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1.
S. Mentus Dijana Jelić Veselinka Grudić 《Journal of Thermal Analysis and Calorimetry》2007,90(2):393-397
Thermal decomposition of lanthanum nitrate to lanthanum oxide was carried out by both temperature programmed heating (TPH)
and citrate-gel combustion. The temperature programmed heating was carried out under flow of oxidizing (air), neutral (nitrogen)
and reducing (25 vol.% hydrogen+argone mixture) gases, and the processes were controlled by simultaneous thermogravimetry
and differential thermal analysis. It was shown that hydrogen atmosphere helps to reduce temperatures of all decomposition
steps. The results of TPH were utilized to check the nature of residues in the products of lanthanum nitrate-to-oxide conversion
performed via citrate-gel combustion technique. 相似文献
2.
Kaloustian J Pauli A-M Lechene de la Porte P Lafont H Portugal H 《Journal of Thermal Analysis and Calorimetry》2003,71(2):341-351
Cholesterol constitutes the major component of most gallstones. It was identified and determined, in gallstones, issued from
eleven patients, by thermal analysis: differential scanning calorimetry (DSC), with the use of the melting temperature and
enthalpy, thermogravimetry (TG), with the mass loss of water. Anhydrous cholesterol (ChA) was characterized by two endothermic
peaks (polymorphic, melting) and cholesterol monohydrate (ChH) by two endothermic peaks (dehydration, melting), too. Cha needle
and Chh plate crystals were observed under polarizing light microscopy. The numerous stones obtained from nine patients were
cholesterol stones: the ChA was higher 45 and lower 96%. ChH was present in stones of three patients.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
3.
4.
复盐法制备无水氯化镁的热解机理及动力学研究 总被引:4,自引:0,他引:4
The complex compound (MgCl2·C6H5NH2·HCl·6H2O) was prepared by reaction of C6H5NH2·HCl with MgCl2·6H2O. Reaction mechanism and kinetics of the compounds decomposition were studied by means of the TG-DTA-MS coupling technique and the TG-DTA technique. The results show that there are four steps in the complex′s thermal decomposition, the first two steps correspond to the loss of six crystal waters and the last two steps loss one Aniline hydrochloride. The first three steps belong to the R2 mechanism with 2-dimentional phase boundary reaction as the control step, and the last step belongs to the D3 with 3-dimensional diffusion (sphere Jander equ.) as the control step. The apparent active energy of four steps are, 127.4 kJ·mol-1, 124.8 kJ·mol-1, 142.3 kJ·mol-1 and 329.0 kJ·mol-1, respectively and the frequency factor are 1.28 × 1018 s-1, 7.94 × 1015 s-1, 5.98 × 1016 s-1 and 4.39 × 1034 s-1, respectively. 相似文献
5.
J. Kaloustian Paulette Lechene De La Porte T. El-Moselhy H. Lafont H. Portugal 《Journal of Thermal Analysis and Calorimetry》2005,82(2):331-338
Summary Cholesterol constitutes the major component of most gallstones. It was identified and determined in gallstones by thermal
analysis technique (DSC and TG-DTA), mainly by the use of the melting temperature (Tonset=145°C and Tmax=149°C) and by DTG peak decomposition (Tmax=364°C). Cholesterol anhydrous (ChA), which showed endothermic polymorphic peak, Tmax=40°C, without mass loss, was differentiated from cholesterol monohydrate (ChH), which showed a broad endothermic peak, Tmax=59°C, attributed to loss of water of crystallization (theoretical 4.45%). Morphological studies of gallstones were performed
by optical microscopy and scanning electron microscopy (SEM). The stones consisted of a pigmented core with a variably-sized
irregular central cavity, surrounded by a radially arranged deposits of plate-like ChH. The outer part of the stones showed
ChA crystal arborescences. X-ray microanalysis gave a typical spectrum rich in C and O, and in some instances the presence
of P, which was attributed to the presence of phospholipids. CaCO3 was easily characterized by TG with the use of DTG decomposition peak at 674°C. 相似文献
6.
Sh. Sh. Nabiev I. I. Ostroukhova N. V. Revina L. P. Sukhanov 《Russian Chemical Bulletin》1998,47(3):417-422
The Raman spectra of ClOF2
+ cation in solutions of anhydrous HF were studied. In the ClOF2
+HF2
− and ClOF2
+BF4
−−HF systems, this cation exists as a pyramidal structure (C
s
symmetry), while in the ClOF2
+AuF6
−−HF system, it exists as a planar structure (C
2v
symmetry). Based on nonempirical calculations by the Hartree-Fock-Roothaan method, an explanation for the dependence of the
structure of the ClOF2
+ cation on the nature of the anion was proposed. For the Cl−O bond vibrations, the correlation functions of vibrational and
rotational relaxations were calculated, and the characteristic times of these processes were determined. The main contribution
to the formation of the band contours corresponding to the above-mentioned modes is made by the vibrational dephasing.
Translated fromIzvestiya Akademii Nauk, Seriya Khimicheskaya, No. 3, pp. 432–437, March, 1998. 相似文献
7.
有机溶剂法无水氯化镁的制备与表征 总被引:6,自引:0,他引:6
Ammonium carnallite was synthesized by hydrated magnesium chloride in salt lake and ammonium chloride solution. Dehydrated ammonium carnallite was dissolved in methanol under low temperature by feeding ammonia, to prepare anhydrous magnesium chloride. The results show that anhydrous magnesium chloride contains magnesium oxide in an amount less than 0.1% by weight, the yield of magnesium chloride was above 99.5%. Ammonium carnallite, ammoniation magnesium chloride and anhydrous magnesium chloride were characterized by thermoanalysis, X-ray powder diffraction and scanning electron microscopy. 相似文献
8.
Acylation of cholest-5-ene and cholest-5-ene 3-one with anhydrides in the presence of zinc chloride and characterization of products thus obtained on the basis of elemental analysis, spectral data, and chemical transformations are reported. 相似文献
9.
Wan-Feng Zhang Xiao-Ping Xia Takahashi Eiichi Li Li Qing Yang Yan-Qiang Zhang Ya-Nan Yang Ming-Liang Liu Chunkit Lai 《Surface and interface analysis : SIA》2020,52(5):224-233
Secondary ion mass spectrometry (SIMS) has a wide range of applications in Earth Science research, thanks to its high precision and sensitivity, and its capacity in direct insitu micromeasurement. The technique is operated in ultra-high vacuum (UHV) conditions, especially for the measurement of volatiles such as hydrogen, or the water content in nominally anhydrous minerals (NAMs). To minimize the water background and obtain accurate and precise water contents in NAMs (eg, olivine) critical parameters such as presputtering time, field aperture (FA), dynamic transfer on/off, and primary beam current intensity were investigated for a CAMECA IMS 1280-HR system. When the chamber vacuum reaches approximately 2 × 10−9 mbar, we set the DTOS OFF, raster size to 50 μm and primary beam current to 5 nA, and used 2000 μm FA and 170-second presputtering time. Consequently, an approximately 1.2 ppmw water background and 3.6 ppmw limit of detection (LOD) were yielded, from analyzing the San Carlos olivine. Meanwhile, the water content and homogeneity of a range of olivine minerals were characterized for potential use as reference materials for SIMS water content measurement. Olivine water content calibration curve was also established by comparing the Fourier transform infrared (FTIR) results with the SIMS-measured 16O1H−/16O− ratios. Accuracy and precision of water content measurement were estimated to be better than approximately 10% in this study. 相似文献
10.
Bongiorno D Ceraulo L Giorgi G Indelicato S Ferrugia M Ruggirello A Liveri VT 《Journal of mass spectrometry : JMS》2011,46(2):195-201
Self-assembling of amphiphilic molecules under electrospray ionization (ESI) conditions is characterized by quite unexpected phenomenology. The noticeable differences with respect to the condensed phase are attributable to the absence of the surfactant-solvent interactions, the presence of net charge in the aggregates, and the strong deviation from equilibrium conditions. Aiming to investigate the effects of the net charge on abundance and stability of supramolecular surfactant aggregates, positively and negatively charged aggregates of sodium bis(2-ethylhexyl)sulfosuccinate (AOT) and sodium methane sulfonate (MetS), butane sulfonate (ButS) and octane sulfonate (OctS) have been studied by ESI mass spectrometry, energy resolved mass spectrometry and density functional theory calculations. The negatively charged aggregates are found to be less stable than their positive counterparts. The results are consistent with a self-assembling pattern dominated by electrostatic interactions involving the counterions and head groups of the investigated amphiphilic compounds while the alkyl chains point outwards, protecting the aggregates from unlimited growth processes. 相似文献