Electrospinning of poly(ethylene-co-vinyl acetate)/clay nanocomposite fibers

Poly(ethylene-co-vinyl acetate)/clay nanocomposite fibers were fabricated using electrospinning. The fiber diameters were controlled by varying the polymer/chloroform concentration, which resulted in fibers with diameters ranging from 1 to 15 μm. The clay concentration was varied from 0.35 to 6.6 wt %. Scanning electron microscopy revealed that the fiber diameter increased with increasing clay concentration, whereas beading decreased. Transmission electron microscopy revealed a disruption of the spherulite structures by clay, which is consistent with heterogeneous nucleation. Shear modulus force microscopy indicated a reduction in melting point (T_m) with decreasing diameter for fibers thinner than 15 μm, which was confirmed by temperature dependent X-ray diffraction data. For fibers thinner than 8 μm, the presence of clay further enhanced the reduction of T_m. © 2009 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 47: 2501–2508, 2009     

Melt-electrospinning of PMMA

<正>The melt electrospinning of PMMA was investigated.The averaged fiber diameter thus obtained was reduced from 34.0μm to 19.7μm by adding di-(2-ethylhexyl)phthalate to reduce viscosity of the molten PMMA,and it further lowered down to 4.0μm when a KCl/ice-water solution was used as collection media.A comparison study on the PMMA fibers made through melt electrospinning and done by solution electrospinning was made.It was found that solution electrospinning was capable of fabricating very thin fibers as small as to a nanometer size,but resulted in a much wider fiber diameter range than melt-electrospinning did.In general,within some extent an increase in applied voltage and amount of the additive or a decrease in collection distance can give rise to a decreased fiber diameter and improved mechanical performance for the PMMA fibers by melt electrospinning.It was also indicated that the mechanical properties of the PMMA fibers made through melt-electrospinning were superior to those by solution elctropspinning.     

A method for investigating size distributions of aqueous droplets in the range 0.5–10 μm produced by pneumatic nebulizers

A novel method is described for the measurement of the droplet size distributions produced by nebulizers commonly employed in analytical atomic spectroscopy. It is shown theoretically that, at sufficiently high concentrations of dissolved sodium chloride, the evaporation of water from droplets as small as 0.5 μm in diameter may be reduced to a negligible level. When evaporation is reduced by the presence of a dissolved salt, a conventional cascade impactor may be used to elucidate the droplet size distribution. Empirical observations confirm that, at a sodium concentration of 10,000 μg ml^?1, evaporation is negligible: the method may be used to study particle size distributions over the size range 0.5–10 μm.     

Virginia Tobacco Leaves (CTA-VTL-2) – new Polish CRM for inorganic trace analysis including microanalysis

Preparation and certification of a new Polish reference material (CTA-VTL-2) for inorganic trace analysis including microanalysis is described. Virginia Tobacco Leaves of Bulgarian origin were hand picked, dried, comminuted and sieved at conditions preventing contamination of the material with metals. Ca. 13 kg of the material with particle size φ≤ 80 μm was prepared. Certification was based on world-wide interlaboratory comparison in which 60 laboratories from 18 countries participated. Data evaluation was done using an approach which includes rejection of outliers by concurrent use of four different outlier tests followed by calculation of overall means, confidence intervals etc. Several criteria were employed to qualify or disqualify the obtained overall mean as a certified or information value, respectively. 33 elements were certified and information values were established for 10 others. Particle size distribution of CTA-VTL-2 was investigated microscopically. The modal particle diameter was in the range of 15–35 μm. Extensive homogeneity checking by neutron activation analysis revealed that the material is sufficiently homogeneous for mg sample sizes.     

Laser Microprobe Mass Analysis of Individual Antarctic Aerosol Particles

Abstract

Individual Antarctic aerosol particles in the 0.5–4 μm aerodynamic diameter range were analyzed using laser microprobe mass analysis (LAMMA). As they were sampled near the ocean, the great majority consists of seasalt, transformed to various degrees in the atmosphere. Major alterations include the association of an excess sulfate and methane sulfonate with these particles. Sulfate-rich particles containing little or no chloride were found mostly in the smallest size fraction (0.5–1 μm), where they account for some 5% of all particles: they are most likely highly transformed seasalt. Aluminosilicates, on the other hand, only appear among the coarser particles: they represent 2% of the particulates in the 2–4 μm range. The remainder of the aerosol consists of organic, Fe-rich, K-rich and Zn-rich particles. The latter groups have very low abundances: always less than 1% of the population of the impactor stage(s) onto which they were collected.     

Matrix-Effekt und Korngrößenverteilung bei der Röntgenfluorescenzanalyse von Feststoffen der Gewässer

The intensity of the fluorescence of heavy metal traces, such as zinc, in waters can be described as a function of grain size distribution. Contrary to that of pure metals, it increases with grain size. For a parameter, the sample component in the grain diameter range below 6 μm is suited best. In the sediments of waste polluted waters, the same parameter is frequently found in close correlation to the zinc content of the samples. The analytical and practical consequences are discussed in the present paper.     

Si-Zr-C-O纤维的耐高温抗氧化性能研究

以聚硅碳硅烷(PSCS)与乙酰丙酮锆为原料合成聚锆碳硅烷(PZCS),采用先驱体转化法制备了Si-Zr-C-O纤维.通过元素分析、扫描电镜(SEM)、X射线衍射(XRD)和俄歇电子能谱(AES)等分析测试手段研究了Si-Zr-C-O纤维的组成结构及其耐高温抗氧化性能.结果表明:Si-Zr-C-O纤维的元素组成为SiC1.24HxO0.56Zr0.0129,平均强度2.5GPa,平均直径11μm,纤维表面光滑平坦,没出现孔洞、裂纹、沟槽等缺陷,直径均匀.该纤维耐超高温性能良好,在1450和1600℃处理后,强度保留率分别为72%和36%,1800℃处理后Si-Zr-C-O纤维的化学式为SiC0.99HxO0.1Zry,纤维氧含量大大降低;纤维抗氧化性能良好,空气中1000℃热处理20h后,强度保留率为71.2%,热处理100h后,强度保留率为50%.     

New low-cost tubular ceramic microfiltration membrane based on natural sand for tangential urban wastewater treatment

In wastewater treatment, the development of low-cost separation methods is of significant importance. Low-cost membranes based on natural materials have become a highly active research topic in recent years. Herein, using low-cost natural Moroccan sand, new ceramic supports have been developed and characterized using different techniques such as X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, thermogravimetric analysis (TGA), differential thermal analysis (DTA), along with scanning electron microscope (SEM). Plastic paste (average particle size ≤125 µm) was blended with organic additives and water, then the obtained paste was extruded into porous tubular supports. The support had a porosity of 43%, water permeability of 1928 L/h m² bar, excellent chemical and mechanical properties and an average pore diameter in the range of 8–15 µm after firing at 950 °C/2 h. As per SEM analysis, the tubular supports had a smooth and crack-free surface. The slip casting process was used to create a microfiltration layer from the same natural sand powder (average particle size ≤63 µm) using a mixture of powder sand, water, and polyvinyl alcohol solution. The water permeability of the microfiltration membrane sintered at 950 °C/2 h was 1052 L/h m² bar, the average pore size diameter was about 0.90 µm and 82% of pores had a diameter ≤1.00 µm. The obtained microfiltration membrane was tested for the treatment of urban wastewater. The membrane showed excellent separation performance in turbidity removal and chemical oxygen demand.     

Influence of drug on the structure and segmental mobility of poly(3-hydroxybutyrate) ultrafine fibers

Ultrafine fibers of biodegradable natural polyester such as poly(3-hydroxybutyrate) containing dipyridamole at various concentrations as a drug are prepared by the electrospinning method. It is shown by scanning electron microscopy that the absence of dipyridamole or its low concentrations (from 0 to 1%) provide the complex morphology of fibers composed of cylindrical regions 1–3 μm in diameter and thickened spindle-like ones 5–7 μm in average diameter. An increase in the concentration of dipyridamole in fibers leads to disappearance of the latter regions, with the morphology being cylindrical. The features of the crystalline and amorphous structures of poly(3-hydroxybutyrate) and its mixtures with dipyridamole are examined via DSC and EPR probe techniques. It is shown that the addition of dipyridamole to the poly(3- hydroxybutyrate) polymer matrix results in a sharp increase in the crystallinity and a slowdown of the molecular mobility in amorphous regions of ultrafine fibers. The heat treatment (annealing) of fibers leads to a sharp increase in the polymer crystallinity and a reduction of the segmental mobility in intercrystalline regions of the initial poly(3-hydroxybutyrate) fibers and those containing 1% of dipyridamole. All results including the influence of the drug concentration on the shape of fibers and their dynamic characteristics agree well with the thermal and physical parameters and should be used in the design of therapeutic systems for targeted and sustained delivery of bioactive compounds.     

微米级单分散共聚物微球的制备

用分散聚合法制备了苯乙烯 甲基丙烯酸甲酯微米级单分散共聚物微球 ,粒径为 5 4 μm .将分散聚合体系与乳液聚合体系进行了比较 ,并对共聚物微球的形貌、粒径分布及共聚情况进行了表征研究 .     

Modeling the liquid filling in capillary well microplates for analyte preconcentration

An attractive advantage of the capillary well microplate approach is the ability to conduct evaporative analyte preconcentration. We advance the use of hydrophobic materials for the wells which apart from reducing material loss through wetting also affords self entry into the well when the droplet size reduces below a critical value. Using Surface Evolver simulation without gravity, we find the critical diameters D(c) fitting very well with theoretical results. When simulating the critical diameters D(c)(G) with gravity included, the gravitational effect could only be ignored when the liquid volumes were small (difference of 5.7% with 5 μL of liquid), but not when the liquid volumes were large (differences of more than 22% with 50 μL of liquid). From this, we developed a modifying equation from a series of simulation results made to describe the gravitational effect. This modifying equation fitted the simulation results well in our simulation range (100°≤θ≤135° and 1 μL≤V≤200 μL). In simulating the condition of multiple wells underneath each droplet, we found that having more holes did not alter the critical diameters significantly. Consequently, the modifying relation should also generally express the critical diameter for multiple wells under a droplet.     

Polydimethylsiloxane Soft Template Assisted Synthesis of Silver Nanoparticles via Vapor‐Solid Reaction Growth

A new route to synthesize silver nanoparticles via vapor‐solid reaction growth (VSRG) is reported. Employing AgCl to react with (Me₃Si)₄Si in a sealed tube (433–673 K) generates silver particles (diameter ≥ 10 μm). Addition of polydimethylsiloxnae (PDMS) to the reaction dramatically reduces the particle size (diameter 60–1200 nm). Moreover, formation of silver nanorods and nanocubes was discovered in some reaction conditions. Adding PDMS and varying the reaction temperature were the key factors influencing the Ag particle size.     

N-Alkanes in an Equatorial Sedimentary Environment: Their Distribution as a Function of Particle Size

Abstract

In order to investigate the biogeochemistry of organic matter deposited in an equatorial deltaic environment, the Mahakam delta, Borneo, analysis of geochemical markers has been realised both on various sediments and on sediments separated as a function of particle size.

Sediments were selected from two levels (-150m and -500m) of a continuous core sampled in the Mahakam delta in 1981 (Misedor Programme) and represent various lithotypes of the deltaic environment and different diagenetic conditions. After separation into sand size (> 50 μm), silt size (50–5 4mUm) and clay size (< 5 μm) fractions, free lipids have been extracted and hydrocarbons isolated by micro-column chromatography, and analysed by capillary gas liquid chromatography. Concentrations and carbon number distributions of n-alkanes are discussed in terms of the relationship between the sedimentary environment and the importance of terrigenous inputs. The distribution patterns of n-alkanes of different sediment size fractions are characterized by the predominance of high molecular weight compounds in the range C23–C37, which are also encountered for the actual deltaic plain flora: mangrove and nipah-nipah. Carbon Preference Index (CPI) values are higher in the coarse and intermediate fractions reflecting their enrichment in continentally-derived vegetation debris.     

The effect of inert gases on the yield and morphology of carbon deposits resulting from methane pyrolysis on fechral catalyst under direct current resistive heating

The effect of the inert component nature (argon, helium) in a gas mixture on the morphology and the amount of carbon deposits formed upon methane pyrolysis on a resistive fechral wire catalyst heated by direct current was studied. The carbon deposits had a similar morphology with fibrous texture in all cases. By varying the gas medium composition, one can obtain either fibers with up to 150 μm length and 2–3 μm diameter or short fibers of 8–10 μm length formed from a dense surface carbon layer. In the presence of helium, the amount of carbon deposited on the surface was virtually proportional to the methane content in the gas mixture, while in argon medium, the carbon formation was markedly retarded.     

Molecular orientation gradients in thermotropic liquid crystalline fiber

The degree of molecular alignment averaged over meso-length scale areas within thermotropic liquid crystalline polymer (LCP) fibers has been intensely studied over recent years. In this work, the degree of molecular orientation is found from spatially-resolved electron diffraction of areas as small as 100 nm in diameter to relieve structural averaging of lower resolution techniques. This investigation reveals that the maximum degree of molecular alignment across a fiber 18 μm in diameter is approximately 1 μm from the fiber surface. Dark-field imaging shows region with little crystallinity adjacent to the fiber surface. The banded structure, typical of TLCP fibers, is also less apparent in the surface region. Copyright © 2003 John Wiley & Sons, Ltd.     

Electrospun fiber mats of poly(3‐hydroxybutyrate), poly(3‐hydroxybutyrate‐co‐3‐hydroxyvalerate), and their blends

Electrospinning of poly(3‐hydroxybutyrate) (PHB), poly(3‐hydroxybutyrate‐co‐3‐hydroxyvalerate) (PHBV), and their blends was first carried out in chloroform at 50 °C on a stationary collector. The average diameter of the as‐spun fiber from PHB and PHBV solutions decreased with increasing collection distance and increased with increasing solution concentration and applied electrical potential. In all of the spinning conditions investigated, the average diameter of the as‐spun pure fibers ranged between 1.6 and 8.8 μm. Electrospinning of PHB, PHBV, and their blends was carried out further at a fixed solution concentration of 14% w/v on a homemade rotating cylindrical collector. Well‐aligned, cross‐sectionally round fibers without beads were obtained. The average diameter of the as‐spun pure and blend fibers ranged between 2.3 and 4.0 μm. The as‐spun fiber mats appeared to be more hydrophobic than the corresponding films and much improvement in the tensile strength and the elongation at break was observed for the blend fiber mats over those of the pure fiber ones. Lastly, indirect cytotoxicity evaluation of the as‐spun pure and blend fiber mats with mouse fibroblasts (L929) indicated that these mats posed no threat to the cells. © 2006 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 44: 2923–2933, 2006     

Fiber‐Optic Probes for Small‐Scale Measurements of Scalar Irradiance

A new method for producing fiber‐optic microprobes for scalar irradiance (=fluence rate) measurements is described. Such fine‐scale measurements are important in many photobiological disciplines. With the new method, it is possible to cast spherical 30–600 μm wide light integrating sensor tips onto tapered or untapered optical fibers. The sensor tip is constructed by first casting a clear polymethyl methacrylate (PMMA) sphere (~80% of the size of the final probe tip diameter) onto the optical fiber via dip‐coating. Subsequently, the clear sphere is covered with light diffusing layers of PMMA mixed with TiO₂ until the fiber probe exhibits a satisfactory isotropic response (typically ±5–10%). We also present an experimental setup for measuring the isotropic response of fiber‐optic scalar irradiance probes in air and water. The fiber probes can be mounted in a syringe equipped with a needle, facilitating retraction of the spherical fiber tip. This makes it, e.g. possible to cut a hole in cohesive tissue with the needle before inserting the probe. The light‐collecting properties of differently sized scalar irradiance probes (30, 40, 100, 300 and 470 μm) produced by this new method were compared to probes produced with previously published methods. The new scalar irradiance probes showed both higher throughput of light, especially for blue light, as well as a better isotropic light collection over a wide spectral range. The new method also allowed manufacturing of significantly smaller scalar irradiance microprobes (down to 30 μm tip diameter) than hitherto possible, and such sensors allow minimally invasive high‐resolution scalar irradiance measurements in thin biofilms, leaves and animal tissues.     

Effect of the surface topography of electrospun poly(ε-caprolactone)/poly(3-hydroxybuterate-co-3-hydroxyvalerate) fibrous substrates on cultured bone cell behavior

The use of electrospun fibrous matrices as substrates for cell/tissue culture has usually been confined to those consisting of smooth fibers. Here, we demonstrated that in vitro responses of mouse-calvaria-derived preosteoblastic cells (MC3T3-E1) that had been cultured on electrospun fibrous substrates made from blend solutions of 50/50 w/w poly(ε-caprolactone) (PCL) and poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) of varying concentrations, ranging from 4 to 14 wt %, depended strongly on the topography of the individual fibers. As the concentration of the blend solutions increased from 4 to 14 wt %, the topography of the individual fibers changed from discrete beads/smooth fibers to beaded fibers/smooth fibers and finally to smooth fibers, and the average diameter of the individual, smooth fibers increased from ～0.4 to ～1.8 μm. The results clearly showed that MC3T3-E1 preferred the smooth hydrophilic surface of the fibrous substrate from 10 wt % PCL/PHBV solution because the cells appeared to attach, proliferate, and differentiate on the surface of this substrate particularly well.     

Free surface electrospinning of fibers containing microparticles

Many materials have been fabricated using electrospinning, including pharmaceutical formulations, superhydrophobic surfaces, catalysis supports, filters, and tissue engineering scaffolds. Often these materials can benefit from microparticles included within the electrospun fibers. In this work, we evaluate a high-throughput free surface electrospinning technique to prepare fibers containing microparticles. We investigate the spinnability of polyvinylpyrrolidone (PVP) solutions containing suspended polystyrene (PS) beads of 1, 3, 5, and 10 μm diameter in order to better understand free surface electrospinning of particle suspensions. PS bead suspensions with both 55 kDa PVP and 1.3 MDa PVP were spinnable at 1:10, 1:5, and 1:2 PS:PVP mass loadings for all particle sizes studied. The final average fiber diameters ranged from 0.47 to 1.2 μm and were independent of the particle size and particle loading, indicating that the fiber diameter can be smaller than the particles entrained and can furthermore be adjusted based on solution properties and electrospinning parameters, as is the case for electrospinning of solutions without particles.     

Chain Orientation in Polyethylene Fibers Prepared by Ethylene Nanoextrusion Polymerization

Summary: Ethylene nanoextrusion polymerization has been demonstrated to be a novel nanofabrication concept for the preparation of polyethylene (PE) fibers directly from ethylene monomers without any post‐processing procedures. For PE fibers, chain orientation is a critical parameter that affects performance and application of the fibrous materials. In this communication, we report an investigation on chain orientation in PE fibrous samples prepared through nanoextrusion polymerization using a two‐dimensional wide angle X‐ray diffraction (2D WAXRD) technique. Two types of fibrous samples, including individual microfibers and microfiber aggregates, were sampled randomly and studied. For individual PE microfibers, anisotropic diffraction patterns were observed, suggesting chain orientation along the microfiber axial direction. Some microfibers showed the most desired diffraction pattern often found in high‐modulus high‐strength PE fibers. These samples possessed a very high degree of chain orientation along the fiber axis. Owing to a random aggregation of anisotropic microfibers, microfiber aggregates exhibited isotropic diffraction patterns. This work provided further experimental evidence for the proposed nanoextrusion polymerization concept.

2D WAXRD diffraction pattern of a PE microfiber.