encapsulated in sonosensitive perfluorocarbon (C{sub 6}F{sub 14} or C{sub 5}F{sub 12}) double emulsions (mean diameter: 2.9±0.1 µm). For in vitro release studies, 0.5 mL ARSs (10 mg/mL fibrin, 1% (v/v) emulsion) were polymerized in 24 well plates and covered with 0.5 mL medium. Starting one day after polymerization, ARSs were exposed to FUS (2.5 MHz, Pr = 8 MPa, 13 cycles, 100 Hz PRF) for 2 min daily. The amount of dextran released into the media wasmore » quantified. For in vivo studies, 0.25 mL ARSs were prepared as described previously and injected subcutaneously in the lower back of BALB/c mice. After polymerization, a subset of the implanted ARSs were exposed to FUS (as previously described). Animals were imaged longitudinally using a fluorescence imaging system to quantify the amount of dextran released from the ARSs. Results: In vitro: Over 6 days, +FUS displayed an 8.2-fold increase in dextran release compared to −FUS (−FUS: 2.7±0.6%; +FUS: 22.2±3.0%) for C{sub 6}F{sub 14} ARSs, and a 6.7-fold increase (−FUS: 5.0±0.8%; +FUS: 38.5±1.6%) for C{sub 5}F{sub 12}:C{sub 6}F{sub 14} ARSs. In vivo: +FUS displayed statistically greater dextran release compared to −FUS one day after implantation for C{sub 5}F{sub 12}:C{sub 6}F{sub 14} ARSs (−FUS: 55.1±1.5%; +FUS: 74.1±2.2%) and three days after implantation for C{sub 6}F{sub 14} ARSs (−FUS: 1.4±6.5%; +FUS: 30.4±5.4%). Conclusion: FUS enables non-invasive control of payload release from an ARS, which could benefit growth factor delivery for tissue regeneration. ARS are versatile due to their tunability (i.e. stiffness, emulsion composition, FUS pressure, FUS frequency, etc.) and can be modified to for optimal payload release. Future work will optimize ARS formulations for in vivo use to minimize payload release in the absence of FUS. This work was supported by NIH Grant R21 AR065010 (M.L. Fabiilli) and the Basic Radiologic Sciences Innovative Research Award (M.L. Fabiilli). A. Moncion is supported by the National Science Foundation Graduate Student Research Fellowship (Grant DGE 1256260).« less

Double emulsion formation through hierarchical flow-focusing microchannel

NASA Astrophysics Data System (ADS)

Azarmanesh, Milad; Farhadi, Mousa; Azizian, Pooya

2016-03-01

A microfluidic device is presented for creating double emulsions, controlling their sizes and also manipulating encapsulation processes. As a result of three immiscible liquids' interaction using dripping instability, double emulsions can be produced elegantly. Effects of dimensionless numbers are investigated which are Weber number of the inner phase (Wein), Capillary number of the inner droplet (Cain), and Capillary number of the outer droplet (Caout). They affect the formation process, inner and outer droplet size, and separation frequency. Direct numerical simulation of governing equations was done using volume of fluid method and adaptive mesh refinement technique. Two kinds of double emulsion formation, the two-step and the one-step, were simulated in which the thickness of the sheath of double emulsions can be adjusted. Altering each dimensionless number will change detachment location, outer droplet size and droplet formation period. Moreover, the decussate regime of the double-emulsion/empty-droplet is observed in low Wein. This phenomenon can be obtained by adjusting the Wein in which the maximum size of the sheath is discovered. Also, the results show that Cain has significant influence on the outer droplet size in the two-step process, while Caout affects the sheath in the one-step formation considerably.

Physicochemical characterisation of β-carotene emulsion stabilised by covalent complexes of α-lactalbumin with (-)-epigallocatechin gallate or chlorogenic acid.

PubMed

Wang, Xiaoya; Liu, Fuguo; Liu, Lei; Wei, Zihao; Yuan, Fang; Gao, Yanxiang

2015-04-15

In this study the impact of covalent complexes of α-lactalbumin (α-La) with (-)-epigallocatechin gallate (EGCG) or chlorogenic acid (CA) was investigated on the physicochemical properties of β-carotene oil-in-water emulsions. EGCG, or CA, was covalently linked to α-La at pH 8.0, as evidenced by increased total phenolic content and declined fluorescence intensity. Compared with those stabilised by α-La alone and α-La-CA or EGCG mixture, the emulsion stabilised by the α-La-EGCG covalent complex exhibited the least changes in particle size and transmission profiles, using a novel centrifugal sedimentation technique, indicating an improvement in the physical stability. The least degradation of β-carotene occurred in the emulsion stabilised with the α-La-EGCG covalent complex when stored at 25 °C. These results implied that protein-polyphenol covalent complexes were able to enhance the physical stability of β-carotene emulsion and inhibit the degradation of β-carotene in oil-in-water emulsion, and the effect was influenced by the types of the phenolic compounds. Copyright © 2014 Elsevier Ltd. All rights reserved.

Protein-based emulsion electrosprayed micro- and submicroparticles for the encapsulation and stabilization of thermosensitive hydrophobic bioactives.

PubMed

Gómez-Mascaraque, Laura G; López-Rubio, Amparo

2016-03-01

This work shows the potential of emulsion electrospraying of proteins using food-grade emulsions for the microencapsulation and enhanced protection of a model thermosensitive hydrophobic bioactive. Specifically, gelatin, a whey protein concentrate (WPC) and a soy protein isolate (SPI) were compared as emulsion stabilizers and wall matrices for encapsulation of α-linolenic acid. In a preliminary stage, soy bean oil was used as the hydrophobic component for the implementation of the emulsion electrospraying process, investigating the effect of protein type and emulsion protocol used (i.e. with or without ultrasound treatment) on colloidal stability. This oil was then substituted by the ω-3 fatty acid and the emulsions were processed by electrospraying and spray-drying, comparing both techniques. While the latter resulted in massive bioactive degradation, electrospraying proved to be a suitable alternative, achieving microencapsulation efficiencies (MEE) of up to ∼70%. Although gelatin yielded low MEEs due to the need of employing acetic acid for its processing by electrospraying, SPI and WPC achieved MEEs over 60% for the non-sonicated emulsions. Moreover, the degradation of α-linolenic acid at 80°C was significantly delayed when encapsulated within both matrices. Whilst less than an 8% of its alkene groups were detected after 27h of thermal treatment for free α-linolenic acid, up to 43% and 67% still remained intact within the electrosprayed SPI and WPC capsules, respectively. Copyright © 2015 Elsevier Inc. All rights reserved.

Hierarchically porous materials from layer-by-layer photopolymerization of high internal phase emulsions.

PubMed

Sušec, Maja; Ligon, Samuel Clark; Stampfl, Jürgen; Liska, Robert; Krajnc, Peter

2013-06-13

A combination of high internal phase emulsion (HIPE) templating and additive manufacturing technology (AMT) is applied for creating hierarchical porosity within an acrylate and acrylate/thiol-based polymer network. The photopolymerizable formulation is optimized to produce emulsions with a volume fraction of droplet phase greater than 80 vol%. Kinetic stability of the emulsions is sufficient enough to withstand in-mold curing or computer-controlled layer-by-layer stereolithography without phase separation. By including macroscale cellular cavities within the build file, a level of controlled porosity is created simultaneous to the formation of the porous microstructure of the polyHIPE. The hybrid HIPE-AMT technique thus provides hierarchically porous materials with mechanical properties tailored by the addition of thiol chain transfer agent. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Comparative Effect of Different Polymerization Techniques on the Flexural and Surface Properties of Acrylic Denture Bases.

PubMed

Gad, Mohammed M; Fouda, Shaimaa M; ArRejaie, Aws S; Al-Thobity, Ahmad M

2017-05-22

Polymerization techniques have been modified to improve physical and mechanical properties of polymethylmethacrylate (PMMA) denture base, as have the laboratory procedures that facilitate denture construction techniques. The purpose of the present study was to investigate the effect of autoclave polymerization on flexural strength, elastic modulus, surface roughness, and the hardness of PMMA denture base resins. Major Base and Vertex Implacryl heat-polymerized acrylic resins were used to fabricate 180 specimens. According to the polymerization technique, tested groups were divided into: group I (water-bath polymerization), group II (short autoclave polymerization cycle, 60°C for 30 minutes, then 130°C for 10 minutes), and group III (long autoclave polymerization cycle, 60°C for 30 minutes, then 130°C for 20 minutes). Each group was divided into two subgroups based on the materials used. Flexural strength and elastic modulus were determined by a three-point bending test. Surface roughness and hardness were evaluated with a profilometer and Vickers hardness (VH) test, respectively. One-way ANOVA and the Tukey-Kramer multiple-comparison test were used for results analysis, which were statistically significant at p ≤ 0.05. Autoclave polymerization showed a significant increase in flexural strength and hardness of the two resins (p < 0.05). The elastic modulus showed a significant increase in the major base resin, while a significant decrease was seen for Vertex Implacryl in all groups (p < 0.05); however, there was no significant difference in surface roughness between autoclave polymerization and water-bath polymerization (p > 0.05). Autoclave polymerization significantly increased the flexural properties and hardness of PMMA denture bases, while the surface roughness was within acceptable clinical limits. For a long autoclave polymerization cycle, it could be used as an alternative to water-bath polymerization. © 2017 by the American College of Prosthodontists.

Ultrasonic energy input influence οn the production of sub-micron o/w emulsions containing whey protein and common stabilizers.

PubMed

Kaltsa, O; Michon, C; Yanniotis, S; Mandala, I

2013-05-01

Ultrasonication may be a cost-effective emulsion formation technique, but its impact on emulsion final structure and droplet size needs to be further investigated. Olive oil emulsions (20wt%) were formulated (pH∼7) using whey protein (3wt%), three kinds of hydrocolloids (0.1-0.5wt%) and two different emulsification energy inputs (single- and two-stage, methods A and B, respectively). Formula and energy input effects on emulsion performance are discussed. Emulsions stability was evaluated over a 10-day storage period at 5°C recording the turbidity profiles of the emulsions. Optical micrographs, droplet size and viscosity values were also obtained. A differential scanning calorimetric (DSC) multiple cool-heat cyclic method (40 to -40°C) was performed to examine stability via crystallization phenomena of the dispersed phase. Ultrasonication energy input duplication from 11kJ to 25kJ (method B) resulted in stable emulsions production (reduction of back scattering values, dBS∼1% after 10days of storage) at 0.5wt% concentration of any of the stabilizers used. At lower gum amount samples became unstable due to depletion flocculation phenomena, regardless of emulsification energy input used. High energy input during ultrasonic emulsification also resulted in sub-micron oil-droplets emulsions (D(50)=0.615μm compared to D(50)=1.3μm using method A) with narrower particle size distribution and in viscosity reduction. DSC experiments revealed no presence of bulk oil formation, suggesting stability for XG 0.5wt% emulsions prepared by both methods. Reduced enthalpy values found when method B was applied suggesting structural modifications produced by extensive ultrasonication. Change of ultrasonication conditions results in significant changes of oil droplet size and stability of the produced emulsions. Copyright © 2012 Elsevier B.V. All rights reserved.

Single Charged Particle Identification in Nuclear Emulsion Using Multiple Coulomb Scattering Method

NASA Astrophysics Data System (ADS)

Tint, Khin T.; Endo, Yoko; Hoshino, Kaoru; Ito, Hiroki; Itonaga, Kazunori; Kinbara, Shinji; Kobayashi, Hidetaka; Mishina, Akihiro; Soe, Myint K.; Yoshida, Junya; Nakazawa, Kazuma

Development of particle identification technique for single charged particles such as Ξ- hyperon, proton, K- and π- mesons is on-going by measuring multiple Coulomb scattering in nuclear emulsion. We generated several thousands of tracks of the single charged particles in nuclear emulsion stacks with GEANT 4 simulation and obtained second difference in constant Sagitta Method. We found that recognition of Ξ- hyperon from π- mesons is well satisfied, although that from K- and proton are a little difficult. On the other hand, the consistency of second difference of real Ξ- hyperon and pi meson tracks and simulation results were also confirmed.

Nanoparticles by spray drying using innovative new technology: the Büchi nano spray dryer B-90.

PubMed

Li, Xiang; Anton, Nicolas; Arpagaus, Cordin; Belleteix, Fabrice; Vandamme, Thierry F

2010-10-15

Spray drying technology is widely known and used to transform liquids (solutions, emulsions, suspension, slurries, pastes or even melts) into solid powders. Its main applications are found in the food, chemical and materials industries to enhance ingredient conservation, particle properties, powder handling and storage etc. However, spray drying can also be used for specific applications in the formulation of pharmaceuticals for drug delivery (e.g. particles for pulmonary delivery). Büchi is a reference in the development of spray drying technology, notably for laboratory scale devices. This study presents the Nano Spray Dryer B-90, a revolutionary new sprayer developed by Büchi, use of which can lower the size of the produced dried particles by an order of magnitude attaining submicron sizes. In this paper, results are presented with a panel of five representative polymeric wall materials (arabic gum, whey protein, polyvinyl alcohol, modified starch, and maltodextrin) and the potentials to encapsulate nano-emulsions, or to formulate nano-crystals (e.g. from furosemide) are also shown. Copyright © 2010 Elsevier B.V. All rights reserved.

Comparison of In Situ Polymerization and Solution-Dispersion Techniques in the Preparation of Polyimide/Montmorillonite (MMT) Nanocomposites

PubMed Central

Ahmad, Mansor Bin; Gharayebi, Yadollah; Salit, Mohd. Sapuan; Hussein, Mohd. Zobir; Shameli, Kamyar

2011-01-01

In this paper, Polyimide/Montmorillonite Nanocomposites (PI/MMT NCs), based on aromatic diamine (4-Aminophenyl sulfone) (APS) and aromatic dianhydride (3,3′,4,4′-benzophenonetetracarboxylic dianhydride) (BTDA) were prepared using in situ polymerization and solution-dispersion techniques. The prepared PI/MMT NCs films were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). The XRD results showed that at the content of 1.0 wt % Organo Montmorillonite (OMMT) for two techniques and 3.0 wt % OMMT for the in situ polymerization technique, the OMMT was well-intercalated, exfoliated and dispersed into polyimide matrix. The OMMT agglomerated when its amount exceeded 10 wt % and 3.0 wt % for solution-dispersion and in situ polymerization techniques respectively. These results were confirmed by the TEM images of the prepared PI/MMT NCs. The TGA thermograms indicated that thermal stability of prepared PI/MMT NCs were increased with the increase of loading that, the effect is higher for the samples prepared by in situ polymerization technique. PMID:22016643

Comparison of in situ polymerization and solution-dispersion techniques in the preparation of Polyimide/Montmorillonite (MMT) Nanocomposites.

PubMed

Ahmad, Mansor Bin; Gharayebi, Yadollah; Salit, Mohd Sapuan; Hussein, Mohd Zobir; Shameli, Kamyar

2011-01-01

In this paper, Polyimide/Montmorillonite Nanocomposites (PI/MMT NCs), based on aromatic diamine (4-Aminophenyl sulfone) (APS) and aromatic dianhydride (3,3',4,4'-benzophenonetetracarboxylic dianhydride) (BTDA) were prepared using in situ polymerization and solution-dispersion techniques. The prepared PI/MMT NCs films were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). The XRD results showed that at the content of 1.0 wt % Organo Montmorillonite (OMMT) for two techniques and 3.0 wt % OMMT for the in situ polymerization technique, the OMMT was well-intercalated, exfoliated and dispersed into polyimide matrix. The OMMT agglomerated when its amount exceeded 10 wt % and 3.0 wt % for solution-dispersion and in situ polymerization techniques respectively. These results were confirmed by the TEM images of the prepared PI/MMT NCs. The TGA thermograms indicated that thermal stability of prepared PI/MMT NCs were increased with the increase of loading that, the effect is higher for the samples prepared by in situ polymerization technique.

Design and evaluation of a novel nanoparticulate-based formulation encapsulating a HIP complex of lysozyme.

PubMed

Gaudana, Ripal; Gokulgandhi, Mitan; Khurana, Varun; Kwatra, Deep; Mitra, Ashim K

2013-01-01

Formulation development of protein therapeutics using polymeric nanoparticles has found very little success in recent years. Major formulation challenges include rapid denaturation, susceptibility to lose bioactivity in presence of organic solvents and poor encapsulation in polymeric matrix. In the present study, we have prepared hydrophobic ion pairing (HIP) complex of lysozyme, a model protein, using dextran sulfate (DS) as a complexing polymer. We have optimized the process of formation and dissociation of HIP complex between lysozyme and DS. The effect of HIP complexation on enzymatic activity of lysozyme was also studied. Nanoparticles were prepared and characterized using spontaneous emulsion solvent diffusion method. Furthermore, we have also investigated release of lysozyme from nanoparticles along with its enzymatic activity. Results of this study indicate that nanoparticles can sustain the release of lysozyme without compromising its enzymatic activity. HIP complexation using a polymer may also be employed to formulate sustained release dosage forms of other macromolecules with enhanced encapsulation efficiency.

The study of size and stability of n-butylcyanoacrylate nanocapsule suspensions encapsulating green grass fragrance

NASA Astrophysics Data System (ADS)

Zhu, G. Y.; Lin, C. T.; Chen, J. M.; Lei, D. M.; Zhu, G. X.

2018-01-01

Green grass fragrance has been widely used in many fields. However, fragrances are volatile compounds that do not last long. In order to prolong its odor, nanocapsules encapsulated green grass fragrance were prepared. The paper deals with the preparation of green grass fragrance nanocapsules by emulsion polymerization. N-butylcyanoacrylate (BCA) with excellent biocompatibility and biodegradability was used as encapsulant. The nanocapsule suspension systems were characterized and its stability was investigated. The physicochemical properties of polymeric nanocapsules (average diameter and polydispersity) were evaluated as a function of time to assess the system stability. The result showed that the system (containing 0.8% of green grass fragrance, with a polydispersity index (PDI) near 0.1 and an average diameter in the range of 20-30 nm) was an ideal state and relatively stable. Besides, the distinction of stability of three nanocapsule suspensions with different green grass fragrance content was also obvious from scanning electron microscopy (SEM).

Development of eco-friendly submicron emulsions stabilized by a bio-derived gum.

PubMed

Pérez-Mosqueda, Luis María; Ramírez, Pablo; Trujillo-Cayado, Luis Alfonso; Santos, Jenifer; Muñoz, José

2014-11-01

Many traditional organic solvents are being gradually replaced by ecofriendly alternatives. D-Limonene is a terpenic (bio)-solvent that fulfils the requirements to be considered a green solvent. D-Limonene sub-micron emulsions suffer from Ostwald ripening destabilization. In this study, we examined the influence of the addition of a natural gum (rosin gum) to D-limonene in order to prevent Ostwald ripening. This contribution deals with the study of emulsions formulated with a mixture of D-limonene and rosin gum as dispersed phase and Pluronic PE9400 as emulsifier. The procedure followed for the development of these formulations was based on the application of product design principles. This led to the optimum ratio rosin gum/D-limonene and subsequently to the optimum surfactant concentration. The combination of different techniques (rheology, laser diffraction and multiple light scattering) was demonstrated to be a powerful tool to assist in the prediction of the emulsions destabilization process. Not only did the addition of rosin gum highly increase the stability of these emulsions by inhibiting the Ostwald ripening, but it also reduced the emulsions droplet size. Thus, we found that stable sub-micron D-limonene-in-water emulsions have been obtained in the range 3-6 wt% Pluronic PE-9400 by means of a single-step rotor/stator homogenizing process. Copyright © 2014 Elsevier B.V. All rights reserved.

Poly(lactic-co-glycolic acid) devices: Production and applications for sustained protein delivery.

PubMed

Lee, Parker W; Pokorski, Jonathan K

2018-03-13

Injectable or implantable poly(lactic-co-glycolic acid) (PLGA) devices for the sustained delivery of proteins have been widely studied and utilized to overcome the necessity of repeated administrations for therapeutic proteins due to poor pharmacokinetic profiles of macromolecular therapies. These devices can come in the form of microparticles, implants, or patches depending on the disease state and route of administration. Furthermore, the release rate can be tuned from weeks to months by controlling the polymer composition, geometry of the device, or introducing additives during device fabrication. Slow-release devices have become a very powerful tool for modern medicine. Production of these devices has initially focused on emulsion-based methods, relying on phase separation to encapsulate proteins within polymeric microparticles. Process parameters and the effect of additives have been thoroughly researched to ensure protein stability during device manufacturing and to control the release profile. Continuous fluidic production methods have also been utilized to create protein-laden PLGA devices through spray drying and electrospray production. Thermal processing of PLGA with solid proteins is an emerging production method that allows for continuous, high-throughput manufacturing of PLGA/protein devices. Overall, polymeric materials for protein delivery remain an emerging field of research for the creation of single administration treatments for a wide variety of disease. This review describes, in detail, methods to make PLGA devices, comparing traditional emulsion-based methods to emerging methods to fabricate protein-laden devices. This article is categorized under: Biology-Inspired Nanomaterials > Protein and Virus-Based Structures Implantable Materials and Surgical Technologies > Nanomaterials and Implants Biology-Inspired Nanomaterials > Peptide-Based Structures. © 2018 Wiley Periodicals, Inc.

Process evaluation and in vitro selectivity analysis of aptamer-drug polymeric formulation for targeted pharmaceutical delivery.

PubMed

Tan, Kei X; Lau, Sie Yon; Danquah, Michael K

2018-05-01

Targeted drug delivery is a promising strategy to promote effective delivery of conventional and emerging pharmaceuticals. The emergence of aptamers as superior targeting ligands to direct active drug molecules specifically to desired malignant cells has created new opportunities to enhance disease therapies. The application of biodegradable polymers as delivery carriers to develop aptamer-navigated drug delivery system is a promising approach to effectively deliver desired drug dosages to target cells. This study reports the development of a layer-by-layer aptamer-mediated drug delivery system (DPAP) via a w/o/w double emulsion technique homogenized by ultrasonication or magnetic stirring. Experimental results showed no significant differences in the biophysical characteristics of DPAP nanoparticles generated using the two homogenization techniques. The DPAP formulation demonstrated a strong targeting performance and selectivity towards its target receptor molecules in the presence of non-targets. The DPAP formulation demonstrated a controlled and sustained drug release profile under the conditions of pH 7 and temperature 37 °C. Also, the drug release rate of DPAP formulation was successfully accelerated under an endosomal acidic condition of ∼pH 5.5, indicating the potential to enhance drug delivery within the endosomal micro-environment. The findings from this work are useful to understanding polymer-aptamer-drug relationship and their impact on developing effective targeted delivery systems. Copyright © 2018 Elsevier Masson SAS. All rights reserved.

Targeted delivery of 10-hydroxycamptothecin to human breast cancers by cyclic RGD-modified lipid-polymer hybrid nanoparticles.

PubMed

Yang, Zhe; Luo, Xingen; Zhang, Xiaofang; Liu, Jie; Jiang, Qing

2013-04-01

Lipid-polymer hybrid nanoparticles (NPs) combining the positive attributes of both liposomes and polymeric NPs are increasingly being considered as promising candidates to carry therapeutic agents safely and efficiently into targeted sites. Herein, a modified emulsification technique was developed and optimized for the targeting lipid-polymer hybrid NPs fabrication; the surface properties and stability of the hybrid NPs were systematically investigated, which confirmed that the hybrid NPs consisted of a poly (lactide-co-glycolide) core with ∼90% surface coverage of the lipid monolayer and a ∼4.4 nm hydrated polyethylene glycol (PEG) shell. Optimization results showed that the lipid:polymer mass ratio and the lipid-PEG:lipid molar ratio could affect the size, lipid association efficiency and stability of hybrid NPs. Furthermore, a model chemotherapy drug, 10-hydroxycamptothecin, was encapsulated into hybrid NPs with a higher drug loading compared to PLGA NPs. Surface modification of the lipid layer and the PEG conjugated targeting ligand did not affect their drug release kinetics. Finally, the cytotoxicity and cellular uptake studies indicated that the lipid coverage and the c(RGDyk) conjugation of the hybrid NPs gained a significantly enhanced ability of cell killing and endocytosis. Our results suggested that lipid-polymer hybrid NPs prepared by the modified emulsion technique have great potential to be utilized as an engineered drug delivery system with precise control ability of surface targeting modification.

Coherent X-ray diffraction imaging of nanoengineered polymeric capsules

NASA Astrophysics Data System (ADS)

Erokhina, S.; Pastorino, L.; Di Lisa, D.; Kiiamov, A. G.; Faizullina, A. R.; Tayurskii, D. A.; Iannotta, S.; Erokhin, V.

2017-10-01

For the first time, nanoengineered polymeric capsules and their architecture have been studied with coherent X-ray diffraction imaging technique. The use of coherent X-ray diffraction imaging technique allowed us to analyze the samples immersed in a liquid. We report about the significant difference between polymeric capsule architectures under dry and liquid conditions.

Bioactive Hybrid Particles from Poly(D,L-lactide-co-glycolide) Nanoparticle Stabilized Lipid Droplets.

PubMed

Joyce, Paul; Whitby, Catherine P; Prestidge, Clive A

2015-08-12

Biodegradable and bioactive hybrid particles composed of poly(D,L-lactide-co-glycolide) (PLGA) nanoparticles and medium-chain triglycerides were prepared by spray drying lipid-in-water emulsions stabilized by PLGA nanoparticles, to form PLGA-lipid hybrid (PLH) microparticles approximately 5 μm in mean diameter. The nanoparticle stabilizer was varied and mannitol was also incorporated during the preparation to investigate the effect of stabilizer charge and cryoprotectant content on the particle microstructure. An in vitro lipolysis model was used to demonstrate the particles' bioactivity by manipulating the digestion kinetics of encapsulated lipid by pancreatic lipase in simulated gastrointestinal fluid. Lipid digestion kinetics were enhanced in PLH and PLGA-lipid-mannitol hybrid (PLMH) microparticles for both stabilizers, compared to a coarse emulsion, in biorelevant media. An optimal digestion rate was observed for the negatively charged PLMH system, evidenced by a 2-fold increase in the pseudo-first-order rate constant compared to a coarse emulsion. Improved microparticle redispersion, probed by dual dye confocal fluorescence microscopy, increased the available surface area of lipid for lipase adsorption, enhancing digestion kinetics. Thereby, lipase action was controlled in hybrid microparticles by altering the surface charge and carbohydrate content. Our results demonstrate that bioactive microparticles composed of versatile and biodegradable polymeric particles and oil droplets have great potential for use in smart food and nutrient delivery, as well as safer and more efficacious oral delivery of drugs and drug combinations.

Newly Developed Techniques on Polycondensation, Ring-Opening Polymerization and Polymer Modification: Focus on Poly(Lactic Acid)

PubMed Central

Hu, Yunzi; Daoud, Walid A.; Cheuk, Kevin Ka Leung; Lin, Carol Sze Ki

2016-01-01

Polycondensation and ring-opening polymerization are two important polymer synthesis methods. Poly(lactic acid), the most typical biodegradable polymer, has been researched extensively from 1900s. It is of significant importance to have an up-to-date review on the recent improvement in techniques for biodegradable polymers. This review takes poly(lactic acid) as the example to present newly developed polymer synthesis techniques on polycondensation and ring-opening polymerization reported in the recent decade (2005–2015) on the basis of industrial technique modifications and advanced laboratory research. Different polymerization methods, including various solvents, heating programs, reaction apparatus and catalyst systems, are summarized and compared with the current industrial production situation. Newly developed modification techniques for polymer properties improvement are also discussed based on the case of poly(lactic acid). PMID:28773260

Separation of oil-water-sludge emulsions coming from palm oil mill process through microwave techniques.

PubMed

Pérez-Páez, Rocío; Catalá-Civera, José Manuel; García-Baños, Beatriz; Castillo, Edgar F; Bastos, Johanna M; Zambrano, Luz S

2008-01-01

The palm oil mills extraction process requires the separation of oil-water-sludge emulsions. For this purpose, the use of sedimentation and/or centrifugation techniques have been required until now. However, significant losses persist in different process flows and new methods are needed to further decrease them, such as methods based on electromagnetic waves application. In the study, emulsions obtained from two flow processes, namely press liquor stream (PL) and recovered stream of the centrifugal step (RC), were exposed to microwave radiation with different exposure times. In the case of the press liquor stream, different oil/water dilution ratios were also studied. The sedimentation speed and efficiency were studied for the irradiated samples and compared to those obtained for the same fluids with no radiation. Also, chromatographic tests were performed on the recovered oil to determine the effect on the oil quality after microwave radiation. The obtained results allow us to conclude that microwave exposure during periods below 1 minute lead to better sedimentation speed and efficiency. It was observed that microwaves facilitate the break of the charges and polarities balances in the emulsions at considerably lower temperatures than the corresponding in the conventional process, without affecting the recovered oil quality.

Synthesis of Calcium Phosphate Composite Organogels by Using Emulsion Method for Dentine Occlusion Materials

NASA Astrophysics Data System (ADS)

Nopteeranupharp, C.; Akkarachaneeyakorn, K.; Songsasaen, A.

2018-03-01

Dentinal hypersensitivity (DH) is one of the most human’s problems caused by the erosion of enamel. There are many methods and materials to solve this problem. Calcium phosphate is an excellent alternative for curing this symptom because of its osteoconductivity, and biocompatibility properties. The low-cost and low-toxicity calcium phosphate nanogel was fabricated by using emulsion method and characterized by using TEM, EDX, and DLS techniques. The results showed that P123 (poly (ethylene oxide)19-block-Poly (propylene oxide)69-block-poly (ethylene oxide)19) has played a major role as template and gel formation, SDS was used as a surfactant to form water-in-oil emulsion nanodroplets with circle-like shape. Moreover, the ability of synthesised organogel to occlude the exposed dentine tubules was tested on the model of human’s dentine slices. The results showed that calcium phosphate composite organogel can be efficiently occluded on dentine slice, characterized by SEM technique, after 1 day.

Preparation of non-porous microspheres with high entrapment efficiency of proteins by a (water-in-oil)-in-oil emulsion technique.

PubMed

Viswanathan, N B; Thomas, P A; Pandit, J K; Kulkarni, M G; Mashelkar, R A

1999-03-08

Emulsification-solvent removal methods have been widely used for encapsulating bioactive macromolecules like proteins and polypeptides in biodegradable polymers. We report, a (water-in-oil)-in-oil emulsion technique wherein proteins and polypeptides differing in molecular weight and shape were encapsulated in polymers of current biomedical interest. When an oil was used as the processing medium in combination with a carefully selected mixed solvent system such that a stable (w/o1/o2 emulsion is formed and solvents are removed by a combination of extraction and evaporation, the entrapment efficiency was high and the product nonporous. The entrapment efficiency of globular proteins exceeded 90% while that of fibrous proteins was around 70%. Fracture studies revealed that the polymer matrix was dense. The mechanism of entrapment involved solvent-induced precipitation of the protein as the microspheres were being formed. The principle of the method will find use in preparation of non-porous polymer microparticles with reduced burst effect.

Hydrolase stabilization via entanglement in poly(propylene sulfide) nanoparticles: stability towards reactive oxygen species.

PubMed

Allen, Brett L; Johnson, Jermaine D; Walker, Jeremy P

2012-07-27

In the advancement of green syntheses and sustainable reactions, enzymatic biocatalysis offers extremely high reaction rates and selectivity that goes far beyond the reach of chemical catalysts; however, these enzymes suffer from typical environmental constraints, e.g. operational temperature, pH and tolerance to oxidative environments. A common hydrolase enzyme, diisopropylfluorophosphatase (DFPase, EC 3.1.8.2), has demonstrated a pronounced efficacy for the hydrolysis of a variety of substrates for potential toxin remediation, but suffers from the aforementioned limitations. As a means to enhance DFPase's stability in oxidative environments, enzymatic covalent immobilization within the polymeric matrix of poly(propylene sulfide) (PPS) nanoparticles was performed. By modifying the enzyme's exposed lysine residues via thiolation, DFPase is utilized as a comonomer/crosslinker in a mild emulsion polymerization. The resultant polymeric polysulfide shell acts as a 'sacrificial barrier' by first oxidizing to polysulfoxides and polysulfones, rendering DFPase in an active state. DFPase-PPS nanoparticles thus retain activity upon exposure to as high as 50 parts per million (ppm) of hypochlorous acid (HOCl), while native DFPase is observed as inactive at 500 parts per billion (ppb). This trend is also confirmed by enzyme-generated (chloroperoxidase (CPO), EC 1.11.1.10) reactive oxygen species (ROS) including both HOCl (3 ppm) and ClO(2) (100 ppm).

Occlusion of Sulfate-Based Diblock Copolymer Nanoparticles within Calcite: Effect of Varying the Surface Density of Anionic Stabilizer Chains.

PubMed

Ning, Yin; Fielding, Lee A; Ratcliffe, Liam P D; Wang, Yun-Wei; Meldrum, Fiona C; Armes, Steven P

2016-09-14

Polymerization-induced self-assembly (PISA) offers a highly versatile and efficient route to a wide range of organic nanoparticles. In this article, we demonstrate for the first time that poly(ammonium 2-sulfatoethyl methacrylate)-poly(benzyl methacrylate) [PSEM-PBzMA] diblock copolymer nanoparticles can be prepared with either a high or low PSEM stabilizer surface density using either RAFT dispersion polymerization in a 2:1 v/v ethanol/water mixture or RAFT aqueous emulsion polymerization, respectively. We then use these model nanoparticles to gain new insight into a key topic in materials chemistry: the occlusion of organic additives into inorganic crystals. Substantial differences are observed for the extent of occlusion of these two types of anionic nanoparticles into calcite (CaCO3), which serves as a suitable model host crystal. A low PSEM stabilizer surface density leads to uniform nanoparticle occlusion within calcite at up to 7.5% w/w (16% v/v), while minimal occlusion occurs when using nanoparticles with a high PSEM stabilizer surface density. This counter-intuitive observation suggests that an optimum anionic surface density is required for efficient occlusion, which provides a hitherto unexpected design rule for the incorporation of nanoparticles within crystals.

A Cost-effective and Reliable Method to Predict Mechanical Stress in Single-use and Standard Pumps

PubMed Central

Dittler, Ina; Dornfeld, Wolfgang; Schöb, Reto; Cocke, Jared; Rojahn, Jürgen; Kraume, Matthias; Eibl, Dieter

2015-01-01

Pumps are mainly used when transferring sterile culture broths in biopharmaceutical and biotechnological production processes. However, during the pumping process shear forces occur which can lead to qualitative and/or quantitative product loss. To calculate the mechanical stress with limited experimental expense, an oil-water emulsion system was used, whose suitability was demonstrated for drop size detections in bioreactors1. As drop breakup of the oil-water emulsion system is a function of mechanical stress, drop sizes need to be counted over the experimental time of shear stress investigations. In previous studies, the inline endoscopy has been shown to be an accurate and reliable measurement technique for drop size detections in liquid/liquid dispersions. The aim of this protocol is to show the suitability of the inline endoscopy technique for drop size measurements in pumping processes. In order to express the drop size, the Sauter mean diameter d32 was used as the representative diameter of drops in the oil-water emulsion. The results showed low variation in the Sauter mean diameters, which were quantified by standard deviations of below 15%, indicating the reliability of the measurement technique. PMID:26274765

Naproxen-imprinted xerogels in the micro- and nanospherical formsby emulsion technique.

PubMed

Ornelas, Mariana; Azenha, Manuel; Pereira, Carlos; Silva, A Fernando

2015-11-27

Naproxen-imprinted xerogels in the microspherical and nanospherical forms were prepared by W/O emulsion and microemulsion, respectively. The work evolved from a sol–gel mixture previously reported for bulk synthesis. It was relatively simple to convert the original sol–gel mixture to one amenable to emulsion technique. The microspheres thus produced presented mean diameter of 3.7 μm, surface area ranging 220–340 m2/g, selectivity factor 4.3 (against ibuprofen) and imprinting factor 61. A superior capacity (9.4 μmol/g) was found, when comparing with imprints obtained from similar pre-gelification mixtures. However, slow mass transfer kinetics was deduced from column efficiency results. Concerning the nanospherical format, which constituted the first example of the production of molecularly imprinted xerogels in that format by microemulsion technique, adapting the sol–gel mixture was troublesome. In the end, nanoparticles with diameter in the order of 10 nm were finally obtained, exhibiting good indications of an efficient molecular imprinting process. Future refinements are necessary to solve serious aggregation issues, before moving to more accurate characterization of the binding characteristics or to real applications of the nanospheres.

The application of pulse field gradient (PFG) NMR methods to characterize the efficiency of separation of water-in-crude oil emulsions.

PubMed

Marques, Debora Salomon; Sørland, Geir; Less, Simone; Vilagines, Regis

2018-02-15

Demulsification of water-in-crude oil emulsions is an essential and sometimes challenging procedure for crude oil processing facilities. Pulse field gradient (PFG) NMR techniques are known to monitor the dynamics of emulsion separation. This method has limitations that restrict its application to some crude oils. A comprehensive methodology applicable to all types of crude oil regardless of its viscosity, without assumptions, and providing a large number of data with fast measurements, is proposed in this paper. The coalescence and sedimentation of unstable emulsions was observed through simultaneous measurements of the evolution of the brine profile and droplet size distribution (DSD). Measurements of emulsions after stabilization, with and without the contribution of the free water layer, revealed the residual emulsified water quantity and location in the sample. A new, faster approach to separate the oil and water overlapping T 2 relaxation signals was demonstrated on real water-in-crude oil emulsions, using the root mean square displacement (RMSD) measured with the spoiler recovery and a loop of 13-interval pulsed field gradient stimulated echo (PFGSTE) oneshot sequences. The residual water within the crude oils after separation was determined and used to quantify the efficiency of the demulsifier used. Copyright © 2017 Elsevier Inc. All rights reserved.

Chromatic changes to artificial irises produced using different techniques

NASA Astrophysics Data System (ADS)

Bannwart, Lisiane Cristina; Goiato, Marcelo Coelho; dos Santos, Daniela Micheline; Moreno, Amália; Pesqueira, Aldiéris Alves; Haddad, Marcela Filié; Andreotti, Agda Marobo; de Medeiros, Rodrigo Antonio

2013-05-01

Ocular prostheses are important determinants of their users' aesthetic recovery and self-esteem. Because of use, ocular prostheses longevity is strongly affected by instability of the iris color due to polymerization. The goal of this study is to examine how the color of the artificial iris button is affected by different techniques of artificial wear and by the application of varnish following polymerization of the colorless acrylic resin that covers the colored paint. We produce 60 samples (n=10) according to the wear technique applied: conventional technique without varnish (PE); conventional technique with varnish (PEV); technique involving a prefabricated cap without varnish (CA); technique involving a prefabricated cap with varnish (CAV); technique involving inverted painting without varnish (PI); and technique involving inverted painting with varnish (PIV). Color readings using a spectrophotometer are taken before and after polymerization. We submitted the data obtained to analyses of variance and Tukey's test (P<0.05). The color test shows significant changes after polymerization in all groups. The PE and PI techniques have clinically acceptable values of ΔE, independent of whether we apply varnish to protect the paint. The PI technique produces the least color change, whereas the PE and CA techniques significantly improve color stability.

Poly-ε-caprolactone microspheres as a drug delivery system for cannabinoid administration: development, characterization and in vitro evaluation of their antitumoral efficacy.

PubMed

Hernán Pérez de la Ossa, D; Ligresti, A; Gil-Alegre, M E; Aberturas, M R; Molpeceres, J; Di Marzo, V; Torres Suárez, A I

2012-08-10

Cannabinoids show promise for the treatment of various medical conditions such as emesis, anorexia, pain, cancer, multiple sclerosis, Parkinson's disease and glaucoma. However, their high lipohilicity and instability complicate their handling and dosing, and restrict their use as pharmaceuticals. The objective of the present work was to assess the feasibility of developing cannabinoid loaded poly-ε-caprolactone (PCL) microparticles prepared by the oil-in-water emulsion-solvent evaporation technique as a suitable dosage form for their administration. Spherical microparticles with a size range of 20-50 μm, and high entrapment efficiency (around 100%) were obtained. Cannabidiol (CBD) dissolved in the polymeric matrix of the microspheres was slowly released in vitro within 10 days. In vitro cell viability studies demonstrated the antitumoral activity of CBD released from microparticles. After 4 and 7 days of incubation, CBD in microspheres significantly inhibited the growth of MDA-MB-231 cells by 60% as compared to the 50% attained with free drug. The results suggest that PCL microparticles could be an alternative delivery system for long-term cannabinoid administration, showing potential therapeutic advantages over free drug. Copyright © 2012 Elsevier B.V. All rights reserved.

Versatile antifouling polyethersulfone filtration membranes modified via surface grafting of zwitterionic polymers from a reactive amphiphilic copolymer additive.

PubMed

Zhao, Yi-Fan; Zhang, Pei-Bin; Sun, Jian; Liu, Cui-Jing; Yi, Zhuan; Zhu, Li-Ping; Xu, You-Yi

2015-06-15

Here we describe the development of versatile antifouling polyethersulfone (PES) filtration membranes modified via surface grafting of zwitterionic polymers from a reactive amphiphilic copolymer additive. Amphiphilic polyethersulfone-block-poly(2-hydroxyethyl methacrylate) (PES-b-PHEMA) was beforehand designed and used as the blending additive of PES membranes prepared by phase inversion technique. The surface enriched PHEMA blocks on membrane surface acted as an anchor to immobilize the initiating site. Poly(sulfobetaine methacrylate) (PSBMA) were subsequently grafted onto the PES blend membranes by surface-initiated atom transfer radical polymerization (SI-ATRP). The analysis of surface chemistry confirmed the successful grafting of zwitterionic PSBMA brushes on PES membrane surface. The resulted PES-g-PSBMA membranes were capable of separating proteins from protein solution and oil from oil/water emulsion efficiently. Furthermore, the modified membranes showed high hydrophilicity and strongly antifouling properties due to the incorporation of well-defined PSBMA layer. In addition, the PES-g-PSBMA membranes exhibited excellent blood compatibility and durability during the washing process. The developed antifouling PES membranes are versatile and can find their applications in protein filtration, blood purification and oil/water separation, etc. Copyright © 2015 Elsevier Inc. All rights reserved.

Castable three-dimensional stationary phase for electric field-driven applications

DOEpatents

Shepodd, Timothy J.; Whinnery, Jr., Leroy; Even, Jr., William R.

2005-01-25

A polymer material useful as the porous dielectric medium for microfluidic devices generally and electrokinetic pumps in particular. The polymer material is produced from an inverse (water-in-oil) emulsion that creates a 3-dimensional network characterized by small pores and high internal volume, characteristics that are particularly desirable for the dielectric medium for electrokinetic pumps. Further, the material can be cast-to-shape inside a microchannel. The use of bifunctional monomers provides for charge density within the polymer structure sufficient to support electroosmotic flow. The 3-dimensional polymeric material can also be covalently bound to the channel walls thereby making it suitable for high-pressure applications.

Castable three-dimensional stationary phase for electric field-driven applications

DOEpatents

Shepodd, Timothy J [Livermore, CA; Whinnery, Jr., Leroy; Even, Jr., William R.

2009-02-10

A polymer material useful as the porous dielectric medium for microfluidic devices generally and electrokinetic pumps in particular. The polymer material is produced from an inverse (water-in-oil) emulsion that creates a 3-dimensional network characterized by small pores and high internal volume, characteristics that are particularly desirable for the dielectric medium for electrokinetic pumps. Further, the material can be cast-to-shape inside a microchannel. The use of bifunctional monomers provides for charge density within the polymer structure sufficient to support electroosmotic flow. The 3-dimensional polymeric material can also be covalently bound to the channel walls thereby making it suitable for high-pressure applications.

Preparation of anionic polyurethane nanoparticles and blood compatible behaviors.

PubMed

Zhu, Qinshu; Wang, Yan; Zhou, Min; Mao, Chun; Huang, Xiaohua; Bao, Jianchun; Shen, Jian

2012-05-01

The anionic polyurethane nanoparticles (APU-NPs) were obtained by an emulsion polymerization method. It was found that the average size of the prepared APU-NPs is about 84 nm, and the APU-NPs have zeta-potential of -38.9 mV. The bulk characterization of synthesized APU-NPs was investigated by FTIR. The blood compatibility of APU-NPs was characterized by in vitro for coagulation tests, complement activation, platelet activation, cytotoxicity experiments, and hemolysis assay. The results showed that the APU-NPs synthesized in this paper are blood compatible with low level of cell cytotoxicity, and the results were significant for their potential use in vivo.

Biodegradable microparticles based on poly(D,L-lactide) as a protective transport system in ruminant digestion.

PubMed

Jay, Steven M; Peevy, Nolan J; Jenkins, Thomas C; Burg, Karen J L

2006-01-01

Despite its abundance in their diet, cattle are unable to directly digest cellulose. The bovine digestive tract overcomes this problem via the rumen, a portion of the stomach containing mixed anaerobic bacteria. These microbes, while breaking down foodstuffs, also perform undesirable processes such as biohydrogenation, in which unsaturated fatty acids become saturated, with deleterious cardiovascular effects. An approach to preventing this saturation entailing the use of polymeric microspheres to encapsulate feed supplements is proposed, with a single emulsion, solvent evaporation method used to formulate poly(D,L-lactide) microparticles for delivery of unsaturated fatty acids to ruminant abomasum.

Preparation, thermal property and morphology analysis of waterborne polyurethane-acrylate

NASA Astrophysics Data System (ADS)

Zhao, Zhenyu; Jing, Zefeng; Qiu, Fengxian; Dai, Yuting; Xu, Jicheng; Yu, Zongping; Yang, Pengfei

2017-01-01

A series of waterborne polyurethane-acrylate (WPUA) dispersions were prepared with isophorone diisocyanate (IPDI), polyether polyol (NJ-210), dimethylol propionic acid (DMPA), hydroxyethyl methyl acrylate (HEMA), different proportions of methyl methacrylate (MMA) and ethyl acrylate (MMA and EA) and initiating agent by the emulsion co-polymerization. The structures, thermal properties and morphology of WPUA films were characterized with FT-IR, DSC, SEM and AFM. Performances of the dispersions and films were studied by means of apparent viscidity, particle size and polydispersity, surface tension and mechanical properties. The obtained WPUA have great potential application such as coatings, leather finishing, adhesives, sealants, plastic coatings and wood finishes.

Atom Transfer Radical Polymerization of Functionalized Vinyl Monomers Using Perylene as a Visible Light Photocatalyst

PubMed Central

Theriot, Jordan C.; Ryan, Matthew D.; French, Tracy A.; Pearson, Ryan M.; Miyake, Garret M.

2016-01-01

A standardized technique for atom transfer radical polymerization of vinyl monomers using perylene as a visible-light photocatalyst is presented. The procedure is performed under an inert atmosphere using air- and water-exclusion techniques. The outcome of the polymerization is affected by the ratios of monomer, initiator, and catalyst used as well as the reaction concentration, solvent, and nature of the light source. Temporal control over the polymerization can be exercised by turning the visible light source off and on. Low dispersities of the resultant polymers as well as the ability to chain-extend to form block copolymers suggest control over the polymerization, while chain end-group analysis provides evidence supporting an atom-transfer radical polymerization mechanism. PMID:27166728

Physicochemical Properties and Chemical Stability of β-Carotene Bilayer Emulsion Coated with Bovine Serum Albumin and Arabic Gum Compared to Monolayer Emulsions.

PubMed

Sheng, Bulei; Li, Lin; Zhang, Xia; Jiao, Wenjuan; Zhao, Di; Wang, Xue; Wan, Liting; Li, Bing; Rong, Hui

2018-02-23

β-carotene is a lipophilic micronutrient that is considered beneficial to human health. However, there are some limitations in utilizing β-carotene in functional foods or dietary supplements currently because of its poor water dispersibility and chemical stability. A new type of β-carotene bilayer emulsion delivery system was prepared by a layer-by-layer electrostatic deposition technique, for which were chosen bovine serum albumin (BSA) as the inner emulsifier and Arabic gum (GA) as the outer emulsifier. The physicochemical properties of bilayer emulsions were mainly characterized by droplet size distribution, zeta potential, rheological behavior, Creaming Index (CI), and encapsulation ratio of β-carotene. Besides this, the effects of processing conditions (pH, thermal treatment, UV radiation, strong oxidant) and storage time on the chemical stability of bilayer emulsions were also evaluated. The bilayer emulsion had a small droplet size (221.27 ± 5.17 nm) and distribution (PDI = 0.23 ± 0.02), strong zeta potential (-30.37 ± 0.71 mV), good rheological behavior (with the highest viscosity that could reduce the possibility of flocculation) and physical stability (CI = 0), high β-carotene encapsulation ratio (94.35 ± 0.71%), and low interfacial tension (40.81 ± 0.86 mN/m). It also obtained better chemical stability under different environmental stresses when compared with monolayer emulsions studied, because it had a dense and thick bilayer structure.

How the multiple antioxidant properties of ascorbic acid affect lipid oxidation in oil-in-water emulsions.

PubMed

Uluata, Sibel; McClements, D Julian; Decker, Eric A

2015-02-18

Lipid oxidation is a serious problem for oil-containing food products because it negatively affects shelf life and nutritional composition. An antioxidant strategy commonly employed to prevent or delay oxidation in foods is to remove oxygen from the closed food-packaging system. An alternative technique is use of an edible oxygen scavenger to remove oxygen within the food. Ascorbic acid (AA) is a particularly promising antioxidant because of its natural label and multiple antioxidative functions. In this study, AA was tested as an oxygen scavenger in buffer and an oil-in-water (O/W) emulsion. The effects of transition metals on the ability of AA to scavenge oxygen were determined. Headspace oxygen decrease less than 1% in the medium-chain triacylglycerol (MCT) O/W emulsion system (pH 3 and 7). AA was able to almost completely remove dissolved oxygen (DO) in a buffered solution. Transition metals (Fe(2+) and Cu(+)) significantly accelerated the degradation of AA; however, iron and copper only increased DO depletion rates, by 10.6-16.4% from day 1 to 7, compared to the control. AA (2.5-20 mM) decreased DO in a 1% O/W emulsion system 32.0-64.0% and delayed the formation of headspace hexanal in the emulsion from 7 to over 20 days. This research shows that, when AA is used in an O/W emulsion system, oxidation of the emulsion system can be delay by multiple mechanisms.

Enhancing the Breadth and Efficacy of Therapeutic Vaccines for Breast Cancer

DTIC Science & Technology

2014-10-01

sequence data produced by the Slansky team following their single-cell emulsion RT-PCR technique; however, it can be packaged and shared for use...cell emulsion RT-PCR. Additional modifications were made to our epitope discovery workflow to increase efficacy of transcript and neoantigen candidate...the MiTCR [8] open source software package developed by MiLaboratory. MiTCR is a highly efficient and fast approach to CDR3 extraction, clonotype

Application of Advanced Nuclear Emulsion Technique to Fusion Neutron Diagnostics

NASA Astrophysics Data System (ADS)

Nakayama, Y.; Tomita, H.; Morishima, K.; Yamashita, F.; Hayashi, S.; Cheon, MunSeong; Isobe, M.; Ogawa, K.; Naka, T.; Nakano, T.; Nakamura, M.; Kawarabayashi, J.; Iguchi, T.; Ochiai, K.

In order to measure the 2.5 MeV neutrons produced by DD nuclear fusion reactions, we have developed a compact neutron detector based on nuclear emulsion. After optimization of development conditions, we evaluated the response of the detector to an accelerator-based DD neutron source. The absolute efficiency at an energy of 2.5 MeV was estimated to be (4.1±0.2)×10-6 tracks/neutron.

Surface Modification of Nanocellulose Substrates

NASA Astrophysics Data System (ADS)

Zoppe, Justin Orazio

Cellulose fibers constitute an important renewable raw material that is utilized in many commercial applications in non-food, paper, textiles and composite materials. Chemical functionalization is an important approach for improving the properties of cellulose based materials. Different approaches are used to graft polymeric chains onto cellulose substrates, which can be classified by two principal routes, namely 'grafting onto' or 'grafting from' methods. Never-dried cellulose nanocrystals (CNCs) or nanowhiskers produced from sulfuric acid hydrolysis of ramie fibers were used as substrates for surface chemical functionalization with various macromolecules. In addition, the use of cellulose nanocrystals to reinforce poly(epsilon-caprolactone) (PCL) nanofibers was studied. Chemical grafting with low molecular weight polycaprolactone diol onto cellulose nanocrystals was carried out in an attempt to improve the interfacial adhesion with the fiber matrix. Significant improvements in the mechanical properties of the nanofibers after reinforcement with unmodified cellulose nanocrystals were confirmed. Fiber webs from PCL reinforced with 2.5% unmodified CNCs showed ca. 1.5-fold increase in Young's modulus and ultimate strength compared to PCL webs. The CNCs were also grafted with poly(N-isopropylacrylamide) (poly(NiPAAm)) brushes via surface-initiated single-electron transfer living radical polymerization (SI-SETLRP) under various conditions at room temperature. The grafting process depended on the initiator and/or monomer concentrations used. No observable damage occurred to the CNCs after grafting, as determined by X-ray diffraction. Size exclusion chromatography analyses of polymer chains cleaved from the cellulose nanocrystals indicated that a higher degree of polymerization was achieved by increasing initiator or monomer loading, most likely caused by local heterogeneities yielding higher rates of polymerization. In addition, the colloidal stability and thermo-responsive behavior of poly(NiPAAm) brushes grafted from nanoparticles of CNCs of varying graft densities and molecular weights was investigated. Halo areas surrounding grafted CNCs that were adsorbed on silica and imaged with an AFM were indicative of the grafted polymer brushes. Aggregation of nanoparticles carrying grafts of high degree of polymerization was observed. The responsiveness of CNCs in liquid medium and as spin-coated films was determined by using light scattering, viscometry and Colloidal Probe Microscopy (CPM). Light transmittance measurements showed temperaturedependent aggregation originating from the different graft densities and molecular weights and a sharp increase in dispersion viscosity as the temperature approached the LCST. The lower critical solution temperature (LCST) of grafted poly(NiPAAm) brushes was found to decrease with the ionic strength as is the case of neat poly(NiPAAm) in aqueous solution. CPM in aqueous media for asymmetric systems consisting of thin films of CNCs and a colloidal silica probe showed the distinctive effects of the grafted polymer brushes on the interaction (repulsive and adhesive) forces. The origin of such forces was mainly electrostatic and steric in the case of bare and grafted CNCs, respectively. A decrease in the onset of attractive and adhesion forces of grafted CNCs films was observed with the ionic strength of the aqueous solution medium. The decreased mobility of polymer brushes upon partial collapse and decreased availability of hydrogen bonding sites with higher electrolyte concentration were hypothesized as main reasons for the less prominent polymer bridging between interacting surfaces. Finally, poly(NiPAAm)-g-CNCs were utilized as a Pickering emulsions stabilizer. All emulsions formed were oil-in-water confirmed by a drop test. Various drop sizes were obtained as characterized by laser scattering particle size analysis and optical microscopy. Anisotropic colloidal assemblies of grafted CNCs at the oil-water interface were observed in freeze-fractured samples via Transmission Electron Microscopy. Emulsions were stable for over three months at the time of writing this thesis, however rapidly broke above the LCST as determined by rheometry.

SHSG processing for three-wavelength HOEs recording in silver halide materials

NASA Astrophysics Data System (ADS)

Kim, Jong Man; Choi, Yoon S.; Bjelkhagen, Hans I.; Phillips, Nicholas J.

2002-06-01

The recording and processing technique for color HOEs in ultrafine-grain panchromatic silver halide emulsions is presented. It is possible to obtain high diffraction efficiency employing the silver halide sensitized gelatin (SHSG) process. SHSG holograms are similar to holograms recorded in dichromated gelatin (DCG). The drawback of DCG is its low sensitivity and limited spectral response. Panchromatic silver halide materials from Slavich can be processed in such a way that the final holograms have properties like a DCG hologram. The processing method or microvoid technique has been optimized for three laser- wavelength recordings in Slavich PFG-03C emulsion. For example, applying this new processing technique high- efficiency white holographic reflectors can be manufactured. The technique is also suitable for producing efficiency color display holograms. In particular, masters for mass production of color holograms or color HOEs can be performed by contact-copying into photopolymer materials because the reconstruction wavelengths are identical to the recording wavelengths.

Synthesis and polymerization of vinyl triazolium ionic liquids

DOEpatents

Luebke, David; Nulwala, Hunaid; Matyjaszewski, Krzysztof; Adzima, Brian

2018-05-15

Herein, we describe polymerized ionic liquids, demonstrate the synthesis of polymerized ionic liquids, and demonstrate the polymerization of triazolium monomers. One embodiment shows the polymeriazation of the triazolium monomers with bis(trifluoromethanesulfonyl)imide anions. In another embodiment we show the feasibility of copolymerizing with commodity monomers such as styrene using free radical polymerization techniques.

Selective boron delivery by intra-arterial injection of BSH-WOW emulsion in hepatic cancer model for neutron capture therapy

PubMed Central

Dewi, Novriana; Higashi, Syushi; Ikushima, Ichiro; Seguchi, Koji; Mizumachi, Ryoji; Murata, Yuji; Morishita, Yasuyuki; Shinohara, Atsuko; Mikado, Shoji; Yasuda, Nakahiro; Fujihara, Mitsuteru; Sakurai, Yuriko; Mouri, Kikue; Yanagawa, Masashi; Iizuka, Tomoya; Suzuki, Minoru; Sakurai, Yoshinori; Masunaga, Shin-ichiro; Tanaka, Hiroki; Matsukawa, Takehisa; Yokoyama, Kazuhito; Fujino, Takashi; Ogura, Koichi; Nonaka, Yasumasa; Sugiyama, Hirotaka; Kajiyama, Tetsuya; Yui, Sho; Nishimura, Ryohei; Ono, Koji; Takamoto, Sinichi; Nakajima, Jun; Ono, Minoru; Eriguchi, Masazumi; Hasumi, Kenichiro; Takahashi, Hiroyuki

2017-01-01

Objective: Boron neutron-capture therapy (BNCT) has been used to inhibit the growth of various types of cancers. In this study, we developed a 10BSH-entrapped water-in-oil-in-water (WOW) emulsion, evaluated it as a selective boron carrier for the possible application of BNCT in hepatocellular carcinoma treatment. Methods: We prepared the 10BSH-entrapped WOW emulsion using double emulsification technique and then evaluated the delivery efficacy by performing biodistribution experiment on VX-2 rabbit hepatic tumour model with comparison to iodized poppy-seed oil mix conventional emulsion. Neutron irradiation was carried out at Kyoto University Research Reactor with an average thermal neutron fluence of 5 × 1012 n cm−2. Morphological and pathological analyses were performed on Day 14 after neutron irradiation. Results: Biodistribution results have revealed that 10B atoms delivery with WOW emulsion was superior compared with those using iodized poppy-seed oil conventional emulsion. There was no dissemination in abdomen or lung metastasis observed after neutron irradiation in the groups treated with 10BSH-entrapped WOW emulsion, whereas many tumour nodules were recognized in the liver, abdominal cavity, peritoneum and bilateral lobes of the lung in the non-injected group. Conclusion: Tumour growth suppression and cancer-cell-killing effect was observed from the morphological and pathological analyses of the 10BSH-entrapped WOW emulsion-injected group, indicating its feasibility to be applied as a novel intra-arterial boron carrier for BNCT. Advances in knowledge: The results of the current study have shown that entrapped 10BSH has the potential to increase the range of therapies available for hepatocellular carcinoma which is considered to be one of the most difficult tumours to cure. PMID:28406315

Chemical approach to solvent removal during nanoencapsulation: its application to preparation of PLGA nanoparticles with non-halogenated solvent

NASA Astrophysics Data System (ADS)

Lee, Youngme; Sah, Eric; Sah, Hongkee

2015-11-01

The objective of this study was to develop a new oil-in-water emulsion-based nanoencapsulation method for the preparation of PLGA nanoparticles using a non-halogenated solvent. PLGA (60-150 mg) was dissolved in 3 ml of methyl propionate, which was vortexed with 4 ml of a 0.5-4 % polyvinyl alcohol solution. This premix was sonicated for 2 min, added into 30 ml of the aqueous polyvinyl alcohol solution, and reacted with 3 ml of 10 N NaOH. Solvent removal was achieved by the alkaline hydrolysis of methyl propionate dissolved in an aqueous phase into water-soluble methanol and sodium propionate. It was a simple but effective technique to quickly harden nanoemulsion droplets into nanoparticles. The appearing PLGA nanoparticles were recovered by ultracentrifugation and/or dialysis, lyophilized with trehalose, and redispersed by water. This nanoencapsulation technique permitted a control of their mean diameters over 151.7 ± 3.8 to 440.2 ± 22.2 nm at mild processing conditions. When the aqueous polyvinyl alcohol concentration was set at ≥1 %, nanoparticles showed uniform distributions with polydispersity indices below 0.1. There were no significant changes in their mean diameters and size distribution patterns before and after lyophilization. When mestranol was encapsulated into nanoparticles, the drug was completely nanoencapsulated: depending on experimental conditions, their encapsulation efficiencies were determined to be 99.4 ± 7.2 to 105.8 ± 6.3 %. This simple, facile nanoencapsulation technique might have versatile applications for the preparation of polymeric nanoparticulate dosage forms.

The calcium phosphate coating of soy lecithin nanoemulsion with performance in stability and as an oxygen carrier

NASA Astrophysics Data System (ADS)

Han, Kyu B.

This work studied the relationship between surfactant, oil, and water, by building ternary phase diagrams, the goal of which was to identify the oil-in-water phase composition. The resulting nano-sized emulsion was coated with dicalcium phosphate by utilizing the ionic affinity between calcium ions and the emulsion surface. Since the desired function of the particle is as an oxygen carrier, the particle stability, oxygen capacity, and oxygen release rate were investigated. The first step in the process was to construct ternary phase diagrams with 1,2-dioleoyl-sn-glycero-3-phosphate (DOPA) and soy derived lecithin. The results showed that the lecithin surfactant formed an oil-in-water phase region that was 36 times greater than that of DOPA. With the desired phase composition set, the lecithin emulsion was extruded, resulting in a well-dispersed nanosized particle. A pH titration study of the emulsion found an optimized calcium phosphate coating condition at pH 8.8, at which, the calcium ion had a greater affinity for the emulsion surface than phosphate. A Hill plot was used to show calcium cooperativeness on the emulsion surface which suggested one calcium ion binds to one lecithin molecule. The lecithin emulsion particles were then coated with calcium phosphate using a layering technique that allowed for careful control of the coating thickness. The overall particle hydrodynamic radius was consistent with the growth of the calcium phosphate coating, from 8 nm to 28 nm. This observation was further supported with cryo-TEM measurements. The stability of the coated emulsion was tested in conditions that simulate practical thermal, physical, and time-dependent conditions. Throughout the tests, the coated emulsion exhibited a constant mono-dispersed particle size, while the uncoated emulsion size fluctuated greatly and exhibited increased polydispersion. The fast mixing method with the stopped-flow apparatus was employed to test the product as an oxygen carrier, and it was shown that particles with thicker calcium phosphate coatings released smaller amounts of oxygen in a given timeframe. This study proved the hypothesis by showing a fundamental understanding of emulsion science, coating the flexible emulsion surface with a biocompatible material, and a strong particle performance with regard to stability and as an oxygen carrier.

Fabrication of novel silicone capsules with tunable mechanical properties by microfluidic techniques.

PubMed

Vilanova, Neus; Rodríguez-Abreu, Carlos; Fernández-Nieves, Alberto; Solans, Conxita

2013-06-12

A novel approach for the synthesis of silicone capsules using double W/O/W emulsions as templates is introduced. The low viscosity of the silicone precursors enables the use of microfluidic techniques to accurately control the size and morphology of the double emulsion droplets, which after cross-linking result in the desired monodisperse silicone capsules. Their shell thickness can be finely tuned, which in turn allows control over their permeability and mechanical properties; the latter are particularly important in a variety of practical applications where the capsules are subjected to large external forces. The potential of these capsules for controlled release is also demonstrated using a model hydrophilic substance.

Polymer/Pristine graphene based composites: from emulsions to strong, electrically conducting foams

DOE PAGES

Woltornist, Steven J.; Carrillo, Jan-Michael Y.; Xu, Thomas O.; ...

2015-01-21

The unique electrical, thermal, and mechanical properties of graphene make it a perfect candidate for applications in graphene/graphite based polymer composites, yet challenges due to the lack of solubility of pristine graphene/graphite in water and common organic solvents have limited its practical utilization. In this paper, we report a scalable and environmentally friendly technique to form water-in-oil type emulsions stabilized by overlapping pristine graphene sheets, enabling the synthesis of open cell foams containing a continuous graphitic network. Our approach utilizes the insolubility of graphene/graphite in both water and organic solvents and so does not require oxidation, reduction, surfactants, high boilingmore » solvents, chemical functionalization, or the input of large amounts of mechanical energy or heat. At the heart of our technique is the strong attraction of graphene to high-energy oil and water interfaces. This allows for the creation of stable water-in-oil emulsions with controlled droplet size and overlapping graphene sheets playing the role of surfactant by covering the droplet surface and stabilizing the interfaces with a thin graphitic skin. Finally, these emulsions are used as templates for the synthesis of open cell foams with densities below 0.35 g/cm 3 that exhibit remarkable mechanical and electrical properties including compressive moduli up to ~100 MPa, compressive strengths of over 8.3 MPa (1200 psi), and bulk conductivities approaching 7 S/m.« less

Optimization of cyanide extraction from wastewater using emulsion liquid membrane system by response surface methodology.

PubMed

Xue, Juan Qin; Liu, Ni Na; Li, Guo Ping; Dang, Long Tao

To solve the disposal problem of cyanide wastewater, removal of cyanide from wastewater using a water-in-oil emulsion type of emulsion liquid membrane (ELM) was studied in this work. Specifically, the effects of surfactant Span-80, carrier trioctylamine (TOA), stripping agent NaOH solution and the emulsion-to-external-phase-volume ratio on removal of cyanide were investigated. Removal of total cyanide was determined using the silver nitrate titration method. Regression analysis and optimization of the conditions were conducted using the Design-Expert software and response surface methodology (RSM). The actual cyanide removals and the removals predicted using RSM analysis were in close agreement, and the optimal conditions were determined to be as follows: the volume fraction of Span-80, 4% (v/v); the volume fraction of TOA, 4% (v/v); the concentration of NaOH, 1% (w/v); and the emulsion-to-external-phase volume ratio, 1:7. Under the optimum conditions, the removal of total cyanide was 95.07%, and the RSM predicted removal was 94.90%, with a small exception. The treatment of cyanide wastewater using an ELM is an effective technique for application in industry.

Surface modification of carbon fibers by a polyether sulfone emulsion sizing for increased interfacial adhesion with polyether sulfone

NASA Astrophysics Data System (ADS)

Yuan, Haojie; Zhang, Shouchun; Lu, Chunxiang

2014-10-01

Interests on carbon fiber-reinforced thermoplastic composites are growing rapidly, but the challenges with poor interfacial adhesion have slowed their adoption. In this work, a polyether sulfone (PES) emulsion sizing was prepared successfully for increased interfacial adhesion of carbon fiber/PES composites. To obtain a high-quality PES emulsion sizing, the key factor, emulsifier concentration, was studied by dynamic light scattering technique. The results demonstrated that the suitable weight ratio of PES to emulsifier was 8:3, and the resulting PES emulsion sizing had an average particle diameter of 117 nm and Zeta potential of -52.6 mV. After sizing, the surface oxygen-containing functional groups, free energy and wettability of carbon fibers increased significantly, which were advantageous to promote molecular-level contact between carbon fiber and PES. Finally, short beam shear tests were performed to evaluate the interfacial adhesion of carbon fiber/PES composites. The results indicated that PES emulsion sizing played a critical role for the enhanced interfacial adhesion in carbon fiber/PES composites, and a 26% increase of interlaminar shear strength was achieved, because of the improved fiber surface wettability and interfacial compatibility between carbon fiber and PES.

A general computation model based on inverse analysis principle used for rheological analysis of W/O rapeseed and soybean oil emulsions

NASA Astrophysics Data System (ADS)

Vintila, Iuliana; Gavrus, Adinel

2017-10-01

The present research paper proposes the validation of a rigorous computation model used as a numerical tool to identify rheological behavior of complex emulsions W/O. Considering a three-dimensional description of a general viscoplastic flow it is detailed the thermo-mechanical equations used to identify fluid or soft material's rheological laws starting from global experimental measurements. Analyses are conducted for complex emulsions W/O having generally a Bingham behavior using the shear stress - strain rate dependency based on a power law and using an improved analytical model. Experimental results are investigated in case of rheological behavior for crude and refined rapeseed/soybean oils and four types of corresponding W/O emulsions using different physical-chemical composition. The rheological behavior model was correlated with the thermo-mechanical analysis of a plane-plane rheometer, oil content, chemical composition, particle size and emulsifier's concentration. The parameters of rheological laws describing the industrial oils and the W/O concentrated emulsions behavior were computed from estimated shear stresses using a non-linear regression technique and from experimental torques using the inverse analysis tool designed by A. Gavrus (1992-2000).

An alkyl polyglucoside-mixed emulsifier as stabilizer of emulsion systems: the influence of colloidal structure on emulsions skin hydration potential.

PubMed

Savic, Snezana; Lukic, Milica; Jaksic, Ivana; Reichl, Stephan; Tamburic, Slobodanka; Müller-Goymann, Christel

2011-06-01

To be considered as a suitable vehicle for drugs/cosmetic actives, an emulsion system should have a number of desirable properties mainly dependent on surfactant used for its stabilization. In the current study, C(12-14) alkyl polyglucoside (APG)-mixed emulsifier of natural origin has been investigated in a series of binary (emulsifier concentration 10-25% (w/w)) and ternary systems with fixed emulsifier content (15% (w/w)) with or without glycerol. To elucidate the systems' colloidal structure the following physicochemical techniques were employed: polarization and transmission electron microscopy, X-ray diffraction (WAXD and SAXD), thermal analysis (DSC and TGA), complex rheological, pH, and conductivity measurements. Additionally, the emulsion vehicles' skin hydration potential was tested in vivo, on human skin under occlusion. In a series of binary systems with fixed emulsifier/water ratios ranging from 10/90 to 25/75 the predominance of a lamellar mesophase was found, changing its character from a liquid crystalline to a gel crystalline type. The same was observed in gel emulsions containing equal amounts of emulsifier and oil (15% (w/w)), but varying in glycerol content (0-25%). Different emulsion samples exhibited different water distribution modes in the structure, reflecting their rheological behavior and also their skin hydration capacity. Copyright © 2011 Elsevier Inc. All rights reserved.

Switchable Pickering Emulsions Stabilized by Awakened TiO2 Nanoparticle Emulsifiers Using UV/Dark Actuation.

PubMed

Zhang, Qing; Bai, Rui-Xue; Guo, Ting; Meng, Tao

2015-08-26

In this work, switchable Pickering emulsions that utilize UV/dark manipulation employ a type of smart TiO2 nanoparticle as emulsifiers. The emulsifiers can be awakened when needed via UV-induced degradation of grafted silanes on TiO2 nanoparticles. By tuning the surface wettability of TiO2 nanoparticles in situ via UV/dark actuation, emulsions stabilized by the nanoparticles can be reversibly switched between the water-in-oil (W/O) type and oil-in-water (O/W) type for several cycles. Due to the convertible wettability, the smart nanoparticle emulsifiers can be settled in either the oil phase or the water phase as desired during phase separation, making it convenient for recycling. The present work provides a facile and noninvasive method to freely manipulate the formation, breakage, and switching of the emulsion; this method has promising potential as a powerful technique for use in energy-efficient and environmentally friendly industries.

Influence of polysaccharides on the rheology and stabilization of α-pinene emulsions.

PubMed

García, Ma Carmen; Alfaro, Ma Carmen; Calero, Nuria; Muñoz, José

2014-05-25

This work focuses on the need to include polysaccharides in a slightly concentrated O(α-pinene)/W emulsion, formulated with amphiphilic copolymers as emulsifiers. Rheology, laser diffraction and multiple light scattering were the main techniques used to assess the performance of gellan gum, xanthan gum and a mixture of both hydrocolloids as stabilizers. Small amplitude oscillatory shear results were consistent with the existence of three distinct microstructures and relaxation mechanisms, which depended on the hydrocolloid system used. The mechanical spectrum of the emulsion containing both polysaccharides signalled the occurrence of thermodynamic incompatibility between the two. Flow curves fitted to the Carreau-Yasuda model demonstrated a negative synergistic effect between gellan and xanthan gums. The droplet size distribution was similar for these systems, which highlighted the importance of the continuous phase for emulsion stability. Multiple light scattering illustrated that creaming was practically eliminated by the incorporation of polysaccharides, coalescence being the main destabilization mechanism. Copyright © 2014 Elsevier Ltd. All rights reserved.

Fabrication of magnetic hydroxypropyl cellulose-g-poly(acrylic acid) porous spheres via Pickering high internal phase emulsion for removal of Cu(2+) and Cd(2.).

PubMed

Zhu, Yongfeng; Zheng, Yian; Zong, Li; Wang, Feng; Wang, Aiqin

2016-09-20

A series of magnetic hydroxypropyl cellulose-g-poly(acrylic acid) porous spheres were prepared via O/W Pickering high internal phase emulsions (HIPEs) integrated precipitation polymerization. The structure and composition of modified Fe3O4 and porous structures were characterized by TEM, XRD, TGA and SEM. The results indicated that the silanized Fe3O4 can influence greatly the pore structure of magnetic porous sphere in addition to non-negligible impacts of the proportion of mixed solvent and co-surfactant. The adsorption experiment demonstrated that the adsorption equilibrium can be reached within 40min and the maximal adsorption capacity was 300.00mg/g for Cd(2+) and 242.72mg/g for Cu(2+), suggesting its fast adsorption kinetics and high adsorption capacity. After five adsorption-desorption cycles, no significant changes in the adsorption capacity were observed, suggesting its excellent reusability. The magnetic porous sphere can be easily separated from the solution and then find its potential as a recyclable material for highly efficient removal of heavy metals. Copyright © 2016 Elsevier Ltd. All rights reserved.

Influences of MAA on the porous morphology of P(St-MAA) latex particles produced by batch soap-free emulsion polymerization followed by stepwise alkali/acid post-treatment.

PubMed

Deng, Wei; Li, Ronglong; Zhang, Mengjun; Gong, Lixiang; Kan, Chengyou

2010-09-01

Soap-free P(St-MAA) latex particles with variable styrene (St)/methacrylic acid (MAA) ratio were synthesized by batch emulsion copolymerization at 70 degrees C for 7h, and the particles with porous structure were obtained after stepwise alkali/acid post-treatment. The effects of MAA amount on the particle morphologies after the alkali and the stepwise alkali/acid post-treatments were investigated by transmission electron microscopy (TEM) and scanning electron microscopy (SEM). Results indicated that the alkali-treated latex particles showed anomalous structure with rough surface, and no hollow was clearly identified inside them. When these alkali-treated particles were further treated with acid solution, the particle surface became much smoother, and porous morphology appeared. It was found that when the MAA amount was less than or equal to 4mol%, no obvious morphological variation was observed; while the latex particles showed clearly porous structure as the MAA amount increased to 6mol%; with the further increase of MAA amount to 8mol%, the pore size decreased distinctly. Copyright 2010 Elsevier Inc. All rights reserved.

Preparation and in vitro evaluation of heparin-loaded polymeric nanoparticles.

PubMed

Jiao, Y Y; Ubrich, N; Marchand-Arvier, M; Vigneron, C; Hoffman, M; Maincent, P

2001-01-01

Nanoparticles of a highly soluble macromolecular drug, heparin, were formulated with two biodegradable polymers (poly-E-caprolactone [PCL] and poly (D, L-lactic-co-glycolic-acid) 50/50 [PLAGA]) and two nonbiodegradable positively charged polymers (Eudragit RS and RL) by the double emulsion and solvent evaporation method, using a high-pressure homogenization device. The encapsulation efficiency and heparin release profiles were studied as a function of the type of polymers employed (alone or in combination) and the concentration of heparin. Optimal encapsulation efficiency was observed when 5000 IU of heparin were incorporated in the first emulsion. High drug entrapment efficiency was observed in both Eudragit RS and RL nanoparticles (60% and 98%, respectively), compared with PLAGA and PCL nanoparticles (<14%). The use of the two types of Eudragit in combination with PCL and PLAGA increased the encapsulation efficiency compared with these two biodegradable polymers used alone; however, the in vitro drug release was not modified and remained low. On the other hand, the addition of esterase to the dissolution medium resulted in a significant increase in heparin release. The in vitro biological activity of released heparin, evaluated by measuring the anti-Xa activity by a colorimetric assay, was conserved after the encapsulation process.

Sustained release formulations of citronella oil nanoemulsion using cavitational techniques.

PubMed

Agrawal, Naveen; Maddikeri, Ganesh L; Pandit, Aniruddha B

2017-05-01

Nanoemulsion synthesis has proven to be an effective way for transportation of immobile, insoluble bioactive compounds. Citronella Oil (lemongrass oil), a natural plant extract, can be used as a mosquito repellent and has less harmful effects compared to its available market counterpart DEET (N, N-Diethyl-meta-toluamide). Nanoemulsion of citronella oil in water was prepared using cavitation-assisted techniques while investigating the effect of system parameters like HLB (Hydrophilic Lipophilic Balance), surfactant concentration, input energy density and mode of power input on emulsion quality. The present work also examines the effect of emulsification on release rate to understand the relationship between droplet size and the release rate. Minimum droplet size (60nm) of the emulsion was obtained at HLB of 14, S/O 1 ratio of 1.0, ultrasound amplitude of 50% and irradiation time of 5min. This study revealed that hydrodynamic cavitation-assisted emulsification is more energy efficient compared to ultrasonic emulsification. It was also found that the release rate of nanoemulsion enhanced as the droplet size of emulsion reduced. Copyright © 2016 Elsevier B.V. All rights reserved.

Measurements of 12C ions beam fragmentation at large angle with an Emulsion Cloud Chamber

NASA Astrophysics Data System (ADS)

Alexandrov, A.; De Lellis, G.; Di Crescenzo, A.; Lauria, A.; Montesi, M. C.; Pastore, A.; Patera, V.; Sarti, A.; Tioukov, V.

2017-08-01

Hadron radiotherapy is a powerful technique for the treatment of deep-seated tumours. The physical dose distribution of hadron beams is characterized by a small dose delivered in the entrance channel and a large dose in the Bragg peak area. Fragmentation of the incident particles and struck nuclei occurs along the hadron path. Knowledge of the fragment energies and angular distributions is crucial for the validation of the models used in treatment planning systems. We report on large angle fragmentation measurements of a 400 MeV/n 12C beam impinging on a composite target at the GSI laboratory in Germany. The detector was made of 300 micron thick nuclear emulsion films, with sub-micrometric spatial resolution and large angle track detection capability, interleaved with passive material. Thanks to newly developed techniques in the automated scanning of emulsions it was possible to extend the angular range of detected particles. This resulted in the first measurement of the angular and momentum spectrum for fragments emitted in the range from 34o to 81o.

Light-responsive polymer microcapsules as delivery systems for natural active agents

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bizzarro, Valentina; Carfagna, Cosimo; Cerruti, Pierfrancesco

2016-05-18

In this work we report the preparation and the release behavior of UV-responsive polymeric microcapsules containing essential oils as a core. The oil acted also as a monomer solvent during polymerization. Accordingly, the potentially toxic organic solvent traditionally used was replaced with a natural active substance, resulting in a more sustainable functional system. Polymer shell was based on a lightly cross-linked polyamide containing UV-sensitive azobenzene moieties in the main chain. The micro-sized capsules were obtained via interfacial polycondensation in o/w emulsion, and their mean size was measured via Dynamic Light Scattering. Shape and morphology were analyzed through Scanning Electron andmore » Optical Microscopy. UV-responsive behavior was evaluated via spectrofluorimetry, by assessing the release kinetics of a fluorescent probe molecule upon UV light irradiation (λ{sub max}=360 nm). The irradiated samples showed an increase in fluorescence intensity, in accordance with the increase of the probe molecule concentration in the release medium. As for the un-irradiated sample, no changes could be detected demonstrating the effectiveness of the obtained releasing system.« less

Waterborne Polyurethane Coatings with Covalently Linked Black Dye Sudan Black B

PubMed Central

Sun, Wei; Xu, Haiyan; Xu, Fei

2017-01-01

Colored waterborne polyurethanes have been widely used in paintings, leathers, textiles, and coatings. Here, a series of black waterborne polyurethanes (WPUs) with different ratios of black dye, Sudan Black B (SDB), were prepared by step-growth polymerization. WPU emulsions as obtained exhibit low particle sizes and remarkable storage stability at the same time. At different dye loadings, essential structural, statistical and thermal properties are characterized. FTIR (fourier transform infrared) spectra indicate that SDB is covalently linked into waterborne polyurethane chains. All of the WPUs with covalently linked SDB show better color fastness and resistance of thermal migration than those with SDB mixed physically. Besides, WPUs incorporated SDB covalently with different polymeric diols, polytetramethylene ether glycol (PTMG), polypropylene glycol (PPG), poly-1, 4-butylene adipate glycol (PBA) and polycaprolactone glycol (PCL), were prepared to obtain different properties to cater to a variety of practical demands. By a spraying method, the black WPUs can be directly used as metal coatings without complex dyeing process by simply mixing coating additive and other waterborne resins, which exhibit excellent coating performance. PMID:29143785

Preparation and encapsulation of white/yellow dual colored suspensions for electrophoretic displays

NASA Astrophysics Data System (ADS)

Han, Jingjing; Li, Xiaoxu; Feng, Yaqing; Zhang, Bao

2014-11-01

C.I. Pigment Yellow 181 (PY181) composite particles encapsulated by polyethylene (PE) were prepared by dispersion polymerization method, and C.I. Pigment Yellow 110 (PY110) composite particles encapsulated by polystyrene (PS) with mini-emulsion polymerization method were achieved, respectively. The modified pigments were characterized by fourier transform infrared spectroscopy, scanning electron microscope and transmission electron microscope. Compared with the PE-coated PY 181 pigments, the PS-coated PY-110 particles had a narrow particle size distribution, regular spherical and average particle size of 450 nm. Suspension 1 and suspension 3 were prepared by the two composite particles dispersed in isopar M. A chromatic electrophoretic display cell consisting of yellow particles was successfully fabricated using dispersions of yellow ink particles in a mixed dielectric solvent with white particles as contrast. The response behavior and the contrast ratio to the electric voltage were also examined. The contrast ratio of pigments modified by polystyrene was 1.48, as well as the response time was 2 s, which were better than those of pigments modified by polyethylene.

Carried by History: Cesar Lattes, Nuclear Emulsions, and the Discovery of the Pi-meson

NASA Astrophysics Data System (ADS)

Vieira, Cássio Leite; Videira, Antonio Augusto Passos

2014-03-01

We analyze the role played by the Brazilian physicist Cesar Lattes (1924-2005) in the historical development of the nuclear emulsion technique and in the co-discovery of the pion. His works influenced and gave impetus to the development of experimental physics in Brazil, the foundation of a national center dedicated to physics research, the beginnings of Brazilian "Big Science," and the inauguration of a long-lasting collaboration between Brazil and Japan in the field of comic ray physics.

Formulation and evaluation of targeted nanoparticles for breast cancer theranostic system.

PubMed

Dadras, Pegah; Atyabi, Fatemeh; Irani, Shiva; Ma'mani, Leila; Foroumadi, Alireza; Mirzaie, Zahra Hadavand; Ebrahimi, Marzieh; Dinarvand, R

2017-01-15

Theranostic polymeric NPs developed for both cancer diagnosis and cancer therapy. This multifunctional polymeric vehicle was prepared by a single emulsion evaporation method, using carboxyl-terminated PLGA. LHRH as a targeting moiety, was conjugated to the surface of polymeric carrier by applying polyethylene glycol. The results indicated that the diameter of NPs was ~185.4±4.6nm as defined by DLS. The entrapment efficacy of docetaxel, silibinin, and SPIONs was 84.6±4.1%, 80.6±2.7%, and 77.9±4.3%, respectively. The NPs showed a triphasic in-vitro drug release pattern. MTT assay was done on two cell lines, MCF-7 and SKOV-3. Enhanced cellular uptake ability of the targeted NPs to MCF-7 was evaluated in-vitro by confocal laser scanning microscopy. The results indicated that compared to non-targeted NPs, the LHRH targeted NPs had significant efficacy at IC50 concentration. The effect of the NPs on VEGF expression in MCF-7 and SKOV-3 cells was investigated by Real-Time PCR method. VEGF mRNA level expression in MCF-7 cell line reduced by 83% in comparison to control cell line. The designed NPs can be used as promising multifunctional platform for detection and targeted drug delivery in breast cancer. Copyright © 2016 Elsevier B.V. All rights reserved.

Utilizing stretch-tunable thermochromic elastomeric opal films as novel reversible switchable photonic materials.

PubMed

Schäfer, Christian G; Lederle, Christina; Zentel, Kristina; Stühn, Bernd; Gallei, Markus

2014-11-01

In this work, the preparation of highly thermoresponsive and fully reversible stretch-tunable elastomeric opal films featuring switchable structural colors is reported. Novel particle architectures based on poly(diethylene glycol methylether methacrylate-co-ethyl acrylate) (PDEGMEMA-co-PEA) as shell polymer are synthesized via seeded and stepwise emulsion polymerization protocols. The use of DEGMEMA as comonomer and herein established synthetic strategies leads to monodisperse soft shell particles, which can be directly processed to opal films by using the feasible melt-shear organization technique. Subsequent UV crosslinking strategies open access to mechanically stable and homogeneous elastomeric opal films. The structural colors of the opal films feature mechano- and thermoresponsiveness, which is found to be fully reversible. Optical characterization shows that the combination of both stimuli provokes a photonic bandgap shift of more than 50 nm from 560 nm in the stretched state to 611 nm in the fully swollen state. In addition, versatile colorful patterns onto the colloidal crystal structure are produced by spatial UV-induced crosslinking by using a photomask. This facile approach enables the generation of spatially cross-linked switchable opal films with fascinating optical properties. Herein described strategies for the preparation of PDEGMEMA-containing colloidal architectures, application of the melt-shear ordering technique, and patterned crosslinking of the final opal films open access to novel stimuli-responsive colloidal crystal films, which are expected to be promising materials in the field of security and sensing applications. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Free-Standing and Self-Crosslinkable Hybrid Films by Core-Shell Particle Design and Processing.

PubMed

Vowinkel, Steffen; Paul, Stephen; Gutmann, Torsten; Gallei, Markus

2017-11-15

The utilization and preparation of functional hybrid films for optical sensing applications and membranes is of utmost importance. In this work, we report the convenient and scalable preparation of self-crosslinking particle-based films derived by directed self-assembly of alkoxysilane-based cross-linkers as part of a core-shell particle architecture. The synthesis of well-designed monodisperse core-shell particles by emulsion polymerization is the basic prerequisite for subsequent particle processing via the melt-shear organization technique. In more detail, the core particles consist of polystyrene (PS) or poly(methyl methacrylate) (PMMA), while the comparably soft particle shell consists of poly(ethyl acrylate) (PEA) and different alkoxysilane-based poly(methacrylate)s. For hybrid film formation and convenient self-cross-linking, different alkyl groups at the siloxane moieties were investigated in detail by solid-state Magic-Angle Spinning Nuclear Magnetic Resonance (MAS, NMR) spectroscopy revealing different crosslinking capabilities, which strongly influence the properties of the core or shell particle films with respect to transparency and iridescent reflection colors. Furthermore, solid-state NMR spectroscopy and investigation of the thermal properties by differential scanning calorimetry (DSC) measurements allow for insights into the cross-linking capabilities prior to and after synthesis, as well as after the thermally and pressure-induced processing steps. Subsequently, free-standing and self-crosslinked particle-based films featuring excellent particle order are obtained by application of the melt-shear organization technique, as shown by microscopy (TEM, SEM).

Dye-attached magnetic poly(hydroxyethyl methacrylate) nanospheres for albumin depletion from human plasma.

PubMed

Gökay, Öznur; Karakoç, Veyis; Andaç, Müge; Türkmen, Deniz; Denizli, Adil

2015-02-01

The selective binding of albumin on dye-affinity nanospheres was combined with magnetic properties as an alternative approach for albumin depletion from human plasma. Magnetic poly(hydroxyethyl methacrylate) (mPHEMA) nanospheres were synthesized using mini-emulsion polymerization method in the presence of magnetite powder. The specific surface area of the mPHEMA nanospheres was found to be 1302 m(2)/g. Subsequent to Cibacron Blue F3GA (CB) immobilization onto mPHEMA nanospheres, a serial characterization processing was implemented. The quantity of immobilized CB was calculated as 800 μmol/g. Ultimately, albumin adsorption performance of the CB-attached mPHEMA nanospheres from both aqueous dissolving medium and human plasma were explored.

Mechanistic examination of pre-exfoliating confinement of surface-active polystyrene nanobeads within pristine clay.

PubMed

Khvan, Svetlana; Kim, Junkyung; Lee, Sang-Soo

2007-02-01

Hydrophobic polymer (PS) nanoparticles preformed through an emulsifier-free emulsion polymerization method were successfully incorporated into a gallery of pristine sodium montmorillonite via interfacial cation exchange. The polymer beads confined between clay nanosheets were capable of (1) preventing the silicate layers from restacking and (2) maintaining the exfoliated state of clay. The increase in the abundance of surface groups promoted adsorption of the nanobeads onto the silicate surface and eventually led to the establishment of strong polymer-clay interactions. These findings suggest that, on the basis of the obtained pre-exfoliated clay masterbatch, the presence of strong polymer-clay interactions could improve the mechanical performance of nanocomposites.

Probing of cosolvents in polymer latex materials by using solvatochromic fluorescence.

PubMed

Brouwer, Albert M; Raja, Tanzeela N; Biemans, Koen; Nabuurs, Tijs; Tennebroek, Ronald

2008-01-01

The process of film formation is of great importance for the application of organic coatings. In waterborne coatings, organic cosolvents are still indispensable, but regulations force the industry to reduce their amounts. Here we describe a method that uses the solvatochromic fluorescence of a probe molecule copolymerized in an emulsion polymerization process with different monomers to shed light on the partitioning of cosolvents in polymer latex materials. The formulation of the latex with organic cosolvents that are not very water soluble leads to a quantifiable redshift of the emission of the probe. The transfer of the cosolvent upon mixing of cosolvent-containing and cosolvent-free compartments can also be monitored.

Characteristics of low polymerization shrinkage flowable resin composites in newly-developed cavity base materials for bulk filling technique.

PubMed

Nitta, Keiko; Nomoto, Rie; Tsubota, Yuji; Tsuchikawa, Masuji; Hayakawa, Tohru

2017-11-29

The purpose of this study was to evaluate polymerization shrinkage and other physical properties of newly-developed cavity base materials for bulk filling technique, with the brand name BULK BASE (BBS). Polymerization shrinkage was measured according to ISO/FDIS 17304. BBS showed the significantly lowest polymerization shrinkage and significantly higher depth of cure than conventional flowable resin composites (p<0.05). The Knoop hardness, flexural strength and elastic modulus of that were significantly lower than conventional flowable resin composites (p<0.05). BBS had the significantly greatest filler content (p<0.05). SEM images of the surface showed failure of fillers. The lowest polymerization shrinkage was due to the incorporation of a new type of low shrinkage monomer, which has urethane moieties. There were no clear correlations between inorganic filler contents and polymerization shrinkage, flexural strength and elastic modulus. In conclusion, the low polymerization shrinkage of BBS will be useful for cavity treatment in dental clinics.

A colloidal assembly approach to synthesize magnetic porous composite nanoclusters for efficient protein adsorption

NASA Astrophysics Data System (ADS)

Yang, Qi; Lan, Fang; Yi, Qiangying; Wu, Yao; Gu, Zhongwei

2015-10-01

A combination strategy of the inverse emulsion crosslinking approach and the colloidal assembly technique is first proposed to synthesize Fe3O4/histidine composite nanoclusters as new-type magnetic porous nanomaterials. The nanoclusters possess uniform morphology, high magnetic content and excellent protein adsorption capacity, exhibiting their great potential for bio-separation.A combination strategy of the inverse emulsion crosslinking approach and the colloidal assembly technique is first proposed to synthesize Fe3O4/histidine composite nanoclusters as new-type magnetic porous nanomaterials. The nanoclusters possess uniform morphology, high magnetic content and excellent protein adsorption capacity, exhibiting their great potential for bio-separation. Electronic supplementary information (ESI) available: Experimental details. See DOI: 10.1039/c5nr05800g

Click polymerization for the synthesis of reduction-responsive polymeric prodrug

NASA Astrophysics Data System (ADS)

Zhang, Xiaojin; Wang, Hongquan; Dai, Yu

2018-05-01

Click polymerization is a powerful polymerization technique for the construction of new macromolecules with well-defined structures and multifaceted functionalities. Here, we synthesize reduction-responsive polymeric prodrug PEG- b-(PSS- g-MTX)- b-PEG containing disulfide bonds and pendant methotrexate (MTX) via two-step click polymerization followed by conjugating MTX to pendant hydroxyl. MTX content in polymeric prodrug is 13.5%. Polymeric prodrug is able to form polymeric micelles by self-assembly in aqueous solution. Polymeric micelles are spherical nanoparticles with tens of nanometers in size. Of note, polymeric micelles are reduction-responsive due to disulfide bonds in the backbone of PEG- b-(PSS- g-MTX)- b-PEG and could release pendant drugs in the presence of the reducing agents such as dl-dithiothreitol (DTT).

Heterofunctional Glycopolypeptides by Combination of Thiol-Ene Chemistry and NCA Polymerization.

PubMed

Krannig, Kai-Steffen; Schlaad, Helmut

2016-01-01

Glycopolypeptides are prepared either by the polymerization of glycosylated amino acid N-carboxyanhydrides (NCAs) or by the post-polymerization functionalization of polypeptides with suitable functional groups. Here we present a method for the in-situ functionalization and (co-) polymerization of allylglycine N-carboxyanhydride in a facile one-pot procedure, combining radical thiol-ene photochemistry and nucleophilic ring-opening polymerization techniques, to yield well-defined heterofunctional glycopolypeptides.

Influence of the ratio of amphiphilic copolymers used as emulsifiers on the microstructure, physical stability and rheology of α-pinene emulsions stabilized with gellan gum.

PubMed

García, Maria Carmen; Alfaro, Maria Carmen; Muñoz, José

2015-11-01

α-Pinene is a terpenic solvent whose use in the formulation of emulsions entails a double benefit from the environmental point of view since it is a green solvent, easily biodegradable, which also has certain antimicrobial properties. In this work a combination of Atlas™ G-5000 and Atlox™ 4913 amphiphilic copolymers was used to obtain O/W emulsions formulated with α-pinene and gellan gum. These emulsions may find applications related to the design of complex biotechnological systems with different uses. In order to investigate the microstructure and the physical stability of these emulsions, a combination of different techniques such as rheology, microscopy, laser diffraction and multiple light scattering turn out to be a useful methodology. The results demonstrated the need to include a minimum amount of Atlas™ G-5000 copolymer in the formulation of these emulsions to improve their stability. These results were supported by the information revealed by optical micrographs, according to which Atlas™ G-5000 is directed to the continuous medium to structure water (this surfactant is particularly effective at forming hydrogen bonds with water). On the other hand Atlox™ 4913 is preferentially adsorbed at the α-pinene-water interface, such that a high Atlox™ 4913/Atlas™ G-5000 mass ratio slows down the kinetics of coalescence as shown by multiple light scattering. However, a very low relative concentration of Atlas™ G-5000 causes creaming to become the dominant destabilization mechanism. Increasing the Atlas™ G-5000/Atlox™ 4913 mass ratio yields emulsions with enhanced viscosity and viscoelasticity. Copyright © 2015 Elsevier B.V. All rights reserved.

Anti-inflammatory and analgesic activity of novel oral aspirin-loaded nanoemulsion and nano multiple emulsion formulations generated using ultrasound cavitation.

PubMed

Tang, Siah Ying; Sivakumar, Manickam; Ng, Angela Min-Hwei; Shridharan, Parthasarathy

2012-07-01

The present study investigated the anti-inflammatory and analgesic activities of novel aspirin oil-in-water (O/W) nanoemulsion and water-in-oil-in-water (W/O/W) nano multiple emulsion formulations generated using ultrasound cavitation techniques. The anti-inflammatory activities of nanoemulsion and nano multiple emulsion were determined using the λ-carrageenan-induced paw edema model. The analgesic activities of both nanoformulations were determined using acetic acid-induced writhing response and hot plate assay. For comparison, the effect of pretreatment with blank nanoemulsion and reference aspirin suspension were also studied for their anti-inflammatory and antinociceptive activities. The results showed that oral administration of nanoemulsion and nano multiple emulsion containing aspirin (60 mg/kg) significantly reduced paw edema induced by λ-carrageenan injection. Both nanoformulations decreased the number of abdominal constriction in acetic acid-induced writhing model. Pretreatment with nanoformulations led to a significant increase in reaction time in hot plate assay. Nanoemulsion demonstrated an enhanced anti-inflammatory and analgesic effects compared to reference suspension while nano multiple emulsion exhibited a mild inhibitory effects in the three experimental animal model tests. The results obtained for nano multiple emulsion were relatively lower than reference. However, administration of blank nanoemulsion did not alter the nociceptive response significantly though it showed slight anti-inflammatory effect. These experimental studies suggest that nanoemulsion and nano multiple emulsion produced a pronounced anti-inflammatory and analgesic effects in rats and may be candidates as new nanocarriers for pharmacological NSAIDs in the treatment of inflammatory disorders and alleviating pains. Copyright © 2012 Elsevier B.V. All rights reserved.

Direct electron-pair production by high energy heavy charged particles

NASA Technical Reports Server (NTRS)

Takahashi, Y.; Gregory, J. C.; Hayashi, T.; Dong, B. L.

1989-01-01

Direct electron pain production via virtual photons by moving charged particles is a unique electro-magnetic process having a substantial dependence on energy. Most electro-magnetic processes, including transition radiation, cease to be sensitive to the incident energy above 10 TeV/AMU. Thus, it is expected, that upon establishment of cross section and detection efficiency of this process, it may provide a new energy measuring technique above 10 TeV/AMU. Three accelerator exposures of emulsion chambers designed for measurements of direct electron-pains were performed. The objectives of the investigation were to provide the fundamental cross-section data in emulsion stacks to find the best-fit theoretical model, and to provide a calibration of measurements of direct electron-pairs in emulsion chamber configurations. This paper reports the design of the emulsion chambers, accelerator experiments, microscope measurements, and related considerations for future improvements of the measurements, and for possible applications to high energy cosmic ray experiments. Also discussed are the results from scanning 56m of emulsion tracks at 1200x magnification so that scanning efficiency is optimized. Measurements of the delta-ray range spectrum were also performed for much shorter track lengths, but with sufficiently large statistics in the number of measured delta-rays.

Emulsification of oil in water as affected by different parameters.

PubMed

Baloch, Musa Kaleem; Hameed, Gulzar

2005-05-15

The aim of this investigation was to develop a basic understanding of the emulsification process by considering simple systems such as n-hexane, n-heptane, n-decane, and kerosene oil in water. The technique employed for the purpose was ultrasonification. The effect of ultrasonification time, chain length, viscosity, surface tension, oil content, and ionic strength of the media on the quality of emulsion has been studied. The emulsions were viewed through microscope to measure the number, size, and size distribution of droplets. Quantification of turbidity and viscosity was also used to characterize the emulsions. It has been found that the number and size of the droplets vary with the time of ultrasonification, contents of oils, molecular mass of the oils, and ionic strength of the media, and hence the quality of the emulsion is influenced by these parameters. The droplet size decreases, whereas the number of drops increases with the time of emulsification, approaching an optimum distribution at about 15 min of ultrasonification. Further, the increase in the molecular mass of the oil increases the size of the droplets and hence decreases the stability of the emulsion. The addition of electrolytes encourages coalescence and enhances the instability in the system. The results are in accord with the equations proposed by us.

Synthesis of Biocompatible Surfaces by Different Techniques

DTIC Science & Technology

2002-04-01

production . In the other hand, polymers are widely used in bone/cartilage implants, both, as polymeric materials themselves and as a polymeric surface on a...focus on the production of HA scaffolds by a sol-gel method using different drying processes, and on the study of the plasma polymerization technique to...precursor at 3. SA-stoichiometric amount (to maintain Ca/P= 1,67) of the calcium precursor solution (3 M solution in anhidrous etanol ) was added dropwise

DH and ESPI laser interferometry applied to the restoration shrinkage assessment

NASA Astrophysics Data System (ADS)

Campos, L. M. P.; Parra, D. F.; Vasconcelos, M. R.; Vaz, M.; Monteiro, J.

2014-01-01

In dental restoration postoperative marginal leakage is commonly associated to polymerization shrinkage effects. In consequence the longevity and quality of restorative treatment depends on the shrinkage mechanisms of the composite filling during the polymerization. In this work the development of new techniques for evaluation of those effects under light-induced polymerization of dental nano composite fillings is reported. The composite resins activated by visible light, initiate the polymerization process by absorbing light in wavelengths at about 470 nm. The techniques employed in the contraction assessment were digital holography (DH) and Electronic Speckle Pattern Interferometry (ESPI) based on laser interferometry. A satisfactory resolution was achieved in the non-contact displacement field measurements on small objects concerning the experimental dental samples. According to a specific clinical protocol, natural teeth were used (human mandibular premolars). A class I cavity was drilled and restored with nano composite material, according to Black principles. The polymerization was monitored by DH and ESPI in real time during the cure reaction of the restoration. The total displacement reported for the material in relation of the tooth wall was 3.7 μm (natural tooth). The technique showed the entire tooth surface (wall) deforming during polymerization shrinkage.

The therapeutic effect of nano-encapsulated and nano-emulsion forms of carvacrol on experimental liver fibrosis.

PubMed

Hussein, Jihan; El-Banna, Mona; Mahmoud, Khaled F; Morsy, Safaa; Abdel Latif, Yasmin; Medhat, Dalia; Refaat, Eman; Farrag, Abdel Razik; El-Daly, Sherien M

2017-06-01

The present study aimed to compare the therapeutic efficiency of nano-encapsulated and nano-emulsion carvacrol administration on liver injury in thioacetamide (TAA) treated rats. To fulfill our target, we used sixty male albino rats classified into six groups as follow: control, nano-encapsulated carvacrol, nano-emulsion carvacrol, thioacetamide, treated nano-encapsulated carvacrol and treated nano-emulsion carvacrol groups. Blood samples were collected from all groups and the separated serum was used for analysis of the following biochemical parameters; aspartate aminotransferase (AST), alanine aminotransferase (ALT), S100 B protein, alpha fetoprotein (AFP) and caspase-3. The levels of malondialdehyde (MDA), reduced glutathione (GSH), nitric oxide (NO), monocyte chemoattractant protein-1(MCP-1) and hydroxyproline content were all evaluated in liver tissue homogenate. Histopathological examinations for liver tissues were also performed. Thioacetamide induced hepatic damage in rats as revealed by the significant increase in the levels of serum ALT, AST and produced oxidative stress as displayed by the significant elevation in the levels of hepatic MDA and NO concomitant with a significant decrease in GSH. In addition, thioacetamide significantly increased serum S100B protein, alpha fetoprotein and caspase-3 along with hepatic MCP-1 and hydroxyproline; these results were confirmed by the histopathological investigation. In contrast, nano-encapsulated and nano-emulsion carvacrol were able to ameliorate these negative changes in the thioacetamide injected rats. However, the effect of the nano-encapsulated form of carvacrol was more prominent than the nano-emulsion form. Nano-encapsulated and nano-emulsion carvacrol can ameliorate thioacetamide induced liver injury. These results could be attributed to the potential anti-inflammatory, antioxidant, and anti-apoptotic activities of carvacrol in addition to the effectiveness of the encapsulation technique that can protect carvacrol structure and increase its efficiency and stability. Moreover, nano-encapsulation of carvacrol is more efficient than nano-emulsion. Copyright © 2017 Elsevier Masson SAS. All rights reserved.

Dimensional change in complete dentures fabricated by injection molding and microwave processing.

PubMed

Keenan, Phillip L J; Radford, David R; Clark, Robert K F

2003-01-01

Acrylic resin complete dentures undergo dimensional changes during polymerization. Techniques with injection molding and polymerization and microwave polymerization are reported to reduce these changes and thereby improve clinical fit. These dimensional changes need to be quantified. The purpose of this study was to compare differences in dimensional changes of simulated maxillary complete dentures during polymerization and storage in water after injection molding and conventional polymerization, or microwave polymerization against a control of conventionally packed and polymerized simulated maxillary complete dentures. Forty identical maxillary denture bases were prepared in dental wax with anatomic teeth. They were invested and the wax eliminated from the molds. Ten specimens each were randomly assigned to 1 of 4 groups. Group 1 was compression molded and conventionally polymerized; group 2 was injection molded and conventionally polymerized (Success); group 3 was injection molded and microwave polymerized (Acron MC); and group 4 was injection molded and microwave polymerized (Microbase). Intermolar width and changes in vertical dimension of occlusion, were determined after polymerization and after storage in water for 28 days. Measurements in triplicate were made between points scribed on the second molar teeth with a traveling microscope (accurate to 0.005 mm). Vertical dimension of occlusion was measured between points scribed on the upper and lower members of an articulator by use of an internal micrometer (accurate to 0.05 mm). Data were analyzed by use of a 1-way analysis of variance with Tukey post-hoc contrasts (P <.05). Polymerization contractions (intermolar widths) for each group were: group 1, -0.24%; group 2, -0.27%; group 3, -0.35%; and group 4, -0.37%. The Microbase specimens had greater shrinkage than conventionally polymerized specimens, but there were no significant differences between the groups. All injection methods had less postpolymerization increase in vertical dimension of occlusion (0.63 to 0.41 mm) than the conventional Trevalon control (0.74 mm), but only group 4 was significantly different (P<.004). After storage in water for 28 days, all specimens increased in vertical dimension of occlusion (0.10% to 0.16%) from polymerization techniques, but there were no significant differences between groups. Within the limitations of this study, injection molding resulted in a slightly less increase of vertical dimension of occlusion than conventional polymerization techniques, the difference being significant for Microbase compared with the conventional Trevalon control.

Hierarchical Biomolecular Emulsions Using 3-D Microfluidics with Uniform Surface Chemistry.

PubMed

Toprakcioglu, Zenon; Levin, Aviad; Knowles, Tuomas P J

2017-11-13

Microfluidic devices can be used to produce single, double and higher order emulsions, where droplet sizes can be precisely controlled and modulated. Such emulsions have great potential for the storage and study of biomolecules, including peptides and proteins. However, advancement of this technique has remained challenging due to the tendency of various biomolecules to adhere to the surface of the formed channels, resulting in changes in surface wetting and fouling on the micrometer scale. Thus, precise control of surface wettability plays a crucial role in the processes that govern droplet formation. Here, we report an approach for producing both water-oil-water (w/o/w) and oil-water-oil (o/w/o) double emulsions without any need for surface modification, an enabling feature for biomolecular encapsulation. Using this strategy, we show that the number of monodisperse encapsulated internal droplets can be controlled systematically and reproducibly by suitable adjustment of the relevant flow rates, and ranges from 1 to 40 in the case of w/o/w emulsions. We further demonstrate that the number of internal droplets scales linearly with the reciprocal flow rate of the outer continuous phase, when the inner and middle phase flow rates are kept constant. We demonstrate that this approach is suitable for forming double emulsions where the inner phase consists of reconstituted silk protein solution whereby incubation of the internal droplets can be induced to form a gel resulting in silk fibroin microgels surrounded by an external oil shell. Finally, for o/w/o emulsions, we show that single or multiple monodisperse internal droplets can be encapsulated with a size that ranges over 1 order of magnitude, from ca. 10 μm to >100 μm. Moreover, o/w/o emulsions where the middle phase consists of silk fibroin solution were prepared and by allowing the protein to aggregate, a core-shell structure was formed. This microfluidic strategy allows for multiple emulsions to be generated drop by drop for biomolecular solutions with potential applications in the biomedical and pharmaceutical fields.

In-Situ Swelling For Holographic Color Control

NASA Astrophysics Data System (ADS)

Walker Parker, Julie L.; Benton, Stephen A.

1989-05-01

Deliberate variations of the emulsion thickness between holographic exposures and reconstruction produce a range of output wavelengths from a fixed exposure wavelength, a technique known as "pseudo-color" multi-color reflection holography. Usual methods require the removal of the film or plate from the holographic setup between exposures for imbibition of a swelling agent, followed by drying and replacement, so that a retention of the swelling agent forces a physical increase in the thickness of the emulsion. The density (and hence the thickness) of the gelatin binder can also be varied by changing its electrolytic environment. By immersing the holographic emulsion in a suitable solution, allowing it to come to a new equilibrium thickness, and exposing with a long-wavelength laser, shorter wavelength reconstructions can be obtained without removing the film or plate from the setup. Accurate changes of solution can make a precise sequence of swellings possible, producing multiple reconstruction colors from a set of constant-wavelength recordings. Here we describe pre-treatments of the emulsion that make rapid and stable equilibria possible, and swelling bath sequences that produce color primaries suitable for full-color computer-graphic holographic imagery.

Preparation of a reversed-phase/anion-exchange mixed-mode spherical sorbent by Pickering emulsion polymerization for highly selective solid-phase extraction of acidic pharmaceuticals from wastewater.

PubMed

Huang, Chaonan; Li, Yun; Yang, Jiajia; Peng, Junyu; Jin, Jing; Dhanjai; Wang, Jincheng; Chen, Jiping

2017-10-27

The present work represents a simple and effective preparation of a novel mixed-mode anion-exchange (MAX) sorbent based on porous poly[2-(diethylamino)ethyl methacrylate-divinylbenzene] (poly(DEAEMA-DVB)) spherical particles synthesized by one-step Pickering emulsion polymerization. The poly(DEAEMA-DVB) particles were quaternized with 1,4-butanediol diglycidyl ether (BDDE) followed by triethylamine (TEA) via epoxy-amine reaction to offer strong anion exchange properties. The synthesized MAX sorbent was characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy, nitrogen adsorption-desorption measurements and elemental analysis. The MAX sorbent possessed regular spherical shape and narrow diameter distribution (15-35μm), a high IEC of 0.54meq/g, with carbon and nitrogen contents of 80.3% and 1.62%, respectively. Compared to poly(DEAEMA-DVB), the MAX sorbent exhibited decreased S BET (390.5 vs. 515.3m 2 g -1 ), pore volume (0.74 vs. 0.85cm 3 g -1 ) and pore size (16.8 vs. 17.3nm). Moreover, changes of N content for producing the MAX sorbent reveal a successful two-step quaternization, which can be highly related to such a high IEC. Finally, the MAX sorbent was successfully evaluated for selective isolation and purification of some selected acidic pharmaceuticals (ketoprofen, KEP; naproxen, NAP; and ibuprofen, IBP) from neutral (hydrocortisone, HYC), basic (carbamazepine, CAZ; amitriptyline, AMT) pharmaceuticals and other interferences in water samples using solid phase extraction (SPE). An efficient analytical method based on the MAX-based mixed-mode SPE coupled with HPLC-UV was developed for highly selective extraction and cleanup of acidic KEP, NAP and IBP in spiked wastewater samples. The developed method exhibited good sensitivity (0.009-0.085μgL -1 limit of detection), satisfactory recoveries (82.1%-105.5%) and repeatabilities (relative standard deviation < 7.9%, n=3). Copyright © 2017 Elsevier B.V. All rights reserved.

Investigation of Solution Polymerizations in Microgravity and 1 G

NASA Technical Reports Server (NTRS)

Kennedy, Alvin P.

1998-01-01

The in-situ dielectric spectra for the solution polymerization of polydiacetylene has been successfully measured. The results show a distinct difference between the response for the bulk solution and surface polymerization. It also shows a low frequency peak in the dissipation factor which is present in both the bulk and surface polymerizations. These features may prove to be significant indicators for important polymerization processes. Future studies will investigate the mechanisms responsible for these dielectric responses. This technique will eventually be used to monitor microgravity polymerizations and provide in-situ data on how microgravity affects solution polymerization.

Determining the Effective Density and Stabilizer Layer Thickness of Sterically Stabilized Nanoparticles

PubMed Central

2016-01-01

A series of model sterically stabilized diblock copolymer nanoparticles has been designed to aid the development of analytical protocols in order to determine two key parameters: the effective particle density and the steric stabilizer layer thickness. The former parameter is essential for high resolution particle size analysis based on analytical (ultra)centrifugation techniques (e.g., disk centrifuge photosedimentometry, DCP), whereas the latter parameter is of fundamental importance in determining the effectiveness of steric stabilization as a colloid stability mechanism. The diblock copolymer nanoparticles were prepared via polymerization-induced self-assembly (PISA) using RAFT aqueous emulsion polymerization: this approach affords relatively narrow particle size distributions and enables the mean particle diameter and the stabilizer layer thickness to be adjusted independently via systematic variation of the mean degree of polymerization of the hydrophobic and hydrophilic blocks, respectively. The hydrophobic core-forming block was poly(2,2,2-trifluoroethyl methacrylate) [PTFEMA], which was selected for its relatively high density. The hydrophilic stabilizer block was poly(glycerol monomethacrylate) [PGMA], which is a well-known non-ionic polymer that remains water-soluble over a wide range of temperatures. Four series of PGMAx–PTFEMAy nanoparticles were prepared (x = 28, 43, 63, and 98, y = 100–1400) and characterized via transmission electron microscopy (TEM), dynamic light scattering (DLS), and small-angle X-ray scattering (SAXS). It was found that the degree of polymerization of both the PGMA stabilizer and core-forming PTFEMA had a strong influence on the mean particle diameter, which ranged from 20 to 250 nm. Furthermore, SAXS was used to determine radii of gyration of 1.46 to 2.69 nm for the solvated PGMA stabilizer blocks. Thus, the mean effective density of these sterically stabilized particles was calculated and determined to lie between 1.19 g cm–3 for the smaller particles and 1.41 g cm–3 for the larger particles; these values are significantly lower than the solid-state density of PTFEMA (1.47 g cm–3). Since analytical centrifugation requires the density difference between the particles and the aqueous phase, determining the effective particle density is clearly vital for obtaining reliable particle size distributions. Furthermore, selected DCP data were recalculated by taking into account the inherent density distribution superimposed on the particle size distribution. Consequently, the true particle size distributions were found to be somewhat narrower than those calculated using an erroneous single density value, with smaller particles being particularly sensitive to this artifact. PMID:27478250

Fluctuation analysis of relativistic nucleus-nucleus collisions in emulsion chambers

NASA Technical Reports Server (NTRS)

Mcguire, Stephen C.

1988-01-01

An analytical technique was developed for identifying enhanced fluctuations in the angular distributions of secondary particles produced from relativistic nucleus-nucleus collisions. The method is applied under the assumption that the masses of the produced particles are small compared to their linear momenta. The importance of particles rests in the fact that enhanced fluctuations in the rapidity distributions is considered to be an experimental signal for the creation of the quark-gluon-plasma (QGP), a state of nuclear matter predicted from the quantum chromodynamics theory (QCD). In the approach, Monte Carlo simulations are employed that make use of a portable random member generator that allow the calculations to be performed on a desk-top computer. The method is illustrated with data taken from high altitude emulsion exposures and is immediately applicable to similar data from accelerator-based emulsion exposures.

Efficient synthesis of PMMA@Co0.5Ni0.5Fe2O4 organic-inorganic hybrids containing hyamine 1622 - Physicochemical properties, cytotoxic assessment and antimicrobial activity.

PubMed

Zachanowicz, E; Pigłowski, J; Grzymajło, M; Poźniak, B; Tikhomirov, M; Pierunek, N; Śniadecki, Z; Idzikowski, B; Marycz, K; Marędziak, M; Kisała, J; Hęclik, K; Pązik, R

2018-09-01

The PMMA@Co 0.5 Ni 0.5 Fe 2 O 4 ferrite containing hybrid nanomaterials with hyamine were prepared using emulsion polymerization method. Structural and morphological properties were evaluated using XRD, FT-IR, SEM techniques. The TGA and DTA analysis were performed in order to study the thermal properties of hybrid materials in contrast to reference material. Magnetic properties were studied using Quantum Design PPMS (VSM option) in a constant external magnetic field equal (100 Oe and 1000 Oe) in the temperature range from 2 to 380 K. Both the pure Co 0.5 Ni 0.5 Fe 2 O 4 and the sample with 85% of PMMA exhibit superparamagnetic behavior whereas blocking temperatureT B decreases with increase of PMMA content. The cytotoxicity assessment of PMMA@Co 0.5 Ni 0.5 Fe 2 O 4 with hyamine in J774.E murine macrophages and U2OS human osteosarcoma cell lines was performed. Additionally, sensitivity of bacteria Escherichia coli ATCC 8739 and Staphylococcus aureus ATCC 25923 to hybrid materials (with/without hyamine) was investigated using a of Kirby-Bauer disc method. Copyright © 2018. Published by Elsevier B.V.

Polyacrylamide medium for the electrophoretic separation of biomolecules

DOEpatents

Madabhushi, Ramakrishna S.; Gammon, Stuart A.

2003-11-11

A polyacryalmide medium for the electrophoretic separation of biomolecules. The polyacryalmide medium comprises high molecular weight polyacrylamides (PAAm) having a viscosity average molecular weight (M.sub.v) of about 675-725 kDa were synthesized by conventional red-ox polymerization technique. Using this separation medium, capillary electrophoresis of BigDye DNA sequencing standard was performed. A single base resolution of .about.725 bases was achieved in .about.60 minute in a non-covalently coated capillary of 50 .mu.m i.d., 40 cm effective length, and a filed of 160 V/cm at 40.degree. C. The resolution achieved with this formulation to separate DNA under identical conditions is much superior (725 bases vs. 625 bases) and faster (60 min. vs. 75 min.) to the commercially available PAAm, such as supplied by Amersham. The formulation method employed here to synthesize PAAm is straight-forward, simple and does not require cumbersome methods such as emulsion polymerizaiton in order to achieve very high molecular weights. Also, the formulation here does not require separation of PAAm from the reaction mixture prior to reconstituting the polymer to a final concentration. Furthermore, the formulation here is prepared from a single average mol. wt. PAAm as opposed to the mixture of two different average mo. wt. PAAm previously required to achieve high resolution.

Facile fabrication of bowl-shaped microparticles for oral curcumin delivery to ulcerative colitis tissue.

PubMed

Chen, Qiubing; Gou, Shuangquan; Huang, Yamei; Zhou, Xin; Li, Qian; Han, Moon Kwon; Kang, Yuejun; Xiao, Bo

2018-05-05

Oral microparticles (MPs) have been considered as promising drug carriers in the treatment of ulcerative colitis (UC). Here, a facile strategy based on a conventional emulsion-solvent evaporation technique was used to fabricate bowl-shaped MPs (BMPs), and these MPs loaded with anti-inflammatory drug (curcumin, CUR) during the fabrication process. The physicochemical properties of the resultant BMPs were characterized by dynamic light scattering, scanning electron microscope, confocal laser scanning microscope and X-ray diffraction as well as contact angle goniometer. Results indicated that BMPs had a desirable hydrodynamic diameter (1.84 ± 0.20 μm), a negative zeta potential (-26.5 ± 1.13 mV), smooth surface morphology, high CUR encapsulation efficiency and controlled drug release profile. It was found that CUR molecules were dispersed in an amorphous state within the polymeric matrixes. In addition, BMPs showed excellent hydrophilicity due to the presence of Pluronic F127 and poly(vinyl alcohol) on their surface. More importantly, orally administered BMPs could efficiently alleviate UC based on a dextran sulfate sodium-induced mouse model. These results collectively suggest that BMP can be exploited as a readily scalable oral drug delivery system for UC therapy. Copyright © 2018 Elsevier B.V. All rights reserved.

A Pressure Control Method for Emulsion Pump Station Based on Elman Neural Network

PubMed Central

Tan, Chao; Qi, Nan; Yao, Xingang; Wang, Zhongbin; Si, Lei

2015-01-01

In order to realize pressure control of emulsion pump station which is key equipment of coal mine in the safety production, the control requirements were analyzed and a pressure control method based on Elman neural network was proposed. The key techniques such as system framework, pressure prediction model, pressure control model, and the flowchart of proposed approach were presented. Finally, a simulation example was carried out and comparison results indicated that the proposed approach was feasible and efficient and outperformed others. PMID:25861253

Synthesis and Characterization of Cholesterol Nano Particles by Using w/o Microemulsion Technique

NASA Astrophysics Data System (ADS)

Vyas, Poorvesh M.; Vasant, Sonal R.; Hajiyani, Rakesh R.; Joshi, Mihir J.

2010-10-01

Cholesterol is one of the most abundant and well known steroids in the animal kingdom. Cholesterol rich micro-emulsions and nano-emulsions are useful for the treatment of breast cancer and gynecologic cancers. The nano particles of cholesterol and other pharmaceutically important materials have been reported. In the present investigation, the nano particles of cholesterol were synthesized by direct precipitation technique using triton X-100/water/n-butanol micro-emulsion. The average particle size of cholesterol nano particles was estimated by applying Scherrer's formula to the powder X-ray diffraction pattern, which was found to be 22 nm. The nanoparticles of cholesterol were observed by using TEM and the particle size was found within the range from 15 nm-31 nm. The distribution of particle size was studied through DLS. The nanoparticles of cholesterol were characterized by using FT-IR spectroscopy and the force constant was also calculated for O-H, C-H and C-O bonds. The thermal response of nanoparticles of cholesterol was studied by TGA, which showed that the nanoparticles were stable up to 200 °C and then decomposed. Kinetic and thermodynamic parameters of decomposition process were also calculated by applying Coats and Redfern formula to thermo-gram.

A new solution to emulsion liquid membrane problems by non-Newtonian conversion

DOE Office of Scientific and Technical Information (OSTI.GOV)

Skelland, A.H.P.; Meng, X.

1996-02-01

Surfactant-stabilized emulsion liquid membrane processes constitute an emerging separation technology that has repeatedly been shown to be highly suited for such diverse separation processes as metal recovery or removal from dilute aqueous solutions; separations in the food industry; removal of organic bases and acids from water; and separation of hydrocarbons. Emulsion liquid membrane separation processes remain excessively vulnerable to one or more of four major problems. Difficulties lie in developing liquid membranes that combine high levels of both stability and permeability with acceptably low levels of swelling and ease of subsequent demulsification for membrane and solute recovery. This article providesmore » a new technique for simultaneously overcoming the first three problems, while identifying physical indications that the proposed solution may have little adverse effect on the fourth problem (demulsification) and may even alleviate it. Numerous benefits of optimized conversion of the membrane phase into suitable non-Newtonian form are identified, their mechanisms outlined, and experimental verifications provided. These include increased stability, retained (or enhanced) permeability, reduced swelling, increased internal phase volume, and increased stirrer speeds. The highly favorable responsiveness of both aliphatic and aromatic membranes to the new technique is demonstrated.« less

Chemical projectile-target interaction and liquid immiscibility in impact glass from the Wabar craters, Saudi Arabia

NASA Astrophysics Data System (ADS)

Hamann, Christopher; Hecht, Lutz; Ebert, Matthias; Wirth, Richard

2013-11-01

Impact glasses are usually strongly affected by secondary alteration and chemical weathering. Thus, in order to understand relevant formation processes, detailed petrographic studies on unweathered impact glasses are necessary as preserved heterogeneities in quenched impact glasses may serve as a tool to better understand their genesis. Here, we report on petrography and microchemistry of impact glasses from the Wabar impact craters (Saudi Arabia) that, with an age of ∼300 years, are among the youngest terrestrial impact craters. The fact that parts of the IIIAB iron meteorite have survived impact and subsequent weathering is granting Wabar a special role among the presently 184 confirmed terrestrial impact structures. Electron microprobe analysis (EMPA) and transmission electron microscopy (TEM) obtained on the black impact melt/glass variety at Wabar suggest that meteoritic Fe was selectively mixed with high-silica target melt at high temperatures due to selective oxidation, resulting in high Fe/Ni ratios for the black melt (37 on average, individual values range from 13 to 449) and low Fe/Ni ratios for projectile droplets ("FeNi spheres" with a Fe/Ni ratio of 3 on average; Fe/Ni ratio for the meteorite is ∼12). The black melt shows emulsion textures that are the result of silicate liquid immiscibility. Liquid-liquid phase-separation resulted in the formation of a poorly polymerized, ultrabasic melt (Lfe) rich in divalent cations like Fe2+, Ca2+, or Mg2+, that is dispersed in a highly polymerized, high-silica melt (Lsi) matrix. The typical Wabar black melt emulsion displays a spheres-in-a-matrix texture of ∼10-20% Lfe homogeneously dispersed in the form of two sets of spheres and droplets (10-30 nm and 0.1-0.4 μm in diameter) in ∼80-90% Lsi matrix, plus occasionally disseminated FeNi spheres. Around large (>10 μm) FeNi spheres, however, the typical emulsion texture changes to ∼21% Lsi dispersed in ∼79% Lfe. This change of texture is interpreted as evidence for the transfer of meteoritic Fe from the meteoritic FeNi spheres into the target melt due to selective oxidation of Fe over Ni and Co. Variations in the bulk composition of Wabar black melt largely depend on the volume ratios between immiscible ultrabasic Lfe, felsic Lsi, and remains of meteoritic FeNi spheres. Based on natural occurrences of phase-separated glasses (this work and literature) and quenching experiments (literature), there is growing evidence that liquid immiscibility is a major process in the formation of glassy impactites.

Capreomycin oleate microparticles for intramuscular administration: Preparation, in vitro release and preliminary in vivo evaluation.

PubMed

Cambronero-Rojas, Adrián; Torres-Vergara, Pablo; Godoy, Ricardo; von Plessing, Carlos; Sepúlveda, Jacqueline; Gómez-Gaete, Carolina

2015-07-10

Capreomycin sulfate (CS) is a second-line drug used for the treatment of multidrug-resistant tuberculosis (MDR-TB). The adverse effects profile and uncomfortable administration scheme of CS has led to the development of formulations based on liposomes and polymeric microparticles. However, as CS is a water-soluble peptide that does not encapsulate properly into hydrophobic particulate matrices, it was necessary to reduce its aqueous solubility by forming the pharmacologically active capreomycin oleate (CO) ion pair. The aim of this research was to develop a new formulation of CO for intramuscular injection, based on biodegradable microparticles that encapsulate CO in order to provide a controlled release of the drug with reduced local and systemic adverse effects. The CO-loaded microparticles prepared by spray drying or solvent emulsion-evaporation were characterized in their morphology, encapsulation efficiency, in vitro/in vivo kinetics and tissue tolerance. Through scanning electron microscopy it was confirmed that the microparticles were monodisperse and spherical, with an optimal size for intramuscular administration. The interaction between CO and the components of the microparticle matrix was confirmed on both formulations by X-ray powder diffraction and differential scanning calorimetry analyses. The encapsulation efficiencies for the spray-dried and emulsion-evaporation microparticles were 92% and 56%, respectively. The in vitro kinetics performed on both formulations demonstrated a controlled and continuous release of CO from the microparticles, which was successfully reproduced on an in vivo rodent model. The results of the histological analysis demonstrated that none of the formulations produced significant tissue damage on the site of injection. Therefore, the results suggest that injectable CO microparticles obtained by spray drying and solvent emulsion-evaporation could represent an interesting therapeutic alternative for the treatment of MDR-TB. Copyright © 2015 Elsevier B.V. All rights reserved.

Achieving interconnected pore architecture in injectable PolyHIPEs for bone tissue engineering.

PubMed

Robinson, Jennifer L; Moglia, Robert S; Stuebben, Melissa C; McEnery, Madison A P; Cosgriff-Hernandez, Elizabeth

2014-03-01

Template polymerization of a high internal phase emulsion (polyHIPE) is a relatively new method to produce tunable high-porosity scaffolds for tissue regeneration. This study focuses on the development of biodegradable injectable polyHIPEs with interconnected porosity that have the potential to fill bone defects and enhance healing. Our laboratory previously fabricated biodegradable polyHIPEs that cure in situ upon injection; however, these scaffolds possessed a closed-pore morphology, which could limit bone ingrowth. To address this issue, HIPEs were fabricated with a radical initiator dissolved in the organic phase rather than the aqueous phase of the emulsion. Organic-phase initiation resulted in macromer densification forces that facilitated pore opening during cure. Compressive modulus and strength of the polyHIPEs were found to increase over 2 weeks to 43±12 MPa and 3±0.2 MPa, respectively, properties comparable to cancellous bone. The viscosity of the HIPE before cure (11.0±2.3 Pa·s) allowed for injection and filling of the bone defect, retention at the defect site during cure under water, and microscale integration of the graft with the bone. Precuring the materials before injection allowed for tuning of the work and set times. Furthermore, storage of the HIPEs before cure for 1 week at 4°C had a negligible effect on pore architecture after injection and cure. These findings indicate the potential of these emulsions to be stored at reduced temperatures and thawed in the surgical suite before injection. Overall, this work highlights the potential of interconnected propylene fumarate dimethacrylate polyHIPEs as injectable scaffolds for bone tissue engineering.

Effect of polymerization technique and glass fiber addition on the surface roughness and hardness of PMMA denture base material.

PubMed

Gad, Mohammed M; Rahoma, Ahmed; Al-Thobity, Ahmad M

2018-06-20

The current study evaluated the effects of autoclave polymerization both with and without glass fiber (GF) reinforcement on the surface roughness and hardness of acrylic denture base material. Ninety disc specimens (30×2.5 mm) were prepared from Vertex resin and divided according to polymerization techniques into a water bath, short and long autoclave polymerization groups. Tested groups were divided into three subgroups according to the GF concentration (0, 2.5, and 5 wt%). Profilometer and Vickers hardness tests were performed to measure surface roughness and hardness. ANOVA and Tukey-Kramer multiple comparison tests analyzed the results, and p≤0.05 was considered statistically significant. Autoclave polymerization significantly decreased the surface roughness and increased the hardness of acrylic resin without GF reinforcement (p<0.05). However, 5 wt% GF addition significantly increased surface roughness and decreased hardness of the autoclave polymerized denture base resin (p<0.05). Surface properties of Polymethyl methacrylate (PMMA) denture base material improved with autoclave polymerization and negatively affected with GFs addition.

Technique for the polymerization of monomers for PPQ/graphite fiber composites

NASA Technical Reports Server (NTRS)

Serafini, T. T.; Delvigs, P.; Vannucci, R. D.

1973-01-01

Impregnation of fiber prior to appreciable polymerization completely eliminates impregnation problems encountered with use of high viscosity high molecular weight polyphenylquinoxalines (PPQ) solutions. Major part of polymerization of reactant mixture is conducted on fiber during solvent removal and final curing stages.

Two-Photon Polymerization of Defects in Photonic Crystals

DTIC Science & Technology

2006-01-01

technique employs two-photon polymerization (TPP) (for description, see Section 2.2) to fabricate high-resolution 3D embedded polymer features within... polymer , and therefore does not influence the polymerization . The image contrast is from the different reflectivities of the interfaces in the system due...Spectroscopy also confirmed for the first time the successful polymerization of a uniform, dense polymer feature throughout the thickness of the

A thin porous substrate using bonded particles for reverse-emulsion electrophoretic displays

NASA Astrophysics Data System (ADS)

Ahumada, M.; Bryning, M.; Cromer, R.; Hartono, M.; Lee, S. J.

2012-03-01

A thin porous layer of bonded ceramic microparticles has been developed to provide structural integrity and a stationary matrix for use in reflective-mode reverse-emulsion electrophoretic displays (REED), based on self-assembled nanodroplets dispersed in a non-polar liquid. REED ink uses low-cost materials and manufacturing processes, yet is capable of video speed and low voltage operation below 10 V. Porous layers of titanium dioxide (TiO2) are prepared as thin as 10 microns by fluidizing the particles in a water-based slurry with polymeric adhesive. The slurry is distributed between glass shear plates, one of which serves as the substrate for the working device. Particle morphology is examined using scanning electron microscopy and layer uniformity is characterized by opacity measurements using a throughbeam fiber optic sensor. Performance of the bonded matrix with REED ink is compared to baseline performance of a paste mixture, comprised of the same ink and unbonded TiO2 particles. Results show that at 25% volume fraction, the bonded substrate improves image bistability and is better able to maintain both light and dark intensity after extensive switching. The same bonded substrate also improves image bistability when power is disconnected, even compared to a paste with 40% volume fraction of TiO2.

Synthesis and electrorheological characteristics of polyaniline/organoclay nanoparticles via Pickering emulsion polymerization

NASA Astrophysics Data System (ADS)

Fang, F. F.; Liu, Y. D.; Choi, H. J.

2010-12-01

Conducting polymer/inorganic composite particles have been regarded as a potential candidate material for electrorheological (ER) fluids when dispersed in non-conducting oils due to their synergistic physical properties such as enhanced thermal stability and high dielectric properties. In this study, we fabricated polyaniline (PANI)/clay nanoparticles with unique core-shell structure via Pickering emulsion in the phase of toluene by adopting exfoliated clay as a stabilizer. Successfully synthesized PANI nanospheres which were initialized by oil-soluble benzoyl peroxide possess a polydispersed size distribution of particles ranging from 200 nm to 1 µm. Surface morphology was revealed by SEM images in which some clay sheets were found to wrap the PANI nanoparticles compactly. TEM images explicitly confirm the position of exfoliated clay layers around the nanospheres. In addition, some nano-scaled particles showed an irregular shape because clay plates are difficult to bend while wrapping the very tiny PANI nanoparticles, so the x-ray diffraction (XRD) pattern did not indicate any obvious sharp peak, demonstrating the nearly completely exfoliated clay layers. Besides these, thermal gravimetric analysis (TGA) data also gave additional information on thermal stability and composition. Finally, the ER fluid was prepared by dispersing PANI/clay nanoparticles in silicone oil and the ER performance was investigated via a rotational rheometer under an applied electric field.

Fabrication of sub-micrometer-sized jingle bell-shaped hollow spheres from multilayered core-shell particles.

PubMed

Gu, Shunchao; Kondo, Tomohiro; Mine, Eiichi; Nagao, Daisuke; Kobayashi, Yoshio; Konno, Mikio

2004-11-01

Jingle bell-shaped hollow spheres were fabricated starting from multilayered particles composed of a silica core, a polystyrene inner shell, and a titania outer shell. Composite particles of silica core-polystyrene shell, synthesized by coating a 339-nm-sized silica core with a polystyrene shell of thickness 238 nm in emulsion polymerization, were used as core particles for a succeeding titania-coating. A sol-gel method was employed to form the titania outer shell with a thickness of 37 nm. The inner polystyrene shell in the multilayered particles was removed by immersing them in tetrahydrofuran. These successive procedures could produce jingle bell-shaped hollow spheres that contained a silica core in the titania shell.

Low-power upconversion in dye-doped polymer nanoparticles.

PubMed

Simon, Yoan C; Bai, Shuo; Sing, Michelle K; Dietsch, Hervé; Achermann, Marc; Weder, Christoph

2012-04-13

Examples of nanoscale low-power upconverting systems are rapidly increasing because of their potential application in numerous areas such as bioimaging or drug delivery. The fabrication of dye-doped cross-linked rubbery nanoparticles that exhibit upconversion even at relatively low power densities is reported here. The nanoparticles were prepared by surfactant-free emulsion polymerization of n-butylacrylate with divinylbenzene as a cross-linker, followed by dyeing of the resulting particles with a two-chromophore system composed of a palladium porphyrin sensitizer, and diphenylanthracene. Blue emission (≈440 nm) of these systems was observed upon excitation at 532 nm. In addition to their optical properties, the particles were characterized by electron microscopy and dynamic light scattering. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The impact of size on particulate vaccine adjuvants.

PubMed

Shah, Ruchi R; O'Hagan, Derek T; Amiji, Mansoor M; Brito, Luis A

2014-12-01

Particulate adjuvants have been successful at inducing increased immune responses against many poorly immunogenic antigens. However, the mechanism of action of these adjuvants often remains unclear. As more potential vaccine targets are emerging, it is becoming necessary to broaden our knowledge on the factors involved in generating potent immune responses to recombinant antigens with adjuvants. While composition of adjuvants is integral in defining the overall performance of an adjuvant, some physical parameters such as particle size, surface charge and surface modification may also contribute to the potency. In this review, we will try to highlight the role of particle size in controlling the immune responses to adjuvanted vaccines, with a focus on insoluble aluminum salts, oil-in-water emulsions, polymeric particles and liposomes.

Electrokinetic properties of polymer colloids

NASA Technical Reports Server (NTRS)

Micale, F. J.; Fuenmayor, D. Y.

1986-01-01

The surface of polymer colloids, especially polystyrene latexes, were modified for the purpose of controlling the electrokinetic properties of the resulting colloids. Achievement required a knowledge of electrical double layer charging mechanism, as a function of the electrolyte conditions, at the polymer/water interface. The experimental approach is to control the recipe formulation in the emulsion polymerization process so as to systematically vary the strong acid group concentration on the surface of the polymer particles. The electrophoretic mobility of these model particles will then be measured as a function of surface group concentration and as a function of electrolyte concentration and type. An effort was also made to evaluate the electrophoretic mobility of polystyrene latexes made in space and to compare the results with latexes made on the ground.

Symposium on Explosives and Pyrotechnics, 13th, Hilton Head Island, SC, Dec. 2-4, 1986, Proceedings

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

1987-01-01

The present conference on explosive and pyrotechnic technologies discusses the shock-sensitivity of RDX, the thermodynamic properties of RDX, TNT, nitroglycerine, and HMX energetic molecules, the dynamic resistivity of exploding conductors, the decomposition of azides, the critical shock-initiation energy of emulsion explosives, actuator valve optimization, pyrotechnic aerosolization from novel imbibed liquid matrices, tetrazole initiators, and polymeric binders for red phosphorus pellets. Also discussed are channel-effect studies, the dynamic desensitization of coal mine explosives, the electromagnetic and electrostatic protection of explosives, the reliability of fuze explosive trains, the hazardous properties of explosive chemicals, the emulsification of an explosive with a chemical foamingmore » agent, and low energy ignition of HMX using a foil bridge.« less

Synthesis and characterization of nanomagnetite particles and their polymer coated forms.

PubMed

Utkan, Guldem Guven; Sayar, Filiz; Batat, Pinar; Ide, Semra; Kriechbaum, Manfred; Pişkin, Erhan

2011-01-15

Superparamagnetic nanoparticles were prepared by coprecipitation of ferrous (Fe(2+)) and ferric (Fe(3+)) aqueous solution by a base. Nanomagnetite particles were coated with poly(St/PEG-EEM/DMAPM) and poly(St/PEG-MA/DMAPM) layer by emulsifier-free emulsion polymerization. Chemical structure of nanoparticles was characterized by both FTIR and (1)H NMR. Particle morphologies were determined by Zeta Sizer, DLS, XRD and SAXS. Structural analysis showed that after polymer coating nanomagnetite particles kept their superparamagnetic property. Besides the synthesized magnetites, polymer coated forms of these particles are more biocompatible, well dispersable and uniform. These properties make them a very strong candidate for bioengineering applications, such as bioseparation, gene transfer. Copyright © 2010 Elsevier Inc. All rights reserved.

Ca (OH)2Nanoparticles Based on Acrylic Copolymers for the consolidation and protection of Ancient Egypt Calcareous Stone Monuments

NASA Astrophysics Data System (ADS)

Al-Dosari, Mohammad A.; Darwish, Sawsan S.; Adam, Mahmoud A.; Elmarzugi, Nagib A.; Al-Mouallimi, Nadia; Ahmed, Sayed M.

2017-04-01

The deterioration of calcareous stones materials used in artistic/architectural field is one of the most serious problems facing conservation today. The aim of this study was to evaluate the effectiveness of nanosized particles of calcium hydroxide (slaked lime) as a consolidation and protection material dispersed in acrylic copolymer, poly ethylmethacrylate/methylacrylate (70:30) (Poly (EMA/MA), for calcareous stone monuments and painted surfaces affected by different kinds of decay. The synthesis process of Ca (OH)2 nanoparticles/polymer nanocomposites have been prepared by in situ emulsion polymerization system. The prepared nanocomposite containing 5% of Ca (OH)2 nanoparticles showed obvious transparency features and represent nanocomposites coating technology with hydrophobic, consolidating and well protection properties.

The hypertriglyceridemic clamp technique. Studies using long-chain and structured triglyceride emulsions in healthy subjects.

PubMed

Nordenström, Jörgen; Thörne, Anders; Aberg, Wiveca; Carneheim, Claes; Olivecrona, Thomas

2006-11-01

In a randomized crossover study, plasma kinetics of 2 different types of fat emulsions were studied in 8 healthy volunteers by using a hypertriglyceridemic clamp technique. The method involves the stabilization of serum triglyceride (TG) concentration during 180 minutes at a predetermined level (4 mmol/L) by adjustment of TG infusion rate by repeated online measurements of serum TG concentration. The fat emulsions under study were a long-chain fatty acid triglyceride (LCT) emulsion (Intralipid 20%, Fresenius Kabi, Sweden) and a structured triglyceride (STG) emulsion (Structolipid 20%, Fresenius Kabi) where medium- and long-chain fatty acids have been interesterified within a TG molecule. The hypertriglyceridemic clamp was found to have acceptable reproducibility when tested in 3 healthy individuals on 2 different occasions, as similar steady-state TG levels were obtained by infusing similar amounts of fat. The average (+/-SEM) TG concentration during the 180-minute clamp was similar for STGs and LCTs (4.0 +/- 0.1 vs 3.9 +/- 0.1 mmol/L; not significant), but the amount of fat that had to be infused was significantly higher during STG than during LCT clamping (0.31 +/- 0.04 vs 0.21 +/- 0.02 g TG per minute; P < .05). Higher serum levels of free fatty acids (1.80 +/- 0.13 vs 0.96 +/- 0.09 mmol/L; P < .05), free glycerol (1.30 +/- 0.07 vs 0.76 +/- 0.08 mmol/L; P < .001), and beta-OH butyrate (1.61 +/- 0.44 vs 1.17 +/- 0.23 mmol/L; not significant) were obtained at the end of the clamp during infusion of STGs compared with LCTs. During infusion of STGs the medium-chain fatty acids octanoic (C:8) and decanoic acid (C:10) constituted approximately half of circulating fatty acids that correspond to the compositional ratio of the emulsion. Plasma lipoprotein lipase (LPL) concentration was higher during STG than during LCT clamping (6.06 +/- 0.62 vs 3.15 +/- 0.40 mU/mL; P < .05), and there was a positive correlation between the mean LPL concentration and the amount of infused TG during the steady-state period (r = 0.58; P < .05). In conclusion, the hypertriglyceridemic clamp method was found to give reproducible results and could be considered for comparison of metabolic clearance properties of different types of fat emulsions. The capacity of healthy subjects to eliminate STGs from blood was greater than for LCTs. An increased LPL activity induced by the higher TG infusion rate may have contributed to the increased metabolic clearance of STGs.

Correlation of individual cosmic ray nuclei with the observation of light flashes by Apollo astronauts. [nuclear emulsion detector design and operation

NASA Technical Reports Server (NTRS)

Pinsky, L. S.; Osborne, W. Z.; Bailey, J. V.

1975-01-01

A nuclear emulsion detector known as the Apollo Light Flash Moving Emulsion Detector (ALFMED) was designed: (1) to record tracks of primary cosmic rays; (2) to provide time-of-passage information via a relative plate translation technique; (3) to provide particle trajectory information; and (4) to fit into a masklike device that could be located about the head and eyes of an astronaut. An ALFMED device was worn by an astronaut observing light flashes for 60 minutes on each of the last two Apollo missions. During the Apollo 17 experiment seventeen separate flashes were reported by the observer. With one-third of the total plate area completely analyzed, two definite correlations have been found between Z greater than 8 cosmic ray nuclei traversing an eye and the reports of visual sensations.

Synthesis and characterization of cationic lipid coated magnetic nanoparticles using multiple emulsions as microreactors

NASA Astrophysics Data System (ADS)

Akbaba, Hasan; Karagöz, Uğur; Selamet, Yusuf; Kantarcı, A. Gülten

2017-03-01

The aim of this study was to develop a novel iron oxide nanoparticle synthesis method with in-situ surface coating. For this purpose multiple emulsions were used as microreactors for the first time and magnetic iron oxide particles synthesized in the core of cationic solid lipid nanoparticles. DLS, SEM, TEM, VSM, Raman Spectrometer, XRD, and XPS techniques were performed for characterization of the magnetic nanoparticles. Obtained magnetic nanoparticles are superparamagnetic and no additional process was needed for surface adjustments. They are positively charged as a result of cationic lipid coating and has appropriate particle size (<30 nm) for drug or nucleic acid delivery. Structure analysis showed that magnetic core material is in the form of magnetite. Saturation magnetization value was measured as 15-17 emu g-1 for lipid coated magnetic nanoparticles obtained by multiple emulsion method which is reasonably sufficient for magnetic targeting.

NMR relaxation dispersion of Miglyol molecules confined inside polymeric micro-capsules.

PubMed

Nechifor, Ruben; Ardelean, Ioan; Mattea, Carlos; Stapf, Siegfried; Bogdan, Mircea

2011-11-01

Frequency dependent NMR relaxation studies have been carried out on Miglyol molecules confined inside core shell polymeric capsules to obtain a correlation between capsule dimension and the measurable parameters. The polymeric capsules were prepared using an interfacial polymerization technique for three different concentrations of Miglyol. It was shown that the variation of Miglyol concentration influences the capsule dimension. Their average size was estimated using the pulsed field gradient diffusometry technique. The relaxation dispersion curves were obtained at room temperature by a combined use of a fast field cycling instrument and a high-field instrument. The frequency dependence of relaxation rate shows a transition from a diffusion-limited to a surface-limited relaxation regime. Copyright © 2011 John Wiley & Sons, Ltd.

Evaluation of the color stability of two techniques for reproducing artificial irides after microwave polymerization

PubMed Central

GOIATO, Marcelo Coelho; dos SANTOS, Daniela Micheline; MORENO, Amália; GENNARI-FILHO, Humberto; PELLIZZER, Eduardo Piza

2011-01-01

The use of ocular prostheses for ophthalmic patients aims to rebuild facial aesthetics and provide an artificial substitute to the visual organ. Natural intemperate conditions promote discoloration of artificial irides and many studies have attempted to produce irides with greater chromatic paint durability using different paint materials. Objectives The present study evaluated the color stability of artificial irides obtained with two techniques (oil painting and digital image) and submitted to microwave polymerization. Material and Methods Forty samples were fabricated simulating ocular prostheses. Each sample was constituted by one disc of acrylic resin N1 and one disc of colorless acrylic resin with the iris interposed between the discs. The irides in brown and blue color were obtained by oil painting or digital image. The color stability was determined by a reflection spectrophotometer and measurements were taken before and after microwave polymerization. Statistical analysis of the techniques for reproducing artificial irides was performed by applying the normal data distribution test followed by 2-way ANOVA and Tukey HSD test (α=.05). Results Chromatic alterations occurred in all specimens and statistically significant differences were observed between the oil-painted samples and those obtained by digital imaging. There was no statistical difference between the brown and blue colors. Independently of technique, all samples suffered color alterations after microwave polymerization. Conclusion The digital imaging technique for reproducing irides presented better color stability after microwave polymerization. PMID:21625733

Synthesis and characterization of fluorinated polyacrylate latex emulsified with novel surfactants.

PubMed

Zhang, Cuifeng; Xu, Tingting; Bao, Zhongbin; Chen, Lijun

2017-01-01

The fluorinated polyacrylate latex were successfully prepared with semi- continuous seeded emulsion polymerization of butyl acrylate (BA), methyl methacrylate (MMA) and hexafluorobutyl methacrylate (HFMA) which was initiated with potassium persulfate (KPS) initiator and emulsified with the novel mixed surfactants of sodium lauryl glutamate (SLG) and alkylphenol ethoxylates (OP-10). The structure of the resultant latex was confirmed by Fourier transform infrared spectroscopy (FTIR). The particle size of the latex was measured by Zetatrac dynamic light scattering detector. The film of latex was tested by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and contact angle (CA). The optimum conditions of preparing the novel fluorinated polyacrylate latex are optimized and the results are as follows: the amount of emulsifiers is 4.0%; mass ratio of SLG to OP-10 is 1:1, the amount of the initiator is 0.6%. The mass ratio of MMA to BA is 1:1 and the amount of HFMA is 7.0%. In this case, the conversion is high and the polymerization stability is good. In addition, the water resistance and thermal properties of the latex films were improved significantly in comparison with the film of the latex prepared without the fluorinated monomer.

Synthesis and characterization of fluorinated polyacrylate latex emulsified with novel surfactants

PubMed Central

Zhang, Cuifeng; Xu, Tingting; Bao, Zhongbin; Chen, Lijun

2017-01-01

Abstract The fluorinated polyacrylate latex were successfully prepared with semi- continuous seeded emulsion polymerization of butyl acrylate (BA), methyl methacrylate (MMA) and hexafluorobutyl methacrylate (HFMA) which was initiated with potassium persulfate (KPS) initiator and emulsified with the novel mixed surfactants of sodium lauryl glutamate (SLG) and alkylphenol ethoxylates (OP-10). The structure of the resultant latex was confirmed by Fourier transform infrared spectroscopy (FTIR). The particle size of the latex was measured by Zetatrac dynamic light scattering detector. The film of latex was tested by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and contact angle (CA). The optimum conditions of preparing the novel fluorinated polyacrylate latex are optimized and the results are as follows: the amount of emulsifiers is 4.0%; mass ratio of SLG to OP-10 is 1:1, the amount of the initiator is 0.6%. The mass ratio of MMA to BA is 1:1 and the amount of HFMA is 7.0%. In this case, the conversion is high and the polymerization stability is good. In addition, the water resistance and thermal properties of the latex films were improved significantly in comparison with the film of the latex prepared without the fluorinated monomer. PMID:29491785

A modified emulsion gelation technique to improve buoyancy of hydrogel tablets for floating drug delivery systems.

PubMed

Yom-Tov, Ortal; Seliktar, Dror; Bianco-Peled, Havazelet

2015-10-01

The use of buoyant or floating hydrogel tablets is of particular interest in the sustained release of drugs to the stomach. They have an ability to slow the release rates of drugs by prolonging their absorption window in the upper part of the gastrointestinal (GI) tract. In this study we synthesized bioactive hydrogels that have sustainable release rates for drugs in the stomach based on a hydrogel preparation technique that employs emulsifying surfactants. The emulsion gelation technique, which encapsulates oil droplets within the hydrogels during crosslinking, was used to decrease their specific gravity in aqueous environments, resulting in floating drug release depots. Properties such as swelling, buoyancy, density and drug release were manipulated by changing the polymer concentrations, surfactant percentages and the oil:polymer ratios. The relationship between these properties and the hydrogel's floating lag time was documented. The potential for this material to be used as a floating drug delivery system was demonstrated. Copyright © 2015 Elsevier B.V. All rights reserved.

Preparation of Eleutherine americana-Alginate Complex Microcapsules and Application in Bifidobacterium longum

PubMed Central

Phoem, Atchara N; Chanthachum, Suphitchaya; Voravuthikunchai, Supayang P

2015-01-01

Microencapsulation using extrusion and emulsion techniques was prepared for Bifidobacterium longum protection against sequential exposure to simulated gastric and intestinal juices, refrigeration storage and heat treatment. Eleutherine americana was used as the co-encapsulating agent. Hydrolysis of E. americana by gastric and intestinal juices was also determined. E. americana and its oligosaccharide extract demonstrated their resistance to low pH and partial tolerance to human α-amylase. Microencapsulated B. longum with E. americana and oligosaccharide extract prepared by the extrusion technique survived better than that by the emulsion technique under adverse conditions. Survival of microencapsulated cells after exposure to the juices and refrigeration storage was higher than free cells at Weeks 2 and 4. In addition, the viability of microencapsulated cells was better than free cells at 65 °C for 15 min. This work suggested that microencapsulated B. longum with E. americana offers the effective delivery of probiotics to colon and maintains their survival in food products. PMID:25629556

A study of the radiation environment on board the space shuttle flight STS-57

NASA Technical Reports Server (NTRS)

Badhwar, G. D.; Atwell, W.; Benton, E. V.; Frank, A. L.; Keegan, R. P.; Dudkin, V. E.; Karpov, O. N.; Potapov, V.; Akopova, A. B.; Magradze, N. V.

1995-01-01

A joint NASA-Russian study of the radiation environment inside a SPACEHAB 2 locker on space shuttle flight STS-57 was conducted. The shuttle flew in a nearly circular orbit of 28.5 deg inclination and 462 km altitude. The locker carried a charged particle spectrometer, a tissue equivalent proportional counter (TEPC), and two area passive detectors consisting of combined NASA plastic nuclear track detectors (PNTD's) and thermoluminescent detectors (TLD's), and Russian nuclear emulsions, PNTD's, and TLD's. All the detector systems were shielded by the same shuttle mass distribution. This makes possible a direct comparison of the various dose measurement techniques. In addition, measurements of the neutron energy spectrum were made using the proton recoil technique. The results show good agreement between the integral LET spectrum of the combined galactic and trapped particles using the tissue equivalent proportional counter and track detectors between about 15 keV/micron and 200 keV/micron. The LET spectrum determined from nuclear emulsions was systematically lower by about 50%, possibly due to emulsion fading. The results show that the TEPC measured an absorbed dose 20% higher than TLD's, due primarily to an increased TEPC response to neutrons and a low sensitivity of TLD's to high LET particles under normal processing techniques. There is a significant flux of high energy neutrons that is currently not taken into consideration in dose equivalent calculations. The results of the analysis of the spectrometer data will be reported separately.

Trace detection of perchlorate in industrial-grade emulsion explosive with portable surface-enhanced Raman spectroscopy.

PubMed

Nuntawong, N; Eiamchai, P; Limwichean, S; Wong-ek, B; Horprathum, M; Patthanasettakul, V; Leelapojanaporn, A; Nakngoenthong, S; Chindaudom, P

2013-12-10

Recent analyses by ion-exchange chromatography (IC) showed that, beside nitrate, the majority of the industrial-grade emulsion explosives, extensively used by most separatists in the southern Thailand insurgency, contained small traces of perchlorate anions. In demand for the faster, reliable, and simple detection methods, the portable detection of nitrate and perchlorate became the great interest for the forensic and field-investigators. This work proposed a unique method to detect the trace amount of perchlorate in seven industrial-grade emulsion explosives under the field tests. We utilized the combination of the portable Raman spectroscope, the developed surfaced-enhanced Raman substrates, and the sample preparation procedures. The portable Raman spectroscope with a laser diode of 785 nm for excitation and a thermoelectric-cooled CCD spectrometer for detection was commercially available. The SERS substrates, with uniformly distributed nanostructured silver nanorods, were fabricated by the DC magnetron sputtering system, based on the oblique-angle deposition technique. The sample preparation procedures were proposed based on (1) pentane extraction technique and (2) combustion technique, prior to being dissolved in the purified water. In comparison to the ion chromatography and the conventional Raman measurements, our proposed methods successfully demonstrated the highly sensitive detectability of the minimal trace amount of perchlorate from five of the explosives with minimal operating time. This work was therefore highly practical to the development for the forensic analyses of the post-blast explosive residues under the field-investigations. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

Mitigation of NOx and smoke emissions in a diesel engine using novel emulsified lemon peel oil biofuel.

PubMed

Bragadeshwaran, Ashok; Kasianantham, Nanthagopal; Balusamy, Saravanan; Muniappan, SenthilKumar; Reddy, Dandu Madhu Sudan; Subhash, Randive Vishal; Pravin, Nashte Adarsh; Subbarao, Rayapati

2018-06-25

Lemon peel oil (LPO) is considered to be a viable alternative fuel for diesel engine applications due to its wider availability, renewable nature, easy extraction process, almost equivalent calorific value as neat diesel, and low viscosity. The present work aims to investigate the effect of novel emulsified LPO in a diesel engine in order to reduce the NOx emission without compromising the engine performance. A new ionic surfactant is introduced in the present study, namely methyl-dihydroxy propyl imidazolium chloride due to its higher hydrophilic-lipophilic balance value which helps to prepare stable water in oil emulsion. Also, Span 80 has been selected as another suitable surfactant for water in oil emulsion. Four emulsified fuel samples have been prepared using LPO, water, and different concentrations of surfactants. All the fuel samples are tested for their stability through gravitational technique for 7 days. Among the emulsified samples, 92% LPO + 5% water + 2% Span 80 + 1% methyl-dihydroxy propyl imidazolium chloride by volume (LPOE2) and 93.5% LPO + 5% water + 1.5% surfactant Span 80 by volume (LPOE4) have showed better stability when compared to other emulsion fuel samples. It is also revealed that the stability of LPO emulsion is improved by the addition of two emulsions. The experimental results showed that the brake thermal efficiency of LPO emulsion is reduced to 29.87 from 34.58% of pure LPO at full load condition. Oxides of nitrogen emission and smoke emission are reduced by 21-32 and 6-15% for the LPO emulsion samples compared to pure LPO. Moreover, the diesel engine operation with emulsified form of LPO increases the HC emission about 0.1 g/kWh for LPOE4 and 0.15 g/kWh for LPOE2 fuels from 0.053 g/kW for pure LPO at maximum power output condition. The reformulation of LPO into emulsified form increases the CO emission by 25-53% compared to pure LPO. Moreover, the reformulation of LPO into emulsions has resulted in lower cylinder pressure and heat release rate compared to pure LPO and diesel fuels.

Electric field mediated breakdown of thin liquid films separating microscopic emulsion droplets

NASA Astrophysics Data System (ADS)

Mostowfi, Farshid; Khristov, Khristo; Czarnecki, Jan; Masliyah, Jacob; Bhattacharjee, Subir

2007-04-01

The authors present a microfluidic technique for electrically induced breakup of thin films formed between microscopic emulsion droplets. The method involves creating a stationary film at the intersection of two microchannels etched onto a glass substrate. After stabilizing the film, a ramped potential is applied across it. The electrical stresses developed at the film interfaces lead to its rupture above a threshold potential. The potential difference at which the film ruptures assesses the film stability. This approach is employed to demonstrate how surfactant (lecithin) adsorption imparts stability to an ultrathin oil film formed between two water droplets.

Spray dried microparticles of chia oil using emulsion stabilized by whey protein concentrate and pectin by electrostatic deposition.

PubMed

Noello, C; Carvalho, A G S; Silva, V M; Hubinger, M D

2016-11-01

Chia seed oil has a high content of α-linolenic acid (60%) and linoleic acid (20%). Use of this oil in different products is limited due to its liquid state, and the presence of insaturation is a trigger for oxidation. In this context, to facilitate the incorporation of chia oil in food products and increase its protection against oxidation, the aim of this work was to produce chia oil microparticles by spray drying using emulsions stabilized by whey protein concentrate (ζ-potential +13.4 at pH3.8) and pectin (ζ-potential -40.4 at pH3.8) through the electrostatic layer-by-layer deposition technique and emulsions prepared with only whey protein concentrate. Emulsions stabilized by whey protein concentrate and stabilized by whey protein concentrate-pectin were prepared using maltodextrin (10 DE) and modified starch (Hi-Cap® 100). They were characterized in relation to stability, droplet size, ζ-Potential and optical microscopy. The microparticles were characterized in relation to moisture content, water activity, particle size, microstructure and oxidative stability by the Rancimat method. Emulsions stabilized by whey protein concentrate-pectin with added maltodextrin 10 DE and emulsions stabilized by whey protein concentrate with added modified starch (Hi-Cap® 100) were stable after 24h. Emulsions stabilized by whey protein concentrate and by whey protein concentrate-pectin showed droplets with mean diameter ranging from 0.80 to 1.31μm, respectively and ζ-potential varying from -6.9 to -27.43mV, respectively. After spray drying, the microparticles showed an mean diameter ranging from 7.00 to 9.00μm. All samples presented high encapsulation efficiency values, above 99%. Microparticles produced with modified starch showed a smoother spherical surface than particles with maltodextrin 10 DE, which presented a wrinkled surface. All microparticles exhibited higher oxidative stability than chia oil in pure form. Copyright © 2016 Elsevier Ltd. All rights reserved.

Acute administration of n-3 rich triglyceride emulsions provides cardioprotection in murine models after ischemia-reperfusion.

PubMed

Zirpoli, Hylde; Abdillahi, Mariane; Quadri, Nosirudeen; Ananthakrishnan, Radha; Wang, Lingjie; Rosario, Rosa; Zhu, Zhengbin; Deckelbaum, Richard J; Ramasamy, Ravichandran

2015-01-01

Dietary n-3 fatty acids (FAs) may reduce cardiovascular disease risk. We questioned whether acute administration of n-3 rich triglyceride (TG) emulsions could preserve cardiac function and decrease injury after ischemia/reperfusion (I/R) insult. We used two different experimental models: in vivo, C57BL/6 mice were exposed to acute occlusion of the left anterior descending coronary artery (LAD), and ex-vivo, C57BL/6 murine hearts were perfused using Langendorff technique (LT). In the LAD model, mice treated with n-3 TG emulsion (1.5 g/kg body weight), immediately after ischemia and 1 h later during reperfusion, significantly reduced infarct size and maintained cardiac function (p<0.05). In the LT model, administration of n-3 TG emulsion (300 mg TG/100 ml) during reperfusion significantly improved functional recovery (p<0.05). In both models, lactate dehydrogenase (LDH) levels, as a marker of injury, were significantly reduced by n-3 TG emulsion. To investigate the mechanisms by which n-3 FAs protects hearts from I/R injury, we investigated changes in key pathways linked to cardioprotection. In the ex-vivo model, we showed that n-3 FAs increased phosphorylation of AKT and GSK3β proteins (p<0.05). Acute n-3 TG emulsion treatment also increased Bcl-2 protein level and reduced an autophagy marker, Beclin-1 (p<0.05). Additionally, cardioprotection by n-3 TG emulsion was linked to changes in PPARγ protein expression (p<0.05). Rosiglitazone and p-AKT inhibitor counteracted the positive effect of n-3 TG; GSK3β inhibitor plus n-3 TG significantly inhibited LDH release. We conclude that acute n-3 TG injection during reperfusion provides cardioprotection. This may prove to be a novel acute adjunctive reperfusion therapy after treating patients with myocardial infarction.

Acute Administration of n-3 Rich Triglyceride Emulsions Provides Cardioprotection in Murine Models after Ischemia-Reperfusion

PubMed Central

Zirpoli, Hylde; Abdillahi, Mariane; Quadri, Nosirudeen; Ananthakrishnan, Radha; Wang, Lingjie; Rosario, Rosa; Zhu, Zhengbin; Deckelbaum, Richard J.; Ramasamy, Ravichandran

2015-01-01

Dietary n-3 fatty acids (FAs) may reduce cardiovascular disease risk. We questioned whether acute administration of n-3 rich triglyceride (TG) emulsions could preserve cardiac function and decrease injury after ischemia/reperfusion (I/R) insult. We used two different experimental models: in vivo, C57BL/6 mice were exposed to acute occlusion of the left anterior descending coronary artery (LAD), and ex-vivo, C57BL/6 murine hearts were perfused using Langendorff technique (LT). In the LAD model, mice treated with n-3 TG emulsion (1.5g/kg body weight), immediately after ischemia and 1h later during reperfusion, significantly reduced infarct size and maintained cardiac function (p<0.05). In the LT model, administration of n-3 TG emulsion (300mgTG/100ml) during reperfusion significantly improved functional recovery (p<0.05). In both models, lactate dehydrogenase (LDH) levels, as a marker of injury, were significantly reduced by n-3 TG emulsion. To investigate the mechanisms by which n-3 FAs protects hearts from I/R injury, we investigated changes in key pathways linked to cardioprotection. In the ex-vivo model, we showed that n-3 FAs increased phosphorylation of AKT and GSK3β proteins (p<0.05). Acute n-3 TG emulsion treatment also increased Bcl-2 protein level and reduced an autophagy marker, Beclin-1 (p<0.05). Additionally, cardioprotection by n-3 TG emulsion was linked to changes in PPARγ protein expression (p<0.05). Rosiglitazone and p-AKT inhibitor counteracted the positive effect of n-3 TG; GSK3β inhibitor plus n-3 TG significantly inhibited LDH release. We conclude that acute n-3 TG injection during reperfusion provides cardioprotection. This may prove to be a novel acute adjunctive reperfusion therapy after treating patients with myocardial infarction. PMID:25559887

Phospholipid hydrolysis in a pharmaceutical emulsion assessed by physicochemical parameters and a new analytical method.

PubMed

Rabinovich-Guilatt, Laura; Dubernet, Catherine; Gaudin, Karen; Lambert, Gregory; Couvreur, Patrick; Chaminade, Pierre

2005-09-01

The aim of this work was to develop a simple high-performance liquid chromatography (HPLC) technique with evaporative light scattering detection (ELSD) for the separation and quantification of the major phospholipid (PL) and lysophospholipid (LPL) classes contained in a pharmaceutical phospholipid-based emulsion. In the established method, phosphatidylcholine (PC), phosphatidylethanolamine (PE), sphingomyeline (SM), lysophosphatidylcholine (LPC) and lysophosphatidylethanolamine (LPE) were separated with a PVA-Sil stationary phase and a binary gradient from pure chloroform to methanol:water (94:6 v/v) at 3.4%/min. The ELSD detection was enhanced using 0.1% triethylamine and formic acid in each gradient mobile phases. Factors such as stationary phase and ELSD drift tube temperature were optimized, concluding in optimal temperatures of 25 degrees C for separation and 50 degrees C for evaporation. This HPLC-ELSD method was then applied to a PL-emulsion exposed to autoclaving and accelerated thermal conditions at 50 degrees C. Hydrolysis of PC and PE followed first-order kinetics, representing only 45% of the total lipid mass after 3 months. The chemical stability was correlated to commonly measured formulation physical and physico-chemical parameters such as droplet size, emulsion pH and zeta-potential.

The effect of butter grains on physical properties of butter-like emulsions.

PubMed

Rønholt, Stine; Buldo, Patrizia; Mortensen, Kell; Andersen, Ulf; Knudsen, Jes C; Wiking, Lars

2014-01-01

Milk fat exists as globules in its natural state in milk. The potential of using globular fat to modulate the rheological properties and crystallization behavior in butter-like emulsions was studied in the present work. We conducted a comparative study of butter-like emulsions, with a fat phase consisting of 0, 10, 25, 50, or 100% anhydrous milk fat (AMF), the remaining fat being butter grains, and all samples containing 20% water, to obtain systematic variation in the ratio of globular fat. All emulsions were studied over 4wk of storage at 5°C. By combining small and large deformation rheology, we conducted a detailed characterization of the rheological behavior of butter-like emulsions. We applied differential scanning calorimetry to monitor thermal behavior, confocal laser scanning microscopy for microstructural analysis, and low-field pulsed nuclear magnetic resonance spectrometry to measure solid fat content. By combining these techniques, we determined that increasing the fraction of globular fat (by mixing with butter grains) decreases the hardness of butter-like emulsions up to an order of magnitude at d 1. However, no difference was observed in thermal behavior as a function of butter grain content, as all emulsions containing butter grains revealed 2 endothermal peaks corresponding to the high (32.7°C ± 0.6) and medium (14.6°C ± 0.1) melting fractions of fatty acids. In terms of microstructure, decreasing the amount of butter grains in the emulsions resulted in formation of a denser fat crystal network, corresponding to increased hardness. Moreover, microstructural analysis revealed that the presence of butter grains resulted in faster formation of a continuous fat crystal network compared with the 100% AMF sample, which was dominated by crystal clusters surrounded by liquid oil. During storage, hardness remained stable and no changes in thermal behavior were observed, despite an increase in solid fat content of up to 5%. After 28d of storage, we observed no difference in either microstructural or rheological properties, indicating that formation of primary bonds occurs primarily within the first day of storage. The rheological behavior of butter-like emulsions is not determined solely by hardness, but also by stiffness related to secondary bonds within the fat crystal network. The complex rheological behavior of milk fat-based emulsions is better characterized using multiple parameters. Copyright © 2014 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

A multi-module microfluidic platform for continuous pre-concentration of water-soluble ions and separation of oil droplets from oil-in-water (O/W) emulsions using a DC-biased AC electrokinetic technique.

PubMed

Das, Dhiman; Phan, Dinh-Tuan; Zhao, Yugang; Kang, Yuejun; Chan, Vincent; Yang, Chun

2017-03-01

A novel continuous flow microfluidic platform specifically designed for environmental monitoring of O/W emulsions during an aftermath of oil spills is reported herein. Ionized polycyclic aromatic hydrocarbons which are toxic are readily released from crude oil to the surrounding water phase through the smaller oil droplets with enhanced surface area. Hence, a multi-module microfluidic device is fabricated to form ion enrichment zones in the water phase of O/W emulsions for the ease of detection and to separate micron-sized oil droplets from the O/W emulsions. Fluorescein ions in the water phase are used to simulate the presence of these toxic ions in the O/W emulsion. A DC-biased AC electric field is employed in both modules. In the first module, a nanoporous Nafion membrane is used for activating the concentration polarization effect on the fluorescein ions, resulting in the formation of stable ion enrichment zones in the water phase of the emulsion. A 35.6% amplification of the fluorescent signal is achieved in the ion enrichment zone; corresponding to 100% enrichment of the fluorescent dye concentration. In this module, the main inlet is split into two channels by using a Y-junction so that there are two outlets for the oil droplets. The second module located downstream of the first module consists of two oil droplet entrapment zones at two outlets. By switching on the appropriate electrodes, either one of the two oil droplet entrapment zones can be activated and the droplets can be blocked in the corresponding outlet. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

α-Tocopherol/chitosan-based nanoparticles: characterization and preliminary investigations for emulsion systems application

NASA Astrophysics Data System (ADS)

Aresta, Antonella; Calvano, Cosima Damiana; Trapani, Adriana; Zambonin, Carlo Giorgio; De Giglio, Elvira

2014-02-01

The processes of lipids oxidation represent a great concern for the consumer health because they are one of the major causes of quality deterioration in fat-containing products. One of the most effective methods of delaying lipid oxidation consists in incorporating antioxidants. The present investigation describes the formulation of chitosan and novel glycol chitosan nanoparticles (NPs) loaded with α-Tocopherol (αToc-NPs). The obtained NPs were characterized by various techniques, such as particle size (showing mean diameters in the range 335-503 nm) and zeta potential measurements, X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy. The NPs were, then, added in the preparation of oil-in-water simple emulsion both to make the lipophilic αToc available in an aqueous medium and to prevent emulsion oxidation. For this purpose, a new highly sensitive, simple and solvent-free method based on a solid phase microextraction (SPME) coupled to gas chromatography mass spectrometry was developed for the determination of αToc in aqueous medium. All the parameters influencing SPME, including fiber coating, time and temperature extraction, pH, ionic strength and desorption conditions, have been carefully screened. The method was successfully applied to the determination of vitamin in the αToc-NPs and its release from NPs-enriched simple emulsion formulations. SPME provided high recovery yields and the limits of detection and of quantification in emulsion were 0.1 and 0.5 μg/mg, respectively. The precision of the method has been also estimated. The delay of the lipid oxidation by the proposed formulations has been evaluated exploiting the Kreis test on αToc-NPs-enriched emulsions.

Synthesis and biodistribution of novel magnetic-poly(HEMA-APH) nanopolymer radiolabeled with iodine-131 and investigation its fate in vivo for cancer therapy

NASA Astrophysics Data System (ADS)

Avcıbaşı, Uğur; Avcıbaşı, Nesibe; Akalın, Hilmi Arkut; Ediz, Melis; Demiroğlu, Hasan; Gümüşer, Fikriye Gül; Özçalışkan, Emir; Türkcan, Ceren; Uygun, Deniz Aktaş; Akgöl, Sinan

2013-10-01

Herein, we investigated the biological uptake, distribution, and radiopharmaceutical potential of a novel molecule based on 2-hydroxyethyl methacrylate (HEMA) and anilinephtalein (APH) in the metabolism of Albino Wistar rats. In order to achieve this, we synthesized APH using organic synthesis methods and copolymerized APH with HEMA using a common polymerization method, surfactant-free emulsion polymerization. In the presence of Fe3O4 particles, we obtained a new generation magnetic-nano-scale polymer, magnetic-poly(HEMA-APH). This new molecule was chemically identified and approved by several characterization methods using Fourier transform infrared spectroscopy, scanning electron microscope, energy dispersive X-ray spectroscopy, electron spin resonance, atomic force microscope, and Zeta particle-size analysis. To evaluate the biological activity in live metabolism and anti-cancer potential of mag-poly(HEMA-APH), molecule was radioiodinated by a widely used labeling technique, iodogen method, with a gamma diffuser radionuclide, 131I. Thin-layer radiochromatography experiments demonstrated that 131I binded to nanopolymer with the labeling yield of 90 %. Lipophilicity and stability experiments were conducted to determine the condition of cold and labeled mag-poly(HEMA-APH) in rat blood and lipid medium. Results demonstrated that radioiodinated molecule stayed as an intact complex in rat metabolism for 24 h and experimental lipophilicity was determined as 0.12 ± 0.02. In vivo results obtained by imaging and biological distribution experiments indicated that mag-poly(HEMA-APH) labeled with 131I [131I-mag-poly(HEMA-APH)] highly incorporated into tissues of the uterus, the ovarian, the prostate, and the lungs in rat metabolism. Based on these results, it may be evaluated that novel mag-poly(HEMA-APH) molecule labeled with 131I is a compound which has a significant potential for being used as an anti-cancer agent. Certain results can only be obtained whether this molecule is applied to adenocarcinoma cell models and tumor-bearing animals.

Free Radical Polymerization of Styrene: A Radiotracer Experiment

ERIC Educational Resources Information Center

Mazza, R. J.

1975-01-01

Describes an experiment designed to acquaint the chemistry student with polymerization reactions, vacuum techniques, liquid scintillation counting, gas-liquid chromatography, and the handling of radioactive materials. (MLH)

Application of neutron capture autoradiography to Boron Delivery seeking techniques for selective accumulation of boron compounds to tumor with intra-arterial administration of boron entrapped water-in-oil-in-water emulsion

NASA Astrophysics Data System (ADS)

Mikado, S.; Yanagie, H.; Yasuda, N.; Higashi, S.; Ikushima, I.; Mizumachi, R.; Murata, Y.; Morishita, Y.; Nishimura, R.; Shinohara, A.; Ogura, K.; Sugiyama, H.; Iikura, H.; Ando, H.; Ishimoto, M.; Takamoto, S.; Eriguchi, M.; Takahashi, H.; Kimura, M.

2009-06-01

It is necessary to accumulate the 10B atoms selectively to the tumor cells for effective Boron Neutron Capture Therapy (BNCT). In order to achieve an accurate measurement of 10B accumulations in the biological samples, we employed a technique of neutron capture autoradiography (NCAR) of sliced samples of tumor tissues using CR-39 plastic track detectors. The CR-39 track detectors attached with the biological samples were exposed to thermal neutrons in the thermal column of the JRR3 of Japan Atomic Energy Agency (JAEA). We obtained quantitative NCAR images of the samples for VX-2 tumor in rabbit liver after injection of 10BSH entrapped water-in-oil-in-water (WOW) emulsion by intra-arterial injection via proper hepatic artery. The 10B accumulations and distributions in VX-2 tumor and normal liver of rabbit were investigated by means of alpha-track density measurements. In this study, we showed the selective accumulation of 10B atoms in the VX-2 tumor by intra-arterial injection of 10B entrapped WOW emulsion until 3 days after injection by using digitized NCAR images (i.e. alpha-track mapping).

Hydrophilic microspheres from water-in-oil emulsions by the water diffusion technique.

PubMed

Trotta, Michele; Chirio, Daniela; Cavalli, Roberta; Peira, Elena

2004-08-01

In this study, we developed and evaluated a novel method to produce insulin-loaded hydrophilic microspheres allowing high encapsulation efficiency and the preservation of peptide stability during particle processing. The preparation method used the diffusion of water by an excess of solvent starting from a water-in-solvent emulsion. The water dispersed phase containing albumin or lactose, or albumin-lactose in different weight ratios, and insulin was emulsified in water-saturated triacetin with and without emulsifiers, producing a water-in-triacetin emulsion. An excess of triacetin was added to the emulsion so that water could be extracted into the continuous phase, allowing the insulin-loaded microsphere precipitation. Insulin stability within the microspheres after processing was evaluated by reverse-phase and size-exclusion high-performance liquid chromatography. The water diffusion extraction process provided spherical microparticles of albumin or albumin-lactose. The mean diameter of the microspheres prepared with or without emulsifiers ranged from 2 to 10 microm, and the encapsulation efficiency of insulin was between 60% and 75%, respectively. The analysis of microsphere content after processing showed that insulin did not undergo any chemical modification within microspheres. The use of lactose alone led to the formation of highly viscous droplets that coalesced during the purification step. The water extraction procedures successfully produced insulin-loaded hydrophilic microspheres allowing the preservation of peptide stability. The type of excipient and the size of the disperse phase of the primary w/o emulsion were crucial determinants of microsphere characteristics.

Improvement studies on emission and combustion characteristics of DICI engine fuelled with colloidal emulsion of diesel distillate of plastic oil, TiO2 nanoparticles and water.

PubMed

Karisathan Sundararajan, Narayanan; Ammal, Anand Ramachandran Bhagavathi

2018-04-01

Experimentation was conducted on a single cylinder CI engine using processed colloidal emulsions of TiO 2 nanoparticle-water-diesel distillate of crude plastic diesel oil as test fuel. The test fuel was prepared with plastic diesel oil as the principal constituent by a novel blending technique with an aim to improve the working characteristics. The results obtained by the test fuel from the experiments were compared with that of commercial petro-diesel (CPD) fuel for same engine operating parameters. Plastic oil produced from high density polyethylene plastic waste by pyrolysis was subjected to fractional distillation for separating plastic diesel oil (PDO) that contains diesel range hydrocarbons. The blending process showed a little improvement in the field of fuel oil-water-nanometal oxide colloidal emulsion preparation due to the influence of surfactant in electrostatic stabilization, dielectric potential, and pH of the colloidal medium on the absolute value of zeta potential, a measure of colloidal stability. The engine tests with nano-emulsions of PDO showed an increase in ignition delay (23.43%), and decrease in EGT (6.05%), BSNO x (7.13%), and BSCO (28.96%) relative to PDO at rated load. Combustion curve profiles, percentage distribution of compounds, and physical and chemical properties of test fuels ascertains these results. The combustion acceleration at diffused combustion phase was evidenced in TiO 2 emulsion fuels under study.

Production, deformation and mechanical investigation of magnetic alginate capsules

NASA Astrophysics Data System (ADS)

Zwar, Elena; Kemna, Andre; Richter, Lena; Degen, Patrick; Rehage, Heinz

2018-02-01

In this article we investigated the deformation of alginate capsules in magnetic fields. The sensitivity to magnetic forces was realised by encapsulating an oil in water emulsion, where the oil droplets contained dispersed magnetic nanoparticles. We solved calcium ions in the aqueous emulsion phase, which act as crosslinking compounds for forming thin layers of alginate membranes. This encapsulating technique allows the production of flexible capsules with an emulsion as the capsule core. It is important to mention that the magnetic nanoparticles were stable and dispersed throughout the complete process, which is an important difference to most magnetic alginate-based materials. In a series of experiments, we used spinning drop techniques, capsule squeezing experiments and interfacial shear rheology in order to determine the surface Young moduli, the surface Poisson ratios and the surface shear moduli of the magnetically sensitive alginate capsules. In additional experiments, we analysed the capsule deformation in magnetic fields. In spinning drop and capsule squeezing experiments, water droplets were pressed out of the capsules at elevated values of the mechanical load. This phenomenon might be used for the mechanically triggered release of water-soluble ingredients. After drying the emulsion-filled capsules, we produced capsules, which only contained a homogeneous oil phase with stable suspended magnetic nanoparticles (organic ferrofluid). In the dried state, the thin alginate membranes of these particles were rather rigid. These dehydrated capsules could be stored at ambient conditions for several months without changing their properties. After exposure to water, the alginate membranes rehydrated and became flexible and deformable again. During this swelling process, water diffused back in the capsule. This long-term stability and rehydration offers a great spectrum of different applications as sensors, soft actuators, artificial muscles or drug delivery systems.

Strategies to overcome polymerization shrinkage--materials and techniques. A review.

PubMed

Malhotra, Neeraj; Kundabala, M; Shashirashmi, Acharya

2010-03-01

Stress generation at tissue/resin composite interfaces is one of the important reasons for failure of resin-based composite (RBC) restorations owing to the inherent property of polymerization shrinkage. Unrelieved stresses can weaken the bond between the tooth structure and the restoration, eventually producing a gap at the restoration margins. This can lead to postoperative sensitivity, secondary caries, fracture of the restorations, marginal deterioration and discoloration. As polymerization shrinkage cannot be eliminated completely, various techniques and protocols have been suggested in the manipulation of, and restorative procedures for, RBCs to minimize the shrinkage and associated stresses. Introduction of various newer monomer systems (siloranes) may also overcome this problem of shrinkage stress. This review emphasizes the various material science advances and techniques advocated that are currently available or under trial/testing phase to deal with polymerization shrinkage in a clinical environment. Minimizing the shrinkage stresses in RBC restorations may lead to improvement in the success rate and survival of restorations. Thus, it is important for dental practitioners to be aware of various techniques and materials available to reduce these shrinkage stresses and be updated with the current knowledge available to deal with this issue.

Effects of process variables on the encapsulation of oil in ca-alginate capsules using an inverse gelation technique.

PubMed

Abang, Sariah; Chan, Eng-Seng; Poncelet, Denis

2012-01-01

The objective of this study was to investigate the effects of process variables on the encapsulation of oil in a calcium alginate membrane using an inverse gelation technique. A dispersion of calcium chloride solution in sunflower oil (water-in-oil emulsion) was added dropwise to the alginate solution. The migration of calcium ions to the alginate solution initiates the formation of a ca-alginate membrane around the emulsion droplets. The membrane thickness of wet capsules and the elastic modulus of dry capsules increased following first-order kinetics with an increasing curing time. An increase in the calcium chloride concentration increased the membrane thickness of wet capsules and the elastic modulus of dry capsules. An increase in the alginate concentration decreased the mean diameter of wet capsules but increased the elastic modulus of dry capsules.

Synthesis and characterization of monodispersed polymer/polydiacetylene nanocrystal composite particles.

PubMed

Wei, Zhong; Ujiiye-Ishii, Kento; Masuhara, Akito; Kasai, Hitoshi; Okada, Shuji; Matsune, Hideki; Asahi, Tsuyoshi; Masuhara, Hiroshi; Nakanishi, Hachiro

2005-06-01

Monodispersed polymer/polydiacetylenecomposite particles were synthesized by soap-free seeded emulsion polymerization of styrene andmethyl methacrylate; the products were characterized by XRD, SEM, TEM, UV-visible spectroscopy, and single particle scattering spectroscopy. In the synthesis process, polydiacetylene nanocrystals were found to act as inhibitor, and consequently a relatively low concentration was necessary. Different monomers lead to the differences in reaction condition and particle morphology; the PMMA composite particles were simpler in preparation than polystyrene particles, but the latter havebetter spherical morphology. The composite particles were composed of polymer shells and polydiacetylene cores, which kept their crystal structure and optical properties. A high percentage of cored particles could be achieved with optimized reaction conditions where the amount of seed was sufficient and the oily oligomer by-product was suppressed.

Scaffolds for Controlled Release of Cartilage Growth Factors.

PubMed

Morille, Marie; Venier-Julienne, Marie-Claire; Montero-Menei, Claudia N

2015-01-01

In recent years, cell-based therapies using adult stem cells have attracted considerable interest in regenerative medicine. A tissue-engineered construct for cartilage repair should provide a support for the cell and allow sustained in situ delivery of bioactive factors capable of inducing cell differentiation into chondrocytes. Pharmacologically active microcarriers (PAMs), made of biodegradable and biocompatible poly (D,L-lactide-co-glycolide acid) (PLGA), are a unique system which combines these properties in an adaptable and simple microdevice. This device relies on nanoprecipitation of proteins encapsulated in polymeric microspheres with a solid in oil in water emulsion-solvent evaporation process, and their subsequent coating with extracellular matrix protein molecules. Here, we describe their preparation process, and some of their characterization methods for an application in cartilage tissue engineering.

Data Analysis for the Scintillating Optical Fiber Calorimeter (SOFCAL)

NASA Technical Reports Server (NTRS)

Christl, Mark J.

1997-01-01

The scintillating optical fiber calorimeter is a hybrid instrument with both active and passive components for measuring the proton and helium cosmic ray spectra from 0.2 to IO TeV kinetic energy. A thin emulsion/x-ray film chamber is situated between a cerenkov counter and an imaging calorimeter. Scintillating optical fibers sample the electromagnetic showers that develop in the calorimeter and identify the trajectory of cosmic rays that interact in SOFCAL. The emulsion/x-ray film data provide an in flight calibration for SOFCAL. The data reduction techniques used will be discussed and interim results of the analysis from a 20 hour balloon flight will be presented.

Imipenem/cilastatin encapsulated polymeric nanoparticles for destroying carbapenem-resistant bacterial isolates.

PubMed

Shaaban, Mona I; Shaker, Mohamed A; Mady, Fatma M

2017-04-11

Carbapenem-resistance is an extremely growing medical threat in antibacterial therapy as the incurable resistant strains easily develop a multi-resistance action to other potent antimicrobial agents. Nonetheless, the protective delivery of current antibiotics using nano-carriers opens a tremendous approach in the antimicrobial therapy, allowing the nano-formulated antibiotics to beat these health threat pathogens. Herein, we encapsulated imipenem into biodegradable polymeric nanoparticles to destroy the imipenem-resistant bacteria and overcome the microbial adhesion and dissemination. Imipenem loaded poly Ɛ-caprolactone (PCL) and polylactide-co-glycolide (PLGA) nanocapsules were formulated using double emulsion evaporation method. The obtained nanocapsules were characterized for mean particle diameter, morphology, loading efficiency, and in vitro release. The in vitro antimicrobial and anti adhesion activities were evaluated against selected imipenem-resistant Klebsiella pneumoniae and Pseudomonas aeruginosa clinical isolates. The obtained results reveal that imipenem loaded PCL nano-formulation enhances the microbial susceptibility and antimicrobial activity of imipenem. The imipenem loaded PCL nanoparticles caused faster microbial killing within 2-3 h compared to the imipenem loaded PLGA and free drug. Successfully, PCL nanocapsules were able to protect imipenem from enzymatic degradation by resistant isolates and prevent the emergence of the resistant colonies, as it lowered the mutation prevention concentration of free imipenem by twofolds. Moreover, the imipenem loaded PCL eliminated bacterial attachment and the biofilm assembly of P. aeruginosa and K. pneumoniae planktonic bacteria by 74 and 78.4%, respectively. These promising results indicate that polymeric nanoparticles recover the efficacy of imipenem and can be considered as a new paradigm shift against multidrug-resistant isolates in treating severe bacterial infections.

Fabrication of silver nanoparticles in pH responsive polymer microgel dispersion for catalytic reduction of nitrobenzene in aqueous medium

NASA Astrophysics Data System (ADS)

Farooqi, Zahoor H.; Begum, Robina; Naseem, Khalida; Rubab, Uma; Usman, Muhammad; Khan, Abbas; Ijaz, Aysha

2016-12-01

Copolymer microgels based on N-isopropylacrylamide (NIPAM) and methacrylic acid (MAA) have been synthesized by free radical emulsion polymerization using N, N-methylenebisacrylamide (BIS) as a cross-linker. Synthesized microgels were characterized by Fourier transform infrared spectroscopy (FTIR). Then silver nanoparticles were fabricated in the synthesized microgels by in-situ reduction of AgNO3 with NaBH4. The formation of silver nanoparticles was confirmed by UV-Vis spectroscopy. The pH sensitivity of the copolymer microgels was investigated using dynamic light scattering technique (DLS). Hydrodynamic radius of P (NIPAM-MAA) microgels increases with increase in pH of the medium at 25°C. Surface plasmon resonance wavelength (λSPR) of silver nanoparticles increases with increase in hydrodynamic radius due to change in pH of the medium. The catalytic activity for the reduction of nitrobenzene (NB), an environmental pollutant, into aniline was investigated by UV-Vis spectroscopy in excess of NaBH4 using hybrid microgels as catalyst. The value of apparent rate constant ( k app) of the reaction was calculated using pseudo first order kinetic model and it was found to be linearly related to the amount of catalyst. The results were compared with literature data. The system was found to be an effective catalyst for conversion of NB into aniline.

Curcumin loaded pH-sensitive nanoparticles for the treatment of colon cancer.

PubMed

Prajakta, Dandekar; Ratnesh, Jain; Chandan, Kumar; Suresh, Subramanian; Grace, Samuel; Meera, Venkatesh; Vandana, Patravale

2009-10-01

The investigation was aimed at designing pH-sensitive, polymeric nanoparticles of curcumin, a natural anti-cancer agent, for the treatment of colon cancer. The objective was to enhance the bioavailability of curcumin, simultaneously reducing the required dose through selective targeting to colon. Eudragit S100 was chosen to aid targeting since the polymer dissolves at colonic pH to result in selective colonic release of the entrapped drug. Solvent emulsion-evaporation technique was employed to formulate the nanoparticles. Various process parameters were optimized and the optimized formulation was evaluated for particle size distribution and encapsulation efficiency before subjecting to freeze-drying. The freeze dried product was characterized for particle size, drug content, DSC studies, particle morphology. Anti-cancer potential of the formulation was demonstrated by MTT assay in HT-29 cell line. Nanometric, homogeneous, spherical particles were obtained with encapsulation efficiency of 72%. Freeze-dried nanoparticles exhibited a negative surface charge, drug content of > 99% and presence of drug in amorphous form which may result in possible enhanced absorption. MTT assay demonstrated almost double inhibition of the cancerous cells by nanoparticles, as compared to curcumin alone, at the concentrations tested. Enhanced action may be attributed to size influenced improved cellular uptake, and may result in reduction of overall dose requirement. Results indicate the potential for in vivo studies to establish the clinical application of the formulation.

The synthesis of desired functional groups on PEI microgel particles for biomedical and environmental applications

NASA Astrophysics Data System (ADS)

Sahiner, Nurettin; Demirci, Sahin; Sahiner, Mehtap; Al-Lohedan, Hamad

2015-11-01

Polyethyleneimine (PEI) microgels were synthesized by micro emulsion polymerization technique and converted to positively charged forms by chemical treatments with various modifying agents with different functional groups, such as 2-bromoethanol (-OH), 4-bromobutyronitrile (-CN), 2-bromoethylamine hydrobromide (-NH2), and glycidol (-OH). The functionalization of PEI microgels was confirmed by FT-IR, TGA and zeta potential measurements. Furthermore, a second modification of the modified PEI microgels was induced on 4-bromo butyronitrile-modified PEI microgels (PEI-CN) by amidoximation, to generate new functional groups on the modified PEI microgels. The PEI and modified PEI microgels were also tested for their antimicrobial effects against various bacteria such as Bacillus subtilis ATCC 6633, Escherichia coli ATCC 8739 and Staphylococcus aureus ATCC 25323. Moreover, the PEI-based particles were used for removal of organic dyes such as methyl orange (MO) and congo red (CR). The absorption capacity of PEI-based microgels increased with modification from 101.8 mg/g to 218.8 mg/g with 2-bromoethylamine, 216.2 m/g with 1-bromoethanol, and 224.5 mg/g with 4-bromobutyronitrile for MO. The increase in absorption for CR dyes was from 347.3 mg/g to 390.4 mg/g with 1-bromoethanol, 399.6 mg/g with glycidol, and 349.9 mg/g with 4-bromobutyronitrile.

New generation ion-imprinted nanocarrier for removal of Cr(VI) from wastewater

NASA Astrophysics Data System (ADS)

Uygun, Murat; Feyzioğlu, Esra; Özçalışkan, Emir; Caka, Müşerref; Ergen, Aygen; Akgöl, Sinan; Denizli, Adil

2013-08-01

The purpose of this study was to prepare a novel ion-imprinted nanoparticle to remove Cr(VI) ions from waste water. For this, Cr(VI) ions were complexed with 2-methacryloylamido histidine (MAH) and then Cr(VI)-imprinted poly(HEMAH) nanoparticles were synthesized by surfactant-free emulsion polymerization technique. The templates, Cr(VI) ions, were removed from the nanoparticles using 0.1 M of HNO3 solution. The specific surface area of the Cr(VI)-imprinted poly(HEMAH) nanoparticles was found to be 1,397.85 m2/g, and the particle size was calculated as 155.3 nm. These Cr(VI)-imprinted nanoparticles were used for the adsorption/desorption of Cr(VI) ions from its aqueous solutions. The effects of initial Cr(VI) concentration and medium pH on the Cr(VI) adsorption capacity were also studied. The maximum adsorbed amount of Cr(VI) on the imprinted nanoparticles was found to be 3,830.58 mg/g nanoparticle in pH 4.0. In order to investigate the selectivity of the imprinted nanoparticle, adsorption studies were repeated using Cr(III) ions. The selectivity results demonstrated that Cr(VI)-imprinted poly(HEMAH) nanoparticles showed high affinity for the Cr(VI) ions than Cr(III). The Cr(VI)-imprinted nanoparticles were used several times without decreasing their Cr(VI) adsorption capacities.

Magnetic poly(lactide-co-glycolide) (PLGA) and cellulose particles for MRI-based cell tracking

PubMed Central

Nkansah, Michael K.; Thakral, Durga; Shapiro, Erik M.

2010-01-01

Biodegradable, superparamagnetic micro- and nanoparticles of poly(lactide-co-glycolide) (PLGA) and cellulose were designed, fabricated and characterized for magnetic cell labeling. Monodisperse nanocrystals of magnetite were incorporated into micro- and nanoparticles of PLGA and cellulose with high efficiency using an oil-in-water single emulsion technique. Superparamagnetic cores had high magnetization (72.1 emu/g). The resulting polymeric particles had smooth surface morphology and high magnetite content (43.3 wt% for PLGA and 69.6 wt% for cellulose). While PLGA and cellulose nanoparticles displayed highest r2* values per millimole of iron (399 s-1mM-1 for cellulose and 505 s-1mM-1 for PLGA), micron-sized PLGA particles had a much higher r2* per particle than either. After incubation for a month in citrate buffer (pH 5.5), magnetic PLGA particles lost close to 50% of their initial r2* molar relaxivity, while magnetic cellulose particles remained intact, preserving over 85% of their initial r2* molar relaxivity. Lastly, mesenchymal stem cells and human breast adenocarcinoma cells were magnetically labeled using these particles with no detectable cytotoxicity. These particles are ideally suited for non-invasive cell tracking in vivo via MRI and due to their vastly different degradation properties, offer unique potential for dedicated use for either short (PLGA-based particles) or long term (cellulose-based particles) experiments. PMID:21404328

Evaluation of shrinkage polymerization and temperature of different acrylic resins used to splinting transfer copings in indirect impression technique

NASA Astrophysics Data System (ADS)

Franco, Ana Paula G. O.; Karam, Leandro Z.; Galvão, José R.; Kalinowski, Hypolito J.

2015-09-01

The aim of the present study was evaluate the shrinkage polymerization and temperature of different acrylic resins used to splinting transfer copings in indirect impression technique. Two implants were placed in an artificial bone, with the two transfer copings joined with dental floss and acrylic resins; two dental resins are used. Measurements of deformation and temperature were performed with Fiber Braggs grating sensor for 17 minutes. The results revealed that one type of resin shows greater values of polymerization shrinkage than the other. Pattern resins did not present lower values of shrinkage, as usually reported by the manufacturer.

Single chain technology: Toward the controlled synthesis of polymer nanostructures

NASA Astrophysics Data System (ADS)

Lyon, Christopher

A technique for fabricating advanced polymer nanostructures enjoying recent popularity is the collapse or folding of single polymer chains in highly dilute solution mediated by intramolecular cross-linking. We term the resultant structures single-chain nanoparticles (SCNP). This technique has proven particularly valuable in the synthesis of nanomaterials on the order of 5 -- 20 nm. Many different types of covalent and non-covalent chemistries have been used to this end. This dissertation investigates the use of so-called single-chain technology to synthesize nanoparticles using modular techniques that allow for easy incorporation of functionality or special structural or characteristic features. Specifically, the synthesis of linear polymers functionalized with pendant monomer units and the subsequent intramolecular polymerization of these monomer units is discussed. In chapter 2, the synthesis of SCNP using alternating radical polymerization is described. Polymers functionalized with pendant styrene and stilbene groups are synthesized via a modular post-polymerization Wittig reaction. These polymers were exposed to radical initiators in the presence (and absence) of maleic anhydride and other electron deficient monomers in order to form intramolecular cross-links. Chapter 3 discusses templated acyclic diene metathesis (ADMET) polymerization using single-chain technology, starting with the controlled ring-opening polymerization of a glycidyl ether functionalized with an ADMET monomer. This polymer was then exposed to Grubbs' catalyst to polymerize the ADMET monomer units. The ADMET polymer was hydrolytically cleaved from the template and separated. Upon characterization, it was found that the daughter ADMET polymer had a similar degree of polymerization, but did not retain the low dispersity of the template. Chapter 4 details the synthesis of aldehyde- and diol-functionalized polymers toward the synthesis of SCNP containing dynamic, acid-degradable acetal cross-links. SCNP fabrication with these materials is beyond the scope of this dissertation.

Miniemulsion polymerization as a versatile tool for the synthesis of functionalized polymers

PubMed Central

Crespy, Daniel

2010-01-01

Summary The miniemulsion technique is a particular case in the family of heterophase polymerizations, which allows the formation of functionalized polymers by polymerization or modification of polymers in stable nanodroplets. We present here an overview of the different polymer syntheses within the miniemulsion droplets as reported in the literature, and of the current trends in the field. PMID:21160567

Charge patterns as templates for the assembly of layered biomolecular structures.

PubMed

Naujoks, Nicola; Stemmer, Andreas

2006-08-01

Electric fields are used to guide the assembly of biomolecules in predefined geometric patterns on solid substrates. Local surface charges serve as templates to selectively position proteins on thin-film polymeric electret layers, thereby creating a basis for site-directed layered assembly of biomolecular structures. Charge patterns are created using the lithographic capabilities of an atomic force microscope, namely by applying voltage pulses between a conductive tip and the sample. Samples consist of a poly(methyl methacrylate) layer on a p-doped silicon support. Subsequently, the sample is developed in a water-in-oil emulsion, consisting of a dispersed aqueous phase containing biotin-modified immunoglobulinG molecules, and a continuous nonpolar, insulating oil phase. The electrostatic fields cause a net force of (di)electrophoretic nature on the droplet, thereby guiding the proteins to the predefined locations. Due to the functionalization of the immunoglobulinG molecules with biotin-groups, these patterns can now be used to initiate the localized layer-by-layer assembly of biomolecules based on the avidin-biotin mechanism. By binding 40 nm sized biotin-labelled beads to the predefined locations via a streptavidin linker, we verify the functionality of the previously deposited immunoglobulinG-biotin. All assembly steps following the initial deposition of the immunoglobulinG from emulsion can conveniently be conducted in aqueous solutions. Results show that pattern definition is maintained after immersion into aqueous solution.

Plasma polymerized high energy density dielectric films for capacitors

NASA Technical Reports Server (NTRS)

Yamagishi, F. G.

1983-01-01

High energy density polymeric dielectric films were prepared by plasma polymerization of a variety of gaseous monomers. This technique gives thin, reproducible, pinhole free, conformable, adherent, and insoluble coatings and overcomes the processing problems found in the preparation of thin films with bulk polymers. Thus, devices are prepared completely in a vacuum environment. The plasma polymerized films prepared all showed dielectric strengths of greater than 1000 kV/cm and in some cases values of greater than 4000 kV/cm were observed. The dielectric loss of all films was generally less than 1% at frequencies below 10 kHz, but this value increased at higher frequencies. All films were self healing. The dielectric strength was a function of the polymerization technique, whereas the dielectric constant varied with the structure of the starting material. Because of the thin films used (thickness in the submicron range) surface smoothness of the metal electrodes was found to be critical in obtaining high dielectric strengths. High dielectric strength graft copolymers were also prepared. Plasma polymerized ethane was found to be thermally stable up to 150 C in the presence of air and 250 C in the absence of air. No glass transitions were observed for this material.

Fabrication of iron (III) oxide doped polystyrene shells

NASA Astrophysics Data System (ADS)

Cai, Pei-Jun; Tang, Yong-Jian; Zhang, Lin; Du, Kai; Feng, Chang-Gen

2004-03-01

A type of iron (III) oxide doped plastic shell used for inertial confinement fusion experiments has been fabricated by emulsion techniques. Three different phases of solution (W1, O, and W2) are used for the fabrication process. The W1 phase is a 1 wt % of sodium lauryl sulfate in water. This W1 phase solution is mixed with a 3 wt % Fe2O3-polystyrene (PS) solution in benzene-dichloroethane (O phase) while stirring. The resulting emulsion (W1/O) is poured into a 3 wt % aqueous polyvinyl alcohol solution (W2 phase) while stirring. The resulting emulsion (W1/O/W2) is then heated to evaporate benzene and dichloroethane, and thus a solid Fe2O3-PS shell is formed. The diameter and wall thickness of the shells range from 150 to 500 μm and 5 to 15 μm, respectively. The average surface roughness of the shells is 40 nm, similar to that of the usual PS shells. .

Fragmentation of relativistic nuclei in peripheral interactions in nuclear track emulsion

DOE Office of Scientific and Technical Information (OSTI.GOV)

Artemenkov, D. A., E-mail: artemenkov@lhe.jinr.ru; Bradnova, V.; Chernyavsky, M. M.

2008-09-15

The technique of nuclear track emulsions is used to explore the fragmentation of light relativistic nuclei down to the most peripheral interactions: nuclear 'white' stars. A complete pattern of the relativistic dissociation of a 8B nucleus with target fragment accompaniment is presented. Relativistic dissociation {sup 9}Be {yields} 2{alpha} is explored using significant statistics, and a relative contribution of {sup 8}Be decays from 0+ and 2+ states is established. Target fragment accompaniments are shown for relativistic fragmentation {sup 14}N {yields} 3He +H and {sup 22}Ne {yields} 5He. The leading role of the electromagnetic dissociation on heavy nuclei with respect to breakupsmore » on target protons is demonstrated in all these cases. It is possible to conclude that the peripheral dissociation of relativistic nuclei in nuclear track emulsion is a unique tool to study many-body systems composed of the lightest nuclei and nucleons in the energy scale relevant for nuclear astrophysics.« less