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1.
Solid-phase microextraction (SPME) with a disposable ionic liquid (IL) coating was developed for headspace extraction of benzene, toluene, ethylbenzene, and xylenes (BTEX) in paints. The SPME fiber was coated with IL prior to every extraction, then the analytes were extracted and desorbed on the injection port of gas chromatography, and finally the IL coating on the fiber was washed out with solvents. The coating and washing out of IL from the fiber can be finished in a few minutes. This disposable IL-coated fiber was applied to determine BTEX in water-soluble paints with results in good agreement with that obtained by using commercially available SPME fibers. For all the four studied paints samples, the benzene contents were under the detection limits, but relatively high contents of toluene, ethylbenzene and xylenes (56-271 microg g(-1)) were detected with spiked recoveries in the range of 70-114%. Compared to the widely used commercially available SPME fibers, this proposed disposable IL-coated fiber has much lower cost per determination, comparable reproducibility (RSD < 11%), and no carryover between each determination. Considering that IL possess good extractability for various organic compounds and metals ions, and that task-specific IL can be designed and synthesized for selective extraction of target analytes, this disposable IL coating SPME might has great potential in sample preparation. 相似文献
2.
In the presence of n-Bu4NBr acting as phase-transfer reagent, n-Bu4N+ salts of organophosphoryl polyoxotungstate derivatives [RP(O)]2X
n+W11O39
(8–n)– [R = PhCH2CH2P(O), X = P, Si; R = C6H11P(O); X = Ge, Ga] have been prepared and characterized by elemental analysis, i.r., 31P- and 183W-n.m.r. spectroscopy. According to the elemental analysis and spectroscopic data, the hybrid anions consist of an -[XW11O39] framework on which are grafted two equivalent organophosphoryl groups through P—O—W bridges; these new species still retain the Keggin structure. The six-line 183W spectrum indicates that hybrid anions possess C
s symmetry in MeCN. 相似文献
3.
Jin Yang Guo-Li Zheng Li Li Fang-Fang Li Yong-Mei Zhang Jing-Fu Liu 《Journal of solid state chemistry》2003,174(1):116-124
A series of divalent transition metal phosphonates containing hydrogen-bonded layers of phosphonate anions, namely [M(phen)3]·C6H5PO3·11H2O [M=Co(1), Ni(2), Cu(3)] and [Cd(phen)3]·C6H5PO3H·Cl·7H2O (4) have been synthesized, structurally characterized by single-crystal X-ray diffraction method. These compounds all crystallize in the triclinic system, space group P-1. The lattice parameters are a=12.1646(5), b=12.4155(6), c=15.4117(10) Å, α=78.216(2), β=79.735(3), γ=77.8380(3)°, V=2205.1(2) Å3, Z=2 for 1; a=12.097(2), b=12.606(3), c=15.742(3) Å, α=76.66(3), β=80.04(3), γ=77.75(3)°, V=2263.4(8) Å3, Z=2 for 2; a=12.058(2), b=12.518(3), c=15.781(3) Å, α=77.77(3), β=80.02(3), γ=77.91(3)°, V=2255.5(8) Å3, Z=2 for 3 and a=12.47680(10), b=12.6693(2), c=16.1504(3) Å, α=82.600(1), β=71.122(1), γ=77.355(1)°, V=2352.37(6) Å3, Z=2 for 4. All structures are refined by full-matrix least-squares methods [for 1, R1=0.0602 using 6458 independent reflections with I>2σ(I); for 2, R1=0.0632 using 4657 independent reflections with I>2σ(I); for 3, R1=0.0634 using 6221 independent reflections with I>2σ(I); for 4, R1=0.0400 using 7930 independent reflections with I>2σ(I)]. In the crystal structures, the phenylphosphonate anions and water molecules are hydrogen-bonded to form layers, and there exist the cationic species [M(phen)3]2+ between the adjacent layers of anions and water. Luminescence, thermal analysis as well as IR spectroscopic studies are also presented. 相似文献
4.
5.
纳米尺寸多酸脂质体复合物的合成及抗肿瘤活性研究 总被引:3,自引:0,他引:3
合成了杂多化合物α-K8H6[Si2W18Ti6O77](α-Si2W18Ti6)的脂质体纳米粒子.通过红外、固体核磁和极谱对其结构进行了表征,使用透射电镜和粒径分析仪研究了纳米粒子的形态和粒径分布.所合成的纳米粒子中多酸化合物仍保持母体的结构,纳米粒子的粒径在60~150nm之间.用MTT法测定了不同粒径纳米粒子的体外抗肿瘤活性.发现多酸化合物形成脂质体纳米粒子后稳定性和活性都有所提高. 相似文献
6.
A whole impulsive control scheme of nonlinear systems with time-varying delays, which is an extension for impulsive control of nonlinear systems without time delay, is presented in this paper. Utilizing the Lyapunov functions and the impulsive-type comparison principles, we establish a series of different conditions under which impulsively controlled nonlinear systems with time-varying delays are asymptotically stable. Then we estimate upper bounds of impulse interval and time-varying delays for asymptotically stable control. Finally a numerical example is given to illustrate the effectiveness of the method. 相似文献
7.
Studies on the redox properties of the heteropolytungstosilicates substituted by transition elements
The redox properties of the tri-heteropolytungstosilicates of transition elements KnSiZ(H2O)W11O39 (Z ? Mn2+, Fe3+, Co2+, Ni2+, Zn2+, Cd2+). In solution have been studied with polarography and cyclic voltammetry as well as with ultraviolet spectroscopy and X-ray photoelectron spectroscopy. The order of the polarographic half-wave potentials (E1/2) of these heteropolyanions is as follows: Z?Ni2+>Co2+>Zn2+>Fe2+>Mn2+. We have found that the E1/2 of heteropolyanions could be correlated linearly with both the electronegativities X of the transition elements and the logarithm of the rate constants (log ke) of reaction of transition metal ions with hydrated electrons. The reduction mechanism and effects of transition elements on the redox properties of the heteropolyanions have been discussed. 相似文献
8.
Yan-Jun Li Peng Wang Jing-Fu Ni Liang Meng Xiao-Bo Wang Chun-Qi Sheng Hong-Nian Li Wen-Hua Zhang Yang Xu Fa-Qiang Xu Jun-Fa Zhu 《Journal of Electron Spectroscopy and Related Phenomena》2011,184(7):414-419
We have measured and analyzed the photoemission spectra (PES) of a C70 film in the photon energy region from 13.4 eV to 98.4 eV. The photoelectron intensities of two C 2p π-derived features (denoted by A and B) oscillate regularly in the whole energy region with some fine structures below ∼30 eV. To obtain the detailed information of the oscillations, we have developed a sophisticated but practical procedure for intensity calculation. The procedure consists of two core concepts. The first is ascribing the PES features to their corresponding molecular orbitals with the help of density functional calculations. The second is a background subtraction algorithm. With this procedure, we obtained the oscillating behavior for individual features (A and B), which is by and large consistent with the predictions based on the spherical symmetric approximation although C70 has the ellipsoidal shape. Owing to the solid state effect, the oscillating amplitudes of the A/B intensity ratios are smaller than those of gas phase C70, but an orbital shift reported recently was not observed on our sample. The oscillating curve of a deeper feature, which consists of both σ and π states, are also reported. 相似文献
9.
A static and exhaustive extraction mode of hollow fiber-supported liquid membrane was developed for field sample passive pretreatment of environmental water samples. The extraction device was prepared by immobilizing dihexyl ether in the wall of a polypropylene hollow fiber membrane (60 cm length, 50 μm wall thickness, and 280 μm id) as liquid membrane and filling the fiber lumen with 0.1 M NaOH as acceptor, and closing the two ends of the fiber with an aluminum foil. Passive extraction was conducted by immersing the device into 15 mL water samples modified with 0.01 M HCl and 20% m/v NaCl. Model analytes including 4-chlorophenol, 2,4-dichlorophenol, and 2,4,6-trichlorophenol were transferred into acceptor with extraction efficiencies over 79% in 10 h at room temperature, and determined by high-performance liquid chromatography. The proposed method has the enrichment factor of 394-498 and LOD of 0.3-0.4 μg/L for the three chlorophenols. Humic acid and salinity in the environmentally relevant range had no significant influence on the extraction, and chlorophenols in various environmental waters were determined with spike recoveries between 71.6 and 120%. The static passive extraction nature benefited field sample pretreatment without power, whereas the exhaustive extraction mode effectively eliminated the sample matrix effects. 相似文献
10.
Xiao-Ting Liu Lu-Yi Zou Ai-Min Ren Jing-Fu Guo Ying Sun Shuang Huang Ji-Kang Feng 《Theoretical chemistry accounts》2011,130(1):37-50