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Abstract

The hydration heat of pure cement, fly ash single-doped cement, as well as fly ash and fluorgypsum co-doped cement were investigated by means of micro-calorimetry with an eight-channel micro-calorimeter. The results showed that the hydration heat and the hydration rate could be reduced significantly by fly ash and fluorgypsum. However, the reduction was not proportional to the loading of dopant. The exothermic peak of the co-doped cement was appeared earlier than that of the single-doped cement. As the temperature decreased, the hydration heat and the hydration rate of both the doped cement were reduced, and the exothermic peak appeared later. The effect of fly ash and fluorgypsum on the compressive strength of cement was also investigated. The results revealed that the early compressive strength of concrete made up of the co-doped cement was largely higher than that of the single-doped cement. Based on the experiment results obtained in this article, we could conclude that fluorgypsum is a suitable additive for the single-doped cement.

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Abstract

A new potential enantioselective catalyst derived from ferrocene, 1-{(R)-1-[(S)-2-(diphenylphosphino)ferrocenyl]ethyl}-benzimidazole (DPFEB), was prepared and its absolute structure was characterized by means of single crystal X-ray diffraction. The molar heat capacity of DPFEB was measured by means of temperature modulated differential scanning calorimetry over the temperature range of 200–530 K, and the thermodynamic functions of [H TH 298.15] and [S TS 298.15] were calculated. Further more, thermogravimetry experiment revealed that DPFEB exhibited a three step thermal decomposition process with the final residual of 28.7%.

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Journal of Thermal Analysis and Calorimetry
Authors: Ju-Lan Zeng, Sai-Bo Yu, Bo Tong, Li-Xian Sun, Zhi-Cheng Tan, Zhong Cao, Dao-Wu Yang, and Jing-Nan Zhang

Abstract

An N-tert-butyloxycarbonylated organic synthesis intermediate, (S)-tert-butyl 1-phenylethylcarbamate, was prepared and investigated by means of differential scanning calorimetry (DSC) and thermogravimetry (TG). The molar heat capacities of (S)-tert-butyl 1-phenylethylcarbamate were precisely determined by means of adiabatic calorimetry over the temperature range of 80-380 K. There was a solid–liquid phase transition exhibited during the heating process with the melting point of 359.53 K. The molar enthalpy and entropy of this transition were determined to be 29.73 kJ mol−1 and 82.68 J K−1 mol−1 based on the experimental C pT curve, respectively. The thermodynamic functions, [ ] and [ ], were calculated from the heat capacity data in the temperature range of 80–380 K with an interval of 5 K. TG experiment showed that the pyrolysis of the compound was started at the temperature of 385 K and terminated at 510 K within one step.

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Journal of Thermal Analysis and Calorimetry
Authors: Li-Fang Song, Chun-Hong Jiang, Jian Zhang, Li-Xian Sun, Fen Xu, Wan-Sheng You, Yi Zhao, Zhi-Heng Zhang, Mei-Han Wang, Yutake Sawada, Zhong Cao, and Ju-Lan Zeng

Abstract  

A novel metal-organic frameworks [Cu2(OH)(2,2′-bpy)2(BTC) · 2H2O]n (CuMOF, BTC = benzene-1,3,5-tricarboxylic acid, 2,2′-bpy = 2,2′-bipyridine) has been synthesized hydrothermally and characterized by single crystal XRD, FT-IR spectra. The low-temperature molar heat capacities were measured by temperature modulated differential scanning calorimetry (TMDSC) for the first time. The thermodynamic parameters such as entropy and enthalpy relative to reference temperature 298.15 K were derived based on the above molar heat capacity data. Moreover, the thermal stability and the decomposition mechanism of CuMOF were investigated by TG-MS (thermogravimetry-mass spectrometer). A four-stage mass loss was observed in the TG curve. MS curve indicated that the gas products for oxidative degradation of CuMOF were H2O, CO2, NO and NO2.

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Journal of Thermal Analysis and Calorimetry
Authors: Chun-Hong Jiang, Li-Fang Song, Jian Zhang, Li-Xian Sun, Fen Xu, Fen Li, Qing-Zhu Jiao, Zhen-Gang Sun, Yong-Heng Xing, Yong Du, Ju-Lan Zeng, and Zhong Cao

Abstract

A novel metal organic framework [Co (BTC)1/3 (DMF) (HCOO)]n (CoMOF, BTC = 1,3,5-benzene tricarboxylate, DMF = N,N-dimethylformamide) has been synthesized solvothermally and characterized by single crystal X-ray diffraction, X-ray powder diffraction, and FT-IR spectra. The molar heat capacity of the compound was measured by modulated differential scanning calorimetry (MDSC) over the temperature range from 198 to 418 K for the first time. The thermodynamic parameters such as entropy and enthalpy versus 298.15 K based on the above molar heat capacity were calculated. Moreover, a four-step sequential thermal decomposition mechanism for the CoMOF was investigated through the thermogravimetry and mass spectrometer analysis (TG-DTG-MS) from 300 to 800 K. The apparent activation energy of the first decomposition step of the compound was calculated by the Kissinger method using experimental data of TG analysis.

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