Sharif Digital Repository

A magnetic polyurethane (PU) nanocomposite was synthesized by an electrospinning technique and applied for isolation and preconcentration of fluoxetine from aquatic and biological samples. The nanocomposite was electrospun using a PU polymer solution containing the dispersed magnetic nanoparticles. The magnetic properties of iron nanoparticles, along with the use of an electrospinning technique, led to the formation of a suitable sorbent toward isolation of fluoxetine. The magnetic PU nanofibers could be subsequently removed from the sample solution by applying a permanent magnet. The scanning electron microscopy (SEM) image of the magnetic PU nanofibers confirms that their diameters are in... 

In salting-out liquid-liquid extraction (SALLE) technique, water-miscible organic solvents are used for extraction of polar analytes from saline solutions. In this study, for the first time, a coupled 1-mL syringes system was utilized to perform a miniaturized SALLE method. Sulfanilamide antibiotic was extracted and determined via the developed method followed by high performance liquid chromatography-ultraviolet detection (HPLC-UV). The extraction process was carried out by rapid shooting of acetonitrile as extraction solvent (syringe B) into saline aqueous sample solution (syringe A), and then the shooting was repeated several times at a rate of 1 cycle s-1. Thereby, an extremely large... 

The objective of the work ahead is presentation of a new carbon paste electrode (CPE) modified by TiO2 nanoparticles (TiO2NPs) and 1,2-bis-[o-aminophenyl thio] ethane (APTE) ligand as a selective cation receptor for determination of the Cd (II) ions using differential pulse anodic stripping voltammetry (DPASV). The electrode shows an excellent tendency to Cd (II) ions in presence of some interfering species. Under the optimum conditions, a linear calibration curve was obtained in the concentration range of 2.9 nM to 4.6 μM with a correlation coefficient of 0.9969 in the anodic potential of 0.54 (V vs. Ag/AgCl). The metal detection limit was 2.0 nM after 10 min preconcentration (S/N = 3). The... 

Titanium(IV) tetraisopropoxide was employed as a metal oxide sol-gel precursor to prepare ceramic composite nanofibers by the electrospinning system. To facilitate this process and obtain the desired nanofibers with higher aspect ratios and surface area, poly(vinylpyrrolidone) was added to the sol of titania. Four ceramic nanofibers sheets based on titania were prepared while each sheet contained different transition metals such as Fe-Mn, Fe-Ni, Fe-Co, and Fe-Mn-Co-Ni. The scanning electron microscope images showed good homogeneity for all the prepared ceramic composites with a diameter range of 100-250 nm. The sorption efficiency was investigated by a micro-solid-phase extraction setup in... 

A high-temperature-resisant solid-phase microextraction (SPME) fiber was prepared based on polyetherimide (PEI) by the electrospinning method. The PEI polymeric solution was converted to nanofibers using high voltages and directly coated on a stainless steel SPME needle. The scanning electron microscopy images of PEI coating showed fibers with diameter range of 500-650 nm with a homogeneous and smooth surface morphology. The SPME nanofibers coating was optimized for PEI percentage, electrospinning voltage, and time. The extraction efficiency of the coating was investigated for headspace SPME of some environmentally important polycyclic aromatic hydrocarbons from aqueous samples followed by... 

A horizontally oriented liquid-liquid-liquid microextraction (HOLLLME) setup was developed and applied for the isolation of two major estrogens from aquatic media. In contrast to the conventional procedure, in this setup the extracting microdrop was suspended from a horizontally positioned needle in order to provide much higher stability to the extracting phase. The developed HOLLLME approach was applied to isolate two major selected estrogens from aquatic media followed by high performance liquid chromatography-ultraviolet (HPLC-UV) determination. Estrogens were, initially, extracted from water samples into hexane and subsequently, the back extraction stage was performed with 6 μL of sodium... 

A new and convenient format of single drop microextraction (SDME) was developed and applied for isolation of some selected aryloxyphenoxypropionate herbicides from aquatic media. In contrast to the conventional SDME procedure, in this set-up the extraction microdrop was positioned at the bottom of a conical vial in order to provide much higher stability for the organic extraction phase while a magnetic bar was used for stirring the aqueous solution. A simple magnet was used for positioning the bar on the top of the microdrop prior to stirring. The whole set-up led to the use of any volume of extraction solvent with unlimited stirring rates. Some important extraction parameters such as the... 

A novel Fe3O4-poly(aniline-naphthylamine)-based nanocomposite was synthesized by chemical oxidative polymerization process as a magnetic sorbent for micro solid phase extraction. The scanning electron microscopy images of the synthesized nanocomposite revealed that the copolymer posses a porous structure with diameters less than 50nm. The extraction efficiency of this sorbent was examined by isolation of rhodamine B, a mutagenic and carcinogenic dye, from aquatic media in dispersion mode. Among different synthesized polymers, Fe3O4/poly(aniline-naphthylamine) nanocomposite showed a prominent efficiency. Parameters including the desorption solvent, amount of sorbent, desorption time, sample... 

An immersed solvent microextraction (SME) method was successfully developed for the trace enrichment of aryloxyphenoxypropionate herbicides from aquatic media. A microdrop of toluene was used as the extraction solvent. Some important extraction parameters such as type of solvent, solvent dropsize, stirring rate, ionic strength and extraction time were investigated and optimized. The microdrop volume of 1.5 μL, a sampling time of 25 min, and use of toluene were major parameters for achieving high enrichment factors. The linearity was studied by preconcentration of 4 mL of the water samples spiked with a standard solution of aryloxyphenoxypropionates at the concentration range of 0.15 to 30 ng... 

A new unbreakable solid phase microextraction (SPME) fiber coating based on aniline-silica nanocomposite was electrodeposited on a stainless steel wire. The electropolymerization process was carried out at a constant deposition potential, applied to the corresponding aqueous electrolyte containing aniline and silica nanoparticles. The scanning electron microscopy (SEM) images showed the non-smooth and the porous surface structure of the prepared nanocomposite. The applicability of the new fiber coating was examined by headspace-solid phase microextraction (HS-SPME) of some environmentally important polycyclic aromatic hydrocarbons (PAHs), as model compounds, from aqueous samples.... 

A new method based on the combination of magnetic solid phase extraction (MSPE) and spectrofluorimetric determination was developed for isolation and preconcentration of fluoxetine form aquatic and biological samples using sodium dodecyl sulfate (SDS) coated Fe 3O 4 nanoparticles (NPs) as a sorbent. The unique properties of Fe 3O 4 NPs including high surface area and strong magnetism were utilized effectively in the MSPE process. Effect of different parameters influencing the extraction efficiency of fluoxetine including the amount of Fe 3O 4 and SDS, pH value, sample volume, extraction time, desorption solvent and time were optimized. Under optimized condition, the method was successfully... 

A novel solid phase microextraction (SPME) fiber was fabricated by electrospinning method in which a polymeric solution was converted to nanofibers using high voltages. A thin stainless steel wire was coated by the network of polymeric nanofibers. The polymeric nanofiber coating on the wire was mechanically stable due to the fine and continuous nanofibers formation around the wire with a three dimensional structure. Polyamide (nylon 6), due to its suitable characteristics was used to prepare the unbreakable SPME nanofiber. The scanning electron microscopy (SEM) images of this new coating showed a diameter range of 100-200nm for polyamide nanofibers with a homogeneous and porous surface... 

A headspace adsorptive microextraction technique was developed using a novel polyaniline-nylon-6 (PANI-N6) nanofiber sheet, fabricated by electrospinning. The homogeneity and the porosity of the prepared PANI-N6 sheet were studied using the scanning electron microscopy (SEM) and nanofibers diameters were found to be around 200nm. The novel nanofiber sheet was examined as an extracting medium to isolate some selected chlorobenzenes (CBs), as model compounds, from aquatic media. The extracted analytes were desorbed using μL-amounts of solvent and eventually an aliquot of extractant was injected into gas chromatography-mass spectrometry (GC-MS). Various parameters affecting the extraction and... 

A novel method based on microextraction in packed syringe (MEPS) as sample preparation technique coupled off-line with gas chromatography-mass spectrometry was developed using electrospun nanofibers as sorbent. For electrospinning of polypyrrole/polyamide-based nanofiber, a homogeneous solution containing nylon 6, ferric chloride and pyrrole monomer was prepared and then was drawn into a 2.5-mL syringe. By applying a voltage of 13akV between the needle of the syringe and an aluminum-foil collector, the nanofibers could be formed on the surface of the collector. The prepared sheet was used as the sorbent for MEPS to analyze some selected organophosphorous pesticides. Important parameters... 

Comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC × GC-TOFMS) combined to multivariate curve resolution-alternating least-squares (MCR-ALS) is proposed for the resolution and quantification of very complex mixtures of compounds such as polycyclic aromatic hydrocarbons (PAHs) in heavy fuel oil (HFO). Different GC × GC-TOFMS data slices acquired during the analysis of HFO samples and PAH standards were simultaneously analyzed using the MCR-ALS method to resolve the pure component elution profiles in the two chromatographic dimensions as well as their pure mass spectra. Outstandingly, retention time shifts within and between GC × GC runs were not affecting... 

A new technique for preparation of an unbreakable solid-phase microextraction (SPME) fiber, using sol-gel technology is developed. Primarily, an ultrathin two-dimensional intermediate film was prepared by hydrolysis of 3-(trimethoxysilyl)-1-propanthiol self-assembled monolayer grafted onto gold, then a stationary phase by electrodeposition of 3-(trimethoxysilyl) propylmethacrylate as a precursor, tetramethyl orthosilicate and polyethylene glycol as a coating polymer was produced. The scanning electron microscopy images revealed that the new fiber exhibits a rather porous and homogenous surface. The thermal stability of the fabricated fiber was investigated by thermogravimetric analysis. The... 

Novel unbreakable solid phase microextraction (SPME) fiber coatings were fabricated by electrospinning method in which the polymeric solution was converted to nanofibers using high voltages. Four different polymers, polyurethane (PU), polycarbonate (PC), polyamide (PA) and polyvinyl chloride (PVC) were prepared as the fiber coatings on thin stainless steel wires. The extraction efficiencies of new coatings were investigated by headspace solid-phase microextraction (HS-SPME) of some environmentally important chlorobenzenes from aqueous samples followed by gas chromatography-mass spectrometry (GC-MS) analysis. Among them, PU showed a prominent efficiency. Effects of coating time and polymer... 

In the present work, the roles of inorganic oxide nanoparticles on the extraction efficiency of polyethylene terephthalate-based nanocomposites were extensively studied. Four fiber coatings based on polyethylene terephthalate nanocomposites containing different types of nanoparticles along with a pristine polyethylene terephthalate polymer were conveniently electrospun on stainless steel wires. The applicability of new fiber coatings were examined by headspace-solid phase microextraction of some environmentally important volatile organic compound such as benzene, toluene, ethylbenzene and xylene (BTEX), as model compounds, from aqueous samples. Subsequently, the extracted analytes were... 

In the present research, ultrasonic-assisted emulsification-microextraction (USAEME) coupled with gas chromatography-mass spectrometry (GC-MS) has been proposed for analysis of thirteen environmental protection agency (EPA) polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. Tetrachloroethylene was selected as extraction solvent. The main parameters of USAEME affecting the efficiency of the method were modeled and optimized using a central composite design (CCD). Under the optimum conditions (9 μL for extraction solvent, 1.15% (w/v) NaCl (salt concentration) and 10min for ultrasonication time), preconcentration factor (PF) of the PAHs was in the range of 500-950. In order to have a... 

A nanocomposite of silica-polydiphenylamine doped with silver nanoparticles (Ag-SiO2-PDPA) was successfully synthesized by the sol-gel process. For its preparation, PDPA was mixed with butanethiol capped Ag nanoparticles (NPs) and added to the silica sol solution. The Ag NPs were stabilized as a result of their adsorption on the SiO2 spheres. The surface characteristic of nanocomposite was investigated using scanning electron microscopy (SEM). In this work the Ag-SiO2-PDPA nanocomposite was employed as an efficient sorbent for micro-solid-phase extraction (μ-SPE) of some selected pesticides. An amount of 15 mg of the prepared sorbent was used to extract and...