There are many reactions of interest in which one or more of the reactants belong to some solid phases. Modern thermoanalytical instruments can conveniently provide reaction kinetic data of high precision and accuracy, from which the underlying activation energyE may be derived in principle. Unfortunately, no ‘best' method yet exists for the derivation when the data have been collected with a programmed linear increase in sample temperature, unlike the case of isothermal measurements, which however suffer from experimental limitations . Here we propose a method for extractingE from non-isothermal data, that promises general validity.
Authors:B. Zhang, Y. Li, Q. Li, B. Ma, F. Gan, Z. Zhang, H. Cheng, and F. Yang
External-beam PIXE was used for the non-destructive analysis of early glasses unearthed from the tombs of Warring States (475–221BC) and Han Dynasty (BC 206–AD 220) in south China. It was found that these glasses were basically attributed to PbO—BaO—SiO2 system and K2O—SiO2 system. The results from the cluster analysis showed that some glasses had exactly the same recipe. The source of the K2O flux and the correlation between PbO and BaO are discussed. Some archeological information is revealed.
Authors:Q. Chen, P. Li, B. Li, F. Yuan, X. Li, and J. Zhu
A rapid and sensitive method for the identification and quantification of yohimbine in Pausinystalia yohimbe is described. The method used is liquid chromatography-quadrupole ion trap mass spectrometry (LC-QIT/MS). The yohimbine standard solution was directly infused into the ion trap mass spectrometers (IT/MS) for collecting the MSn spectra. The major fragment ions of yohimbine were confirmed by MSn at m/z 355, 224, 212, and 144, in the positive-ion mode. The possible main fragment ion cleavage pathway was studied. Yohimbine provided good signals corresponding to the protonated molecular ion [M + H]+. The method is reliable and reproducible, and the detection limit is 0.1 ng mL-1. The method was validated in the concentration range 0.1–50 μg mL−1; the intra- and interday precision ranged from 1.36% to 2.73% and the accuracy was 96.5–108.2%. The mean recovery of yohimbine was 97.1–101% with a relative standard deviation (RSD) <1.93%. The LC-IT/MS method was successfully applied to determine the yohimbine in P. yohimbe.
Authors:C. Liu, S. Li, X. Wang, Z. Wang, H. Wang, R. Li, C. Xin, B. Li, L. Jiang, and C. Jia
The migration of 99Tc in unsaturated Chinese loess was investigated in-situ with a tracer method. Quartz containing 3H (HTO) and 99Tc (99TcO4-) was introduced into the bottom of an experimental pit which was then backfilled at the field test site. Then core soil samples were taken and cut vertically into 1 cm long slices. The slice samples were analyzed by liquid scintillation techniques in the laboratory. The results indicate that the migration pattern of 99Tc was quite similar to that of 3H and the vertical diffusion coefficients of 99Tc and 3H were calculated as (4.7±0.4).10-2 cm2/d and (7.8±0.4).10-2 cm2/d, respectively.
Authors:Hanxu Li, Xiang-Zhong Shen, B. Sisk, W. Orndorff, Dong Li, Wei-Ping Pan, and J. Riley
Improved thermoanalytical methods have been developed that are capable of quantitative identification of various components
of fly ash from a laboratory-scale fluidized bed combustion system. The thermogravimetric procedure developed can determine
quantities of H2O, Ca(OH)2, CaCO3, CaSO4 and carbonaceous matter in fly ash with accuracy comparable to more time-consuming ASTM methods. This procedure is a modification
of the Mikhail-Turcotte methods that can accurately analyze bed ash, with higher accuracy regarding the greater amount of
carbonaceous matter in fly ash. In addition, in conjunction with FTIR and SEM/EDS analyses, the reduction mechanism of CaSO4 as CaSO4+4H2 ↔ CaS + 4H2O has been confirmed in this study. This mechanism is important in analyzing and evaluating sulfur capture in fluidized-bed
The title compound 3,3-dinitroazetidinium (DNAZ) 3,5-dinitrosalicylate (3,5-DNSA) was prepared and the crystal structure has
been determined by a four-circle X-ray diffractometer. The thermal behavior of the title compound was studied under a non-isothermal
condition by DSC and TG/DTG techniques. The kinetic parameters were obtained from analysis of the TG curves by Kissinger method,
Ozawa method, the differential method and the integral method. The kinetic model function in differential form and the value
of Ea and A of the decomposition reaction of the title compound are f(α)=4α3/4, 130.83 kJ mol−1 and 1013.80s−1, respectively. The critical temperature of thermal explosion of the title compound is 147.55 °C. The values of ΔS≠, ΔH≠ and ΔG≠ of this reaction are −1.35 J mol−1 K−1, 122.42 and 122.97 kJ mol−1, respectively. The specific heat capacity of the title compound was determined with a continuous Cp mode of mircocalorimeter. Using the relationship between Cp and T and the thermal decomposition parameters, the time of the thermal decomposition from initiation to thermal explosion (adiabatic
time-to-explosion) was obtained.
Cyanocobalamin (CNCbl), a kind of vitamin B12 (cobalamin, Cbl), which has a special binding capability to rapid dividing cells and proliferating tissue, especially tumors, has been modified and labeled by 99mTc. The optimal labeling condition was determined, and the biodistribution of 99mTc-DTPA-b-CNCbl both in normal mice and TA2 mice bearing MA891 mammary tumors were studied. 99mTc-DTPA-b-CNCbl showed low uptake and rapid clearance in nontarget tissues, and renal excretion. About 40% of uptake at 1 hour remained in the tumor at 12 hours p.i. The satisfying ratio of T/NT was acquired at 6 hours p.i.