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- Author or Editor: Jing Zhang x
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Abstract
The reaction of direct transformation of ethanol to ethyl acetate was investigated on reduced Cu/ZrO2 catalysts prepared by a co-precipitation procedure. The catalytic performances of these Cu–Zr mixed oxides were considerably influenced by changing the molar ratio of Cu to Zr. The highest selectivity to ethyl acetate was found over Cu/ZrO2(1) catalyst (molar ratio of Cu to Zr was 1). A variety of characterization techniques, such as N2 adsorption, XRD, XPS, TPR and NH3-TPD were carried out on the catalysts. The results revealed that the presence of a certain amount of Cu+ species may play very important role in improving the selectivity to ethyl acetate of the Cu/ZrO2 catalysts.
Abstract
Non-isothermal crystallization kinetics and subsequent melting behavior for three kinds of ethylene-acrylic acid copolymer (EAA) are investigated via differential scanning calorimetry (DSC). From the Jeziorny method, the crystallization rate of the primary stage is significantly influenced by the competitive mobility of chains. While the crystallization rate in the secondary stage decreases in order of acrylic acid (AA) content in copolymers. Mo’s method can also provide a good fitting. Difference between the Jeziorny method and Mo’s method analysis is because of a higher effect of non-crystallizable chain ends. The effective activation energy is also determined via Kissinger’s method.
Abstract
Through placement in a few hours after collecting radioaerosol samples (in Shanghai) after Fukushima nuclear power plant (NPP) accident, radionuclides with gamma-emitting rays can be found to be nuclides (132I/132Te, 129I/129Te) other than 131I, 134,137Cs because of the decrease in background baseline after the daughter nuclides (i.e. 214Bi, 214Pb and etc.) of radon makes decay sharply. Based on aerosol sample collected by passing through 1,300 M3 air in 24 h, the lower limit of detection (LLD) of 132I/132Te, 129I/129Te can be decreased from 6.11 × 10−5, 3.46 × 10−4 Bq m−3 after half an hour sampling to 1.64 × 10−5, 8.19 × 10−5 Bq m−3 after sampling 48 h sampling. Similarly, LLD can be decreased from 9.63 × 10−5 to 1.41 × 10−5 Bq m−3 for 131I, 7.72 × 10−5 to 9.96 × 10−6 Bq m−3 for 134Cs and 9.67 × 10−5 to 1.45 × 10−5 Bq m−3 for 137Cs after the same time sampling. In the same time, the activities of daughter nuclides such as 214Pb and 212Bi from the decay of their parent nuclides 222Rn and 220Rn can sharply decrease from 2.45 × 10−2, 2.57 × 10−2 Bq m−3 to be ~10−4 Bq m−3 while the activities of the concerned nuclides 132I/132Te, 129Te, 131I, 134,137Cs were almost constant. As our knowledge, it is the first time to report such case which is very helpful to monitor the leaked nuclides from NPP by aerosol sampling in both normal operation case and emergency case.
Abstract
Non-isothermal crystallization kinetics of the ethylene–acrylic acid copolymer (EAA) in diluents during thermally induced phase separation (TIPS) process was investigated via differential scanning calorimetry (DSC). Dioctyl phthalate (DOP), diphenyl ester (DPE), and peanut oil were used as diluents. Kinetic models, such as Jeziorny theory, Ozawa theory, and Mo’s approach, were utilized for description. The effective activation energy of EAA component in mixture was calculated by Friedman’s method. In the results, the Jeziorny theory and Mo’s approach could obtain good linear fitting relationship with the primary crystallization behavior of EAA, but the Ozawa theory failed to get a suitable result. The homogeneous nucleation of EAA proceeded at the end of liquid–liquid phase separation, while the non-isothermal crystallization developed within a solid–liquid phase separation environment. In the mixtures, the molecular weight, polar groups, and conformation of the diluent molecules would affect the nucleation of EAA, and its growth rate. Comparing with the non-isothermal crystallization of neat EAA, EAA in diluents obtained a higher Avrami index n, and comparatively lower crystallization rate. Peanut oil facilitated the homogeneous nucleation of EAA, leading to a higher melting peak temperature of EAA in the subsequent melting endotherms. The largest EAA’s Avrami index obtained in peanut oil also indicated a higher crystal growth dimensional geometry. The crystallization rate and crystallinity of EAA during the non-isothermal process decreased in the sequence: EAA/DPE > EAA/DOP > EAA/peanut oil.
In this paper a semi-automatic sample applicator made in an ordinary laboratory without help from others is described in detail. All the components of the applicator are available commercially at low cost and the process of assembly of the applicator is very simple and practical, especially the spraying head and the applicator mechanism. Factors that could affect the function of the applicator, for example the type and position of the spraying head, the gas pressure, and the application speed were tested. The type and position of the spraying head have a discernible effect whereas gas pressure does not. The relative standard deviation of band length and band width are <1% and <2.5%, respectively. The errors mainly arise from the clearance of the screw used for transmission of the shaft. The mechanism of the processes affecting band uniformity were researched and are described in detail. The application speed is an important factor, the faster the application speed, the better.
Abstract
The study was aimed to validate and optimize high performance liquid chromatographic (HPLC) method for the determination of coumarin-3-carboxylic acid (C3A) in the heart and liver issue of Sprague-Dawley (SD) rats after intragastric administration of extractive of leaves of Ficus virens var sublanceolata. And simple ADME and target prediction analyses were performed for C3A. Ethyl acetate was employed to precipitate protein with appropriate sensitivity and acceptable matrix effects. The satisfactory separation was developed on an ODS2 column (4.6 mm × 250 mm, 5 μm) by gradient elution with a methanol-acetic acid solution (pH = 3.0) as the mobile phase. The flow rate was 1.0 mL min−1, the column temperature was maintained at 30 ± 2 °C, the injection volume was 20 μL, and the detection wavelength was set as 309 nm. The method was fully validated in terms of selectivity, linearity, accuracy, precision, extraction recovery and stability. The results of the ADME analysis found that C3A has excellent characteristics of drug-likeness, consistent with good bio-absorption. And the predicted 12 target protein belongs to the amine oxidoreductase and carbonic anhydrase target class. This method is simple, rapid, sensitive, and accurate for the determination of coumarin-3-carboxylic acid in the heart and liver tissue of SD rats.
Dauricine is the major bioactive component isolated from the roots of Menispermum dauricum D.C., a bisbenzylisoquinoline alkaloid derivative, and has shown multiple pharmacological properties. In this work, a sensitive and selective ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was developed for determination of dauricine in rat plasma and its application to pharmacokinetic study of dauricine after intravenous and oral administration in rats. After addition of daurisoline as an internal standard (IS), protein precipitation by acetonitrile was used to prepare samples. Chromatographic separation was achieved on a UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm) with 0.1% formic acid and acetonitrile as the mobile phase with gradient elution. An electrospray ionization source was applied and operated in positive ion mode; multiple reactions monitoring (MRM) mode was used for quantification. Calibration plots were linear throughout the range 2–600 ng mL−1 for dauricine in rat plasma. Relative standard deviation (RSD) of intra-day and inter-day precision was less than 13%. The accuracy of the method was between 95.8% and 105.9%. Matrix effect of dauricine in rat plasma ranged from 88.0% to 90.3%. Mean recoveries of dauricine in rat plasma ranged from 91.5% to 95.1%. The method was successfully applied to pharmacokinetic study of dauricine after intravenous and oral administration in rats. The bioavailability of dauricine was found to be 55.4% for the first time.
Abstract
The stability of the inclusion complex of β-CD with cinnamic aldehyde was investigated by means of TG and DSC. The mass loss takes place in three stages: dehydration occurs at 50–120°C; dissociation of β-CD·C9H8O proceeds in the range 200–260°C; and decomposition of β-CD begins at 280°C. The kinetics of the dissociation of β-CD·C9H8O was studied by means of thermogravimetry both at constant temperature and with linearly increasing temperature. The results demonstrate that the dissociation of β-CD·C9H8O is dominated by a one-dimensional diffusion process. The activation energyE is 160 kJ mol−1, and the pre-exponential factorA is 5.8×1014 min−1. Scanning electron microscope observations and the results of crystal structure analysis are in good agreement with those of thermogravimetry.
Abstract
In this study, a gamma–gamma coincidence spectrometry was developed and examined for environmental low-level cosmogenic 22Na monitoring purposes. The spectrometry consists of two bismuth germanate scintillators (BGO) and XIA LLC Digital Gamma Finder (DGF)/Pixie-4 software and card package. The developed spectrometry was optimized according to the considerations of output count rate and gamma peak energy resolution. This spectrometry provides a more sensitive and effective way to quantify even trace amounts of 22Na with critical detection limit of 9 mBq. A sophisticated computer simulation was also created with the goal of obtaining a better understanding of the experimental results and gamma–gamma coincidence efficiencies at different sample geometries.
Abstract
This paper reports on initial efforts for uranium isotopic analysis using gamma-rays and X-ray fluorescence coincidence. In this study, a gamma–gamma coincidence spectrometry was developed. The spectrometry consists of two NaI(Tl) scintillators and XIA LLC Digital Gamma Finder (DGF)/Pixie-4 software and card package. The developed spectrometry was optimized according to the considerations of output count rate and gamma peak energy resolution. It has been demonstrated that the spectrometry provides an effective method of assessing the content of uranium isotopes for nuclear materials. The main advantages of this approach over the conventional gamma spectrometry include the fact that 235U enrichment can be graphically characterized by its unique coincidence “fingerprints”. The method could be further developed for fast uranium isotope verification with an established gamma–gamma coincidence spectral imaging library by various nuclear materials.
