High frequency circular translation pin-on-disc wear testing of UHMWPE using a ball-on-flat contact along a hypotrochoidal track

To intensify experimental research within the field of orthopaedic tribology, a three-station, dual motion, high frequency (25.3 Hz) circular translation pin-on-disc wear test device was recently introduced. In the present study, the pins were CoCr with a spherical, polished bearing surface of 28 mm radius, whereas the flat discs were conventional UHMWPE. This configuration was intended to simulate the wear mechanisms of total knee prostheses. The number of wear cycles run was as high as 200 million. The mean wear rate was 0.35 mg per one million cycles (0.77 mg/24 h) which corresponded to a mean wear factor of 3.5 × 10⁻⁶ mm³/Nm. The study provided further proof that a wear test for orthopaedic implant materials can be accelerated by substantially increasing the cycle frequency, provided that the sliding velocity remains close to the values obtained from biomechanical studies. Hence, the moderate frictional heating will not lead to unrealistic wear mechanisms.     

Accelerated solvent extraction and pH‐zone‐refining counter‐current chromatographic purification of yunaconitine and 8‐deacetylyunaconitine from Aconitum vilmorinianum Kom

This study aimed to seek an efficient method to extract and purify yunaconitine and 8‐deacetylyunaconitine from Aconitum vilmorinianum Kom. by accelerated solvent extraction combined with pH‐zone‐refining counter‐current chromatography. The major extraction parameters for accelerated solvent extraction were optimized by an orthogonal test design L₉ (3)⁴. Then a separation and purification method was established using pH‐zone‐refining counter‐current chromatography with a two‐phase solvent system composed of petroleum ether/ethyl acetate/methanol/water (5:5:2:8, v/v) with 10 mM triethylamine in the upper phase and 10 mM HCl in the lower phase. From 2 g crude extract, 224 mg of 8‐deacetylyunaconitine (I) and 841 mg of yunaconitine (II) were obtained with a purity of over 98.0%. The chemical structures were identified by ESI‐MS and ¹H and ¹³C NMR spectroscopy.     

Perylene-based profluorescent nitroxides for the rapid monitoring of polyester degradation upon weathering: An assessment

A profluorescent nitroxide possessing an isoindoline nitroxide moiety linked to a perylene fluorophore was developed to monitor radical mediated degradation of melamine-formaldehyde crosslinked polyester coil coatings in an industry standard accelerated weathering tester. Trapping of polyester-derived radicals (most likely C-radicals) that are generated during polymer degradation leads to fluorescent closed-shell alkoxy amines, which was used to obtain time-dependent degradation profiles to assess the relative stability of different polyesters towards weathering. The nitroxide probe couples excellent thermal stability and satisfactory photostability with high sensitivity and enables detection of free radical damage in polyesters under conditions that mimic exposure to the environment on a time scale of hours rather than months or years required by other testing methods. There are indications that the profluorescent nitroxide undergoes partial photo-degradation in the absence of polymer-derived radicals. Unexpectedly, it was also found that UV-induced fragmentation of the NO–C bond in closed-shell alkoxy amines leads to regeneration of the profluorescent nitroxide and the respective C-radical. The maximum fluorescence intensity that could be achieved with a given probe concentration is therefore not only determined by the amount of polyester radicals formed during accelerated weathering, but also by the light-driven side reactions of the profluorescent nitroxide and the corresponding alkoxy amine radical trapping products. Studies to determine the optimum probe concentration in the polymer matrix revealed that aggregation and re-absorption effects lowered the fluorescence intensity at higher concentrations of the profluorescent nitroxide, but too low probe concentrations, where these effects would be avoided, were not sufficient to trap the amount of polyester radicals formed upon weathering. The optimized experimental conditions were used to assess the impact of temperature and UV irradiance on polymer degradation during accelerated weathering.     

The Extraction of Polycyclic Aromatic Hydrocarbons from Atmospheric Particulate Matter Samples by Accelerated Solvent Extraction (ASE)

Abstract

The Accelerated solvent extraction (ASE) of PAHs (23 2- to 6-ring species) spiked onto glass fibre filters (GFFs) was studied as a function of variable extraction solvents, pressure, temperature and extraction times. Acceptable recoveries (85% ± 15%) were obtained for certain combinations of conditions and a tentative method (1500 psi, 150°C, 70:30 hexane:acetone mixture, 7 min heat-up time, 5 min static extraction time, 60% flush volume, 2 static cycles was selected for further testing. However, this method did not prove as effective as the traditional Soxhlet method of extraction when these parameters were used to extract native PAHs from ambient atmospheric particulate matter collected on a GFF by Integrated Atmospheric Deposition Network (IADN) sampling protocols. The extraction recovery study for spiked GFFs was repeated using slightly different extraction conditions: 2000 psi, 100°C, 70:30 hexane:acetone, 5 min heat-up time, 5 min static extraction time, 150% flush volume, 3 static cycles. When this method was applied to the extraction of native PAHs from ambient atmospheric particulate matter collected on GFFs, the results showed equivalent or better recoveries to that of the Soxhlet method. The total time of extraction was 25 min requiring only 30 mL of solvent. This ASE method is presently used to quantitatively determine PAHs in IADN particle-phase samples.     

Optimum step-stress accelerated degradation test for Wiener degradation process under constraints

To assess a product's reliability for subsequent managerial decisions such as designing an extended warranty policy and developing a maintenance schedule, Accelerated Degradation Test (ADT) has been used to obtain reliability information in a timely manner. In particular, Step-Stress ADT (SSADT) is one of the most commonly used stress loadings for shortening test duration and reducing the required sample size. Although it was demonstrated in many previous studies that the optimum SSADT plan is actually a simple SSADT plan using only two stress levels, most of these results were obtained numerically on a case-by-case basis. In this paper, we formally prove that, under the Wiener degradation model with a drift parameter being a linear function of the (transformed) stress level, a multi-level SSADT plan will degenerate to a simple SSADT plan under many commonly used optimization criteria and some practical constraints. We also show that, under our model assumptions, any SSADT plan with more than two distinct stress levels cannot be optimal. These results are useful for searching for an optimum SSADT plan, since one needs to focus only on simple SSADTs. A numerical example is presented to compare the efficiency of the proposed optimum simple SSADT plans and a SSADT plan proposed by a previous study. In addition, a simulation study is conducted for investigating the efficiency of the proposed SSADT plans when the sample size is small.     

Wastes from Wood Extraction Used in Composite Materials: Behavior after Accelerated Weathering

New materials were obtained by incorporating in polypropylene (PP) matrix 60% wood wastes resulting after extraction with supercritical carbon dioxide, water, and ethanol. Structural, mechanical, thermal, and rheological characterizations, as well as moisture uptake of the composites, were evaluated before and after accelerated weathering. It was found that the extraction method influenced the composite properties due to the hydrophilic-hydrophobic balance. The addition of extracted fibers results in an increase in hardness and tensile properties and a decrease of impact strength as compared to PP.     

A comparison of the increased temperature accelerated degradation of Poly(d,l-lactide-co-glycolide) and Poly(l-lactide-co-glycolide)

Bioresorbable polymers composed of Poly(lactide), Poly(glycolide) and their related copolymers have become increasingly popular for the preparation of bone substitute constructs. In vitro tests assessing the degradative changes in physicochemical, mechanical, and biological properties of bioresorbable polymers are generally carried out at 37 °C, in pH 7.4 phosphate-buffered saline (PBS). However, long degradation times, varying from months to years make it difficult to assess these polymers at their late stages of degradation. An increased temperature accelerated degradation methodology, that simulates the long-term degradation of Poly(d,l-lactide-co-glycolide) and Poly(l-lactide-co-glycolide), has been validated in this study. Samples were degraded in PBS, under sterile conditions. Degradation temperatures of 47 °C, 57 °C and 70 °C were selected and compared to physiological temperature, 37 °C. At predetermined time intervals, samples were retrieved and evaluated for changes in mass, swelling, molecular weight, crystallinity, and thermal properties. The results from this study suggest that the degradation mechanism at elevated temperatures is similar to that observed at 37 °C. It is recommended that 47 °C is adopted by the research community to accelerate the degradation of these polymers. It is hoped the application of this methodology could be used as a valuable tool, prior to the assessment of the long-term biocompatibility of these polymers.     

一种新型平板彩色显示器件的制备和光谱分析

以MEH-PPV(聚[2-甲氧基-5-(2′-乙基己氧基-对苯乙烯)])和Alq₃作为发光层, 成功制备出ITO/SiO₂/MEH-PPV/SiO₂/Al结构和ITO/SiO₂/Alq₃ /SiO₂/Al结构的固态阴极射线器件。通过分析SSCL光谱,认为这些高速电子激发有机材料后形成Frenkel激子。当器件两个电极之间加的电压比较低时,有机薄膜层的场强也比较低,这些激子被解离的概率很小,从而产生的是激子发光的长波发射;当器件两个电极之间加的电压比较高时,有机薄膜层的场强很高, 在有机层形成的激子大部分被解离, 解离后的电子直接跃迁至LUMO(lowest unoccupancied molecular orbit),这些电子弛豫后从LUMO能级到HOMO(highest occupancied molecular orbit )能级直接辐射跃迁, 接着重新复合发光,从而产生短波发射。制作的固态阴极射线器件可以实现全色发光, 提高发光效率和加强蓝光发射。作者可以预期所研制出的这种SSCL器件必将引发平板显示领域一场新的革命性变革。     

Solubility study and intensification of extraction of phenolic and anthocyanin compounds from Oryza sativa L. ‘Violet Nori’

Oryza sativa L. ‘Violet Nori’ is an Italian cultivar of spontaneous growing aromatic purple rice which is particularly rich in polyphenolic compounds, especially anthocyanins, conferring it an excellent antioxidant capacity. The present study aimed at increasing the extraction yields of its antioxidant compounds with green strategies and it is divided into two steps. The first step concerned a solubility study of the targeted polyphenols in different ethanol:water mixtures by means of a theoretical prediction method, using the simulation program COSMO-RS, and the subsequently confirmation of the computational results by practical experiments. Once the best extraction mixture was identified, the second step of the work was performed, with the purpose of intensifying the extraction yield. Therefore, various innovative green extraction techniques, including ultrasound, using both the probe system and the ultrasonic bath, bead milling, microwave and accelerated solvent extractions were tested and compared to conventional maceration.Results, expressed in terms of total phenolic and total monomeric anthocyanin contents, showed that the best extracting solvent for ‘Violet Nori’ rice was the mixture ethanol:water (60:40 v/v), being COSMO-RS computational predictions in good correlation with the experimental results. Moreover, the most efficient techniques to extract the antioxidant compounds resulted to be both ultrasound-assisted extraction probe and bead milling, that in only 5 min got the same extractive efficiency obtained after 3 h of conventional maceration.     

沉积物中壬基苯酚类雌性激素化合物的加速溶剂提取方法研究

为了同时提取和检测沉积物中的雌性激素化合物对壬基苯酚(NP)、对壬基苯酚一乙氧醚(NP1EO)和对壬基苯酚二乙氧醚(NP2EO),对加速溶剂提取体系的各种条件和对壬基苯酚类化合物的硅烷基化反应条件等进行了优化。在丙酮和丙酮-二氯甲烷混合液(丙酮含量≥60%)介质中,这些化合物的硅烷基化反应很快达到反应终点。加速溶剂提取体系的最佳提取条件是120℃、8.4MPa、两次循环提取;最佳提取溶剂是二氯甲烷。与索氏提取和酸化悬浮液液提取比较,明显提高了提取率、重现性和准确性。平均添标回收率在89.3%~95.7%之间,相对标准偏差为2.3%~13.4%。本方法对壬基苯酚、对壬基苯酚一乙氧醚和对壬基苯酚二乙氧醚化合物的检出限分别为10、30、35ng/gdw(干重)。