Sharif Digital Repository

The aim of this study is to introduce an extractive phase based on gradient concept by continuous changing in chemical functional groups for non–targeted analysis. For this purpose, three different two–component coatings containing (3–aminopropyl)trimethoxysilane (APTES) as polar and either phenyltriethoxysilane (PTES), octyl–trimethoxysilane (OTMS) or methyltrimethoxysilane (MTMS) as nonpolar precursors were formed on the modified stainless steel wires using controlled rate infusion (CRI) method. The presence of polar and/or non–polar functional groups on the surface of substrate was evaluated by Fourier–transform infrared spectroscopy (FTIR) together with contact angles determined... 

In this study, cellulose acetate (CA) fibers were prepared using different solvent systems in electrospinning. The recorded scanning electron microscopy micrographs indicated that the morphology of the prepared fibers is closely associated with the type of electrospinning solvents. The prepared CA fibers were used as an extractive phase for on–line micro–solid phase extraction (μ-SPE) of nonsteroidal–inflammatory drugs (NSAIDs) in biological samples pursued by HPLC–UV determination. Work conducted on this research ascertained that the use of dichloromethane:acetone (3:1, v/v) solvent system in the CA dissolution for electrospinning, leads to the formation of porous ribbon–like fibers and... 

There are high attractions in the development of conducting polymer (CP) coatings to improve the electrochemical properties and biocompatibility of electrodes in the area of biosensors. A new type of the modified electrodes is prepared in a layer-by-layer process by using multi-walled carbon nanotube (MWCNT) and poly-pyrrole. In this procedure, the glassy carbon electrode is casted by a drop suspension of MWCNT, which leads to form a thin film of nanotube on its surface. In the second step, electrochemical polymerization of pyrrole in the presence of tiron (used as doping anion) is performed on the surface of the MWCNT pre-coated electrode. The modification procedure led to fabrication of a... 

In this study, firstly, a double-reservoir and switchable prototype of a micro-chip along with the respective holders were fabricated. A cyclic desorption process using microliter volume of organic solvent was adopted to prevent any outdoor contamination. As extractive phases, two identical sheets of electrospun polyamide/polypyrrole/titania nanofibers were synthesized using core–shell electro-spinning technique and utilized for determination of memantine in plasma samples. Field emission scanning electron microscopy images showed a high degree of porosity and homogeneity throughout the sheet structure. Also, energy dispersive X-ray analysis confirmed the presence of titania, while the... 

A cryogel–based semi–interpenetrating polymer network (Cryo–SIPN) was prepared in which conductive polymers such as polyaniline (PANI) and polypyrrole (PPy) were formed within the super porous network of acrylic acid cryogel. For completion of cryo-polymerization, all the constituent solutions were severely mixed and placed into the plastic straws and kept at -20°C and then the synthesized cyrogels were cut into the 1-cm length and freeze dried after washing with water. The Cryo–SIPN polymeric composite was applied in micro solid phase extraction (µSPE) of some selected antibiotic residues from various samples. The µSPE method combined with a high performance liquid... 

A method based on solid-phase microextraction (SPME) followed by on-fiber derivatization and gas chromatography-mass spectrometry detection (GC-MS) for determination of phenol in air was developed. Three different types of SPME fibers, polar and non-polar poly(dimethylsiloxane) (PDMS) and polyethylene glycol (PEG) were synthesized using sol-gel technology and their feasibility to the sampling of phenol were investigated. Different derivatization reagents for post on-fiber derivatization of phenol were studied. Important parameters influencing the extraction and derivatization process such as type of fiber coating, type and volume of derivatizing reagent, derivatization time and temperature,... 

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 sensitive glutamate biosensor is prepared based on glutamate dehydrogenase/vertically aligned carbon nanotubes (GLDH, VACNTs). Vertically aligned carbon nanotubes were grown on a silicon substrate by direct current plasma enhanced chemical vapor deposition (DC-PECVD) method. The electrochemical behavior of the synthesized VACNTs was investigated by cyclic voltammetry and electrochemical impedance spectroscopic methods. Glutamate dehydrogenase covalently attached on tip of VACNTs. The electrochemical performance of the electrode for detection of glutamate was investigated by cyclic and differential pulse voltammetry. Differential pulse voltammetric determinations of glutamate are performed... 

In this work a novel unbreakable sol-gel-based in-tube device for on-line solid phase microextraction (SPME) was developed. The inner surface of a copper tube, intended to be used as a high performance liquid chromatography (HPLC) loop, was electrodeposited by metallic Cu followed by the self assembled monolayers (SAM) of 3-(mercaptopropyl) trimethoxysilane (3MPTMOS). Then, poly (ethyleneglycol) (PEG) was chemically bonded to the -OH sites of the SAM already covering the inner surface of the copper loop using sol-gel technology. The homogeneity and the porous surface structure of the SAM and sol-gel coatings were examined using the scanning electron microscopy (SEM) and adsorption/desorption... 

In this study, a low–cost microfluidic device from polymethyl methacrylate was fabricated by laser engraving technique. The device is consisted of a central chip unit with an aligned microchannel. Both sides of the engraved microchannel were sandwiched by two synthesized sheets from polyamide/titania (PA/TiO2) hollow nanofibers as extractive phases. The inlet and outlet of the device were connected to the polyether ether ketone tubes, while a peristaltic pump was used to deliver both sample and desorbing solvent through the microchannel. The recorded scanning electron microscopy images from the surface of the synthesized PA/TiO2 nanofibers, exhibit a good degree of homogeneity and porosity... 

In this research, an attempt was made toward synthesizing a sol–gel–based silica aerogel and its subsequent coating on a copper wire by phase separation of polystyrene. Adaption of this new approach enabled us to coat the metallic wire with powder materials. The use of this method for coating, led to the formation of a porous and thick structure of silica aerogel. The coated wire was placed in a needle and used as the sorbent for in–tube solid phase microextraction of chlorobenzenes (CBs). The superhydrophobicity of sorbent on extraction efficiency was investigated by using different ratios of tetraethylorthosilicate/methyltrimethoxysilane. The surface coated with the prepared silica aerogel... 

We synthesized a titanium dioxide–polyaniline core–shell nanocomposite and implemented it as an efficient sorbent for the needle-trap extraction of some volatile organic compounds from urine samples. Polyaniline was synthesized, in the form of the emeraldine base, dissolved in dimethyl acetamide followed by diluting with water at pH 2.8, using the interfacial polymerization method. The TiO2 nanoparticles were encapsulated inside the conducting polymer shell, by adapting the in situ dispersing approach. The surface characteristics of the nanocomposite were investigated by Fourier transform infrared spectrometry, scanning electron microscopy, and transmission electron microscopy. After... 

A headspace solid-phase dynamic extraction (HS-SPDE) technique was developed by the use of polypyrrole (PPy) sorbent, electropolymerized inside the surface of a needle, as a possible alternative to solid-phase microextraction (SPME). Thermal desorption was subsequently, employed to transfer the extracted analytes into the injection port of a gas chromatography-mass spectrometry (GC-MS). The PPy sorbent including polypyrrole-dodecyl sulfate (PPy-DS) was deposited on the interior surface of a stainless steel needle from the corresponding aqueous electrolyte by applying a constant deposition potential. The homogeneity and the porous surface structure of the coating were examined using the... 

Multi-walled carbon nanotube decorated with silver nanoparticles (AgNPs-MWCNT) is used as an effective strategy for modification of the surface of pyrolytic graphite electrode (PGE). This modification procedure improved colloidal dispersion of the decorated MWCNTs in water, affording uniform and stable thin films for altering the surface properties of the working electrode. Robust electrode for sensing applications is obtained in a simple solvent evaporation process. The electrochemical behavior of sumatriptan (Sum) at the bare PGE and AgNPs-MWCNT modified PGE is investigated. The results indicate that the AgNPs-MWCNT modified PGE significantly enhanced the oxidation peak current of Sum. A... 

Multi-walled carbon nanotubes (MWCNTs) were immobilised with cobalt nanoparticles and analyzed by transmission electron microscopy. This modification procedure substantially improved colloidal dispersion of the immobilised MWCNTs in water and organic solvents, yielding uniform and stable thin films for modification of the glassy carbon electrode surface. The modified electrode showed an efficient catalytic role for the electrochemical oxidation of thioridazine (TR), leading to remarkable decrease in its oxidation overpotential of approximately 100 mV and enhancement of the kinetics of the electrode reaction, which can be confirmed by increasing in the peak current and sharpness of the peak.... 

Implementation of metal organic frameworks (MOFs) in the separation science has attracted many researchers attention. In this study, the role of metal, ligand, the reaction condition and modification on the extraction efficiency of some MOFs was investigated. Among the prevalent reported MOFs, some members of the MIL and MOF–5 families were chosen, and eleven MOF–based sorbents were prepared by changing the metal and ligand type, reaction condition, and/or functionality through post synthetic modification (PSM). MIL–101 and MIL–101–NH2 based structures were initially synthesized based on the chromium and iron salts. Also, three zinc–based structures including MOF–5, [NH2(CH3)2]2... 

In this survey, a reliable and applicable Y–Y shaped micro–channel in a microfluidic device was designed and manufactured. A number of micro–scaled hedges were precisely fabricated inside the micro–channel to facilitate the immobilization of synthesized core–shell Fe3O4@SiO2 magnetic nanoparticles (MNPs), functionalized by triethoxyphenylsilane (TEPS) by sol-gel technique. Both sample and reagents were introduced into the microfluidic device by a syringe pump to perform the extraction and desorption steps. The functionalized MNPs were characterized by transmission electron microscopy, X-ray diffraction spectroscopy and Fourier transform infrared spectroscopy. By adopting the strategy of...