Inorganic Sol-Gel Preparation of Medium Sized Microparticles of Li2TiO3 from TiCl4 as Tritium Breeding Material for Fusion Reactors

Microspheres of Li₂TiO₃ were fabricated by a classical, inorganic sol-gel process from commercially available TiCl₄. Elaborated process consists of the following main steps: (1) dissolving of TiCl₄ in concentrated aqueous HCl and addition of LiOH; (2) formation of sol emulsion in 2-ethylhexanol-1 containing the surfactant SPAN-80 (EH); (3) gelation of emulsion drops by extraction of water with partially dehydrated EH; (4) impregnation of gel to Li:Ti molar ratio MR = 2; (5) thermal treatment at 1200°C in order to receive chloride free product. This temperature can be significantly lowered (to 750°C) by dechlorination starting solution TiCl₄ by chemical treatment of the with nitric acid to form of nitrate-stabilized titania sols. Tritium release from sol-gel made Li₂TiO₃ microspheres were found very close to that observed for other traditional materials, however for the first sample process starts slightly earlier.     

Temperature measurements by H2-CARS in the reactive zone of a plasma test reactor for hydrocarbon synthesis

The application of coherent anti-Stokes Raman spectroscopy (CARS) to an electric are test reactor is described in which acetylene synthesis in analogy to the large-scale industrial process is .studied. We report on spatially resolved measurements of H₂-CARS spectra, the comparison with calculated spectra, and the determination of temperatures in the reaction zone.Dedicated to Prof. Rudolf Wienecke on the occasion of his 65 birthday.     

~(13)C代谢通量分析

代谢通量分析(metabolic flux analysis,MFA)是通过确定代谢网络中代谢流分布来表征细胞代谢状态的强有力的工具。鉴于计量学代谢通量分析在处理复杂代谢网络时表现出的局限性,发展了以13C标记实验为基础的13C MFA。本文介绍了13C MFA的原理与方法,总结和评述了13C MFA在实验与数据分析方面的最新进展以及MFA在功能基因组研究中的重要地位,同时对代谢通量分析的发展前景进行了展望。     

Use of non-segmented flow,post-columns reaction detection with miniaturized HPLC systems

Summary The use of non-segmented flow, post-column reaction detection is evaluated for use with miniaturized HPLC. Non-segmented open-tubular reactors with internal diameters 0.1 mm to 0.25 mm and packed-bed reactors with internal diameters of 1 mm, filled with 5 and 10 m particles are evaluated theoretically and experimentally with respect to band broadening and pressure drop characteristics. An integrated system consisting of miniaturized HPLC (1 mm i. d.) columns and compatible hardware is described. An example of the separation of catecholamines is given.     

Composite poly(dimethylsiloxane)/glass microfluidic system with an immobilized enzymatic particle-bed reactor and sequential sample injection for chemiluminescence determinations

A three-layer poly(dimethylsiloxane) (PDMS)/glass microfluidic system for performing on-chip solid-phase enzymatic reaction and chemiluminescence (CL) reaction was used for the determination of glucose as a model analyte. A novel method for the immobilization of controlled-pore-glass based reactive particles on PDMS microreactor beds was developed, producing an on-chip solid-phase reactor that featured large reactive surface and low flow impedance. Efficient mixing of reagent/sample/carrier streams was achieved by incorporating chaotic mixer structures in the microfluidic channels. A conventional sequential injection (SI) system was adapted for direct coupling with the microfluidic system, and combined with hydrostatic delivery of reagents to achieve efficient and reproducible sample introduction at 10 μl levels. A detection limit of 10 μM glucose (3σ), and a precision of 3.1% RSD (n=7, 0.2 mM glucose) were obtained using the SI-microfluidic-CL system integrated with a glucose oxidase (GOD) reactor. Carryover was <5% at a throughput of 20 samples/h.     

Comparative Effect of UV,UV/H2O2 and UV/H2O2/Fe on Terbuthylazine Degradation in Natural and Ultrapure Water

Different advanced oxidation processes (AOPs) (ultraviolet radiation, hydrogen peroxide photolysis and photo-Fenton) were applied to test the degradation of terbuthylazine in three types of water: (a) ultrapure water, (b) surface water from the Gaditana area (Los Hurones reservoir, Cádiz, Spain) and (c) groundwater from the Tempul spring in Jerez de la Frontera (Cádiz, Spain). The experiments were carried out on a laboratory scale, using two different types of reactors, batch and semi-continuous. In batch reactors, the most efficient process for the experiments carried out with both ultrapure water and underground groundwater was ultraviolet radiation, whereas for surface water from the Gaditana area, the process that obtained the best results was the photolysis of hydrogen peroxide with 2.5 mg L⁻¹ of H₂O₂. In semi-continuous reactors, the most efficient process was the photolysis of hydrogen peroxide with 2.5 mg L⁻¹ of H₂O₂ for all the matrices studied. In both types of reactors, terbuthylazine degradation percentages higher than 90% were achieved; the main difference was in the reaction time, which varied from minutes in the batch reactor to seconds in the semi-continuous reactor. In all the applied AOPs, N-terbutyl-6-hydroxy-N′ethyl-1,3,5-triazine-2,4-diamine (TBA-212) was generated as a reaction intermediate.     

A Cyclodextrin Molecular Reactor for the Regioselective Synthesis of 1,5-disubstituted-1,2,3-triazoles

6^A-Deoxy-6^A-propynamido-β-cyclodextrin reacts with 4-tert-butylphenyl azide in aqueous solution, to form the 5-(aminocarbonyl)-substituted triazole in preference to the 4-(aminocarbonyl)-substituted analogue, in a ratio of 25:1. The cyclodextrin moiety templates the reaction through the formation of a host-guest complex of the dipole with the dipolarophile, controlling the regioselectivity of cycloaddition. In a control reaction under similar conditions, with propiolamide instead of the cyclodextrin derivative, 5- and 4-(aminocarbonyl)-1-(4-tert-butylphenyl)-1,2,3-triazole were formed in a ratio of 1:4. As well as reversing the regioselectivity, the cyclodextrin substituent increases the rate of cycloaddition, by at least two orders of magnitude for the reaction to give the 5-substituted cycloadduct. Even the rate of formation of the 4-substituted cycloadduct is increased by a factor of two. Less marked effects are observed with phenyl azide and 4-tert-butylbenzyl azide as dipoles.     

Batch versus Flow Photochemistry: A Revealing Comparison of Yield and Productivity

The use of flow photochemistry and its apparent superiority over batch has been reported by a number of groups in recent years. To rigorously determine whether flow does indeed have an advantage over batch, a broad range of synthetic photochemical transformations were optimized in both reactor modes and their yields and productivities compared. Surprisingly, yields were essentially identical in all comparative cases. Even more revealing was the observation that the productivity of flow reactors varied very little to that of their batch counterparts when the key reaction parameters were matched. Those with a single layer of fluorinated ethylene propylene (FEP) had an average productivity 20 % lower than that of batch, whereas three‐layer reactors were 20 % more productive. Finally, the utility of flow chemistry was demonstrated in the scale‐up of the ring‐opening reaction of a potentially explosive [1.1.1] propellane with butane‐2,3‐dione.     

生产99Mo、131I和89Sr医用同位素的水溶液堆

99Mo1、31I和89Sr等医用同位素对人类健康和医学的发展具有非常重要的作用。与靶辐照反应堆相比,用水溶液堆生产99Mo1、31I和89Sr具有安全性好,结构简单,经济价值高,无靶件制备、溶解工艺,产生废物少等优点,用水溶液堆生产医用同位素具有很好的发展前景。由于多堆芯水溶液堆、高功率水溶液堆均能显著提高产率,低富集度235U水溶液堆符合核不扩散条约中对235U浓缩度的要求,因此这三种堆是水溶液堆未来的发展方向。     

Intensification of delignification of Tectona grandis saw dust as sustainable biomass using acoustic cavitational devices

Delignification of sawdust was studied using ultrasound assisted alkali peroxide approach using longitudinal horn for the first time and the efficacy compared with more commonly used configurations of ultrasonic reactors. Comparison with the conventional approach based on stirring has also been presented to establish the process intensification benefits. Effect of different operating parameters such as sodium carbonate concentration (0.1, 0.15, 0.2, 0.25 M), hydrogen peroxide concentration (0.2, 0.4, 0.6, 0.8, 1 M) and biomass loading (2, 4, 6, 8, 10 wt%), on the efficacy of lignin extraction has been investigated for different ultrasonic reactors. The optimum conditions for probe type ultrasonic horn were established as 150 W, 50% duty cycle and 80% amplitude with optimum process conditions as Na₂CO₃ concentration as 0.2 M, H₂O₂ concentration as 1 M, biomass loading of 10 wt% and operating time of 70 min. Longitudinal horn resulted in best efficacy (both in terms of yield and energy requirements) followed by ultrasonic horn and ultrasonic bath whereas the conventional approach was least effective. The obtained lignin was also analyzed using different characterization techniques. The presence of peaks at wavelength range of 875–817, 1123–1110, and at 1599 cm⁻¹ for the extracted sample confirmed the presence of lignin. Increase in the crystallinity index of the processed sample (maximum for longitudinal horn) also confirmed the lignin removal as lignin is amorphous in nature. Overall it has been concluded that ultrasound can be effectively used for delignification with longitudinal horn as best configuration.