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  • Author or Editor: L. Zhu x
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Abstract  

A novel method that spent nuclear fuel is converted into nitrates with N2O4, and then nitrates are extracted with TBP in supercritical CO2 (SC-CO2), has been developed for reprocessing of spent nuclear fuel, which has a potential prospect because of its potential to decrease generation of the secondary liquid waste. In this paper, conversion of Nd2O3 with N2O4 into its nitrate under various conditions and extraction of the conversion product with TBP in SC-CO2 were investigated. When temperature was 60–120 °C, the molar ratio of H2O to Nd2O3 was from 1 to 6, and molar ratio of N2O4 to Nd2O3 was above 8, complete conversion of Nd2O3 into its nitrate was achieved. The conversion product was characterized by thermal analysis (TG-DTA), X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FT-IR) and Raman spectroscopy. Quantitative extraction of the conversion product with TBP in supercritical CO2 was also achieved under experimental conditions.

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Abstract  

Thermal, chemical and rheological properties of ultraviolet aged asphalt binder were characterized by differential scanning calorimetry (DSC), Fourier transform infrared (FTIR) and dynamic shear rheometer (DSR), respectively. Asphalt binder samples were made with different film thickness (50, 100, 200 and 500 μm) and suffered different ageing time (0, 48, 96 and 144 h), at a certain UV radiant intensity of 20 w m–2 in a self-made accelerated ageing oven. The results indicate that the UV light ageing would lead to the improvement of thermal behavior and the growth of the glass transition temperature of asphalt binder. This type of ageing can be also reflected from the FTIR spectra in terms of the characteristic peaks of the carbonyl groups and sulphoxides. The UV light ageing can change some rheological parameters of asphalt binder, such as complex modulus and phase angle. The ageing degrees of asphalt binder by this type of ageing test are mainly related to the ageing time and film thickness of the sample.

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Abstract  

To develop potential new Tc radiopharmaceuticals, a novel compound [99mTc(CO)2(NO)(EHIDA)]0 (EHIDA: 2,6-diethylphenylcarbamoylmethyliminodiacetic acid) has been prepared by reacting [99mTc(CO)3)(EHIDA)] with NOBF4 both in water and acetonitrile. The conversion of [99mTc(CO)3)(EHIDA)] to [99mTc(CO)2(NO)(EHIDA)]0 was supported by TLC, HPLC and eletrophoresis. The radiochemical purity (more than 99%) was proved by TLC and HPLC. The biodistribution in mice demonstrated that [Tc(CO)2(NO)(EHIDA)]0 showed higher uptake in blood, kidney and lung (15 min, blood: 19.24±2.95; kidney: 13.61±3.49; lung: 10.81±1.09.) but a lower uptake in liver (15 min, 5.73±0.74). The slower clearances (120 min, blood: 12.75±1.34; kidney: 13.61±3.49) from blood and kidney were also found. This research describes two methods for the conversion of [99mTc(CO)3]+ into [99mTc(CO)2)(NO)]2+ by using NOBF4 as the source of NO+ both in organic solvent and water. The latter method offers the possibility to introduce the NO-group in high yield in water.

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Abstract  

The dilution enthalpies of D-mannitol and D-sorbitol in aqueous sodium chloride solution at various concentrations have been determined by isothermal microcalorimetry at 298.15 K. The homogeneous enthalpic interaction coefficients over a quite large range of concentration of aqueous sodium chloride solutions have been calculated according to the excess enthalpy concept. The results show that enthalpic pairwise interaction coefficients (h 2) of D-mannitol and D-sorbitol are positive in aqueous sodium chloride solution and become more positive with increase of the concentration of sodium chloride. The results are interpreted in terms of the different conformations of the two polyols, solute-solute and solute-solvent interactions involved by solvent effects.

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Abstract  

Uniformly carbon-covered alumina (CCA) was prepared via the carbonisation of sucrose highly dispersed on the alumina surface. Using special thermogravimetry and sorptometry methods physicochemical properties of carbon-covered alumina surfaces were investigated. A numerical and analytical procedure for the evaluation of total heterogeneous properties (desorption energy distribution and pore-size distribution functions) on the basis of liquid thermodesorption from the sample surfaces under the quasi-equilibrium conditions are presented. The desorption energy distribution was derived from the mass loss Q-TG and the differential mass loss Q-DTG curves of thermodesorption of pre-adsorbed polar and apolar liquid films. For the first time, the evaluation of the fractal dimensions of carbon-covered alumina using the sorptometry, thermogravimetry and AFM data is presented.

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Novel magnetic solid-phase extraction using carboxylated multiwalled carbon nanotubes was proposed with ultra high-performance liquid chromatography–tandem mass spectrometry for the determination of silodosin in biological samples. The effects of various experimental parameters including adsorbent amount, pH, adsorption time, desorption conditions, and adsorbent reusability were systematically validated. Under the optimized conditions, the calibration curve was linear within the concentration range of 1.0–800 ng mL−1 with the correlation coefficient of 0.9997 and the lower limit of detection was 0.3 ng mL−1. The extraction recoveries were over 90.0% with relative standard deviation (RSD) of less than 5.0%. All these results suggested that magnetic extraction method can be used for enrichment and quantification of silodosin in biological samples.

Open access

Epimedium pubescens Maxim. and Epimedium koreanum Nakai. are two common and confused species of Herba Epimedii in Chinese Pharmacopoeia 2010 edition. Different species and growing conditions lead to chemical differences between the two species which may result in the improper clinical usage. In this work, a new method based on rapid-resolution liquid chromatography combined with time-of-flight mass spectrometry (RRLC/TOFMS) has been developed for identification and differentiation of major flavonoids in two kinds of Epimedium extract and rat plasma. The compounds were identified effectively based on the accurate extract masses and formulae acquired by RRLC/TOFMS. The fragmentation rules deduced by collision-induced dissociation (CID) were successfully implemented in distinguishing some of the isomers, further validating the results. By using the combined analytical techniques, a total of 40 major flavonoids in extracts of two kinds of Epimedium were identified within 30 min, including 31 common components and 9 characteristic components. After oral administration, three prototype compounds in rat plasma were detected by comparing the constituents measured in vitro with those in vivo, and five metabolites were identified by contrasting the fragmentation rules. The identification and structural elucidation of the chemical constituents provided essential data for further pharmacological and clinical studies on different species of Epimedium.

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Abstract  

Thermogravimetry (TG) was employed to study the thermal degradation kinetics of poly(etherketone/sulfone)ethylimide (PEK-IE and PES-IE). The corresponding decomposition activation energies and reaction orders were obtained and the comparison was made with their parent polymerspoly(ether-ketone/sulfone) with Cardo group (PEK-C and PES-C). The results show that the degradation activation energies of PEK-IE and PES-IE were lower than that of PEK-C and PES-C; and two stages of the degradation process were found for all the four polymers. For PEK-IE and PES-IE, the activation energies in the first decomposition stage are much lower than that in the second stage and the two stages can be taken as slow induction and fast degradation, whereas for PEK-C and PES-C the activation energies in the first decomposition stage are larger than that in the second stage, and the two stages can both be taken as two fast degradation stages. The decomposition mechanism of the two stages was also speculated.

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Traditional Chinese medicine (TCM) has been widely used in many countries for thousands of years and played an indispensable role in the prevention and treatment of diseases, especially the complicated and chronic ones. However, the application of TCM in diseases is still not fully recognized by people around the world, the main reason is that Chinese herb is a very complex mixture containing hundreds of different components. Thus, it is essential to make quality control and evaluation of TCM. A new quality evaluation method, quantitative analysis of multi-components by single marker (QAMS), was developed to the quality control of alkaloids in TCM, a case study on Radix aconiti lateralis, named Fuzi in Chinese. Six alkaloids, including aconitine, hypaconitine, mesaconitine, benzoylaconine, benzoylmesaconine, and benzoylhypaconine, were selected as main components to evaluate the quality of Radix aconiti lateralis. The feasibility and accuracy of QAMS were checked by the external standard method, and various high-performance liquid chromatographic instruments and chromatographic conditions were investigated to verify its applicability. Using aconitine as the internal reference substance and the content of aconitine was calculated according to relative correction factors by high-performance liquid chromatography. The present results showed that there was no significant difference observed between the QAMS method and the external standard method with the relative average deviations less than 3.0%, and QAMS is an effective way to control the quality of herbal medicines and seems to be a convenient and accurate approach to analyze multi-composition when reference substances are unavailable.

Open access