Sharif Digital Repository

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 high-throughput solid-phase microextraction (SPME) on 96-well plate together with gas chromatography-mass spectrometry (GC-MS) was developed for the determination of some selected pesticides in cucumber samples. Pieces with the length of 1.0cm of silicon tubing were precisely prepared and then coated on the end part of stainless steel wires. The prepared fibers were positioned in a home-made polytetrafluoroethylene (PTFE)-based constructed ninety-six holes block to have the possibility of simultaneous immersion of the SPME fibers into the center of individual wells. Pesticides such as diazinon, penconazol, tebuconazol, bitertanol, malathion, phosalone and chlorpyrifos-methyl were selected... 

A gradient derived base layer extractive phase was synthesized and applied for the determination of volatile organic compounds (VOCs) in saliva samples using the headspace cooled in–tube microextraction (HS–CITME) method. The base layers from three different sols of phenyltriethoxysilane (PTES), octyltrimethoxysilane (OTMS) and methyltrimethoxysilane (MTMS) as nonpolar precursors were individually dip coated on the stainless steel wires (SSW). Then, the hydrolyzed polar precursor aminopropyltriethoxysilane (APTES) reacted with the silanol groups already formed on the surface of SSWs via controlled rate infusion (CRI) method. The presence of polar and non–polar functional groups on the... 

In the present work, an amperometric inhibition biosensor for the determination of sulfide has been fabricated by immobilizing Coprinus cinereus peroxidase (CIP) on the surface of screen printed electrode (SPE). Chitosan/acrylamide was applied for immobilization of peroxidase on the working electrode. The amperometric measurement was performed at an applied potential of -150. mV versus Ag/AgCl with a scan rate of 100. mV in the presence of hydroquinone as electron mediator and 0.1. M phosphate buffer solution of pH 6.5. The variables influencing the performance of sensor including the amount of substrate, mediator concentration and electrolyte pH were optimized. The determination of sulfide... 

Multisensor arrays employing various sensing principles are a rapidly developing field of research as they allow simple and inexpensive quantification of various parameters in complex samples. Quantitative analysis with such systems is based on multivariate regression techniques, and deriving of traditional analytical figures of merit (e.g., sensitivity, selectivity, limit of detection, and limit of quantitation) for such systems is not obvious and straightforward. Nevertheless, it is absolutely needed for further development of the multisensor research field and for introducing these instruments into the general context of analytical chemistry. Here, we report on the protocol for... 

An imprinted interpenetrating polymer network (IPN) was synthesized and used as a medium for isolation of carbamazepine from urine samples. The polymer network consisted of a homogeneous polystyrene–sol gel hybrid constructed by in–situ radical polymerization method. In this process, within the sol–gel reaction duration, styrene monomer could penetrate into the reaction mixture and after the polymerization initiation, a monolithic IPN structure was prepared. The scanning electron microscopy (SEM) image and energy dispersive spectroscopy (EDX) are indications of the polystyrene dispersion at nano- to micro-meter level in the sol gel matrix. Eventually, the synthesized IPN was used as a... 

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... 

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... 

A novel and simple photoelectrochemical (PEC) sensor to detect Cr(VI) based on screen-printed TiO2 modified with gold nanoparticles is presented. The proposed PEC sensor showed a very low detection limit (S/N = 3) of 0.004 μM, over a wide linear concentration range from 0.01 μM to 100 μM with a high sensitivity of 11.88 μA.μM-1 Cr(VI). Results also indicated good anti-interference and superb recovery in natural media application for Cr(VI) sensing  

In this study, a novel approach for sensitive and extremely selective detection of copper ions has been developed based on fluorescence resonance energy transfer (FRET) between AuNPs as an acceptor and fluorescein isothiocyanate (FITC) as a donor. Initially, the fluorescence of the FITC molecule turns-off due to adsorption to the AuNPs surface. However, the fluorescence of the FITC-AuNPs system was switched to turn-on by adding d-Pencillamine (d-PC) to the solution mixtures as FITC molecules are released upon displacement by d-PC on the NPs surface. The higher affinity of d-PC toward the surface of AuNPs was further evidenced by controlling the fluorescence intensity enhancement of the... 

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... 

A new modified electrode formed by carbon nanoparticle/chitosan film (CNP/CS) was used for electrocatalytic reduction of Niclosamide (NA). The electrochemical behavior of NA at the CNP/CS modified electrode was investigated in detail by the means of cyclic voltammetry. The reduction mechanism of NA, corresponds to the redox chemistry of nitro group, was thoroughly investigated. The effect of the experimental parameters e.g. potential and time of accumulation, pH of the buffered solutions and potential sweep rate on the response of the electrode was studied. The prepared electrode showed high stability and uniformity in the composite film, short response time, good reproducibility and an... 

A carbon-paste electrode (CPE) modified with iron(II) phthalocyanine was used for the sensitive voltammetric determination of epinephrine (EN). The electrochemical response characteristics of the modified electrode toward EN, ascorbic acid (AA) and uric acid (UA) were investigated by cyclic and differential pulse voltammetry (CV and DPV). The results show an efficient catalytic activity of the electrode for the electro-oxidation of EN, which leads to improvement of reversibility of the electrode response and lowering its overpotential by more than 100 mV. The effect of pH and potential sweep rate on the mechanism of the electrode process was investigated. The modified electrode exhibits an... 

A novel modified pyrolytic graphite electrode with nano-diamond/graphite was fabricated. The electrochemical response characteristics of the modified electrode toward the epinephrine (EN) and uric acid (UA) were studied by means of cyclic and linear sweep voltammetry. The structural morphology and thickness of the film was characterized by SEM technique. The prepared electrode showed an excellent catalytic activity in the electrochemical oxidation of EN and UA, leading to remarkable enhancements in the corresponding peak currents and lowering the peak potentials. The prepared modified electrode acts as a highly sensitive sensor for simultaneous determination of EN and UA in the presence of... 

This paper reports a simple, low-cost, and effective electrochemical technique for sensing and reducing CrVI based on a Au-Pd bimetallic nanoparticle (BNP)-decorated indium tin oxide (ITO) conducting glass electrode. It was observed that the Au-Pd BNP-decorated ITO electrode could significantly boost the electrochemical reduction of CrVI when compared with either Au nanoparticle- or Pd nanoparticle-decorated ITO electrodes. These BNP-decorated electrodes exhibited a wide linear concentration range of 0.001-100 μM, a very low detection limit (signal-to-noise ratio = 3) of 0.3 nM, and a high sensitivity of 1.701 μA μM-1. From electrochemical impedance spectroscopy, it was revealed that this... 

In this study a novel Pt/Ni nanostructure consisting of nano-bushes and nanocubes was fabricated onto TiO 2 nanotubes. The scanning electron microscopy images showed that a large amount of well-dispersed nano-architectures had uniformly covered all over the surface which made an electrode with high surface area. It was obviously seen that the nanocube structures mainly consists of Ni had been grown on top of each other while the Pt colonies represented bush-like structures. As a non-enzymatic glucose biosensor, the Pt/Ni TiO 2 nanotubes modified electrode exhibited an excellent performance. The proposed biosensor had two linear ranges for detection of glucose from 0 to 0.12 mM (correlation... 

A modified carbon paste electrode was prepared by incorporating the TiO2 nanoparticles in the carbon paste matrix. The electrochemical behavior of gallic acid (GA) is investigated on the surface of the electrode using cyclic voltammetry and differential pulse voltammetry. The surface morphology of the prepared electrode was characterized using the scanning electron microscopy. The results indicate that the electrochemical response of GA is improved significantly at the modified electrode compared with the unmodified electrode. Furthermore, the capabilities of electron transfer on these two electrodes were also investigated by electrochemical impedance spectroscopy. Under the optimized... 

Vertical copper oxide nanoflakes were synthesized on a Cu foil through oxidation in alkaline conditions. X-ray photoelectron spectroscopy showed that after exposing the nanoflakes to an Escherichia coli bacterial suspension, the outermost surface of the nanoflakes was chemically reduced through the glycolysis process of the bacteria. Current-voltage (I-V) characteristics of the nanoflakes (measured perpendicular to surface of the Cu foil by using conductive atomic force microscopy) indicated that electrical resistivity of the nanoflakes increased about one order of magnitude after exposure to the bacterial suspension. The nanoflakes reduced by the bacterial suspension could also be... 

A simple and effective ratiometric fluorescence sensor for selective detection of dopamine (DA) in alkaline media has been developed by simply mixing thioglycolic acid (TGA) functionalized orange fluorescent cadmium telluride (CdTe) quantum dots (QDs) with amino-functionalized blue fluorescent carbon nanodots (CDs). Under a single excitation wavelength of 365 nm, the sensor exhibits dual-emissions centered at 445 and 603 nm. The fluorescence of CdTe QDs is selectively quenched by DA, whereas the fluorescence of CDs is insensitive to the analyte. In the presence of different amounts of DA, the variations in the dual emission intensity ratios exhibit a continuous color change from pink to... 

The promise of graphene for use as a vapor sensor motivated exploration of the vapor responses of graphene nanomesh (GNM) functionalized with single stranded DNA. Devices detected different vapor types, including carboxylic acids, aldehydes, organophosphates, and explosives. As-fabricated GNM field effect transistors (FETs) had larger vapor responses than standard graphene FETs due to the effect of oxidized edges and lattice defects. DNA-GNM devices discriminated between homologous species with detection limits of a few parts per million, with fast response and recovery. Responses varied significantly when the base sequence of the DNA was changed, making the sensor class an intriguing...