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991.
Microwave-assisted thermal desorption (MAD) coupled to headspace solid-phase microextraction (HS-SPME) has been studied for
in-situ, one-step, sample preparation for PAHs collected on XAD-2 adsorbent, before gas chromatography with mass spectrometric
detection. The PAHs on XAD-2 were desorbed into the extraction solution, evaporated into the headspace by use of microwave
irradiation, and absorbed directly on a solid-phase microextraction fiber in the headspace. After desorption from the SPME
fiber in the hot GC injection port, PAHs were analyzed by GC–MS. Conditions affecting extraction efficiency, for example extraction
solution, addition of salt, stirring speed, SPME fiber coating, sampling temperature, microwave power and irradiation time,
and desorption conditions were investigated. Experimental results indicated that extraction of 275 mg XAD-2, containing 10–200 ng
PAHs, with 10-mL ethylene glycol–1 mol L−1 NaCl solution, 7:3, by irradiation with 120 W for 40 min (the same as the extraction time), and collection with a PDMS–DVB
fiber at 35 °C, resulted in the best extraction efficiency. Recovery was more than 80% and RSD was less than 14%. Optimum
desorption was achieved by heating at 290 °C for 5 min. Detection limits varied from 0.02 to 1.0 ng for different PAHs. A
real sample was obtained by using XAD-2 to collect smoke from indoor burning of joss sticks. The amounts of PAHs measured
varied from 0.795 to 2.53 ng. The method is a simple and rapid procedure for determination of PAHs on XAD-2 absorbent, and
is free from toxic organic solvents. 相似文献
992.
Lidia Jasińska A. Balas J. T. Haponiuk G. Nowaczyk S. Jurga 《Journal of Thermal Analysis and Calorimetry》2007,88(2):419-423
New cross-linked poly(esterurethanes) (PEU) based on unsaturated olygo(alkyleneester)diol
(OAE), 4,4’-diphenylmethane diisocyanate (MDI) and styrene or methyl
methacrylate as curing monomers were prepared. The synthesis of PEU was performed
in two steps. In the first step OAE was obtained from adipic acid, maleic
anhydride and ethylene glycol. In the second step a prepolymer was obtained
in a reaction of OAE with different amounts of 4,4’-diphenylmethane
diisocyanate followed by crosslinking using previously mentioned curing monomers.
The influence of structure of the poly(esterurethanes) on thermal and dynamic
mechanical properties is studied. Thermogravimetric analysis shows that cross-linked
poly(esterurethanes) demonstrate high thermal stability. Moreover the dynamic
mechanical thermal analysis shows that the presence of styrene cross-linking
chains in polymers lead to the phase separation in cross-linked poly(esterurethanes). 相似文献
993.
We quantitatively modeled the volume phase transition of a hydrogel containing a crystalline colloidal array with a crown
ether ligand which binds Pb2+. The hydrogel volume response and the wavelength diffracted depend on the Pb2+ concentration and on both the ionic strength and the valence of the nonbinding ionic species. We successfully modeled the
response of this hydrogel Pb2+ sensor to ionic strength and the cation valence of the added salts.
Figure Cation identity dependence of crown ether photonic crystal Pb+ sensing 相似文献
994.
995.
Pérez-Sirvent C Martínez-Sánchez MJ García-Lorenzo M López-García I Hernández-Córdoba M 《Analytical and bioanalytical chemistry》2007,388(2):495-498
Use of small membrane pumps, instead of peristaltic pumps, to introduce sample and reagent solutions into the spectrometer
has several advantages in atomic fluorescence spectrometric determination of mercury. This simple modification results in
a substantial saving in the time required for the measurements and so 90% of reagent solution volumes and 95% of sample solution
volumes are saved, with a consequent decrease in the volume of waste generated. The sampling frequency is almost tripled,
with no deterioration in sensitivity, which is similar to that obtained by use of peristaltic pumps. The relative standard
deviation for ten consecutive measurements of a 1 μg L−1 mercury solution was approximately 2%.
Figure Small membrane pumps for the atomic fluorescene spectro metric determination of mercury 相似文献
996.
Sumit Saxena Archana Asokkumar K Bansi Lal 《Journal of Sol-Gel Science and Technology》2007,41(3):245-248
Terbium Aluminum Garnet (TAG) is an important optically active material and is one of the best materials known for the fabrication
of optical isolators. TAG has a large Verdet constant and has good transmission in the region of 350–1500 nm of the electromagnetic
spectrum. It is also known that TAG melts incongruently at 1840°C. This makes efficient synthesis of TAG important and challenging
and forms the motivation of the present work to develop techniques for the synthesis of TAG at lower temperatures. In the
present work we report the synthesis of TAG using sol-gel techniques following the citrate-nitrate route. The prepared sample
is sintered at various temperatures in presence of air and characterized using X-ray diffraction, FT-IR spectroscopy, energy
dispersive X-ray Analysis and the morphology is observed using the scanning electron microscopy. 相似文献
997.
Stéphanie Etienne C. Becker D. Ruch B. Grignard G. Cartigny C. Detrembleur C. Calberg R. Jerome 《Journal of Thermal Analysis and Calorimetry》2007,87(1):101-104
Silica nanoparticles of various sizes have
been incorporated by melt compounding in a poly(methyl methacrylate) (PMMA)
matrix to enhance its thermal and mechanical properties. In order to improve
nanoparticles dispersion, PMMA grafted particles have been prepared by atom
transfer radical polymerization (ATRP) from well-defined silica nanoparticles.
This strategy was expected to ensure compatibility between both components
of the PMMA nanocomposites. TEM analysis have been performed to evaluate the
nanosilica dispersion whereas modified and non-modified silica/PMMA nanocomposites
thermal stability and mechanical properties have been investigated by both
thermogravimetric and dynamical mechanical analysis. 相似文献
998.
A new liquid-phase microextraction method based on solidification of floating organic drop 总被引:2,自引:0,他引:2
In the present study, a new and versatile liquid-phase microextraction method is described. This method requires very simple and cheap apparatus and also a small amount of organic solvent. Eight microliters of 1-undecanol was delivered to the surface of solution containing analytes and solution was stirred for a desired time. Then sample vial was cooled by inserting it into an ice bath for 5 min. The solidified 1-undecanol was transferred into a suitable vial and immediately melted; then, 2 μL of it was injected into a gas chromatograph for analysis.Some polycyclic aromatic hydrocarbons (PAHs) were used as model compounds for developing and evaluating of the method performance. Analysis was carried out by gas chromatography/flame ionization detection (GC/FID).Several factors influencing the microextraction efficiency, such as the nature and volume of organic solvent, the temperature and volume of sample solution, stirring rate and extraction time were investigated and optimized. The applicability of the technique was evaluated by determination of trace amounts of PAHs in environmental samples. Under the optimized conditions, the detection limits (LOD) of the method were in the range of 0.07-1.67 μg L−1 and relative standard deviations (R.S.D.) for 10 μg L−1 PAHs were <7%. A good linearity (r2 > 0.995) in a calibration range of 0.25-300.00 μg L−1 was obtained. After 30 min extraction duration, enrichment factors were in the range of 594-1940. Finally, the proposed method was applied to the determination of trace amounts of PAHs in several real water samples, and satisfactory results were resulted. Since very simple devices were used, this new technique is affordable, efficient, and convenient for extraction and determination of low concentrations of PAHs in water samples. 相似文献
999.
Czesław Rudowicz Ireneusz Stefaniuk Roman Dziembaj Hitoshi Ohta Marcin Molenda Susumu Okubo Makoto Yoshida 《Research on Chemical Intermediates》2007,33(8):853-862
This paper deals with the analysis of the temperature dependence of high-frequency EMR (HF-EMR) spectra due to Mn3+ and Mn4+ ions in the lithium manganese spinel LiMn2O4. A range of powder samples obtained by the sol-gel method with calcinations in several temperature ranges were prepared for
this study. Based on the initial characterization carried out by a number of techniques, the physicochemical and structural
properties of the samples were earlier determined. Independently, temperature magnetization and HF-EMR measurements were carried
out. The EMR spectra vary strongly between samples, indicating possible structural or chemical changes. Quantitative analysis
of the temperature dependence of the HF-EMR spectra due to Mn3+ and Mn4+ ions in LiMn2O4 is presented in this paper. The spectral analysis concerns the line shape, linewidth, intensity and g-factors. Fittings using the Lorentzian spectral shape and, to a certain extent, the Gaussian spectral shape have been carried
out in order to parameterize the temperature dependence of the HF-EMR spectra. This parameterization of the HF-EMR experimental
data enables a deeper characterization of the samples. Subsequently, a better insight into the role of the Mn3+ and Mn4+ ions in accounting for the characteristics most suitable for application of LiMn2O4 as a cathode material may be gained. 相似文献
1000.
In this study, swelling behavior and mechanical properties of polyelectrolyte cationic hydrogels of poly((2-dimethylamino) ethyl methacrylate) (PDMAEMA), and poly((2-dimethylamino) ethyl methacrylate-co-butyl methacrylate) (P(DMAEMA-co-BMA)), were investigated. Hydrogels were prepared by free-radical solution copolymerization of DMAEMA and BMA using ethylene glycol dimethacrylate (EGDMA) as the crosslinking agent. Compression-strain measurements were used to analyze the mechanical properties of the hydrogels. It was found that increasing the amount of BMA comonomer in the gel structure increases the compression modulus of the material. The results of mechanical measurements were used to characterize the network structure of the hydrogels, namely the effective crosslinking density (. It was found that exceeds the theoretical crosslinking density (νt) calculated from the initial amount of EGDMA used for hydrogel synthesis. These hydrogels demonstrated dual sensitivity to both pH and temperature. It was shown that the pH-sensitive or temperature-sensitive phase transition behavior of the gels can be changed by changing the temperature or pH of the swelling medium at constant hydrogel composition. Increasing the temperature decreased the transition pH of the pH-sensitive phase transition. On the other hand, increasing the pH of the surrounding medium decreased the transition temperature of the temperature-sensitive phase transition. Incorporation of BMA in the gel structure has a significant effect on the transition point of the gel. Increasing the BMA content reduced the transition pH and temperature of the pH- and temperature-sensitive phase transition, respectively. The similar effect of increasing temperature or BMA content can be explained by the role of hydrophobicity in the phase transition behavior of hydrogels. Finally, the results of equilibrium swelling and compression-strain measurements were used to calculate the polymer-solvent interaction parameters of these hydrogels using the Flory-Rehner equation of equilibrium swelling. 相似文献