Novel functionalized mesopore of SBA-15 as prospective sorbent for praseodymium and lutetium

In the present work, results of γ-irradiation on normal and functionalized SBA-15 by aurintricarboxylic acid have been reported. Characterization of normal and functionalized SBA-15 particles before and after γ-irradiation was carried out using Fourier-transform infrared technique. Aurintricarboxylic acid ligand connected to SBA-15 was also analyzed using UV/Vis spectrophotometer. The modified sorbent was then used as a new sorbent for separation of trace amounts of praseodymium and lutetium ions from nuclear waste waters in batch techniques. Based on the results of distribution coefficients determination, and investigation of sorption process in various conditions, the parameters were optimized for separation lanthanides. It can be concluded that the functionalized SBA-15 is a promising sorbent for praseodymium and lutetium cations.     

A novel dichromate-sensitive fluorescent nano-chemosensor using new functionalized SBA-15

A novel fluorescence nano-chemosensor for Cr₂O₇²⁻ anion has been developed by assembly of fluorescent aluminum complex of 8-hydroxyquinoline (AlQ_x) within the channels of modified SBA-15. SBA-SPS-AlQ_x shows a fluorescence emission at 486 nm. The observed remarkable fluorescence of SBA-SPS-AlQ_x quenches in presence of Cr₂O₇²⁻ anion. The results showed that this fluorescent nano-material can be a useful chemo-sensor for determination of dichromate anions in aqueous solutions. The linear detecting range of fluorescent nano-chemosensor for Cr₂O₇²⁻ anion was 0.16–2.9 μmol L⁻¹. The lowest limit of detection (LDL) was also found to be 0.2 ng mL⁻¹ in aqueous solutions. SBA-SPS-AlQ_x showed selectively and sensitively fluorescent quenching response toward Cr₂O₇²⁻ ion in comparison with I₃⁻, NO₃⁻, CN⁻, CO₃²⁻, Br⁻, Cl⁻, F⁻, H₂PO₄⁻ and SO₄²⁻ ions, which was because of the higher stability of its inorganic complex with dichromate ion.     

A study on the formation of strontium hexaferrite nanopowder by a sol–gel auto-combustion method in the presence of surfactant

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.     

A novel Lu fluorescent nano-chemosensor using new functionalized mesoporous structures

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.     

Preparation of a New Solid‐Phase Microextraction Fiber by Coating Silylated Nanoporous Silica on a Copper Wire

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.     

The synthesis and spectroscopic characterization of nano calcium fluorapatite using tetra-butylammonium fluoride

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.     

Selective recognition of monohydrogen phosphate by fluorescence enhancement of a new cerium complex

Bis(8-hydroxy quinoline-5-solphonate) cerium(III) chloride (Ce(QS)(2)Cl) (L) was synthesized and then used as a novel fluorescent sensor for anion recognition. Preliminarily study showed that fluorescence of L enhanced selectively in the presence of HPO(4)(2-) ion. This enhancement is attributed to a 1:1 complex formation between L and HPO(4)(2-) anion. The association constant of 1:1 complex of L-HPO(4)(2-) was calculated as 3.0×10(6). Thus, L was utilized as a basis for a selective detection of HPO(4)(2-) anion in solution. The linear response range of the proposed fluorescent chemo-sensor covers a concentration range of HPO(4)(2-) from 3.3×10(-7) to 5.0×10(-6) mol L(-1) with a detection limit of 2.5×10(-8) mol L(-1). L showed selective and sensitive fluorescence enhancement response toward HPO(4)(2-) ion in comparison with I(3)(-), NO(3)(-), CN(-), CO(3)(2-), Br(-), Cl(-), F(-), H(2)PO(4)(-) and SO(4)(2-) ions. It was probably attributed to the higher stability of the inorganic complex between HPO(4)(2-) ion and L. The method was successfully applied for analysis of phosphate ions in some fertilizers samples.     

A three-dimensional highly stable cobalt(II) metal–organic framework based on terephthalic acid: synthesis, crystal structure, thermal and physical properties

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.     

Photo and Chemical Reduction of Copper onto Anatase‐Type TiO2 Nanoparticles with Enhanced Surface Hydroxyl Groups as Efficient Visible Light Photocatalysts

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.     

Investigation of environmental and concentration effects on fluorescence properties of AlQ<Subscript>3</Subscript> using mesoporous silica and polyacrylate

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.