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Journal of Thermal Analysis and Calorimetry
Authors:
Hong-Ling Li
,
Koichi Takahashi
,
Yusuke Ujihira
,
Mariko Ishiwatari
,
Kurima Kobayashi
,
Takahiko Iriyama
, and
Tokuzo Konishi

Abstract  

The Mössbauer spectra of Sm2Fe17Nx, prepared by the nitrogenation of Sm2Fe17 powders in an ammonia and hydrogen atmosphere, were observed at elevated temperatures to shed light on the thermal behavior of nitrogen in the compounds Sm2Fe17Nx. It was found that there were large differences in thermal behavior between the starting Sm2Fe17, crystalline Sm2Fe17Nx (x≈1.7) and amorphous Sm2Fe17Nx(x∼7). The thermal decomposition behavior of Sm2Fe17N3.2, developed as one of the most promising hard magnetic materials, was found to be different under different atmospheres.

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Abstract  

A series of lanthanum-promoted Pd/Al2O3 catalysts (Pd/La x –Al2O3), for the liquid phase in situ hydrogenation of phenol into cyclohexanone, was prepared by the incipient wetness impregnation method. Addition of lanthanum to Pd/Al2O3 enhances the TOF of the catalyst for the liquid phase in situ hydrogenation of phenol significantly. The conversion of phenol is highly dependent upon the atomic ratio of La/Pd, but the presence of lanthanum has little effect on the selectivity of cyclohexanone. The selectivity of cyclohexanone in the liquid phase in situ hydrogenation of phenol over the Pd/La x –Al2O3 catalyst is as high as 98%, which is quite higher than the hydrogenation using H2 (67.4%). Results from BET, EDS, CO chemosorption, XRD and H2-TPR suggest that the presence of suitable amounts of lanthanum improves the Pd dispersion on the support. The peak temperature for the reduction of PdO in the H2-TPR moves to higher in the presence of lanthanum. Additionally, the Pd particles could adhere to the lanthanum rather than the Al2O3.

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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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Journal of Thermal Analysis and Calorimetry
Authors:
Li-Fang Song
,
Chun-Hong Jiang
,
Jian Zhang
,
Li-Xian Sun
,
Fen Xu
,
Yun-Qi Tian
,
Wan-Sheng You
,
Zhong Cao
,
Ling Zhang
, and
Dao-Wu Yang

Abstract  

A novel two-dimensional metal organic framework MgBTC [MgBTC(OCN)2·2H2O, where BTC = 1,3,5-benzenetricarboxylate] has been synthesized solvothermally and characterized by single crystal XRD, powder XRD, FT-IR spectra. The low-temperature molar heat capacities of MgBTC were measured by temperature modulated differential scanning calorimetry (TMDSC) over the temperature range from 190 to 350 K for the first time. No phase transition or thermal anomaly was observed in the experimental temperature range. The thermodynamic parameters of MgBTC such as entropy and enthalpy relative to reference temperature of 298.15 K were derived based on the above molar heat capacities data. Moreover, the thermal stability and decomposition of MgBTC was further investigated through thermogravimetry (TG)-mass spectrometer (MS). Four stages of mass loss were observed in the TG curve. TG-MS curve indicated that the products of oxidative degradation of MgBTC are H2O, N2, CO2 and CO. The powder XRD showed that the mixture after TG contains MgO and graphite.

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Abstract  

The compound 3-{[4-(4-[18F]fluorophenyl)methyl]piperazin-1-yl}-methyl-1H-pyrrolo[2,3-b]pyridine ([18F]3), which is an analogue of L-745,870 binding D4

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Abstract

The thermal decomposition behavior of composite modified double-base propellant containing hexanitrohexaazaisowurtzitane (CL-20/CMDB propellant) was studied by microcalorimetry. The kinetic and thermodynamic parameters were obtained from the analysis of the heat flow curves. The effect of different proportion of CL-20 to the thermal decomposition behavior, kinetics, and thermal hazard was investigated at the same time. The critical temperature of thermal explosion (T b), the self acceleration decomposition temperature (T SADT), and the adiabatic decomposition temperature rise (ΔT ad) were calculated to evaluate the thermal hazard of the CL-20/CMDB propellant. It shows that the CMDB propellant with 38% CL-20 has relative lower values of E and lgA, and with 18% CL-20 has the highest potential hazard.

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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 T H 298.15] and [S T S 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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Abstract  

The fractional cumulative yields (FCY) of133mTe and133gTe in the spontaneous fission of252Cf were measured for the first time by a radiochemical method. The values ofFCY are 0.533±0.014 and 0.291±0.042 for133mTe and133gTe, respectively. The isomeric state to ground state fractional independent yield (FIY) ratio of133Te,R, was found to be 3.5. The root-mean-square angular momentum of the primary fragment corresponding to the fission product133Te, Jr.m.s.=8.8h, was estimated according to a simple one-parameter statistical model. The fractional cumulative yields from this work together with other literature data in the mass region A=131–141 are compared with the normal yields given by the empiricalZ p model by Whhl. It suggests that both theN=82 neutrons shell and nucleus pairing effects are not apparent for the spontaneous fission of252Cf.

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Abstract

Described in this paper are the synthesis, characterization and catalytic application of H-ZSM-5 zeolites for the conversion of CH3Br into aromatics. The H-ZSM-5 zeolites were fabricated by hydrothermal crystallization using n-butylamine (BTA) as a template and characterized by XRD, SEM and NH3-TPD techniques. The effects of batch SiO2/Al2O3 ratio, alkalinity, NaCl/Al2O3 ratio, seed crystals, and crystallization time on the yield, structure/texture and catalytic performance were systematically studied. Adopting the optimum sol (SiO2/Al2O3 = 70, BTA/SiO2 = 0.2847, Na2O/SiO2 = 0.1237, H2O/SiO2 = 37.4, NaCl/Al2O3 = 60, and seed/SiO2 = 5 wt%) and under the most preferable crystallization conditions of 100 °C/24 h–170 °C/24 h, H-ZSM-5 zeolites of high crystallinity and small size (300–700 nm) were obtained. Good catalytic performance was observed over the H-ZSM-5 zeolites (aromatic yield up to 44.2%). However, unlike the modification of large commercial HZSM-5, the use of MoO3 or PbO as modifying agents for the small-size H-ZSM-5 zeolites results in a decline of catalytic performance. The relationship between the structure and the catalytic efficiency of as-synthesized H-ZSM-5 samples were investigated. It was found that with crystallinity enhancement and/or decline in crystal size, there is improvement of catalytic performance.

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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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