Sharif Digital Repository

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... 

A solution of polyamide (PA) containing polyethylene glycol (PEG) as a side low-molecular-weight polymer was electrospun. After synthesizing the PA-PEG nanofibers, the constituent was subsequently removed (modified PA) and confirmed by Fourier transform infrared spectroscopy. The scanning electron microscopy images showed an average diameter of 640 and 148 nm for PA and PA-PEG coatings, respectively, while the latter coating structure was more homogeneous and porous. The extraction efficiencies of PA, PA-PEG, and the modified PA fiber coatings were assayed by headspace solid-phase microextraction of a number of chlorophenols from real water samples followed by their determination by gas... 

A molecularly imprinted xerogel (MIX) for fentanyl was successfully prepared on the inner surface of a copper tube by sol-gel technology. Primarily, the tube was treated by self-assembly monolayers of 3-(mercaptopropyl) trimethoxysilane and then [3-(2,3-epoxypropoxy)-propyl]-trimethoxysilane was employed as a precursor for imprinting the template molecule in acidic conditions. During the sol-gel process influential parameters including volume and concentration of fentanyl were carefully investigated to obtain the most efficient and appropriate xerogel. In parallel, a non-imprinted xerogel (NIX) was synthesized in the absence of fentanyl. The extraction efficiencies achieved from MIX and NIX,... 

In the present work, a novel microextraction method named in situ solvent formation microextraction (ISFME) using ionic liquids (ILs) for preconcentration of carbaryl and carbofuran in water samples is introduced. In this method, a small amount of sodium hexafluorophosphate (NaPF6), as an ion pairing agent, was added to a sample solution containing a small quantity of 1-hexyl-3-methylimidazolium tetrafluoroborate [Hmim][BF4] as a hydrophobic ionic liquid. A cloudy solution formed as a result of formation of fine droplets of 1-hexyl-3-methylimidazolium hexafluorophosphate [Hmim][PF 6]. After centrifugation, the fine droplets of the extractant phase settled to the bottom of the conical-bottom... 

Molybdenum resources around the world are mainly associated with porphyry copper ores. Molybdenite (MoS2) is the main Mo mineral that has rhenium in its crystal lattice. This paper investigates the recovery of rhenium and molybdenum from a molybdenite concentrate using a hydrometallurgical treatment method. The molybdenite concentrate is leached with nitric acid and subjected to solvent extraction to recover and separate rhenium and molybdenum from the leached liquor. The effects of pH and the chemicals' concentration on extraction characteristics of Mo and Re are investigated to define the best condition for selective extraction of these metals. The tested leached liquor contained of 8.2... 

To evaluate the selectivity and efficiency of solid phase microextraction (SPME) fiber coatings, synthesized by sol-gel technology, roles of precursors and coating polymers were extensively investigated. An on-line combination of capillary microextraction (CME) technique and high performance liquid chromatography (HPLC) was set up to perform the investigation. Ten different fiber coatings were synthesized in which five of them contained only the precursor and the rests were prepared using both the precursor and coating polymer. All the coatings were chemically bonded to the inner surface of copper tubes, intended to be used as the CME device and already functionalized by self-assembly... 

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... 

Experimental design of directly suspended droplet liquid-liquid-liquid microextraction has been used to determine residue of 2,4-D, in environmental water samples. A free suspended droplet of 5.5 μL of receiving phase is delivered to the top-center position of 1-Octanol, which is an immiscible organic solvent, floating on the top of a 2.5 mL aqueous sample while being agitated by a stirring bar to create a mild vortex at the center of the vial. Central composite rotatable design has been used for studying the effect of the parameters, the factors interacting with each other and finding the optimum condition. The chromatographic separation was accomplished on a shim-Pak C18 column using a... 

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... 

A new type of composite material based on carbon nanotubes (CNTs) and sol-gel chemistry was prepared and used as sorbent for needle trap device (NTD). The synthesized composite was prepared in a way to disperse CNTs molecules in a sol-gel polymeric network. CNT/silica composites with different CNT doping levels were successfully prepared, and the extraction capability of each composite was evaluated. Effects of surfactant and the oxidation duration of CNTs on the extraction efficiency of synthesized composites were also investigated. The applicability of the synthesized sorbent was examined by developing a method based on needle trap extraction (NTE) and gas chromatography mass spectrometry... 

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 this study, organic aerogels were synthesized by the sol-gel polycondensation of mixed cresol with formaldehyde in a slightly basic aqueous solution. Carbon aerogels and xerogels are generated by pyrolysis of organic aerogels. The novel sol-gel-based micro-solid-phase extraction sorbent, resorcinol-formaldehyde xerogel, was employed for preconcentration of some selected herbicides. Three herbicides of the aryloxyphenoxypropionate group, clodinafop-propargyl, haloxyfop-etotyl, and fenoxaprop-P-ethyl, were extracted from aqueous samples by micro-solid-phase extraction and subsequently determined by gas chromatography with mass spectrometry. The effect of different parameters influencing the... 

Dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography-mass spectrometry-selective ion monitoring (GC-MS-SIM) was applied to the determination of methyl tert-butyl ether (MTBE) in water samples. The effect of main parameters affecting the extraction efficiency was studied simultaneously. From selected parameters, volume of extraction solvent, volume of dispersive solvent, and salt concentration were optimized by means of experimental design. The statistical parameters of the derived model were R 2=0.9987 and F=17.83. The optimal conditions were 42.0μL for extraction solvent, 0.30mL for disperser solvent and 5% (w/v) for sodium chloride. The calibration linear range... 

In industrial liquid-liquid extraction processes, the feed is not clean liquid but there are various kinds of contaminants in the feed entering the extractors. In this regard, a two-impinging-jets contacting device (TIJCD) was tested through the standard test system recommended by the European Federation of Chemical Engineering (EFCE), namely toluene-acetone-water, in the presence and absence of various types of surface-active agents (SAAs). The influences of anionic, cationic, and nonionic SAAs such as sodium dodecyl sulfate (SDS), dodecyl trimethyl ammonium chloride (DTMAC), and octylphenol decaethylene glycol ether (Triton X-100), respectively, on the extraction efficiency and overall... 

In this research, organic solvent composed of hexane and methanol was used for lipid extraction from dry and wet biomass of Chlorella vulgaris. The results indicated that lipid and fatty acid extraction yield was decreased by increasing the moisture content of biomass. However, the maximum extraction efficiency was attained by applying equivolume mixture of hexane and methanol for both dry and wet biomass. Thermodynamic modeling was employed to estimate the effect of hexane/methanol ratio and moisture content on fatty acid extraction yield. Hansen solubility parameter was used in adjusting the interaction parameters of the model, which led to decrease the number of tuning parameters from 6... 

A superhydrophobic polystyrene hollow fiber was electrospun around a copper spring collector. This approach led to the construction of a hollow fiber membrane, and the copper spring acted as a scaffold. The characteristic properties of the hollow fiber were studied by scanning electron microscopy. The membrane was used as a probe to transfer the extracting solvent from aquatic media to a gas chromatograph. After performing the liquid–liquid microextraction procedure on 10 mL of water sample by octanol, the whole solution was passed through the prepared polystyrene hollow fiber. Propanol, containing 2 mg/L lindane as the internal standard, was used for desorption and an aliquot of 2 μL of the... 

A magnetic nanocomposite consisting of nanoparticles–polybutylene terephthalate (MNPs–PBT) was electrospun and used as an extracting medium for an on-line μ-solid phase extraction (μ–SPE)–high performance liquid chromatography (HPLC) set–up with an ultraviolet (UV) detection system. Due to the magnetic property of the prepared nanofibers, the whole extraction procedure was implemented under an external magnetic field to enhance the extraction efficiencies. The developed method along with the synthesized nanocomposite were found to be appropriate for the determination of trace levels of selected drugs including furosemide, naproxen, diclofenac and clobetasol propionate in the urine sample.... 

A thin film microextraction method using elecrospun magnetic polybutylene terephthalate nanofibers is developed and implemented to isolate some selected triazines. Due to the high mechanical stability of these nanofibers, they are repeatedly used under harsh magnetic stirring and ultrasonic conditions without any damage and structure degradation. The presence of magnetic nanoparticles within the nanofiber structure increases the extraction efficiency while the fibers could be collected by an external magnet. The synthesized nanocomposite showed strong affinity toward the selected analytes. Apart from the concentration of magnetic nanoparticles within the nanocomposite network, the effect of... 

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...