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Abstract  

The method of high-temperature hydrolysis separating fluorine from UF4 is described. The determination of the content of fluorine by different methods is performed and compared.

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Abstract  

The two-dimensional angular correlation of annihilation radiation (2D-ACAR) technique has been developed to measure the hole structure of stretched and oriented polymers. The determination of polymer hole structure is demonstrated in a stretched semi-crystalline polyaryl-ether-ether-ketone (PEEK) sample. The atomic scale anisotropy is found to be consistent with the macroscopic scale stretch ratio. Applications of the 2D-ACAR method to image the three-dimensional hole, free-volume, and cavity structures of molecular systems are discussed.

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Shenqi Fuzheng Injection (SFI) is a traditional Chinese medicine injection, widely used to enhance immune function of clinical cancer patients undergoing chemotherapy. In this study, a high-performance liquid chromatography-diode array detection-evaporative light scattering detection (HPLC-DAD-ELSD) method was established for quality control of SFI, which could simultaneously semiquantitatively reflect the constituents displayed in the chromatographic profile of SFI. The relative retention time and relative peak areas of the 21 common peaks related to the reference peak were calculated. The validity and advantage of this method were validated by systematically comparing chromatograms of 10 batches of SFI samples with the analytical methods of principal component analysis and angle cosine method recommended by the State Food and Drug Administration of China. Moreover, a total of 21 constituents of SFI were identified or tentatively characterized in the fingerprint via ultrafast liquid chromatography-diode array detection-quadrupole time-of-flight (UFLC-DAD-Q-TOF) tandem mass spectrometry technique on the basis of the retention time, ultraviolet spectra, fragmentation patterns, and reported literatures. All the results proved that the technique was useful in comprehensive quality evaluation of SFI and further study.

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Abstract  

The recombination of hydrogen and oxygen in technical gaseous waste of nuclear power plants has been studied. A highly efficient catalyst for reacting H2 with O2 to form water was prepared. Various operating conditions and factors affecting the recombination of H2 and O2 were tested and the best conditions were determined. Results show that the Pd–Al2O3 catalyst prepared had very good characteristics. The recombination rate of H2 and O2 was higher than 98.3% and 99.9%, respectively. After recombination, residual concentrations of H2 and O2 in waste gas were O2<3 ppm, H2<400 ppm. The Pd–Al2O3 catalyst and operating conditions determined for gaseous waste processing of nuclear power plants were satisfactory.

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Abstract  

Positron annihilation lifetime (PAL) experiments are performed in polycarbonate (PC) exposed to CO2 and He gases as a function of time and pressure. In PC/CO2 systems, hole size and fraction reduced from PAL data increase as a function of CO2 pressure and exposure time. Significant hysteresis in positron lifetime data is observed during CO2 abasorption/desorption. In PC/He systems, no variation is observed. Hole size distribution in the CO2-exposed polymers is found to be significantly broader than in unexposed samples. The high sensitivity of PAL results to CO2 exposure of PC is thought to relate to the microstructural changes in the polymer matrix, such as penetrant plasticization, gas hydrostatic pressure effect, and molecular filling and creation of holes.

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Thermodynamic investigation of room temperature ionic liquid

The heat capacity and thermodynamic functions of BMIPF6

Journal of Thermal Analysis and Calorimetry
Authors: Z. Zhang, T. Cui, J. Zhang, H. Xiong, G. Li, L. Sun, F. Xu, Z. Cao, F. Li, and J. Zhao

Abstract  

The molar heat capacities of the room temperature ionic liquid 1-butyl-3-methylimidazolium hexafluoroborate (BMIPF6) were measured by an adiabatic calorimeter in temperature range from 80 to 390 K. The dependence of the molar heat capacity on temperature is given as a function of the reduced temperature (X) by polynomial equations, C P,m (J K−1 mol−1) = 204.75 + 81.421X − 23.828 X 2 + 12.044X 3 + 2.5442X 4 [X = (T − 132.5)/52.5] for the solid phase (80–185 K), C P,m (J K−1 mol−1) = 368.99 + 2.4199X + 1.0027X 2 + 0.43395X 3 [X = (T − 230)/35] for the glass state (195 − 265 K), and C P,m (J K−1 mol−1) = 415.01 + 21.992X − 0.24656X 2 + 0.57770X 3 [X = (T − 337.5)/52.5] for the liquid phase (285–390 K), respectively. According to the polynomial equations and thermodynamic relationship, the values of thermodynamic function of the BMIPF6 relative to 298.15 K were calculated in temperature range from 80 to 390 K with an interval of 5 K. The glass transition of BMIPF6 was measured to be 190.41 K, the enthalpy and entropy of the glass transition were determined to be ΔH g = 2.853 kJ mol−1 and ΔS g = 14.98 J K−1 mol−1, respectively. The results showed that the milting point of the BMIPF6 is 281.83 K, the enthalpy and entropy of phase transition were calculated to be ΔH m = 20.67 kJ mol−1 and ΔS m = 73.34 J K−1 mol−1.

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Journal of Thermal Analysis and Calorimetry
Authors: Z. Xiao, D. Liu, C. Wang, Z. Cao, X. Zhan, Z. Yin, Q. Chen, H. Liu, F. Xu, and L. Sun

Abstract  

The effect of mechanical alloying on Zn-Sb alloy system is investigated with X-ray diffraction (XRD), laser grain size analysis and differential scanning calorimetry (DSC) respectively. The results of laser particle size analysis shows that the particle size decreases with increasing of the grinding time between 0 and 24 h. XRD and DSC results indicate that longer the grinding time of Zn-Sb is, the more content of Zn4Sb3 become in the product in this process.

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Summary

A reversed-phase chiral liquid chromatographic method had been developed and validated for resolution of the enantiomers of racemic fudosteine. The effects on the separation of the amounts of anhydrous cupric sulfate and l-phenylalanine, the methanol content, mobile phase pH, and temperature were investigated. The method was validated for linearity, repeatability, intermediate precision, sample recovery, solution stability, and limits of detection (LOD). l-Phenylalanine and anhydrous cupric sulfate as chiral ligand-exchange complexes were used for separation, isomer identification, related substance investigation, and analysis of fudosteine enantiomers in fudosteine bulk drugs and fudosteine tablets.

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