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151.
Tadashi Arii Kiyoshi Terayama Nobuyuki Fujii 《Journal of Thermal Analysis and Calorimetry》1996,46(6):1821-1836
Controlled-rate thermal analysis (CRTA) and differential scanning calorimetry (DSC) were used to investigate the adsorbed water layers and the surface properties of different commercial activated carbons. A simple method is proposed to obtain information on the properties of the adsorbed water film and the surface heterogeneity of the materials studied. This method utilizes TG mass loss and the first derivative of the DTG mass loss curves with respect to temperature and time, obtained during programmed liquid thermodesorption. The obtained TG mass loss curves, which reflect the energetic heterogeneity, consisted of steps and inflections which were associated with the mechanism of wetting of the solid surfaces. The heights of these steps and inflections depend on the adsorption capacity, the adsorption potential and the nature and number of the active centers of the carbon samples studied. The values of the total porosity and the surface phase capacity obtained by this method are in good agreement with those estimated on the basis of independent methods. The behaviour of water/carbon samples was studied by means of DSC at subambient and elevated temperatures. The experimental results provided novel data on the structural heterogeneity, the thermal stability of the water/carbon interface and its phase and structural transitions.Support from the Research Council of Kent State University (Ohio, USA) is acknowledged. The author is pleased to thank Drs M. Jaroniec, R. K. Gilpin, J. Choma and R. Dobrowolski for fruitful discussions and the active carbon samples. 相似文献
152.
A. S. Rozenberg E. I. Aleksandrova G. I. Dzhardimalieva A. N. Titkov A. D. Pomogailo 《Russian Chemical Bulletin》1993,42(10):1666-1672
The thermal decomposition of iron (III) acrylate, [Fe3O(CH2=CHCOO)6 · 3H2O]OH (FeAcr), a monomer with a complex cluster cation, has been studied at 200–370 °C. Thermal transformations of FeAcr occur
in two temperature regions. The rates of gas evolution in the low temperature region (200–300 °C) and the high temperature
region (300–370 °C) are described by first-order equations withk=4.2 · 1021exp[−59000/(RT)] s−1 andk=1.3 · 106exp[−30500/(RT)] s−1, respectively. A study of the qualitative and quantitative composition of the products of FeAcr thermolysis was carried out.
The thermal transformation of FeAcr is a complex process of dehydration, degradation, and polymerization in the solid phase
followed by decarboxylation of the metal-carboxyl groups of the polymer.
for part 33 see Ref. 1.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 10, pp. 1743–1750, October, 1993. 相似文献
153.
V. Bruder-Hubscher F. LagardeM.J.F. Leroy C. CoughanowrF. Enguehard 《Analytica chimica acta》2002,451(2):285-295
The release of five elements (Cr, Cu, Mn, Pb and Zn) from a municipal solid waste incineration bottom ash (BA) under different extraction conditions has been investigated by performing the three-step sequential extraction procedure proposed by the Standards, Measurements and Testing Program of the European Union. A fourth step (strong acid attack) has been added in order to calculate the mass balance. The results of this study provide information on the potential mobility of the studied elements. Almost all of the Cr and part of the Mn are extracted with strong acid which indicates low potential mobility in the environment. Most of the Cu is extracted under oxidizing conditions. Pb and Zn are released under acidic condition, indicating the possibility of their mobilization by changes in pH. The reproducibility of the sequential extraction procedure is also discussed. 相似文献
154.
Summary The retention of 9 nonylphenyl ethylene oxide oligomers was determined in 15 reversed-phase chromatographic systems using silicone oils of various molecular mass as impregnating agents and silica, cellulose and alumina supports. The data were evaluated with principal component analysis carried out on the covariance and the correlation matrices. The RM values did not follow the additivity rule and they did not change linearly with increasing length of the ethylene oxide chain. This is probably due to the folded state of the chain in the eluent. The molecular mass of the silicone oils had a negligible effect on the retention whereas the retention increased with increasing level of impregnation. The support considerably influenced the lipophilicity values of these nonionic surfactants and cellulose seemed to be the most appropriate support. Calculations proved that the application of a correlation matrix may cause data distortion; therefore, the use of a covariance matrix is strongly proposed. 相似文献
155.
Alexander Standler Andrea Schatzl Christian W. Klampfl Wolfgang Buchberger 《Mikrochimica acta》2004,148(3-4):151-156
A method for the determination of the new insect repellent Bayrepel in bathing lakes and public pools is presented. Sample preconcentration is performed either by solid-phase extraction (SPE) or stir bar sorptive extraction (SBSE). Analysis of the enriched analyte using gas chromatography-mass spectrometry (GC-MS) led to almost identical limits of detection (LOD) of 25ngL–1 for Bayrepel with both extraction methods. Because of the slightly reduced handling effort involved, the method based on preconcentration by SBSE was finally chosen for the analysis of real samples. 相似文献
156.
We studied thermal transitions and physical stability
of oil-in-water emulsions containing different milk fat compositions, arising
from anhydrous milk fat alone (AMF) or in mixture (2:1 mass ratio) with a
high melting temperature (AMF–HMT) or a low melting temperature (AMF–LMT)
fraction. Changes in thermal transitions in bulk fat and emulsion samples
were monitored by differential scanning calorimetry (DSC) under controlled
cooling and reheating cycles performed between 50 and –45°C (5°C
min–1). Comparison between bulk fat samples
and emulsions indicated similar values of melting completion temperature,
whereas initial temperature of fat crystallization (Tonset)
seemed to be differently affected by storage temperature depending on triacylglycerols
(TAG) composition. After storage at 4°C, Tonset
values were very similar for emulsified and non-emulsified AMF–HMT blend,
whereas they were lower (by approx. 6°C) for emulsions containing AMF
or mixture of AMF–LMT fraction. After storage at –30°C, Tonset values of re-crystallization
were higher in emulsion samples than in bulk fat blends, whatever the TAG
fat composition. Light scattering measurements and fluorescence microscopic
observations indicated differences in fat droplet aggregation-coalescence
under freeze-thaw procedure, depending on emulsion fat composition. It appeared
that under quiescent freezing, emulsion containing AMF–LMT fraction
was much less resistant to fat droplet aggregation-coalescence than emulsions
containing AMF or AMF–HMT fraction. Our results indicated the role of
fat droplet liquid-solid content on emulsion stability. 相似文献
157.
M. G. Zuev L. A. Perelyaeva E. V. Arkhipova V. S. Kiiko 《Journal of Structural Chemistry》2003,44(2):206-210
The oxygen nonstoichiometry (x) of LaTa2-2xNb2xVO9- (x = 0–0.1) solid solutions was studied using Xray phase analysis, vibrational spectroscopy, and radiospectroscopy. A correlation was found between (x) and the unit cell volume V(x) of the solid solutions. It was shown that the infrared spectra of LaTa2VO9- change in passing from = 0 to 0. The structural position of the oxygen vacancy in LaTa2-2xNb2xVO9- is discussed. 相似文献
158.
E. Yu. Yagudaeva M. R. Muidinov D. V. Kapustin V. P. Zubov 《Russian Chemical Bulletin》2007,56(6):1166-1173
Polyaniline coatings of the cation-exchange resin Dowex and a synthetic composite material based on silica gel surface-modified
by a sulfated styrene-divinylbenzene copolymer were prepared by precipitative polymerization of aniline on the surface of
the supports. The optimal conditions for the preparation of the polyaniline-containing material providing the formation of
a thin polymeric coating on the support surface were determined. Aniline is predominantly consumed to the formation of a uniform
polymeric coating about 3 nm thick with an increase in the concentration of sulfo groups on the support surface. The efficiency
of using the polyaniline-containing sorbents for the preparative isolation of DNA from plant tissue lysates was demonstrated.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1123–1130, June, 2007. 相似文献
159.
In this study, the cooling effect was applied to an evanescent wave type infrared (IR) chemical sensing method to effectively trap volatile organic compounds (VOCs), which have been absorbed in the hydrophobic film coated around the internal reflection element (IRE). The detection of VOCs in aqueous solutions was taken in the headspace of the aqueous solution. This method eliminates the long-term instability of hydrophobic film soaked in an aqueous solution and the potential spectral interference caused by the matrix of the aqueous solution. Thermal energy has been applied to the aqueous solution to assist in the evaporation of VOCs out of the aqueous matrix. By applying a cooling system to the IRE, the excess thermal energy can be removed leading to more stable IR signals. After examination of organic compounds with vapour pressure (Pv) ranging from 0.017 to 150 Torr, significant differences were found between IR signals from cooled and un-cooled systems. Because the thermal conductivity of the IRE used in IR detection is typically low; the efficiency in removing the thermal energy is limited. By heating the aqueous solutions to different temperatures, the IR signals showed that the sample temperature was limited to around 80 °C. The IR signal determination results for five different volatility organic compounds indicated that the optimal heating temperature was not necessary to match with the volatilities of organic compounds in cooling system. The linear regression coefficient (R2) of the standard curve for sample concentrations in the range 5-200 μg ml−1 was generally higher than 0.991 and the detection limit was around a few hundred ng ml−1, which was two to three times lower than that of un-cooled system. 相似文献
160.
V. Ya. Kavun N. F. Uvarov A. B. Slobodyuk V. K. Goncharuk A. Yu. Kotenkov I. A. Tkachenko A. V. Gerasimenko V. I. Sergienko 《Russian Journal of Electrochemistry》2005,41(5):501-509
Methods of (19F, 1H) NMR and impedance spectroscopy are used to investigate the internal mobility and ionic conduction in solid solutions arising in the system PbF2-ZrF4 and polycrystals KSnZrF7, Li(Na)(NH4)6Zr4F23, and M2ZrF6 (M = K, NH4). Factors responsible for the form of ionic motions and their energetics at 170–550 K are considered. It is established that the phase transitions in these compounds are connected with the crystal transition to a superionic state and that the high ionic (superionic) conductivity of beta phases is due to the diffusion of fluoride ions, ammonium cations, and possibly alkali metal cations. The obtained data testify to a substantial role of chainlike aggregation of anionic groupings and a variableness of structural mechanisms of formation of such chains in fluorozirconates for the development of translational diffusion in these compounds.__________Translated from Elektrokhimiya, Vol. 41, No. 5, 2005, pp. 573–582.Original Russian Text Copyright © 2005 by Kavun, Uvarov, Slobodyuk, Goncharuk, Kotenkov, Tkachenko, Gerasimenko, Sergienko. 相似文献