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Abstract  

The complexes of rare earth bromides with alanine, REBr33AlanH2O (RE=Ce, Pr, Sm, Eu, Gd and Tb, n=3; RE=Dy and Y, n=2.5 Ala=alanine), were prepared and characterized by means of chemical analysis, elemental analysis, molar conductivity, thermogravimetry, IR spectra and X-ray diffraction. The thermal decomposition in N2 of these complexes was studied by means of TG-DTG techniques from ambient temperature to 1000C. During heating, the hydrated complexes of Ce, Pr and Y lose waters in one step, but the hydrated complexes of Sm, Eu, Gd, Tb and Dy lose waters in two steps. Then anhydrous complexes lose 2.5 alanine molecules except the complexes of Eu which lose three alanine molecules. Apparently, only be complex of Eu has an intermediate, EuOBr. All complexes finally decompose to oxides.

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Abstract

The purpose of this study is to simulate the early age concrete behaviors and evaluate the cracking risk with the thermal and thermal stress analysis. A new finite element method program associated with ANSYS program is developed for the computation of thermal field and thermal stress field for early age concrete considering the following characters: degree of hydration, thermal properties (such as specific heat, thermal diffusivity), thermal boundary conditions, and mechanical properties (such as shrinkage, creep) which occur at early age. The results from simulation compared with experimental values found in the literature show a good agreement. Finally, based on this user-developed subroutine, the effects of hydration heat, ambient temperature, wind velocity, shrinkage, and length-height ratio on cracking risk were analyzed for a concrete wall which is one part of the structure of Maridal culvert in Norway. By which, the measures to control the cracking were provided for the engineering application.

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Abstract

A heterogeneous photo-Fenton catalyst was prepared using the complex tris(1,10)-phenanthroline iron(II) loaded on the NaY type of zeolite. The catalyst displayed a feature of the photo-Fenton degradation of methylene blue, and a linear relationship between ln(C0/Ct) and reaction time was obtained, indicating the kinetic characteristics of a pseudo first-order reaction. The repeated cyclic experiments showed that the heterogeneous catalyst was stable and recoverable. Compared with the traditional homogeneous Fenton reagent, the heterogeneous catalyst has the advantage in the neutral or weakly basic medium used because the active component tris(1,10)-phenanthroline iron(II) is a stable chelate compound. The photo-Fenton degradation pathway for methylene blue was given based on the mass spectral data.

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Journal of Thermal Analysis and Calorimetry
Authors: Li Bai Xiao, Xiao Ling Xing, Xue Zhong Fan, Feng Qi Zhao, Zhi Ming Zhou, Hai Feng Huang, Ting An, Hai Xia Hao, and Qing Pei

Abstract

The enthalpies of dissolution for di(N,N-di(2,4,6,-trinitrophenyl)amino)-ethylenediamine (DTAED) in dimethyl sulfoxide (DMSO) and N-methyl pyrrolidone (NMP) were measured using a RD496-2000 Calvet microcalorimeter at 298.15 K. Empirical formulae for the calculation of the enthalpies of dissolution (Δdiss H) were obtained from the experimental data of the dissolution processes of DTAED in DMSO and NMP. The linear relationships between the rate (k) and the amount of substance (a) were found. The corresponding kinetic equations describing the two dissolution processes were for the dissolution of DTAED in DMSO, and for the dissolution of DTAED in NMP, respectively.

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Journal of Radioanalytical and Nuclear Chemistry
Authors: Yalan Liu, Liyong Yuan, Yali Yuan, Jianhui Lan, Zijie Li, Yixiao Feng, Yuliang Zhao, Zhifang Chai, and Weiqun Shi

Abstract  

Uranium is one of the most hazardous heavy metal due to its long half-life radioactivity, high toxicity and mobility as aqueous uranyl ion (UO2 2+) under ordinary environmental conditions. Herein, amino functionalized SBA-15 (APSS) was developed as a rapid and efficient sorbent for removal of U(VI) from the environment. The APSS sample was synthesized by grafting method and was characterized by SEM, NMR, SAXS, and N2 sorption/desorption isothermal experiments. The sorption of U(VI) by APSS was investigated under different conditions of pH, contact time, initial U(VI) concentration, ionic strength and solid–liquid ratio. The results show that the sorption of U(VI) by APSS is strongly dependent on pH but independent of ionic strength and solid–liquid ratios (m/V). The sorption is ultrafast with an equilibrium time of less than 30 min, and the sorption capacity is as large as 409 mg/g at pH 5.3 ± 0.1. Besides, the U(VI) sorption by APSS from extremely diluted solution and the desorption of U(VI) from APSS were also studied. It is found that 100 mg of APSS can almost completely remove the U(VI) ions from 4 L aqueous solution with the U(VI) concentration as low as 4.2 ppb and the sorbed U(VI) can be completely desorbed by 0.1 mol/L nitric acid. The results strongly reveal the high performance of the APSS material in the removal and preconcentration of U(VI) from the aqueous solution.

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Abstract  

The thermal decomposition mechanism of hydrazine 3-nitro-1,2,4-triazol-5-one (HNTO) compound was studied by means of differential scanning calorimetry (DSC), thermogravimetry and derivative thermogravimetry (TG-DTG), and the coupled simultaneous techniques of in situ thermolysis cell with rapid scan Fourier transform infrared spectroscopy (in situ thermolysis/RSFTIR). The thermal decomposition mechanism is proposed. The quantum chemical calculation on HNTO was carried out at B3LYP level with 6-31G+(d) basis set. The results show that HNTO has two exothermic decomposition reaction stages: nitryl group break first away from HNTO molecule, then hydrazine group break almost simultaneously away with carbonyl group, accompanying azole ring breaking in the first stage, and the reciprocity of fragments generated from the decomposition reaction is appeared in the second one. The C–N bond strength sequence in the pentabasic ring (shown in Scheme 1) can be obtained from the quantum chemical calculation as: C3–N4 > N2–C3 > N4–C5 > N1–C5. The weakest bond in NTO is N7–C3. N11–N4 bond strength is almost equal to N4–C5. The theoretic calculation is in agreement with that of the thermal decomposition experiment.

Scheme 1 
Scheme 1 

Scheme of HNTO

Citation: Journal of Thermal Analysis and Calorimetry 100, 2; 10.1007/s10973-009-0416-6

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Abstract

A novel energetic material, 4,5-dihydroxyl-2-(dinitromethylene)-imidazolidine (DDNI), was synthesized by the reaction of FOX-7 and glyoxal in water at 70 °C. Thermal behavior of DDNI was studied with DSC and TG-DTG methods, and presents only an intense exothermic decomposition process. The apparent activation energy and pre-exponential factor of the decomposition reaction were 286.0 kJ mol−1 and 1031.16 s−1, respectively. The critical temperature of thermal explosion of DDNI is 183.78 °C. Specific heat capacity of DDNI was studied with micro-DSC method and theoretical calculation method, and the molar heat capacity is 217.76 J mol−1 K−1 at 298.15 K. The adiabatic time-to-explosion was also calculated to be a certain value between 14.54 and 16.34 s. DDNI presents lower thermal stability, for its two ortho-hydroxyl groups, and its thermal decomposition process becomes quite intense.

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A double-development TLC method has been developed for simultaneous qualitative and quantitative analysis of hydrophilic and lipophilic constituents of Salvia miltiorrhiza (Danshen). The optimized mobile phases dichloromethane-ethyl acetate-formic acid 22:24:10 (ν/ν) and petroleum ether-ethyl acetate-cyclohexane 25:11:14 (ν/ν) were used for the double development on nano-silica gel 60F254 plates. Their characteristic TLC profiles were observed under UV light at 254 and 365 nm and the bands were then revealed by reaction with 5% H2SO4 in EtOH. Quantification of twelve compounds was achieved by densitometry at 260 or 290 nm, with reference at 400 nm. Linearity was quite good (R 2 > 0.99) within the ranges tested. This method could be used for quality control of Danshen.

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Acta Chromatographica
Authors: Feng Wu, Xiuli Zhao, Shumin Wang, Hui Zhou, Shaojie Guo, Siyang Ni, Bo Yang, Lihua Zhang, and Xinde Xu

The aim of this study was to develop and validate a HPLC-MS/MS assay to determine the lutein concentration in plasma samples of human and SD rats. Organic solvent was used for lutein extraction. The extract was injected into a HPLC-MS/MS system. Reversed phase chromatography was performed on a C18 column in gradient mode. Lutein and internal standard (phenytoin sodium) were identified in atmospheric pressure chemical ionization mode using ion transitions of m/z 567.5>549.4 and 205.2>110.8, respectively. The lutein quantification assay was linear over concentrations ranging from 4 to 500 ng/mL. The lower limit of quantification was 4 ng/mL with satisfactory precision and accuracy. The assay presented acceptable intra and inter-batch precision (RSD%) and accuracy (RE%) <8.16% in SD rat plasma and <12.80% in human plasma. The extraction recovery ranged from 50.94 to 60.90% in SD rat plasma and 68.73% in human plasma. The matrix effect for lutein was acceptable and had minimal influence on the results. The method was then applied to determine the lutein concentrations in human plasma after a single oral dose of 20mg lutein. The method described is rapid, selective, sensitive and reproducible. This method can be used for both pharmacokinetic studies and therapeutic drug monitoring purposes.

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Abstract  

To investigate the effects of lanthanum exposure on regional distribution of inorganic elements in rat brain. Wistar rats were exposed to lanthanum chloride through oral administration at 0, 0.1, 2, and 40 mg/kg concentration for 6 months. The elements such as Cl, K, Ca, Fe, Cu, and Zn were identified in the brain slices by synchrotron radiation X-ray fluorescence (SRXRF) analysis. Differences of brain elemental distributions were noticed. Cl, Ca, and Zn were primarily concentrated in hippocampus of the controls. With the increase of the lanthanum dosage, the Ca and Zn levels significantly decreased, while the Cu levels significantly elevated in cortex, hippocampus and thalamus. Our results suggest that subchronic lanthanum exposure in rats appears to change elemental distributions in brain.

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