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Abstract  

Fourteen organic compounds, 1-pentene, 2-methylbutane, 2-methyl-1,3-butadiene (isoprene),n-pentane, 2-chloropropane, ethyl alcohol, 2,2,4-trimethylpentane,n-hexane,n-hepatane, 1,3-difluorobenzene, 1,2-dichloroethane, hexafluorobenzene, cyclohexane and diphenyl ether, as new reference materials for energy and temperature calibrations of differential thermal analysers (DTA) and differential scanning calorimeters (DSC) in the temperature range 100–300 K, were investigated. The purities, triple point and transition temperatures, fusion and transition enthalpies of these compounds were measured using a low-temperature DTA apparatus developed by the CTM of the CNRS in Marseille. The results obtained were compared with those produced by adiabatic precision calorimetry. Our data are in good agreement with literature values. Enthalpies of fusion and transition, triple point and transition temperatures are reproduced within ±1% and ±0.1K, respectively.

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Abstract  

Twenty four male autopsies were obtained from Shanghai, China. The samples of liver, lung, kidney cortex, brain and scalp hair were collected from the autopsies. The elements As, Br, Ca, Cd, Cl, Co, Cr, Cu, Fe, Hg, Mg, Mn, Na, Rb, S, Se and Zn were determined by neutron activation analysis (NAA). The present study shows the distribution of the elements in different tissues and provides the element level for normal persons in the local area. In general, the results are comparable with those of other countries.

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Abstract  

A computerized adiabatic calorimeter for heat capacity measurements in the temperature range 80–400 K has been constructed. The sample cell of the calorimeter, which is about 50 cm3 in internal volume, is equipped with a platinum resistance thermometer and surrounded by an adiabatic shield and a guard shield. Two sets of 6-junction chromel-copel thermocouples are mounted between the cell and the shields to indicate the temperature differences between them. The adiabatic conditions of the cell are automatically controlled by two sets of temperature controller. The reliability of the calorimeter was verified through heat capacity measurements on the standard reference material α-Al2O3. The results agreed well with those of the National Bureau of Standards (NBS): within 0.2% throughout the whole temperature region. The heat capacities of high-purity graphite and polystyrene were precisely measured in the interval 260–370 K by using the above-mentioned calorimeter. The results were tabulated and plotted and the thermal behavior of the two materials was discussed in detail. Polynomial expressions for calculation of the heat capacities of the two substances are presented.

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Abstract  

24 male autopsy cases aged 35–60 years have been collected from Shanghai China to study the relationships between human hair and internal tissues. Autopsy samples of hair, kidney-cortex, liver and lung were analyzed. A radiochemical neutron activation analysis (RNAA) based on a simple group extraction scheme was used for measuring the trace elements As, Cd, Hg, Cu and Zn. Zinc diethyldithiocarbamate Zn(DDC)2 and methly isobutyl ketone-iodide have been chosen as reagent. Trace element of Se was determined by instrumental neutron activation analysis (INAA). A SLOWPOKE reactor with a thermal neutron flux of 8·1011 n·cm–2·s–1 and a swimming pool type reactor with a thermal neutron flux of 1·1013 n·cm–2·s–1 were used for short and long irradiation of samples, respectively. The reliability of methods has been checked by analyzing biological standard reference materials Horse Kidney (IAEA H8), Tomato Leaves (NBS 1573) and Human Hair (NIES-5). The analytical results show that toxic elements As, Cd and Hg exist in a larger individual variability than the essential elements of Cu, Se and Zn for each tissue. A linear regression analysis related to the six elements of primary interest for the IAEA Coordinated Research Program (CRP) has been done by a computer program for each pair of hair-tissue. A positive correlation is found between concentration of As in hair and kidney-cortex, the correlation coefficient r is 0.751 (p<0.01). Positive correlations between concentration of Se in hair and liver, kidney-cortex and lung are also observed in this study. It shows that the elements As and Se in hair may be useful indicators for assessing certain internal tissues of normal persons. A comparison of Cd concentration in lung shows a significant difference between smokers and non-smokers. A significant correlation between element Cd and Zn in kidney-cortex is also presented in this paper.

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Abstract  

In this work, a simple group separation scheme based on extraction for NAA determination of trace of As, Cd, Hg, Cu and Zn in biological materials is described. For this purpose, zinc-diethyldithiocarbamate, Zn(DDC)2, and methyl isobutyl ketone-iodide have been chosen as reagents. The elements can be extracted successively and quantitatively from strong mineral acids without adjusting pH of the solution, and separated into two groups suitable for gamma-ray spectrometry. Samples of 100–200 mg dry weight were double-sealed into polyethylene bags and irradiated in a swimming pool reactor with a thermal neutron flux of 1013n·cm–2·s–1 for 44 hours. After a cooling period of 1–3 days, the samples were digested with microgram quantities of carrier in concentrated nitric acid and sulfuric acid at 150°C for 3.5 hours in a teflon bomb, then extracted as described above. The reliability of the analytical method was checked using reference materials Horse Kidney IAEA H-8, Human Hair NIES-5 and Tomato Leaves NBS-1573. Most of the results obtained for reference materials agreed with the certified values12. Chinese autopsy samples of hair and liver were presented.

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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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