Sharif Digital Repository

A three–dimensional metal organic framework (3D–MOF) and a two–dimensional polyoxometalate (2D–POM), both incorporating nanostructured molybdenum (VI) oxide, were synthesized and implemented for headspace needle trap extraction of traces of chlorobenzenes (CBs). The 3D–MOF of type {(Mo2O6)(4,4′–bpy)}n and the 2D–POM of type [4,4′–bpy][Mo7O22] were synthesized by a solvothermal process and characterized by FT–IR, powder X–ray diffraction, scanning electron microscopy, transmission electron microscopy, thermogravimetry, energy dispersive X–ray, elemental mapping and Brunner–Emmet–Teller adsorption analyses. The 3D–MOF proved to be superior. Following thermal desorption, the CBs... 

In this research, three fibers including cellulose acetate (CA), CA–phenyltriethoxysilane (PTES) prepared via sol–gel electrospinning and sol–gel–based CA fibers immersed in PTES solution (dipped–CA–PTES) were prepared. The composition and morphology of the prepared fibers were evaluated by energy dispersive X-ray spectroscopy and field emission scanning electron microscopy. The prepared fibers were implemented in a home–made needle trap device, followed by thermal desorption of the selected chlorobenzenes (CBs) to a gas chromatography–flame ionization detector. Finally, parameters affecting the extraction methodology such as the amount of sorbent, extraction time and temperature, desorption... 

Three-dimensional (3D) polyamide scaffolds were fabricated by applying a solvent bath as the collecting element. Electrospun nanofibers were immersed into the solvent bath to give a material with a laminated 3D texture. In parallel, 2D nanofibers were synthesized and utilized as microextractive phases in a needle trap device to compare the capabilities of 2D and 3D materials in terms of headspace extraction of various chlorobenzenes (chlorobenzene, 1,2-dichlorobenzene, 1,4-dichlorobenzene, 1,2,4-trichlorobenzene and 1,2,3,4-tetrachlorobenzene). The results demonstrate the superiority of 3D nanofibrous scaffolds over 2D mats. The porosity, morphology, and thermal stability of the 3D scaffolds... 

A superhydrophobic extractive phase was prepared and packed in a needle trap microextraction device for extraction of volatile organic compounds, followed by their determination by gas chromatography. The superhydrophobic phase was prepared by surface modification of melamine formaldehyde (MF) sponge embedded by reduced graphene oxide (rGO). The overall properties of the modified MF along with its high sorption capacity and low cost fabrication were indicative of its feasibility to be highly suitable for extraction of organic pollutants. The determined water contact angle (>150o) from the surface of melamine formaldehyde–reduced graphene oxide (MF–rGO) revealed its high affinity toward... 

The authors have synthesized a superhydrophobic silica aerogel by using a sol-gel technique. The material is shown to be an efficient sorbent for needle trap microextraction of chlorobenzenes. Hydrophobicity affects the performance of the sorbent as shown by altering the ratio between tetraethylorthosilicate (TEOS) and methyltrimethoxysilane when synthesizing the sorbent. The observed contact angle (which is >150°) underpins the superhydrophobic properties of the aerogel. The microstructure of the sorbent was investigated by BET adsorption, revealing a surface area above 1000 m2 g−1. The sorbent was applied to needle trap extraction of chlorobenzenes from aqueous samples, and their... 

In this work, the preparation of a new grafted nanosilica-based sorbent was extensively investigated. An inexpensive modifier, cis-9-octadecenoic acid (oleic acid) was selected to be grafted on the surface of the nanosilica particles as the support. The grafting process was accurately confirmed by Fourier transform infra-red spectrometry (FT-IR). Applicability of the prepared sorbent was thoroughly examined by needle trap extraction (NTE) method. The grafted sorbent was dispersed in the appropriate solvent and carefully packed inside a steel needle. Feasibility of the method was completely examined using polycyclic aromatic hydrocarbons (PAHs), as model compounds. For extraction of analytes... 

A nanocomposite consisting of polythiophene–silver was prepared and implemented as a desired sorbent for headspace needle trap extraction. Colloidal silver nanoparticles (Ag NPs) with narrow size distribution and high stability were synthesized in water–in–oil microemulsion. This simple procedure was adapted to prepare highly monodispersed Ag NPs, starting from an initial synthesis in sodium bis(2-ethylhexyl) sulfosuccinate (AOT) reverse micelles. Polythiophene (PT) was synthesized by chemical oxidative polymerization in the presence of anhydrous ferric chloride while its polymeric structure was confirmed by Fourier transform infrared spectrometry (FTIR). Eventually, the prepared PT was... 

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 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...