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Different Radial Modification Profiles Observed on APPJ-Treated Polypropylene Surfaces according to the Distance between Plasma Outlet and Target
The plasma jet transfer technique relies on a conductive wire at floating potential, which, upon entering in contact with a primary discharge, is capable of igniting a small plasma plume at the distal end of a long flexible plastic tube. In this work, two different long tube configurations were employed for the surface modification of polypropylene (PP) samples using argon as the working gas. One of the jet configurations has a thin copper (Cu) wire, which was installed inside the long tube. In the other configuration, the floating electrode is a metallic mesh placed between two plastic tubes in a coaxial arrangement. In the first case, the tip of the Cu wire is in direct contact with the working gas at the plasma outlet, whereas, in the second, the inner plastic tube provides an additional dielectric barrier that prevents the conductor from being in contact with the gas. Water contact angle (WCA) measurements on treated PP samples revealed that different surface modification radial profiles are formed when the distance (d) between the plasma outlet and target is changed. Moreover, it was found that the highest WCA reduction does not always occur at the point where the plasma impinges the surface of the material, especially when the d value is small. Through X-ray photoelectron spectroscopy (XPS) analysis, it was confirmed that the WCA values are directly linked to the oxygen-functional groups formed on the PP surfaces after the plasma treatment. An analysis of the WCA measurements along the surface, as well as their temporal evolution, together with the XPS data, suggest that, when the treatment is performed at small d values, the plasma jet removes some functional groups at the point where the plasma hits the surface, thus leading to peculiar WCA profiles.
Biological Risk Assessment of Three Dental Composite Materials following Gas Plasma Exposure
Gas plasma is an approved technology that generates a plethora of reactive oxygen species, which are actively applied for chronic wound healing. Its particular antimicrobial action has spurred interest in other medical fields, such as periodontitis in dentistry. Recent work has indicated the possibility of performing gas plasma-mediated biofilm removal on teeth. Teeth frequently contain restoration materials for filling cavities, e.g., resin-based composites. However, it is unknown if such materials are altered upon gas plasma exposure. To this end, we generated a new in-house workflow for three commonly used resin-based composites following gas plasma treatment and incubated the material with human HaCaT keratinocytes in vitro. Cytotoxicity was investigated by metabolic activity analysis, flow cytometry, and quantitative high-content fluorescence imaging. The inflammatory consequences were assessed using quantitative analysis of 13 different chemokines and cytokines in the culture supernatants. Hydrogen peroxide served as the control condition. A modest but significant cytotoxic effect was observed in the metabolic activity and viability after plasma treatment for all three composites. This was only partially treatment time-dependent and the composites alone affected the cells to some extent, as evident by differential secretion profiles of VEGF, for example. Gas plasma composite modification markedly elevated the secretion of IL6, IL8, IL18, and CCL2, with the latter showing the highest correlation with treatment time (Pearson’s r > 0.95). Cell culture media incubated with gas plasma-treated composite chips and added to cells thereafter could not replicate the effects, pointing to the potential that surface modifications elicited the findings. In conclusion, our data suggest that gas plasma treatment modifies composite material surfaces to a certain extent, leading to measurable but overall modest biological effects.
Internal Crack Initiation and Growth Starting from Artificially Generated Defects in Additively Manufactured Ti6Al4V Specimen in the VHCF Regime
The aim of the present work was to investigate the ‘fine granular area’ (FGA) formation based on artificially generated internal defects in additively manufactured Ti6Al4V specimens in the early stage of fatigue crack growth in the ‘very high cycle fatigue’ (VHCF) regime. Fatigue tests were performed with constant amplitude at pure tension-compression loading (R = −1) using an ultrasonic fatigue testing setup. Failed specimens were investigated using optical microscopy, high-resolution ‘scanning electron microscopy’ (SEM), and ‘focused ion beam’ (FIB) techniques. Further, the paper introduces alternative proposals to identify the FGA layer beneath the fracture surfaces in terms of the ‘cross section polishing’ (CSP) technique and metallic grindings with special attention paid to the crack origin, the surrounding microstructure, and the expansion of the nanograin layer beneath the fracture surface. Different existing fracture mechanical approaches were applied to evaluate if an FGA formation is possible. Moreover, the results were discussed in comparison to the experimental findings.
Subcritical fluid chromatography at sub-ambient temperatures for the chiral resolution of ketamine metabolites with rapid-onset antidepressant effects
Chiral metabolites of ketamine exerting rapid-onset yet sustained antidepressant effects may be marketed directly in the future, but require chemo- and enantio-selective chromatographic methods for quality assurance and control. The chromatographic behavior of S-/R-ketamine, S-/R-norketamine, S-/R-dehydronorketamine, and (2R,6R)-/(2S,6S)-hydroxynorketamine in supercritical fluid chromatography (SFC) was investigated computationally and experimentally with the aim of identifying problematic pairs of enantiomers and parameters for chiral resolution. Retention on three different polysaccharide-based chiral stationary phases (Lux Amylose-2, i-Amylose-3, and i-Cellulose-5) provided new information on the significance of halogen atoms as halogen bond donors and hydrogen bond acceptors for enantioselectivity, which could be corroborated in silico by molecular docking studies. Modifiers inversely affected enantioselectivity and retention. Methanol yielded lower run times but superior chiral resolution compared to 2-propanol. Lower temperatures than those conventionally screened did not impair phase homogeneity but improved enantioresolution, at no cost to reproducibility. Thus, sub-ambient temperature subcritical fluid chromatography (SubFC), essentially low-temperature HPLC with subcritical CO2, was applied. The optimization of the SubFC method facilitated the chiral separation of ketamine and its metabolites, which was applied in combination with direct injection and online supercritical fluid extraction to determine the purity of pharmaceutical ketamine formulations for proof of concept. © 2019 by the authors.
Mixed Ionic-Electronic Conductivity, Redox Behavior and Thermochemical Expansion of Mn-Substituted 5YSZ as an Interlayer Material for Reversible Solid Oxide Cells
Manganese-substituted 5 mol.% yttria-stabilized zirconia (5YSZ) was explored as a prospective material for protective interlayers between electrolyte and oxygen electrodes in reversible solid oxide fuel/electrolysis cells. [(ZrO2)0.95(Y2O3)0.05]1−x[MnOy]x (x = 0.05, 0.10 and 0.15) ceramics with cubic fluorite structure were sintered in air at 1600 °C. The characterization included X-ray diffraction (XRD), scanning electron microscopy (SEM)/energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), thermogravimetry and dilatometry in controlled atmospheres, electrical conductivity measurements, and determination of oxygen-ion transference numbers by the electromotive force (EMF) technique. Mn-substituted 5YSZ solid solutions exhibit variable oxygen nonstoichiometry with manganese cations in a mixed 2+/3+ oxidation state under oxidizing conditions. Substitution by manganese gradually increases the extent of oxygen content variation on thermal/redox cycling, chemical contribution to thermal expansion and dimensional changes on reduction. It also deteriorates oxygen-ionic conductivity and improves p-type electronic conductivity under oxidizing conditions, leading to a gradual transformation from predominantly ionic to prevailing electronic transport with increasing x. Mn2+/3+→Mn2+ transformation under reducing atmospheres is accompanied by the suppression of electronic transport and an increase in ionic conductivity. All Mn-substituted 5YSZ ceramics are solid electrolytes under reducing conditions. Prolonged treatments in reducing atmospheres, however, promote microstructural changes at the surface of bulk ceramics and Mn exsolution. Mn-substituted 5YSZ with 0.05 ≤ x < 0.10 is considered the most suitable for the interlayer application, due to the best combination of relevant factors, including oxygen content variations, levels of ionic/electronic conductivity and thermochemical expansion.
Thermal analysis of aliphatic polyester blends with natural antioxidants
The aim of this research was to enhance thermal stability of aliphatic polyester blends via incorporation of selected natural antioxidants of plant origin. Thermal methods of analysis, including differential scanning calorimetry (DSC) and thermogravimetry (TGA), are significant tools for estimating the stabilization effect of polyphenols in a polymer matrix. Thermal stability was determined by analyzing thermogravimetric curves. Polymers with selected antioxidants degraded more slowly with rising temperature in comparison to reference samples without additives. This property was also confirmed by results obtained from differential scanning calorimetry (DSC), where the difference between the oxidation temperatures of pure material and polymer with natural stabilizers was observed. According to the results, the materials with selected antioxidants, including trans-chalcone, flavone and lignin have higher oxidation temperature than the pure ones, which confirms that chosen phytochemicals protect polymers from oxidation. Moreover, based on the colour change results or FT-IR spectra analysis, some of the selected antioxidants, including lignin and trans-chalcone, can be utilized as colorants or aging indicators. Taking into account the data obtained, naturally occurring antioxidants, including polyphenols, can be applied as versatile pro-ecological additives for biodegradable and bio-based aliphatic polyesters to obtain fully environmentally friendly materials dedicated for packaging industry.
Microbial Control of Raw and Cold-Smoked Atlantic Salmon (Salmo salar) through a Microwave Plasma Treatment
The control of the pathogenic load on foodstuffs is a key element in food safety. Particularly, seafood such as cold-smoked salmon is threatened by pathogens such as Salmonella sp. or Listeria monocytogenes. Despite strict existing hygiene procedures, the production industry constantly demands novel, reliable methods for microbial decontamination. Against that background, a microwave plasma-based decontamination technique via plasma-processed air (PPA) is presented. Thereby, the samples undergo two treatment steps, a pre-treatment step where PPA is produced when compressed air flows over a plasma torch, and a post-treatment step where the PPA acts on the samples. This publication embraces experiments that compare the total viable count (tvc) of bacteria found on PPA-treated raw (rs) and cold-smoked salmon (css) samples and their references. The tvc over the storage time is evaluated using a logistic growth model that reveals a PPA sensitivity for raw salmon (rs). A shelf-life prolongation of two days is determined. When cold-smoked salmon (css) is PPA-treated, the treatment reveals no further impact. When PPA-treated raw salmon (rs) is compared with PPA-untreated cold-smoked salmon (css), the PPA treatment appears as reliable as the cold-smoking process and retards the growth of cultivable bacteria in the same manner. The experiments are flanked by quality measurements such as color and texture measurements before and after the PPA treatment. Salmon samples, which undergo an overtreatment, solely show light changes such as a whitish surface flocculation. A relatively mild treatment as applied in the storage experiments has no further detected impact on the fish matrix.
Effect of Cold Atmospheric Plasma Jet Associated to Polyene Antifungals on Candida albicans Biofilms
The increasing incidence of antifungal resistance represents a great challenge in the medical area and, for this reason, new therapeutic alternatives for the treatment of fungal infections are urgently required. Cold atmospheric plasma (CAP) has been proposed as a promising alternative technique for the treatment of superficial candidiasis, with inhibitory effect both in vitro and in vivo. However, little is known on the association of CAP with conventional antifungals. The aim of this study was to evaluate the effects of the association between CAP and conventional polyene antifungals on Candida albicans biofilms. C. albicans SC 5314 and a clinical isolate were used to grow 24 or 48 h biofilms, under standardized conditions. After that, the biofilms were exposed to nystatin, amphotericin B and CAP, separately or in combination. Different concentrations of the antifungals and sequences of treatment were evaluated to establish the most effective protocol. Biofilms viability after the treatments was compared to negative control. Data were compared by One-way ANOVA and post hoc Tukey (5%). The results demonstrate that 5 min exposure to CAP showed more effective antifungal effect on biofilms when compared to nystatin and amphotericin B. Additionally, it was detected that CAP showed similar (but smaller in magnitude) effects when applied in association with nystatin and amphotericin B at 40 µg/mL and 60 µg/mL. Therefore, it can be concluded that the application of CAP alone was more effective against C. albicans biofilms than in combination with conventional polyene antifungal agents.
Efficacy of plasma-polymerized allylamine coating of zirconia after five years
Plasma-polymerized allylamine (PPAAm) coatings of titanium enhance the cell behavior of osteoblasts. The purpose of the present study was to evaluate a PPAAm nanolayer on zirconia after a storage period of 5 years. Zirconia specimens were directly coated with PPAAm (ZA0) or stored in aseptic packages at room temperature for 5 years (ZA5). Uncoated zirconia specimens (Zmt) and the micro-structured endosseous surface of a zirconia implant (Z14) served as controls. The elemental compositions of the PPAAm coatings were characterized and the viability, spreading and gene expression of human osteoblastic cells (MG-63) were assessed. The presence of amino groups in the PPAAm layer was significantly decreased after 5 years due to oxidation processes. Cell viability after 24 h was significantly higher on uncoated specimens (Zmt) than on all other surfaces. Cell spreading after 20 min was significantly higher for Zmt = ZA0 > ZA5 > Z14, while, after 24 h, spreading also varied significantly between Zmt > ZA0 > ZA5 > Z14. The expression of the mRNA differentiation markers collagen I and osteocalcin was upregulated on untreated surfaces Z14 and Zmt when compared to the PPAAm specimens. Due to the high biocompatibility of zirconia itself, a PPAAm coating may not additionally improve cell behavior.
Uncertainty Quantification and Sensitivity Analysis for the Electrical Impedance Spectroscopy of Changes to Intercellular Junctions Induced by Cold Atmospheric Plasma
The influence of pertinent parameters of a Cole-Cole model in the impedimetric assessment of cell-monolayers was investigated with respect to the significance of their individual contribution. The analysis enables conclusions on characteristics, such as intercellular junctions. Especially cold atmospheric plasma (CAP) has been proven to influence intercellular junctions which may become a key factor in CAP-related biological effects. Therefore, the response of rat liver epithelial cells (WB-F344) and their malignant counterpart (WB-ras) was studied by electrical impedance spectroscopy (EIS). Cell monolayers before and after CAP treatment were analyzed. An uncertainty quantification (UQ) of Cole parameters revealed the frequency cut-off point between low and high frequency resistances. A sensitivity analysis (SA) showed that the Cole parameters, R0 and α were the most sensitive, while Rinf and τ were the least sensitive. The temporal development of major Cole parameters indicates that CAP induced reversible changes in intercellular junctions, but not significant changes in membrane permeability. Sustained changes of τ suggested that long-lived ROS, such as H2O2, might play an important role. The proposed analysis confirms that an inherent advantage of EIS is the real time observation for CAP-induced changes on intercellular junctions, with a label-free and in situ method manner.