Authors:G. Xu, L. Zhang, L. Liu, G. Liu, and D. Jia
Thermal behaviors of two mixed-ligand complexes, [Ni(PMPP-SAL)(Py)3] and [Cu(PMPP-SAL)Py]·MeOH, (PMPP-SAL=1-phenyl-3-methyl-4-(salicylidene hydrazide)-propenylidene-pyrazolone-5, Py=pyridine),
were studied by TG-DTG-DTA in dynamic air atmosphere. The complexes show the loss of pyridine molecule is followed by the
decomposition of the PMPP-SAL anion and give respective metal oxides as residues. Meanwhile, the Ozawa-Flynn-Wall model-free
analyses and multivariate non-linear regressions were applied to perform single and overall steps optimization. Kinetic parameters
were given and the most probable mechanism functions were suggested in this study.
The adsorption of 99Tc on the adsorbers Fe, Fe2O3 and Fe3O4 was studied by batch experiments under aerobic and anoxic conditions. The effects of pH and CO32- concentration of the simulated ground water on the adsorption ratios were also investigated, and the valences of Tc in solution after the adsorption equilibrium were studied by solvent extraction. The adsorption isotherms of TcO4- on the adsorbers Fe, Fe2O3 and Fe3O4 were determined. Experimental results have shown that the adsorption ratio of Tc on Fe decreases with the increase of pH in the range of 5-12 and increases with the decrease of the CO32- concentration in the range of 10-8M-10-2M. Under aerobic conditions, the adsorption ratios of 99Tc on Fe2O3 and Fe3O4 were not influenced by pH and CO32-concentration. When Fe was used as adsorbent, Tc existed mainly in the form of Tc(IV) after equilibrium and in the form of Tc(VII) when the adsorbent was Fe2O3 or Fe3O4 under aerobic conditions. The adsorption ratios of Tc on Fe, Fe2O3 and Fe3O4 decreased with the increase of pH in the range of 5-12 and increased with the decrease of the CO32- concentration in the range of 10-8M-10-2M under anoxic conditions. Tc existed mainly in the form of Tc(IV) after equilibrium when Fe, Fe2O3 and Fe3O4 was the adsorbent under anoxic conditions. The adsorption isotherms of TcO4- on the adsorbers Fe, Fe2O3 and Fe3O4 are fairly in agreement with the Freundlich’s equation under both aerobic and anoxic conditions.
Experimental crushed granite column breakthrough curves, using 99Tc as spike tracer and 3H as invariant tracer, were analyzed by different linear regression techniques. Dispersity of crushed granite and the retardation factor of 99TcO4- on the crushed granite were determined simultaneously by one linear regression. Dispersity of crushed granite was also obtained with 3H as invariant tracer by the other linear regression. The dispersities found by spike source and invariant source methods are compared. Experimental results show that the dispersity found by the spike source method is close to that found by the invariant source method. This indicates that dispersity is only a characteristic of the dispersion medium.
Authors:S. Li, L. Liu, H. Jiang, D. Liu, S. Chen, and Z. Yang
The crystal C81H78N12O6Cd3 was synthesized and its structure was determined by single crystal X-ray diffraction method. The complex crystallizes in
the monoclinic system space group P21/n with cell parameters, a=15.959(4) , b=26.222(3) , c=25.907(6) , β=101.60(2). The non-isothermal kinetics of the crystal
was studied by use of non-isothermal TG and DTG curves. The kinetic parameters were analyzed by means of integral and differential
methods, and mechanism functions of the thermal decomposition reaction for its second step were proposed. The kinetic equation
of thermal decomposition is expressed as:
dα/dt=Aexp(-E/RT)1.5(1-α)4/3[1/(1-α)1/3-1]−1. The average values of E(kJ mol−1) and lnA/s−1 are 339.25, 43.95, respectively.
Authors:H.-L. Liu, S.-J. Liu, Z.-L. Xiao, Q.-Y. Chen, and D.-W. Yang
Excess molar enthalpies of binary mixtures for tributyl
phosphate (TBP)+methanol/ethanol were measured with a TAM air Isothermal calorimeter
at 298.15 K and ambient. The results for xTBP+(1–x)CH3OH
are negative in the whole range of composition, while the values for xTBP+(1–x)C2H5OH
change from positive values at low x to
small negative values at high x. The experimental
results have been correlated with the Redlich–Kister polynomial. IR
spectra of the mixtures were measured to investigate the effect of hydrogen
bonding in the mixture.
Poly(AN—co—St) (PAS) and poly(AN—St—MMA)(PASM) were synthetized by emulsion polymerisation. The glass transition temperatures (Tg) of the copolymers and the relationship between Tg and the components of the copolymers were investigated by differential scanning calorimetry. The results show that Tg for the AN—St bipolymers has apeak value in the range 115–118°C at a content of 50 mass% St. When methyl methacrylate was added, the Tg of the terpolymer was decreased by about 2–6°C.The thermostability and the activation energy E of degradation were determined by thermogravimetric analysis.
DSC and TG-DTA techniques were used to investigate micro-sized silver powder particles and the adsorption of ethyl cellulose
on these particles in a solution of ethyl acetate. The apparent specific heat of the silver particles was determined, and
the kinetics of temperature-programmed desorption (TPD) of these adsorbed silver particles was investigated. Results show
that the apparent specific heat and desorption kinetic parameters obtained by thermal analysis techniques could be used to
characterize certain physico-chemical properties of such a particulate system.
Authors:J. Liu, D. He, L. Xu, H. Yang, and Q. Wang
The combustion behavior of Shuangya Mountain (SYM) coal dust has been investigated by means of TG in this paper. The reaction fraction can be obtained from isothermal TG data. The regressions of g(), an integral function of
vs. t for different reaction mechanisms were performed. The mechanism of nucleation and nuclei growth is determined as the controlling step of the coal dust combustion reaction by the correlation coefficient of the regression, and the kinetic equation of the SYM coal dust combustion reaction has been established.
Authors:J. Carpenter, D. Katayama, L. Liu, W. Chonkaew, and K. Menard
The glass transition of lyophilized materials is normally measured by conventional or temperature modulated differential scanning
calorimetry (TMDSC). However, because of the weakness of these transitions when protein concentrations are high, these techniques
are often unable to detect the glass transition (Tg). High ramp rate DSC, where heating rates of 100 K per min and higher are used, has been shown to be able to detect weak
transitions in a wide range of materials and has been applied to these materials in previous work. Dynamic mechanical analysis
(DMA) is also known to be much more sensitive to the presence of relaxations in materials than other commonly used thermal
techniques. The development of a method to handle powders in the DMA makes it now possible to apply this technique to protein
and protein-excipient mixtures. HRR DSC, TMA and DMA were used to characterize the glass transition of lyophilized materials
and the results correlated. DMA is shown to be a viable alternative to HRR DSC and TMA for lyophilized materials.