New large volume hydrothermal reaction cell for studying chemical processes under supercritical hydrothermal conditions using time-resolved in situ neutron diffraction

The design and testing of a new large volume Inconel pressure cell for the in situ study of supercritical hydrothermal syntheses using time-resolved neutron diffraction is introduced for the first time. The commissioning of this new cell is demonstrated by the measurement of the time-of-flight neutron diffraction pattern for TiO(2) (Anatase) in supercritical D(2)O on the POLARIS diffractometer at the United Kingdom's pulsed spallation neutron source, ISIS, Rutherford Appleton Laboratory. The sample can be studied over a wide range of temperatures (25-450 °C) and pressures (1-355 bar). This novel apparatus will now enable us to study the kinetics and mechanisms of chemical syntheses under extreme environments such as supercritical water, and in particular to study the crystallization of a variety of technologically important inorganic materials.     

Influence of Synthesis Conditions for ZSM-5 on the Hydrothermal Stability of Cu-ZSM-5

The influence of syntheses parameters of zeolite ZSM-5 on the lean NO _x reduction activity and hydrothermal stability of Cu-ZSM-5 has been investigated. The hydrothermal stability of Cu-ZSM-5 was found to depend on the aluminium source used and on the presence of Ca(OH)₂ in the synthesis mixture for ZSM-5.     

Adsorption of antifouling booster biocides on metal oxide nanoparticles: Effect of different metal oxides and solvents

Controlling the release rate of biocides (antifouling agents) from a paint coating is a key issue for the development of multi-season antifouling marine coatings. One promising approach is the use of nanoparticles onto which biocides are adsorbed to prevent premature depletion of the biocide. Adsorption of one novel (Medetomidine) and six commercially available and widely used antifouling biocides (Chlorothalonile, Dichlofluanid, Diuron, Irgarol, Seanine, Tolylfluanid) onto oxide nanoparticles (Al₂O₃, CuO, MgO, SiO₂, TiO₂, ZnO) was investigated by HPLC and NMR in different organic solvents. Large differences in adsorption strength depending on the type of nanoparticle and solvent employed were observed. It was shown that nanoparticles coordinate preferentially with the imidazole moiety of Medetomidine. Independent of the type of particle this interaction was considerably stronger in comparison to the other biocides. However, the interaction strength was strongly dependant on the type of solvent, where the largest strongest interaction was achieved in o-xylene. In addition field tests were performed where a considerable decrease in release rate was displayed from coatings containing Medetomidine adsorbed to nanoparticles compared to coatings containing Medetomidine as single additive.     

Assessment of the multi-compound non-equilibrium dissolution behaviour of a coal tar containing PAHs and phenols into water

Herein, an experimental study coupled with a model in order to assess the non-equilibrium and multi-compound dissolution behaviour of a coal tar containing PAHs and phenols into water, is presented. For this aim, two experimental studies has been carried out: (1) coal tar-water partition equilibrium and (2) dissolution dynamics of coal tar under controlled hydrodynamic conditions in percolation columns packed with glass beads. The dissolution amount of the three target constituents (i.e. phenol, naphthalene and phenanthrene) was monitored by UV detection. The dissolution behaviour was modelled using a predictive fraction approach. The partition coefficients have been estimated from experimental data and the obtained results show that the partition coefficient of each constituent between the aqueous phase and the tar depends on the activities of the constituent in both phases and cannot be estimated only from the solubility of the pure compound in water. The non-equilibrium dissolution model was established, applied for the experimental conditions and validated for three target compounds adjusting the effective interfacial area between tar and water. This parameter is specific of the experimental set-up. The global behaviour of coal tar has been modelled taking into account four categories of compounds according to their water solubility and volatilities. The mass transfer parameters have been estimated using available correlations. The results of this paper indicate that a model based on component fractions can be used to assess the non-equilibrium dissolution behaviour of a coal tar.     

Effects of Extrusion Temperature and Plasticizers on the Physical and Functional Properties of Starch Films

Cornstarch, at 20% moisture content (dry basis, d.b.), was mixed with glycerol at 3:1 ratio to form the base material for extruded starch films. Stearic acid, sucrose and urea, at varying concentrations, were tested as secondary plasticizers for the starch‐glycerol mixture. The ingredients were extruded at 110 and 120°C barrel temperatures to determine the effects of extrusion temperature, plasticizer type and their concentrations on the film‐forming characteristics of starch, as well as their effects on selected physical and functional properties of the films. The physical and mechanical properties of the films were studied by scanning electron microscopy (SEM) and tensile testing, while the glass transition and gelatinization properties were analyzed using differential scanning calorimetry (DSC). The interactions between the functional groups of starch and plasticizers were investigated using Fourier‐transform infrared (FTIR) spectroscopy. The water vapor permeability (WVP) properties of starch films were determined using ASTM standard E96‐95. Scanning electron micrographs exhibited the presence of native and partially melted starch granules in the extruded films. The tensile stress, strain at break and Young's modulus of starch films ranged from 0.9 to 3.2 MPa, 26.9 to 56.2% and 4.5 to 67.7 MPa, respectively. DSC scans displayed two glass transitions in the temperature ranges of 0.1 to 1°C and 9.6 to 12°C. Multiple melting endotherms, including that of amylose‐lipid complexes, were observed in the thermoplastic extrudates. The gelatinization enthalpies of the starch in the extruded films varied from 0 to 1.7 J/g, and were dependent largely on the extrusion temperature and plasticizer content. The shift in the FTIR spectral bands, as well as the appearance of double‐peaks, suggested strong hydrogen bonding interactions between the starch and plasticizers. The WVP of starch films ranged from 10.9 to 15.7 g mm h^‐1 m^‐2 kPa^‐1, depending on the extrusion temperature and the type of plasticizer used.     

Toughening of epoxy systems by brominated epoxy

Blends of brominated epoxy (BE) and conventional epoxy resins were studied following curing with aliphatic triethylenetetramine (TETA), etheric (polyether diamine‐ PEA4), and aromatic (3,3′‐diamino diphenyl sulfone [DDS]) hardeners. The addition of BE resulted in an increase in T_g in all tested blends. Blends with 50 wt% BE cured with TETA demonstrated an increase in flexural modulus and flexural strength, while preserving the elongation. Blends with 40 wt% BE cured with PEA4 and 50 wt% BE cured with DDS resulted in a significant enhanced tensile elongation. The shear strength of all cured systems decreased moderately with the addition of BE exhibiting a mixed mode failure. Analysis of the fracture morphology using electron microscopy supported the increase of toughness levels as a result of incorporating BE to conventional epoxy. A unique nodular and rough fracture morphology was obtained, which is related to a toughening mechanism caused by the addition of BE. It was concluded that blends of BE and conventional epoxy could be used as structural adhesives having high T_g, enhanced mechanical properties and increased toughness. POLYM. ENG. SCI., 59:206–215, 2019. © 2018 Society of Plastics Engineers     

Emulsifier Composition of Solid Lipid Nanoparticles (SLN) Affects Mechanical and Barrier Properties of SLN‐Protein Composite Films

Protein films can be applied to improve food quality and to reduce packaging waste. To overcome their poor water barrier properties, lipids are often incorporated. The function of incorporated lipid depends on the interface between filler and matrix. This study aimed to tailor the properties of a protein–lipid film by designing the oil/water interface to see if the concept of inactive/active filler is valid. Therefore, we varied the emulsifier stabilizing solid lipid nanoparticles (SLN) to promote (via β‐lactoglobulin) or to minimize (via Tween 20) interactions between particle surface and protein. SLN were incorporated into protein films and film properties were determined. Addition of SLN led to significantly decreased water vapor permeability (WVP) of protein films. However, WVP was mainly affected by the emulsifiers and not by the lipid. Protein‐stabilized SLN (BS) replaced a lacking protein in the protein network and therefore did not influence the mechanical properties of the films at ambient temperature. BS‐composite films were temperature sensitive, as lipid and sucrose palmitate melted at temperatures above 40 °C. Tween 20‐stabilized SLN (TS) led to reduced tensile strengths, probably due to perturbative effects of TS and plasticizing effects of Tween 20. Dynamic mechanical analysis showed that TS and Tween 20 increased film mobility. Melting of lipid and emulsifiers, and temperature‐dependent behavior of Tween 20 led to a strong temperature dependence of the film stiffness. By designing the interface, particles can be used to tailor mechanical properties of protein films. Tuned edible films could be used to control mass transfers between foods.     

Reduced toxicity of fumonisin B1 in corn grits by single-screw extrusion

Corn grits spiked with 30 microg/g fumonisin B1 and two batches of grits fermented with Fusarium verticillioides (batch 1 contained 33 microg/g, and batch 2 contained 48 microg/g fumonisin B1), which were extruded by a single-screw extruder with and without glucose (10%, dry weight basis) supplementation were fed to rats. Control groups were fed uncontaminated grits. Extrusion with glucose more effectively reduced fumonisin B1 concentrations of the grits (75 to 85%) than did extrusion alone (10 to 28%). With one exception, the fumonisin B1-spiked and fermented extrusion products caused moderately severe kidney lesions and reduced kidney weights, effects typically found in fumonisin-exposed rats. Lesions in rats fed the least contaminated grits (batch 1) after extrusion with 10% glucose were, however, significantly less severe and not accompanied by kidney weight changes. Therefore, extrusion with glucose supplementation is potentially useful for safely reducing the toxicity of fumonisins in corn-based products and studies to determine the optimal conditions for its use are warranted.     

The thermostability, bioactive compounds and antioxidant activity of some vegetables subjected to different durations of boiling: Investigation in vitro

This research was performed in order to compare the water and acetone extracts of raw and boiled for 10, 20, 40 and 60 min Korean lotus roots (KLR) and Polish white onion (PWO) in the contents of their bioactive compounds, antioxidant activity and thermostability.It was found that polyphenols (mg GAE/g), flavanols (μg GAE/g), flavonoids (mg CE/g), anthocyanins (mg CGE/kg) and tannins (mg CE/g) in water extract of raw lotus roots were 14.18 ± 0.7, 8.41 ± 0.5, 1.09 ± 0.06, 21.3 ± 1.2 and 7.29 ± 0.4, and of white onion - 11.11 ± 0.6, 6.78 ± 0.3, 0.71 ± 0.03, 17.00 ± 0.9 and 1.64 ± 0.08, respectively, and significantly higher in KLR (P < 0.05). The antioxidant activity of raw KLR water extract (139.4 ± 6.1, 53.1 ± 3.6 and 89.3 ± 4.6 μmol TE/g for DPPH, CUPRAC and ABTS, respectively) was significantly higher than in white onion (23.84 ± 1.8, 31.9 ± 2.1 and 38.14 ± 2.6 for DPPH, CUPRAC and ABTS, respectively, P < 0.05).The thermostability of the water KLR extract’s of polyphenols, flavanols, flavonoids, anthocyanins and tannins was high and even after 60 min of boiling remains as 40.0, 42.3, 50.5, 41.4 and 41.0%, respectively. After 60 min of boiling the most thermostable compounds were flavonoids - remaining at 50.5% in water extract of KLR. Also after 60 min of boiling the thermostability of the antioxidant activity of water extracts of KLR remained significantly high: 40.6, 42.3, 46.3 and 43.6%, according to DPPH, FRAP, ABTS and CUPRAC assays, respectively.Similar relationship was obtained with acetone extracts, but the value was lower than with the water ones. In conclusion, the contents of some bioactive compounds, the antioxidant activity and the thermostability in water and acetone extracts of KLR are significantly higher than the same indices in PWO. FTIR and fluorimetry can be used as additional markers for the characterization of bioactive compounds in vegetables.     

Measuring oxidative DNA damage and DNA repair using the yeast comet assay

Chromosomal DNA damage can be a result of several processes and agents of endogenous or exogenous origin. These cause strand breaks or oxidized bases that lead to strand breaks, which relax the normally supercoiled genomic DNA and increase its electrophoretic mobility. The extent of DNA damage can be assessed by single cell gel electrophoresis, where the chromosomal DNA migration distance correlates with the extent of DNA damage. This technique has been used for a variety of applications with several organisms, but only a few studies have been reported for Saccharomyces cerevisiae. A possible reason for this absence is that low cellular DNA content could hamper visualization. Here we report an optimization of the comet assay protocol for yeast cells that is robust and sensitive enough to reproducibly detect background DNA damage and oxidative damage caused by hydrogen peroxide. DNA repair was observed and quantified as diminishing comet tail length with time after oxidative stress removal in a process well described by first‐order kinetics with a tail length half‐life of 11 min at 37 °C. This is, to our knowledge, the first quantitative measurement of DNA repair kinetics in S. cerevisiae by this method. We also show that diet antioxidants protect from DNA damage, as shown by a three‐fold decrease in comet tail length. The possibility of assessment of DNA damage and repair in individual cells applied to the model organism S. cerevisiae creates new perspectives for studying genotoxicity and DNA repair. Copyright © 2010 John Wiley & Sons, Ltd.