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  • Author or Editor: X.L. Liu x
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Abstract  

Carburization and coke deposition of unsupported and carbon-supported Fe, Mo and Fe−Mo catalysts in syngas have been studied using thermogravimetry. Compositions of the carbides formed are evaluated on the basis of the amount of metals in the catalysts and amount of carbon deposited during carburization. It is shown that carburization temperature and the nature of the carbides formed (Fe5C2 and Fe2C for iron and Mo2C for molybdenum) depend on the metals but are influenced by the support and metal loading. Coke deposition on these catalysts takes place as soon as carburization is complete.

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Abstract  

The catalytic performance of unsupported and carbon-supported Fe, Mo and Fe−Mo catalysts for Fischer-Tropsch synthesis is greatly influenced by the final reduction states of the catalysts. In this investigation, the reduction process of the catalysts by H2 was studied by using TG-DTG. The reduction process depends not only on the reducibility of metals but also on the nature of the support. Methanation of the support occurred as soon as the supported metals were completely reduced for the carbon-supported catalysts. For these, the reduction temperature should by carefully selected so that the metal oxides are reduced as completely as possible, whilst the methanation of the support must be avoided to obtain optimum reduced catalysts.

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Summary

Rapid high-performance liquid chromatographic methods with evaporative light scattering detection (HPLC-ELSD) and electrospray ionization multistage mass spectrometry (HPLC-ESI-MSn) have been established and validated for simultaneous qualitative and quantitative analysis of eight steroidal saponins in ten batches of Gongxuening capsule (GXN), a widely commercially available traditional Chinese preparation. The optimum chromatographic conditions entailed use of a Kromasil C18 column with acetonitrile-water (30:70 to 62:38, υ/υ) as mobile phase at a flow rate of 1.0 mL min−1. The drift tube temperature of the ELSD was 102°C and the nebulizing gas flow rate was 2.8 L min−1. Separation was successfully achieved within 25 min. LC-ESI-MSn was used for unequivocal identification of the constituents of the samples by comparison with reference compounds. The assay was fully validated for precision, repeatability, accuracy, and stability, then successfully applied to quantification of the eight compounds in samples. The method could be effective for evaluation of the clinical safety and efficacy of GXN.

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Abstract  

The isoquinoline alkaloids were isolated from traditional Chinese drugs of Phellodendri Cortex, Radix Stephaniae Tetrandrae, Corydalis Yanhusuo and Corydalis Bungeana. The power-time curves of growth of E. coli at different concentrations of isoquinoline alkaloid at 37�C were determined by a 2277 Thermal Activity Monitor. The rate constant of bacteriostastic activity was calculated. The relationship between growth rate constant and concentration was established. The optimum bacteriostastic concentration was determined. Experimental results have indicated that all the isoquinoline alkaloids isolated from the four kinds of traditional Chinese drugs have bacteriostastic activity and the order is Phellodendri Cortex>Radix Stephaniae Tetrandrae>Corydalis Yanhusuo>Corydalis Bungeana.

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Abstract  

The thermal decomposition of strontium acetate hemihydrate has been studied by TG-DTA/DSC and TG coupled with Fourier transform infrared spectroscopy (FTIR) under non-isothermal conditions in nitrogen gas from ambient temperature to 600°C. The TG-DTA/DSC experiments indicate the decomposition goes mainly through two steps: the dehydration and the subsequent decomposition of anhydrous strontium acetate into strontium carbonate. TG-FTIR analysis of the evolved products from the non-oxidative thermal degradation indicates mainly the release of water, acetone and carbon dioxide. The model-free isoconversional methods are employed to calculate the E a of both steps at different conversion α from 0.1 to 0.9 with increment of 0.05. The relative constant apparent E a values during dehydration (0.5<α<0.9) of strontium acetate hemihydrate and decomposition of anhydrous strontium acetate (0.5<α<0.9) suggest that the simplex reactions involved in the corresponding thermal events. The most probable kinetic models during dehydration and decomposition have been estimated by means of the master plots method.

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Abstract  

The exfoliated poly(vinyl chloride) (PVC)/montmorillonite (MMT) nanocomposites were synthesized by in situ intercalated polymerization of vinyl chloride (VC) in the presence of organic-intercalated montmorillonite (OMMT). Their structures and thermal properties were characterized. The results showed that layered silicates are well exfoliated and uniformly distributed in PVC matrix during in situ intercalated polymerization of VC in the presence of OMMT. The glass transition temperatures of PVC phases in the PVC/MMT nanocomposites are all lower than that of pristine PVC due to the incorporation of the exfoliated silicate layers in PVC matrix. The 5% mass loss temperature (T 5%), the dehydrochlorination temperature (T max1) of the PVC matrix decreased due to the free and interlayer water in MMT, the low thermal stability, and the enhanced dehydrochlorination of the PVC matrix by alkyl ammonium pre-treated MMT. However, the thermal decomposition temperature of the dehydrochlorinated PVC (T max2) and char at 600C are slightly increased in the presence of silicate layers.

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Summary

A simple hydrolysis method has been developed for determination of phenylethanoid glycosides in Lamiophlomis rotata (L.R.). Different kinds of phenylethanoid glycosides were hydrolyzed in hydrochloric acid solution to produce corresponding phenethyl alcohols and cinnamic acids, mainly containing hydroxytyrosol, homovanillyl alcohol, 3,4-dimethoxyphenethyl alcohol, caffeic acid, fumalic acid and 3,4-dimethoxycinnamic acid. The six analytes could be determined simultaneously by high-performance liquid chromatography (HPLC). The effects of mobile phase, pH and concentration of running buffer, detection wavelength, flow rate and injection volume were also investigated. Under the optimum conditions, the six hydrolyzates could be perfectly separated within 45 min. The response was linear over four orders of magnitude with detection limits (S/N = 3) ranging from 1 × 10−8 to 1.5 × 10−4 mol L−1 for the analytes. The method has been successfully applied to the analysis of real sample Du-Yi-Wei capsule and Qi-Zheng-Yan-Tong patch, with satisfactory results.

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Abstract  

A solid complex of rare-earth compounds with alanine, [ErY(Ala)4(H2O)8](ClO4)6 (Ala=alanine), was synthesized, and a calorimetric study and thermal analysis for it was performed through adiabatic calorimetry and thermogravimetry. The low-temperature heat capacity of [ErY(Ala)4(H2O)8](ClO4)6 was measured with an automated adiabatic precision calorimeter over the temperature range from 78 to 377 K. A solid-solid phase transition was found between 99 and 121 K with a peak temperature at 115.78 k. The enthalpy and entropy of the phase transition was determined to be 1.957 Kj mol-1, 16.90 j mol-1 k-1, respectively. Thermal decomposition of the complex was investigated in the temperature range of 40~550C by use of the thermogravimetric and differential thermogravimetric (TG/DTG) analysis techniques. The TG/DTG curves showed that the decomposition started from 120 and ended at 430C, completed in three steps. A possible mechanism of the thermal decomposition was elucidated.

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Abstract  

A new model has been deduced by assumed autocatalytic reactions. It includes two rate constants, k 1 and k 2, two reaction orders, m and n, and the initial concentration of [OH]. The model proposed has been applied to the curing reaction of a system of bisphenol-S epoxy resin (BPSER), with4,4'-diaminodiphenylmethane (DDM) as a curing agent. The curing reactions were studied by means of differential scanning calorimetry (DSC). Analysis of DSC data indicated that an autocatalytic behavior showed in the curing reaction. The new model was found to fit to the experimental data exactly. Rate constants, k 1 and k 2 were observed to be greater when curing temperature increased. The activation energies for k 1 and k 2 were 95.28 and 39.69 kJ mol–1, respectively. Diffusion control was incorporated to describe the cure in the latter stages.

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Summary  

Accelerator mass spectrometry (AMS) is an ultra-sensitive method to monitor and trace the environmental exposure levels of 14C-labeled molecules in vivo. Nicotine [3-(1-methyl-2-pyrrolidinyl)-pyridine], a major alkaloid in tobacco products, has proven to be a potential genotoxic compound. Using 14C-labeled nicotine and AMS, we have investigated the inhibitory effect of curcumin, garlic squeeze, grapeseed extract, tea polyphenols, vitamin C and vitamin E, respectively, on nicotine-hemoglobin (Hb) adduction in vivo. The results demonstrated that these dietary constituents induced remarkable decrease of nicotine-Hb adducts. The inhibitory fact may afford an important clue of the chemoprevention of the potential nicotine-induced carcinogenesis.

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