This paper presents the thermal behavior of Co, Ni and Fe succinates obtained by sol-gel synthesis using Co(II), Ni(II) and Fe(III) nitrates, 1,4-butanediol and tetraethyl orthosilicate as reactants. The thermal analysis revealed the formation of succinates at 413–453 K and their decomposition to ferrites at 503–623 K. The rate constants for the decomposition of succinates to ferrites, calculated using the isotherms at 473, 523, 573 and 623 K, were used to determine the activation energy of each ferrite (NiFe2O4, Ni0.3Co0.7Fe2O4, Ni0.7Co0.3Fe2O4 and CoFe2O4) embedded in the silica matrix. By increasing the Ni content in the mixed Ni–Co ferrites, the activation energy decreases from 13.530 to 1.944 kJ mol?1. The formation and decomposition of succinate precursors and the formation of silica matrix were confirmed by FT-IR spectroscopy, while the formation of CoFe2O4 and NiFe2O4 single-phases embedded in the silica matrix was confirmed by X-ray diffraction analysis. The nanocrystallites size decreases from 31.7 (CoFe2O4) to 18.5 nm (NiFe2O4). The optical band gap of mixed Co–Ni ferrites was significantly higher than that corresponding to CoFe2O4. The photocatalytic activity of the samples was evaluated against Rhodamine B under visible light. All the samples have photocatalytic activities, the best performance being obtained in the case of Ni0.7Co0.3Fe2O4.
The process of shrinkage of calcium silicate hydrate was investigated by dilatometry up to 350 °C. The properties of this material are based on the formation of C–S–H phases during the reaction at temperatures between 180 and 205 °C and water vapor pressure lower than 16 bars. The main C–S–H phases are 11.3 Å tobermorite and xonotlite. 11.3 Å tobermorite converts to 9.3 Å tobermorite on air at temperatures around 300 °C. The hydrosilicate materials were prepared from quicklime and finely ground sand with different CaO/SiO2 ratios under different hydrothermal conditions. The reaction time was 24 h. Materials based on xonotlite and tobermorite were produced, and the calcium silicate phases were characterized by XRD and TG/DTA methods. Dilatometry measurements were used to study the effect of heating conditions on sample shrinkage. Dehydration of hydrated calcium silicate minerals occurred during heating. The results show that sample shrinkage is dependent on the type and amount of C–S–H phases, the amount of bound water and formation of 9.3 Å tobermorite. All samples showed shrinkage after heating up to 350 °C, but this change was not irreversible for all samples after cooling to room temperature.
A total synthesis of largazole that proceeds in 8 steps from commercial materials is reported, along with some structure-activity relationships. A combination of NMR studies and molecular modeling have also provided a preliminary picture of the conformation of largazole. 相似文献
We present results from high-resolution electron energy loss spectroscopy (HREELS) and XPS studies of self-assembled monolayers of DNA. The monolayers are well-organized and display sharp vibrational peaks in the HREEL spectra. The electrons interact mainly with the backbone of the DNA. The XPS results indicate that, in most of the samples studied, the phosphates on the DNA are not charged. 相似文献
We have developed a method using on-line solid-phase extraction–high-performance liquid chromatography–tandem mass spectrometry
(SPE-HPLC-MS/MS) and isotope dilution quantification to measure atrazine and seven atrazine metabolites in urine. The metabolites
measured were hydroxyatrazine, diaminochloroatrazine, desisopropylatrazine, desethylatrazine, desethylatrazine mercapturate,
atrazine mercaturate and atrazine itself. Our method has good precision (relative standard deviations ranging from 4 to 20%
at 5, 10 and 50 ng/mL), extraction efficiencies of 67 to 102% at 5 and 25 ng/mL, relative recoveries of 87 to 112% at 5, 25,
50 and 100 ng/mL limits of detection (LOD) ranging from 0.03 to 2.80 ng/mL. The linear range of our method spans from the
analyte LOD to 100 ng/mL (40 ng/mL for atrazine and atrazine mercapturate) with R2 values of greater than 0.999 and errors about the slope of less than 3%. Our method is rapid, cost-effective and suitable
for large-scale sample analyses and is easily adaptable to other biological matrices. More importantly, this method will allow
us to better assess human exposure to atrazine-related chemicals.
Figure A schematic representation showing the elution of the analytes from the solid-phase extraction cartridge onto the analytical
column for chromatographic separation prior to MS/MS analysis 相似文献
A series of new complexes with mixed ligands of the type [ML(C3H3O2)2]·nH2O (((1)M=Mn, n=1; (2)M=Co(II), n=2; (3)M=Ni(II), n=4; (4)M=Cu(II), n=1.5; (5)M=Zn(II), n=0; L=3-amino-1,2,4-triazole and (C3H3O2)=acrylate anion) were synthesized and characterised by chemical analysis and IR data. In all complexes the 3-amino-1,2,4-triazole
acts as bridge while the acrylate acts as bidentate ligand except for complex (5) where it is found as unidentate. The thermal behaviour steps were investigated in nitrogen flow. The thermal transformations
are complex processes according to TG and DTG curves including dehydration, acrylate ion and 3-amino-1,2,4-triazole degradation
respectively. The final products of decomposition are the most stable metal oxides, except for complex (4) that leads to metallic copper. 相似文献
Melanosomes are organelles found in a wide variety of tissues throughout the animal kingdom and exhibit a range of different shapes: spheres of up to approximately 1 mum diameters and ellipsoids with lengths of up to approximately 2 mum and varying aspect ratios. The functions of melanosomes include photoprotection, mitigation of the effects of reactive oxygen species, and metal chelation. The melanosome contains a variety of biological molecules, e.g., proteins and lipids, but the dominant constituent is the pigment melanin, and the functions ascribed to melanosomes are uniquely enabled by the chemical properties of the melanins they contain. In the past decade, there has been significant progress in understanding melanins and their impact on human health. While the molecular details of melanin production and how the pigment is organized within the melanosome determine its properties and biological functions, the physical and chemical properties of the surface of the melanosome are central to their range of ascribed functions. Surprisingly, few studies designed to probe this biological surface have been reported. In this article, we discuss recent work using surface-sensitive analytic, spectroscopic, and imaging techniques to examine the structural and chemical properties of many types of natural pigments: sepia melanin granules, human and bovine ocular melanosomes, human hair melanosomes, and neuromelanin. N 2 adsorption/desorption measurements and atomic force microscopy provide novel insights into surface morphology. The chemical properties of the melanins present on the surface are revealed by X-ray photoelectron spectroscopy and photoemission electron microscopy. These technologies are also applied to elucidate changes in surface properties that occur with aging. Specifically, studies of the surface properties of human retinal pigment epithelium melanosomes as a function of age are stimulating the development of models for their age-dependent behaviors. The article concludes with a brief discussion of important unanswered research questions in this field. 相似文献
Here, the effect of solvent on the stability of non-covalent complexes, was studied. These complexes were from previously published S22, S66, and X40 datasets, which include hydrogen-, halogen- and dispersion-bonded complexes. It was shown that the charge transfer in the complex determines whether the complex is stabilized or destabilized in solvent. 相似文献
We classify nondegenerate centers of systems of the form
, where the Pi(x) are polynomials in x, y over . We show that such systems fall naturally into two classes: those with Darboux first integrals, and those which arise from
simpler systems via singular algebraic transformations.
Dedicated to V. I. Arnold on his 70th birthday 相似文献