Sharif Digital Repository

An example of zeolite selectivity (MFI → MOR) driven by synthesis aging time has been studied. Using N,N,N′,N′-tetramethyl-N,N′-dipropyl-ethylenediammonium diiodide (TMDP) as an organic structure-directing agent (OSDA), the zeolite phases obtained at 2 h (MFI 97%), 8 h (MFI 84%, MOR 16%) and 24 h (MFI 43%, MOR 57%) have been characterized by powder X-ray diffraction. The results suggest that at intermediate aging time, namely 8 h and 24 h, the dominant phase (MFI) is displaced by MOR. Different techniques (FT-IR, Raman, 13C MAS NMR, TGA/DTG and HC microanalysis) have been employed to verify the OSDA integrity and occlusion inside the zeolite micropores as well as to quantify the water and... 

Biomass, originates from plant- or animal-based materials with a huge potential to be reused. Here we report a simple, rapid and inexpensive method for preparation of modified biochars derived from the banana peel followed by their applications in pipette-tip micro solid-phase extraction (PT-µSPE). Due to the contribution of various effective parameters on modification of banana peel biochars (BPBs), Taguchi design was used to optimize activation temperature, activation repetition, treatment material and impregnation ratio. Efficiency of the prepared BPBs were studied by extraction of twelve various pesticides, as model analytes with an extended range of log P values (1.4–5.7), followed by... 

The quantities of residues of some triazines such as prometon, propazine, atrazine and simazine in complex matrices of apple samples were determined, using gas chromatography-selected ion mass (GC-SIM) spectrometry. Generalized rank annihilation method (GRAM) as a second-order calibration technique was used for screening, resolving and finally determining the amounts of the residues. Before the GRAM analysis, different steps of data preprocessing such as background correction, de-skewing and standardization for rank alignment was used for every target analyte. The de-skewing and rank alignment algorithms were used for bilinearity and trilinearity corrections, respectively. The two data... 

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... 

This paper focuses on characterization of the components of Iranian rosemary essential oil using gas chromatography-mass spectrometry (GC-MS). Multivariate curve resolution (MCR) approach was used to overcome the problem of background, baseline offset and overlapping/embedded peaks in GC-MS. The analysis of GC-MS data revealed that sixty eight components exist in the rosemary essential oil. However, with the help of MCR this number was extended to ninety nine components with concentrations higher than 0.01%, which accounts for 98.23% of the total relative content of the rosemary essential oil. The most important constituents of the Iranian rosemary are 1,8-cineole (23.47%), α-pinene... 

Volatile components of saffron from different regions of Iran were extracted by ultrasonic-assisted solvent extraction (USE) and were analyzed by gas chromatography-mass spectrometry (GC-MS). Self-modeling curve resolution (SMCR) was proposed for resolving the co-eluted GC-MS peak clusters into pure chromatograms and mass spectra. Multivariate curve resolution-objective function minimization (MCR-FMIN) and multivariate curve resolution-alternating least square (MCR-ALS) were successfully used for this purpose. The accuracy of the qualitative and quantitative results was improved considerably using SMCR techniques. Comparison of the results of saffron from different regions of Iran showed... 

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... 

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... 

Herein, some (modified) paper–based substrates were prepared and utilized as extractive phases in a microfluidic device and their extraction performances examined for analytes with different polarities. Reagents including hexadecyltrimethoxysilane (HDTMS), phenyltrimethoxysilane (PTES), (3-aminopropyl) triethoxysilane (APTES) and 3–(2,3–epoxypropoxy) propyltrimethoxysilane (EPPTMOS) were implemented for the modification process. Due to the induction of different silane functional groups, it was anticipated to have various interactions for the tested analytes. Eventually, the prepared paper sheets were used as extractive phases for solid–phase extraction within a microfluidic system. The... 

FeVO4/CeO2 was applied in the electro-Fenton (EF) degradation of Methyl Orange (MO) as a model of wastewater pollution. The results of the characterization techniques indicate that FeVO4 with triclinic structure and face-centered cubic fluorite CeO2 maintained their structures during the nanocomposite synthesis. The effect of applied current intensity, initial pollutant concentration, initial pH, and catalyst weight was investigated. The MO removal reached 96.31% and chemical oxygen demand (COD) removal 70% for 60 min of the reaction. The presence of CeO2 in the nanocomposite plays a key role in H2O2 electro-generation as a significant factor in the electro-Fenton (EF) system. The metal... 

A novel method for extraction and analysis of volatile compounds of Artemisia haussknechtii Boiss., using simultaneous hydro-distillation and static headspace liquid microextraction followed by gas chromatography-mass spectrometry (SHD-SHLPME-GCMS) is developed. SHLPME parameters including nature of extracting solvent, headspace volume and design, extraction time, sample weight and microdrop volume were optimized. Comparison of hydro-distillation gas chromatography-mass spectrometry and HD-SHLPME-GCMS showed that the latter method is fast, simple, inexpensive and effective for the analysis of volatile compounds of aromatic plants. By using this method, 56 compounds were extracted and... 

A fiber coating from polyaniline (PANI) was electrochemically prepared and employed for solid phase microextraction (SPME) of some polycyclic aromatic hydrocarbons (PAHs) from water samples. The PANI film was directly electrodeposited on the platinum wire surface in sulfuric acid solution using cyclic voltammetry (CV) technique. The applicability of this coating was assessed employing a laboratory-made SPME device and gas chromatography with mass spectrometry (GC-MS) for the extraction of some PAHs from the headspace of aqueous samples. Application of wider potential range in CV led to a PANI with more stability against the temperature. The homogeneity and the porous surface structure of the... 

Gas chromatography-mass spectrometry combined with iterative and non-iterative resolution methods was used to characterize the essential oil components of Iranian cumin and caraway. Orthogonal projection resolution (OPR) as a non-iterative and distance-selection-multivariate curve resolution-alternative least squares (DS-MCR-ALS) as an iterative method were used as auxiliary means to the analysis in the case of overlapping peaks. A total of 19 and 39 components were identified by direct similarity searches for cumin and caraway oils, respectively. These numbers were extended to 49 and 98 components, respectively with the help of chemometric techniques. Major constituents in cumin are... 

An automated technique based on purge-and-trap coupled to gas chromatography with mass spectrometric detection has been developed and optimized for the trace determination of five of the most important water odorants; 2-isopropyl-3-methoxypyrazine, 2-isobutyl-3-methoxypyrazine, 2-methylisoborneol, 2,4,6-trichloroanisole and geosmin. The extraction method was absolutely solvent-free. Analytes were purged from 20 ml of water sample containing sodium chloride at room temperature by a flow of He and trapped on a Tenax sorbent. The desorption step was performed with helium and temperature programming and desorbed analytes were directly transferred to a gas chromatograph coupled to a mass... 

A novel solid-phase microextraction (SPME) method was developed for isolation of dextromethorphan (DM) and its main metabolite dextrorphan (DP) from human plasma followed by GC-MS determination. Three different polymers, poly(dimethylsiloxane) (PDMS), poly(ethylenepropyleneglycol) monobutyl ether (Ucon) and polyethylene glycol (PEG) were synthesized as coated fibers using sol-gel methodologies. DP was converted to its acetyl-derivative prior to extraction and subsequent determination. The porosity of coated fibers was examined by SEM technique. Effects of different parameters such as fiber coating type, extraction mode, agitation method, sample volume, extraction time, and desorption... 

The performances of gas chromatography with mass spectrometry and of comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry are examined through the comparison of Daphnia magna metabolic profiles. Gas chromatography with mass spectrometry and comprehensive two-dimensional gas chromatography with mass spectrometry were used to compare the concentration changes of metabolites under saline conditions. In this regard, a chemometric strategy based on wavelet compression and multivariate curve resolution–alternating least squares is used to compare the performances of gas chromatography with mass spectrometry and comprehensive two-dimensional gas chromatography with... 

An effect-directed analysis (EDA) of fresh and artificially weathered (evaporated, photooxidized) samples of North Sea crude oil and residual heavy fuel oil is presented. Aliphatic, aromatic, and polar oil fractions were tested for the presence of aryl hydrocarbon receptor (AhR) agonist and androgen receptor (AR) antagonist, demonstrating for the first time the AR antagonist effects in the aromatic and, to a lesser extent, polar fractions. An extension of the typical EDA strategy to include an N-way partial least-squares (N-PLS) model capable of relating the comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC × GC-TOFMS) data set to the bioassay data... 

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 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...