New synthesis method of HA/P(D,L)LA composites: study of fibronectin adsorption and their effects in osteoblastic behavior for bone tissue engineering

A novel synthetic method to synthesize hydroxyapatite/poly (D,L) lactic acid biocomposite is presented in this study by mixing only the precursors hydroxyapatite and (D,L) LA monomer without adding neither solvent nor catalyst. Three compositions were successfully synthesized with the weight ratios of 1/1, 1/3, and 3/5 (hydroxyapatite/(D,L) lactic acid), and the grafting efficiency of poly (D,L) lactic acid on hydroxyapatite surface reaches up to 84?%. Scanning electron microscopy and Fourier transform infrared spectroscopy showed that the hydroxyapatite particles were successfully incorporated into the poly (D,L) lactic acid polymer and X ray diffraction analysis showed that hydroxyapatite preserved its crystallinity after poly (D,L) lactic acid grafting. Differential scanning calorimetry shows that Tg of hydroxyapatite/poly (D,L) lactic acid composite is less than Tg of pure poly (D,L) lactic acid, which facilitates the shaping of the composite obtained. The addition of poly (D,L) lactic acid improves the adsorption properties of hydroxyapatite for fibronectin extracellular matrix protein. Furthermore, the presence of poly (D,L) lactic acid on hydroxyapatite surface coated with fibronectin enhanced pre-osteoblast STRO-1 adhesion and cell spreading. These results show the promising potential of hydroxyapatite/poly (D,L) lactic acid composite as a bone substitute material for orthopedic applications and bone tissue engineering.     

Evaluation of the effects of operational parameters in the pretreatment of sugarcane bagasse with diluted sulfuric acid using analysis of variance

The pretreatment of lignocellulosic residues has been extensively studied as a method to disrupt the cellulose–hemicelluloses–lignin complex in biomass to access the sugars in their respective components. In this work, we carried out a study using sulfuric acid pretreatment of sugarcane bagasse by varying the following operational parameters: solid loading (10–30% of bagasse relative to the volume of the sulfuric acid solution), sulfuric acid concentration (0.5–2.5% relative to the dry mass of bagasse), reaction time (5–25?min), and temperature (135–195°C). The obtained solids from each pretreatment condition were submitted to enzymatic hydrolysis under the same process conditions: 0.232?g of Celluclast 1.5?L and 0.052?g of Novozym 188 per g of pretreated sugarcane bagasse, 72?h of hydrolysis, and 200?rpm of agitation at 50°C. Using central composite rotational design configuration in the experiments and analysis of variance, the results indicate that the conditions that produced larger quantities of glucose by enzymatic hydrolysis (0.35?g glucose/g pulp) with minimum amounts of degradation products were as follows: 20% solids loading, 15?min of reaction time, 1.5% sulfuric acid, and a minimum temperature of reaction of 170°C.     

An Effect of Temperature and Notch Geometry on Correlated Toughness of a Stainless Steel

To determine the toughness of materials, Charpy V notch test has been widely used over the world. Originally, the Charpy-V or U tests were used mainly as a quality control tests. In this paper, effects of temperature and notch geometry on variation of toughness/yield stress ratio were investigated. The experimental work has been performed on austenitic stainless steel 316L using Charpy tests and carried out at temperature range from 20 ℃ to 250 ℃ on different dimension of V- and U-notch specimens. Energy of fracture was determined directly from machine tests. Furthermore, Barsoum correlation has been applied to determine toughness/yield stress ratio as function of temperature. In addition, several parameters were investigated namely specimen thickness and notch cut angles. U-notch specimen offers a high resistance comparatively to the V-notch and that toughness depends on temper situation and orientation of notch relative to the rolling direction.     

On polyethylene chain generation through chemical crosslinking of isotactic polypropylene

Crosslinked isotactic polypropylene (iPP) was prepared by reactive blending using dicumyl peroxide and active sulfur. The modified material was characterized by means of several techniques: dynamic mechanical thermal analysis, differential scanning calorimetry, Fourier transform infrared spectroscopy, and nuclear magnetic resonance (¹³C solid state NMR). Analysis of results using the above techniques confirms that, during the crosslinking process, new ethylenic chains are generated at expenses of the initially present iPP. Furthermore, a balance between the amount of missing iPP and the proportion of newly created polyethylene (PE) is observed. The newly formed PE is semicrystalline, having a degree of crystallinity of about 30%. The amorphous component of the generated PE is thought to contribute to the high impact strength of the crosslinked samples when compared to the unmodified iPP. In light of the results obtained by the different techniques, an attempt to describe the emerging structure of the new crosslinked iPP material is proposed. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Effects of hydrothermal ageing on the thermal behaviour of poly(vinyl chloride) filled with wood flour

The hydrothermal ageing of wood‐flour‐filled PVC produced by dry‐blending in a high‐speed mixer in the presence of a plasticizer and other processing additives was carried out to investigate its thermal behaviour, and the results obtained were compared with those for the unfilled material. The dry‐blended compounds were prepared as films by a calendering process. The accelerated hydrothermal ageing was carried out by immersing the samples in boiling water at 100 °C for 110 h. The thermal behaviour of the reference and the aged samples in water was characterized by differential scanning calorimetry (DSC) and determination of the weight changes. The study has shown that during hydrothermal ageing, the samples from the whole formulations absorbed water, for instance, for 30 wt% filled PVC (F30), 16 wt% of water absorption was obtained, while this was only 2.2 wt% for unfilled PVC (F0). It was also noticed that the formulations filled with wood flour up to 10 wt% exhibited similar water absorption kinetics, i.e. the water was mostly absorbed during the first 50 h and the amount absorbed was less than 5 wt%. On the other hand, the 30 wt% filled samples regularly absorbed water up to almost 16 wt% after 100 h of immersion. The DSC data showed that hydrothermal ageing significantly affected the onset temperature of decomposition (T_d) of the unfilled samples by decreasing this temperature from 228 to 215 °C. For the 30 wt% filled samples, only additive migration was observed, while the T_d remained almost unchanged. Furthermore, from the DSC data, processability of the 30 wt% filled PVC samples at elevated temperatures, i.e. 180 to 200 °C was shown. Copyright © 2004 Society of Chemical Industry     

Effect of Hydrothermic Ageing on Dielectric and Mechanical Properties of Rigid Poly(vinyl chloride)

An accelerated hydrothermic ageing (according to N.F.T. 54043 method) was performed on samples of rigid poly(vinyl chloride). The test consisted of sample immersion in boiling water at 100°C for different exposure periods up to 480 h. The samples were removed from the boiling water every two hours for mechanical and dielectric characterization and color test. The dielectric measurements carried out on aged samples, up to 40 h, showed that the permittivity remained almost constant and its value was found to be 2.3 in the range –100 to +62.8°C. However, as the temperature approaches the glass transition (T_g = 88.3°C), the permittivity was observed to increase rapidly. It was also found that the permittivity of aged samples was lower than that of the non‐aged samples. The dielectric loss factor (tan δ) measurements with respect to temperature have confirmed the presence of two relaxations: β at low temperature (around –35°C) and α near the T_g. The combined action of water and temperature reduced the intensity of the corresponding relaxation peaks. The sample color index was evaluated up to 480 h using the SYNMERO scale in order to estimate the degradation extent. Unexpectedly, elongation at break under uniaxial traction remained unaffected by the hydrothermic ageing, meaning that two competing processes were involved simultaneously (sample degradation via chain scission and sample plastification via water absorption).     

Kinetic and wet oxidation of phenol catalyzed by non-promoted and potassium-promoted manganese/cerium oxide

The wet oxidation of organic compounds to CO2 and H2O has been shown to be a very efficient technique in the outflows treatment. This work focuses on the interaction of the chemical element potassium with the catalyst MnO2-CeO2 in the wet degradation of phenol. The reaction has been carried out in an autoclave with a controlled system of agitation, pressure, temperature and sampling of the liquid phase. The experiments were performed in the presence of the catalysts MnO2-CeO2 and K-MnO2-CeO2 in the following operational conditions: temperature of 130 degrees C, P = 20.4 atm, catalyst concentration in the range 1.5-5.0 g/L, initial phenol concentration of 0.5 g/L, initial pH varying between 6.8 and 8.5, and percentage of potassium in the catalyst MnO2-CeO2 ranging between 0% and 10%. Curves indicating the profile of conversion of total organic carbon show that the phenol degradation is favored when the potassium quantity is reduced. This behaviour is confirmed by BET analysis, whereby the catalyst presents larger specific area when compared to the percentages of other components. Regardless of the catalyst used in the phenol oxidation, the kinetic constant of reaction had the same order of magnitude for two parallel stages proposed by a first-order kinetic model.     

Nanostructure and morphology of poly(vinylidene fluoride)/polymethyl (methacrylate)/clay nanocomposites: correlation to micromechanical properties

Nanocomposites based on poly(vinylidene fluoride) (PVDF)/poly(methyl methacrylate) (PMMA) with untreated clay were prepared in one step by reactive melt extrusion. Chemical reactions took place between the polymer matrices, the inorganic clay particles, and three reactive agents, leading to the PVDF/PMMA/clay nanocomposites. The microstructure characterizations were carried out by differential scanning calorimetry and wide-angle X-ray scattering (WAXS). The mechanical behavior was investigated by tensile experiments, impact tests, and microhardness measurements. The morphological characterization was carried out by optical and atomic force microscopy (AFM). The decrease of the melting and crystallization temperatures of the PVDF with the increasing PMMA content is attributed to the interactions between the oxygen of the PMMA carbonyl group and the PVDF’s hydrogen atom. WAXS analysis shows that there is neither an intercalation step nor total exfoliation in any composition. As the PMMA content increases, WAXS diagrams show either the PVDF α-crystallographic form, both, α- and β-forms, or only the β-form. For PMMA contents higher than 40 wt%, the materials became amorphous. The microhardness of the samples decrease for a PMMA content up to 20 wt%. The study by optical microscopy and AFM illustrates the significant effect in the presence of clay on the film’s surface morphology.     

Preparation and characterization of poly(vinyl chloride)/virgin and treated sisal fiber composites

Mechanical property changes, thermal stability, and water absorption capacity of poly(vinyl chloride) (PVC)/sisal fiber composites were assessed with respect to the effect of maleic anhydride chemical treatments of the sisal fiber, for five different sisal fiber contents, varying from 0 to 30% by weight in the composite. The composites prepared with the untreated sisal exhibited higher tensile modulus and hardness than the unloaded resin, while elongation and tensile strength were reduced. The deterioration in the mechanical properties of PVC blended with sisal fiber is attributed to the presence of moisture, interfacial defects at the fiber and polymer interface, and fiber dispersion in the PVC matrix. The amount of absorbed water is a function of the amount of fiber in the composite (F0 = 0 phr, F5 = 0.77 phr, and F20 = 4.83 phr). The comparison of the results of characterization of F5, F20, and F30 formulations prepared with the untreated fibers and the treated ones showed a reduction in absorbed water after the chemical treatment of fiber with maleic anhydride (F0 = 0 phr, F5 = 0.28 phr, and F20 = 2.99 phr), thus improving the mechanical properties of composites prepared with the treated sisal. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 3630–3636, 2007     

Effect of a high calcite filler addition upon microstructural, mechanical, shrinkage and transport properties of a mortar

Sands produced from limestone rock deposits in Algeria contain high proportions of fine 0/100 μm particles (named filler hereafter), which are available in large quantities. This study aims to identify the maximum filler amount which may be added to cementitious materials without performance loss. Performance is quantified here as related to varied properties, either microstructural (density, porosity, pore size distribution, capillary absorption, Klinkenberg effect), mechanical (Young's modulus, compressive and flexural strengths), or indicative of durability (intrinsic gas permeability, drying shrinkage and mass loss). To that purpose, mortars with various amounts of filler, ranging from 15 to 45% sand mass (i.e. 45 to 135% cement mass), have been formulated, tested and compared to a reference mortar. As recommended by J. Baron [J. Baron, Les additions normalisées pour le Béton, Les bétons - Bases et données pour leur formulation, Association technique - industrie des liants hydrauliques (in French), Eyrolles Ed., Paris, 1996, pp. 47-57], substitution to sand is privileged, whereby cement proportion and workability are kept constant while water need varies with increasing filler amount. Preliminary XRD analysis of filler powder shows no other minerals than calcite CaCO₃ and traces of dolomite CaMg(CO₃)₂. Results point out the existence of an optimal performance value and a high effect of filler addition. In particular, for high filler amounts, total porosity increases while bigger pore populations diminish. This is confirmed by SEM examinations of the microstructure as well as by the increase of Klinkenberg coefficient β determined from gas permeability measurements, and by capillary absorption results. Moreover, intrinsic gas permeability, compressive and flexural strengths remain remarkably high whatever the filler proportion. Drying shrinkage and mass loss are not impacted dramatically either.