Environ Sci Pollut Res Int
November 2022
The synthesis of silica gel nanostructures and loading it with copper specie via a hydrothermal process were performed. The sample is treated with an amino-functional reagent 3-aminopropyl triethoxysilane (APTES). The products were characterized by X-ray diffraction (XRD), FT-IR, scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive spectroscopy (EDS), TGA/DSC measurements, and X-ray photoelectron spectroscopy (XPS).
View Article and Find Full Text PDFIn this work, a novel mode of hollow fiber liquid-phase microextraction (HF-LPME) technique namely rotating extraction cell solvent bar microextraction (REC-SBME) was introduced. The proposed method was applied for the preconcentration of methylene blue (MB) and rhodamine 6G (RG) in some real samples, including soft drink, lipstick, environmental water, and wastewater samples. In the extraction setup, two pieces of hollow fibers were fixed on a mechanical support and immersed in a rotating extraction cell containing the sample solution during the extraction process.
View Article and Find Full Text PDFIn this work, trace determination of nitrite in river water samples was studied using solvent stir bar microextraction system with three-hollow fiber configuration (3HF-SSBME) as a preconcentration step prior to UV-Vis spectrophotometry. The obtained results showed that the increase in the number of solvent bars can improve the extraction performance by increasing the contact area between acceptor and sample solutions. The extraction process relies on the well-known oxidation-reduction reaction of nitrite with iodide excess in acidic donor phase to form triiodide, and then its extraction into organic acceptor phase using a cationic surfactant.
View Article and Find Full Text PDFIn this work, for the first time, a revolving solvent bar microextraction (RSBME) system was introduced as an efficient alternative method to conventional SBME. The setup proposed for RSBME provides a stable and repeatable method to increase the preconcentration factor. In order to provide the maximum extraction capacity of the organic acceptor phase, four-hollow fibers were applied.
View Article and Find Full Text PDFThe purpose of this research was to optimize a new method for preconcentration and determination of trace iron concentrations in aqueous solutions. For this purpose, a newly synthesized ligand, 3-(3-hydroxy-2-methyl-4-oxopyridin-1(4H)-yl) benzoic acid (3-OH-3-MOPBA), was used in the dispersive liquid-liquid microextraction (DLLME) method coupled with UV-vis spectroscopy. The experiments considering input variables of extractant volume, disperser volume, salt concentration, and pH were designed with the aid of central composite design (CCD).
View Article and Find Full Text PDFSpectrochim Acta A Mol Biomol Spectrosc
October 2018
In this study, lanthanum-containing mesoporous MCM-41 (La-MCM-41) with different amount of lanthanum were synthesized and were used for colorimetric detection of glucose. As prepared La-MCM-41 were characterized by X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). The quantitative amounts of incorporated lanthanum into MCM-41 structure were estimated by energy dispersive X-ray spectrometry.
View Article and Find Full Text PDFThe aim of this study was to establish a new dispersive liquid-liquid microextraction (DLLME) technique for the determination of iron concentration in aqueous solutions and fruit juices based on the reaction between iron and 3-hydroxy-1-(3-hydroxyphenyl)-2-methylpyridin-4(1H)-one (3-OH-PMPO) as a chelating agent. A central composite design (CCD) was applied to optimize the effects of independent parameters (pH, volume of disperser solvent and extractant solvent and chelating agent concentration) on extraction efficiency. Under the optimized conditions, the analytical curve is linear in a concentration range of 10-750 μgL with a detection limit of 5 μgL.
View Article and Find Full Text PDFAn efficient method was applied for extraction of caffeine in food samples. Three-dimensional graphene-FeO (3D-G-FeO) nanoparticles was successfully synthesized and used as adsorbent in magnetic solid phase extraction (MSPE) step. The properties of synthesized adsorbent were characterized by fourier-transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM), vibrating sample magnetometer (VSM), X-ray diffraction (XRD), Raman spectroscopy, Brunauer-Emmett-Teller (BET) and Barrett-Joyner-Halenda (BJH) methods.
View Article and Find Full Text PDFIn this study dependency of simultaneous adsorption of Congo Red (CR), Phloxine B (BP) and Fast green FCF (FG) onto CuS/ZnS nanocomposites loaded on activated carbon (CuS/ZnS-NCs-AC) to pH, adsorbent mass, sonication time and initial dyes concentration were modeled and optimized, while CuS/ZnS-NCs-AC was identified by XRD, FESEM and EDS analysis. CR, PB and FG concentration determination were undertaken by first and second order derivative spectrophotometry in ternary mixture. According to central composite design (CCD) based on desirability function (DF), the best experimental conditions was set as pH 6.
View Article and Find Full Text PDFA sensitive procedure namely ultrasound-assisted (UA) coupled dispersive nano solid-phase microextraction spectrophotometry (DNSPME-UV-Vis) was designed for preconcentration and subsequent determination of gallic acid (GA) from water samples, while the detailed of composition and morphology and also purity and structure of this new sorbent was identified by techniques like field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD) and Energy-dispersive X-ray spectroscopy (EDX) techniques. Among conventional parameters viz. pH, amount of sorbent, sonication time and volume of elution solvent based on Response Surface Methodology (RSM) and central composite design according to statistics based contour the best operational conditions was set at pH of 2.
View Article and Find Full Text PDFThe current techniques for determining adenine have several shortcomings such as high cost, high time consumption, tedious pretreatment steps and the requirements for highly skilled personnel often restrict their use in routine analytical practice. This paper describes the development and utilization of a new nanocomposite consisting of titanium dioxide nanofibers (TNFs) and graphene oxide nanosheets (GONs) for screen printed carbon electrode (SPCE) modification. The synthesized GONs and TNFs were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR).
View Article and Find Full Text PDFSpectrochim Acta A Mol Biomol Spectrosc
December 2015
A series of silicon incorporated TiO2 with anatase crystalline phase were prepared via sol-gel using ammonium hexafluorosilicate (AHFS). The synthesized products were characterized using X-ray diffraction, FTIR, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), UV-vis diffuse reflectance spectrophotometry (DRS), energy dispersive X-ray analysis (EDX) and BET surface area measurement. Presence of Si-O-Ti bonds is revealed based on the XPS results.
View Article and Find Full Text PDFNanocomposits of zinc oxide co-doped with lanthanum and zirconium were prepared using the modified sol-gel method. The samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), diffuse reflectance spectroscopy (DRS), and BET surface area measurement. For comparison, the La and Zr mono doped ZnO have also been prepared under the same conditions.
View Article and Find Full Text PDFSpectrochim Acta A Mol Biomol Spectrosc
September 2014
Metal-semiconductor compounds, such as Ag/AgX (X=Cl, Br, I), enable visible light absorption and separation of photogenerated electron-hole through surface plasmon resonance (SPR) effect. However, the electron-hole generated and separated by light are vulnerable in Ag/AgX phase because of the occurrence of secondary recombined. In order to more effectively utilize the SPR photocatalytic effect, nanoparticles are located in a matrix.
View Article and Find Full Text PDFSpectrochim Acta A Mol Biomol Spectrosc
April 2014
The synthesis of CuS nanomaterial in MCM-41 matrix has been realized by chemical synthesis between MCM-41, copper sulfate pentahydrate and thiourea via a solvothermal method in ethylene glycol and water, separately. X-ray diffraction analysis (XRD), diffuse reflectance spectroscopy (DRS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and fourier transform infrared (FT-IR) were used to characterize the products. At synthesized CuS/MCM-41 sample in ethylene glycol, X-ray diffraction and diffuse reflectance spectroscopy showed pure covellite phase of copper sulfide with high crystality.
View Article and Find Full Text PDFBiVO4-silica composites were prepared and grafted with sulfonated cobalt phthalocyanine. The structural and chemical properties including crystalline phase, specific surface area, UV-Visible diffuse reflectance behavior, morphology and photocatalytic activity were investigated. Depending on the silica content and subsequently amounts of loaded phthalocyanine, various catalytic activities were observed.
View Article and Find Full Text PDFThis paper describes the development and utilization of a new nanocomposite consisting of Cu(OH)2 nanoparticles, hydrophobic ionic liquid 1-ethyl-3-methylimidazolium hexafluorophosphate (EMIMPF6) and multiwalled carbon nanotubes for glassy carbon electrode modification. The nanocomposite was characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM) along with energy-dispersive X-ray spectroscopy (EDX). The modified electrode was used for electrochemical characterization of diclofenac.
View Article and Find Full Text PDFUltrason Sonochem
September 2012
We demonstrate a sonication procedure for the removal of structure-directing micellar templates from mesoporous MCM-41. The method uses a 28 KHz ultrasound in an alcoholic solvent for disrupting micellar aggregation of the surfactant molecules, cetyltrimethylammonium bromide, which have filled the pores of the as-synthesized MCM-41. The majority (93%) of the surfactant molecules are removed out from the powder MCM-41 within a 15 min one-step sonication at a moderate temperature of 40°C.
View Article and Find Full Text PDFSpectrophotometry in combination with ionic liquid-based dispersive liquid-liquid microextraction (DLLME) was applied for the extraction and determination of formaldehyde in real samples. The method is based on the reaction of formaldehyde with methyl acetoacetate in the presence of ammonia. The variation in the absorbance of the reaction product was measured at 375 nm.
View Article and Find Full Text PDFA PVC membrane La (III) ion-selective electrode has been constructed using ethyl1,2,3,4-tetrahydro-6-methyl-4-phenyl-2-thioxopyrimidine-5-carboxylate (ETMPTC) as a neutral ionophore. This electrode responds to La (III) ion with a sensitivity of 19.9 ± 0.
View Article and Find Full Text PDFThe photocatalytic activity of sulphonated cobalt phthalocyanine immobilized onto MCM-41 was investigated for decomposition of 2,4-dichlorophenol (2,4-DCP) in aqueous solutions. Immobilization of anion sulpho-cobalt phthalocyanine to the walls of MCM-41 was performed by pre-anchorage of 3-(aminopropyl)-triethoxysilane (APTES) onto MCM-41 via post-synthesis method. X-ray diffraction, nitrogen physisorption, diffuse reflectance spectroscopy, energy-dispersive X-ray and FT-IR methods were used to characterize the product.
View Article and Find Full Text PDFThe use of titania-dispersed materials in photocatalytic processes has been proposed as an alternative to the conventional bare TiO(2), in order to modify the surface area and activity of the catalyst. A homogeneously dispersed Keggin unit into TiO(2) was synthesized using tungstophosphoric acid (TPA) and titanium tetraisopropoxide. This compound was then loaded into MCM-41 by dispersing it in a suspension containing the mesoporous phase.
View Article and Find Full Text PDFDiffuse reflectance spectroscopy (DRS) can be used as a rapid and sensitive method for the quantitative determination of low amounts of aluminum. In this analytical technique, the analyte in samples are extracted onto a solid sorbent matrix loaded with a colorimetric reagent and then quantified directly on the adsorbent surface. Alternatively, colored aluminum complexes formed in solution can also be immobilized onto adsorbent surface and be measured by DRS technique.
View Article and Find Full Text PDFA new PVC membrane strontium ion-selective electrode has been constructed using 6-(4-nitrophenyl)-2-phenyl-4,4-dipropyl-3,5-diaza-bicyclo[3,1,0] hex-2-ene (NPDBH) as a neutral ionophore. The electrode was prepared with 7% NPDBH (as ionophore), 57% acetophenone (as plasticizer), 30% PVC and 6% oleic acid (as lipophilic additive). The electrode responds to Sr2+ ion with a sensitivity of 28.
View Article and Find Full Text PDFJ Pharm Biomed Anal
December 2003
A coated wire triamterene-selective electrode based on the incorporation of a triamterene-tetraphenylborate ion-pair in a poly(vinylchloride) coating membrane was constructed. The influence of membrane composition, temperature, pH of the test solution, and foreign ions on the electrode performance were investigated. The electrode showed a Nernstian response over a triamterene concentration range from 1.
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