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Abstract  

A novel solid complex, formulated as Ho(PDC)3 (o-phen), has been obtained from the reaction of hydrate holmium chloride, ammonium pyrrolidinedithiocarbamate (APDC) and 1,10-phenanthroline (o-phenH2O) in absolute ethanol, which was characterized by elemental analysis, TG-DTG and IR spectrum. The enthalpy change of the reaction of complex formation from a solution of the reagents, Δr H m θ (sol), and the molar heat capacity of the complex, c m, were determined as being –19.1610.051 kJ mol–1 and 79.2641.218 J mol–1 K–1 at 298.15 K by using an RD-496 III heat conduction microcalorimeter. The enthalpy change of complex formation from the reaction of the reagents in the solid phase, Δr H m θ(s), was calculated as being (23.9810.339) kJ mol–1 on the basis of an appropriate thermochemical cycle and other auxiliary thermodynamic data. The thermodynamics of reaction of formation of the complex was investigated by the reaction in solution at the temperature range of 292.15–301.15 K. The constant-volume combustion energy of the complex, Δc U, was determined as being –16788.467.74 kJ mol–1 by an RBC-II type rotating-bomb calorimeter at 298.15 K. Its standard enthalpy of combustion, Δc H m θ, and standard enthalpy of formation, Δf H m θ, were calculated to be –16803.957.74 and –1115.428.94 kJ mol–1, respectively.

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Abstract  

Solid complexes of M(His)2Cl2 nH2O (M=Mn, Co, Ni, Cu) of MnCl26H2O, CoCl26H2O, NiCl26H2O, CuCl22H2O and L-α-histidine (His) have been prepared in 95% ethanol solution and characterized by elemental analyses, chemical analyses, IR and TG-DTG. The constant-volume combustion energies of the complexes have been determined by a rotating-bomb calorimeter. And the standard enthalpies of formation of the complexes have been calculated as well.

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The sub-acute toxicity of E. faecalis HZNU P2 was investigated in rats fed with different doses for 14 days. To evaluate the acute oral toxicity of E. faecalis HZNU P2, rats were fed with E. faecalis HZNU P2 at a high dose of 2×1011 CFU kg−1 for 10 days. Results showed that there were no abnormal clinical signs in any of the groups during the experiment. There were no significant differences in live weight gain among rats fed with E. faecalis HZNU P2, compared to those in control group. Macroscopic or microscopic examinations of organs revealed no abnormalities, indicating that E. faecalis HZNU P2 did not adversely affect the health of rats. Results of this study demonstrated that digestion of E. faecalis HZNU P2 in rats did not show any obvious signs of toxicity.

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Journal of Thermal Analysis and Calorimetry
Authors: X.-C. Lv, Z.-C. Tan, Z.-A. Li, Y.-S. Li, J. Xing, Q. Shi, and L.-X. Sun

Abstract  

The (R)-BINOL-menthyl dicarbonates, one of the most important compounds in catalytic asymmetric synthesis, was synthesized by a convenient method. The molar heat capacities C p,m of the compound were measured over the temperature range from 80 to 378 K with a small sample automated adiabatic calorimeter. Thermodynamic functions [H TH 298.15] and [S TS 298.15] were derived in the above temperature range with a temperature interval of 5 K. The thermal stability of the substance was investigated by differential scanning calorimeter (DSC) and a thermogravimetric (TG) technique.

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Abstract  

A novel double -diketone 1,6-bis(1-phenyl-3-methyl-5-oxo-pyrazol-4-yl) hexanedione-[1,6] (BPMOPH) was further studied on its coordination compounds with uranium and thorium, respectively. The IR, UV, and1H-NMR spectra were examined, and the proposed structure is discussed.

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Abstract  

A solid complex Eu(C5H8NS2)3(C12H8N2) has been obtained from reaction of hydrous europium chloride with ammonium pyrrolidinedithiocarbamate (APDC) and 1,10-phenanthroline (o-phen⋅H2O) in absolute ethanol. IR spectrum of the complex indicated that Eu3+ in the complex coordinated with sulfur atoms from the APDC and nitrogen atoms from the o-phen. TG-DTG investigation provided the evidence that the title complex was decomposed into EuS. The enthalpy change of the reaction of formation of the complex in ethanol, Δr H m θ(l), as –22.2140.081 kJ mol–1, and the molar heat capacity of the complex, c m, as 61.6760.651 J mol–1 K–1, at 298.15 K were determined by an RD-496 III type microcalorimeter. The enthalpy change of the reaction of formation of the complex in solid, Δr H m θ(s), was calculated as 54.5270.314 kJ mol–1 through a thermochemistry cycle. Based on the thermodynamics and kinetics on the reaction of formation of the complex in ethanol at different temperatures, fundamental parameters, including the activation enthalpy (ΔH θ), the activation entropy (ΔS θ), the activation free energy (ΔG θ), the apparent reaction rate constant (k), the apparent activation energy (E), the pre-exponential constant (A) and the reaction order (n), were obtained. The constant-volume combustion energy of the complex, Δc U, was determined as –16937.889.79 kJ mol–1 by an RBC-II type rotating-bomb calorimeter at 298.15 K. Its standard enthalpy of combustion, Δc H m θ, and standard enthalpy of formation, Δf H m θ, were calculated to be –16953.379.79 and –1708.2310.69 kJ mol–1, respectively.

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Abstract  

The heat capacities of 2-benzoylpyridine were measured with an automated adiabatic calorimeter over the temperature range from 80 to 340 K. The melting point, molar enthalpy, Δfus H m, and entropy, Δfus S m, of fusion of this compound were determined to be 316.49±0.04 K, 20.91±0.03 kJ mol–1 and 66.07±0.05 J mol–1 K–1, respectively. The purity of the compound was calculated to be 99.60 mol% by using the fractional melting technique. The thermodynamic functions (H TH 298.15) and (S TS 298.15) were calculated based on the heat capacity measurements in the temperature range of 80–340 K with an interval of 5 K. The thermal properties of the compound were further investigated by differential scanning calorimetry (DSC). From the DSC curve, the temperature corresponding to the maximum evaporation rate, the molar enthalpy and entropy of evaporation were determined to be 556.3±0.1 K, 51.3±0.2 kJ mol–1 and 92.2±0.4 J K–1 mol–1, respectively, under the experimental conditions.

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Abstract  

The molar heat capacities C p,m of 2,2-dimethyl-1,3-propanediol were measured in the temperature range from 78 to 410 K by means of a small sample automated adiabatic calorimeter. A solid-solid and a solid-liquid phase transitions were found at T-314.304 and 402.402 K, respectively, from the experimental C p-T curve. The molar enthalpies and entropies of these transitions were determined to be 14.78 kJ mol−1, 47.01 J K−1 mol for the solid-solid transition and 7.518 kJ mol−1, 18.68 J K−1 mol−1 for the solid-liquid transition, respectively. The dependence of heat capacity on the temperature was fitted to the following polynomial equations with least square method. In the temperature range of 80 to 310 K, C p,m/(J K−1 mol−1)=117.72+58.8022x+3.0964x 2+6.87363x 3−13.922x 4+9.8889x 5+16.195x 6; x=[(T/K)−195]/115. In the temperature range of 325 to 395 K, C p,m/(J K−1 mol−1)=290.74+22.767x−0.6247x 2−0.8716x 3−4.0159x 4−0.2878x 5+1.7244x 6; x=[(T/K)−360]/35. The thermodynamic functions H TH 298.15 and S TS 298.15, were derived from the heat capacity data in the temperature range of 80 to 410 K with an interval of 5 K. The thermostability of the compound was further tested by DSC and TG measurements. The results were in agreement with those obtained by adiabatic calorimetry.

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Abstract  

A novel gelling method was studied to stabilize phase change material Na2HPO4 · 12H2O with amylose grafted sodium acrylate. Gelled Na2HPO4 · 12H2O shows stable heat storage performance prepared at optimized conditions: 2.7mass/mass% sodium acrylate, 0.4 mass/mass% amylose, 0.05–0.09 mass/mass% N, N′-methylenebisacrylamide, 0.05–0.09 mass/mass% K2S2O8 and Na2SO3 (mass ratio 1:1), at 50 °C. Na2HPO4 · 12H2O was dispersed in gel network as tiny crystals less than 0.1 mm. Melting points were in the range 35.4 ± 2 °C. Short-term thermal cycling proves the effectiveness of the novel method for eliminating phase separation in the gelled salt. Adiabatic calorimetric measurement of heat capacities shows two phase transitions, which correspond to melting of Na2HPO4 · 12H2O and freezable bond water in gel, respectively. Heat of fusion of pure Na2HPO4 · 12H2O was determined as 260.9 J g−1. Distribution of extra water is: free water:freezable water:nonfreezing water = 0:0.85:0.15.

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High-performance liquid chromatography-mass spectrometry (HPLC-MS) method coupled with radical reaction for screening active ingredients from perennial fujimoto bean whole herb was established. The active ingredients, present in perennial fujimoto bean whole herb, possess scavenging effects towards 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical, superoxide, peroxy radical, and hydroxyl radical. The radical scavenging abilities of these active ingredients were evaluated based on the relative peak areas in the HPLC chromatogram. The results indicate that potent antioxidants are present in the anhydrous methanol extract of perennial fujimoto bean whole herb. Based on HPLC-MS analysis, it was found that the scavenging ability can be mostly attributed to the presence of three compounds: cyanidin-3-o-β-d-glucopyranoside, troxerutin, and rutin. The structures were identified based on the MS and nuclear magnetic resonance (NMR) data. Free radical scavenging activity decreased in the following order: troxerutin > rutin > cyanidin-3-o-β-d-glucopyranoside.

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