LUS‐1 typed nanoporous silica particles were synthesized and silylated with hexamethyldisilazane and investigated as a highly porous fiber coating for solid‐phase microextraction (SPME). The pore size distribution of the prepared Sil‐LUS‐1 was still typical of MCM‐41 and centered at 3 nm with a specific surface area of 720 m2g?1. The SPME fiber was prepared by liming the material on a copper wire. The extraction efficiency of the new fiber was compared with a commercial PDMS fiber for headspace extraction and GC‐MS analysis of phenol, 4‐nitrophenol, 2,4‐dichlorophenol and 4‐chlorophenol in water samples. Due to the high porosity of the prepared fiber it showed a higher sensitivity and better selectivity for the extraction of the target compounds. For optimization of different factors affecting the extraction efficiency, a simplex optimization method was used. The relative standard deviation for the measurements by one fiber was better than 7% for five replicates and the fiber‐to‐fiber reproducibility was about 10% for five fabricated fibers. Detection limits in the range of 0.002 to 0.026 μg mL?1 were obtained for the phenolic compounds. The fiber was successfully applied for the determination of phenolic compounds in natural water samples. 相似文献
A new dipyridyl‐functionalized silica gel (DPSG) was synthesized. The potentiometric response of silver ion was investigated at a carbon paste electrode chemically modified with functionalized nanoporous silica gel. The electrodes with a DPSG proportions of 10.1% (w/w), showed very stable potential. Calibration plots with Nernstian slopes for Ag+ were observed, 58.7 (±0.9) mV decade?1, over a wide linear range of concentration (5.0×10?7 to 1.0×10?1 M). The electrode has a detection limit of 1.0×10?7 M. The selectivity coefficients measured by the match potential method in acetate buffer, pH 5.5, were investigated. The electrode has fast response time, high performance, high sensitivity in wide cation activity ranges, and good long term stability (more than 6 months). The method was satisfactory and used to determine the concentration of silver ion in waste waters contaminated by this metal. 相似文献
CMK-3 nanoporous carbon was prepared and used as an efficient sorbent for microextraction in packed syringe of rosmarinic acid in Rosmarinus officinalis L. (rosemary). In the proposed method, only 2 mg of the nanoporous material, inserted between a syringe’s barrel and needle, was sufficient for the extraction with minimum consumption of organic solvents. Sample preparation was performed on the packed bed using a laboratory-made programmable apparatus. The apparatus was designed and used for automation of the conditioning, sampling, washing and elution steps of the method, and increasing the reproducibility of the experiments. For optimization of the experimental parameters, a central composite design method was used. Under the optimized conditions (i.e., number of adsorption cycles 14 times, number of elution cycles ten times and volume of elution 100 μL), an extraction recovery of 90 (±4.5) % was obtained for rosmarinic acid. The same packing bed could be used for at least 80 extractions without significant changes in its properties. The efficiency of the nanoporous sorbent was found to be superior to that of activated carbon, by a factor of about 17. The proposed method was successfully applied to the extraction of three rosemary samples before analysis by HPLC.
In this study, the photocatalytic efficiency of anatase‐type TiO2 nanoparticles synthesized using the sol–gel low‐temperature method, were enhanced by a combined process of copper reduction and surface hydroxyl groups enhancement. UV–light‐assisted photo and NaBH4‐assisted chemical reduction methods were used for deposition of copper onto TiO2. The surface hydroxyl groups of TiO2 were enhanced with the assistance of NaOH modification. The prepared catalysts were immobilized on glass plates and used as the fixed‐bed systems for the removal of phenazopyridine as a model drug contaminant under visible light irradiation. NaOH‐modified Cu/TiO2 nanoparticles demonstrated higher photocatalytic efficiency than that of pure TiO2 due to the extending of the charge carriers lifetime and enhancement of the adsorption capacity of TiO2 toward phenazopyridine. The relationship of structure and performance of prepared nanoparticles has been established by using various techniques, such as XRD, XPS, TEM, EDX, XRF, TGA, DRS and PL. The effects of preparation variables, including copper content, reducing agents rate (NaBH4 concentration and UV light intensity) and NaOH concentration were investigated on the photocatalytic efficiency of NaOH‐modified Cu/TiO2 nanoparticles. 相似文献
A metal?Corganic framework complex, [Co(??3?Ctp)(??2?pyz)]n, where H2tp?=?1,4-benzenedicarboxylic acid (terephthalic acid) and pyz?=?pyrazine, has been synthesized under hydrothermal conditions and characterized by physico-chemical and spectroscopic methods, thermogravimetric analysis and single-crystal X-ray diffraction. Each Co(II) center is surrounded by four carboxylate oxygen atoms from three tp ligands and two nitrogen atoms from two pyrazine ligands, giving a distorted octahedral geometry. The entire framework is made up of two-dimensional sheets of dicobalt ions linked via terephthalate ligands to form rectangles. The sheets are then linked into each other via the axial pyrazine ligands, forming an interlocked 3-D network, which is finally arranged as an ABAB interconnected pattern. Photoluminescence measurements for the polymer in the solid state show an emission at 414?nm, which suggests this complex as a potential blue-light material. The electrochemical behavior of a modified carbon paste electrode prepared from the complex has been studied by cyclic voltammetry, indicating quasi-reversible redox behavior. 相似文献
A new Lu3+ sensitive fluorescent chemosensor is designed using 8-hydroxyquinoline functionalized mesoporous silica with highly ordered structure (LUS-SPS-Q). The characterization of LUS-SPS-Q showed that the organized structure has been preserved after the post grafting procedure. The synthesized material showed a selective interaction with Lu3+ ion, most probably due to the presence of the fluorophore moiety at its surface. The emission intensity of the Lu3+-bound mesoporous material increases with an increase in concentrations of Lu3+ ion. Addition of other mono-, di-, trivalent ions resulted in insignificant change in the fluorescent intensity. The enhancement of fluorescence is attributed to the strong covalent binding of Lu3+ ion. The linear response range of Lu3+ chemo-sensor was from 1.6 × 10−7 to 1.0 × 10−5 mol L−1. The Limit of detection obtained was 8.2 × 10−8 mol L−1 and the pH range which the proposed chemo-sensor can be applied was 3.3–8.3. 相似文献
In this work, for the first time, control over the position of maximum emission peak for fluorophore, using embedded tris(8-hydroxyquinoline) aluminum (AlQ3) complexes into different types of host materials, can be achieved. Moreover, the environmental and concentration effects on luminescent properties were studied. In this regard, different concentrations of AlQ3 were embedded into the poly(methyl methacrylate-co-butyl acrylate) (PMMA-co-PBuA) nanoparticles as organic host materials by emulsion polymerization. It is established that the dilution of AlQ3 in the polymer matrix leads to blue-shift of the luminescence maximum up to 0.32 eV compared to pure AlQ3. Moreover, AlQ3 was embedded in SBA-15 type mesoporous silica as an inorganic host material by physical adsorption. Finally, this functionalized mesoporous silica was incorporated into PMMA-co-PBuA transparent matrix by blending method to obtain Co-Poly-AlQ3-SBA-15 as organic–inorganic composite material. It was found that there is no significant wavelength shift on the maximum emission peak of the organic–inorganic composite at various concentrations of AlQ3-SBA-15. The prepared materials were characterized by powder X-ray diffraction (XRD), N2 adsorption–desorption, NMR, Fourier transform infrared (FT-IR), dynamic light scattering (DLS), scanning electron microscopy (SEM) and fluorescence spectra. 相似文献
Strontium hexaferrite is a hard magnetic material and has been extensively used as a permanent magnet. In this work, a novel sol–gel auto-combustion method was used to synthesize ultra-fine strontium hexaferrite, and the effect of the surfactant on the crystallite size of the final product was investigated for the first time. The DTA/TGA plot exhibited the formation temperature of hexaferrite. The XRD results show that adding surfactant to the sol does not change the composition of the combustion product and the surfactant burns completely during the combustion process. The average crystallite size of hexaferrite powders was also measured by the X-ray line broadening technique employing the Scherrer formula. The results show that adding surfactant to the gel makes the particle size of the final product much smaller. 相似文献
Pure homogeneous nano sized biocompatible fluorapatite (FAp) particles were synthesized by a wet chemical procedure using water soluble tetra-butylammonium fluoride (TBAF) without using high temperatures and any purification processes. Combination of the Bragg's law and the plane-spacing equation for the two high intensity lines, namely, (002) and (300), gives a=9.3531 ?, c=6.8841 ?, confirms the identity of the highly crystalline synthetic material as well as its purity. The effect of various pH's in crystal formation and on their size was also evaluated. The calculated crystallinities were excellent with a rate around 5.0. The synthesized nano FAp was fully characterized by spectroscopic techniques (XRD, SEM, EDS, BET, FT-IR and ICP-AES). The nitrogen adsorption-desorption isotherm showed a type IV diagram and calculation of the surface area was investigated as well. 相似文献