Application of dispersive liquid-liquid microextraction and spectrophotometric detection to the rapid determination of rhodamine 6G in industrial effluents

A rapid and effective preconcentration method for extraction of rhodamine 6G was developed by using a dispersive liquid-liquid microextraction (DLLME) prior to UV-vis spectrophotometry. In this extraction method, a suitable mixture of acetone (disperser solvent) and chloroform (extractant solvent) was injected rapidly into a conical test tube containing aqueous solution of rhodamine 6G. Therefore, a cloudy solution was formed. After centrifugation of the cloudy solution, sedimented phase was evaporated, reconstituted with methanol and measured by UV-vis spectrophotometry. Different operating variables such as type and volume of extractant solvent, type and volume of disperser solvent, pH of the sample solution, salt concentration and extraction time were investigated. The optimized conditions (extractant solvent: 300 μL of chloroform, disperser solvent: 3 mL of acetone, pH: 8 and without salt addition) resulted in a linear calibration graph in the range of 5-900 ng mL⁻¹ of rhodamine 6G in initial solution with R² = 0.9988 (n = 5). The Limits of detection and quantification were 2.39 and 7.97 ng mL⁻¹, respectively. The relative standard deviation for 50 and 250 ng mL⁻¹ of rhodamine 6G in water were 2.88% and 1.47% (n = 5), respectively. Finally, the DLLME method was applied for determination of rhodamine 6G in different industrial waste waters.     

Naked Eye Chemosensor and In Vivo Chelating Activity of Iron (III) By Bromopyridine Quinoxaline (BPQ)

Journal of Fluorescence - A wide variety of medical, biomedical, and industrial applications has been reported for quinoxalines derivatives. In this work, a novel quinoxaline derivative was...     

Application of stabilized zero valent iron nanoparticles for immobilization of lead in three contrasting spiked soils

Research on Chemical Intermediates - This study was conducted to synthesize and characterize the ZVINs stabilized with acid ascorbic (AAS-ZVINs) and to assess their ability to immobilize Pb2+ in...     

Electrocatalytic determination of sulfite using a modified carbon nanotubes paste electrode: application for determination of sulfite in real samples

This paper introduces a carbon paste electrode modified with ferrocene and carbon nanotubes as a voltammetric sensor for determination of sulfite at pH 7.0. The results showed that under the optimum condition (pH 7.0) in cyclic voltammetry, the oxidation of sulfite occurred at a potential about 280?mV less positive than the unmodified carbon paste electrode. Kinetic parameters such as electron transfer coefficient (??) and heterogeneous rate constant (k) for sulfite were also determined using electrochemical approaches. Under the optimized conditions, the electrocatalytic oxidation peak current of sulfite showed two linear dynamic ranges with a detection limit of 0.1???M for sulfite. The proposed method was examined as a selective, simple, and precise method for voltammetric determination of sulfite in some real samples such as weak liquor from wood and paper industry, boiler water, river water, industrial water, and tap water.     

Pyridine-2-yl Quinoxaline (2-CPQ) Derivative As a Novel Pink Fluorophore: Synthesis,and Chemiluminescence Characteristics

Quinoxaline derivatives are well-known N-heterocycles with pharmacological and fluorescence activities. Almost all quinoxaline derivatives with extensive π-conjugation have been introduced as fluorophores which emit blue and green light. For the first time, we designed and synthesized 6-chloro-2,3 di(Pyridine-2yl) quinoxaline (2-CPQ) as a pink fluorophore in acetonitrile medium by simple route at room temperature whitin 30 min. The synthesized quinoxaline was identified using ¹H, ¹³C NMR, MS, and FT-IR spectroscopy. Our results showed that the iodine-catalyzed method for both oxidation and cyclization during the synthesis of quinoxaline from pyridine 2-carbaldehyde was straightforward, efficient, and clean. All of the mentioned characterization devices confirmed the synthesis of 2-CPQ.

Moreover, we studied the photophysical properties of the synthesized fluorophore in which The UV–Vis absorption spectrum of 2-CPQ in DMF were three peaks at 451, 518 and 556 nm. Based on photophysical properties investigation, 2-CPQ shows good fluorescence with maximum peaks 607 and 653 nm in DMF as solvent (ф_F?=?0.21). Hence, the fluorophore was applied in the peroxyoxalate chemiluminescence system. The reaction of imidazole, H₂O_2, and bis (2,4,6-trichlorophenyl) oxalate (TCPO) can transfer energy to a 6-chloro-2,3 di(pyridine-2yl) quinoxaline. In this process, dioxetane was synthesized, which chemically initiated the electron exchange luminescence (CIEEL) mechanism and led to pink light emission. We anticipate our synthesized fluorophores 2-CPQ will have great potential applications in imaging and medical markers.

     

室温下Cu掺杂的ZnO纳米粉末催化多组分一锅法合成完全取代的茚并[1,2-b]吡啶(英文)

Cu doped ZnO nanocrystalline powder(10 mol%) has been found to be an efficient catalyst for the one‐pot multi‐component synthesis of fully substituted new indeno[1,2‐b]pyridines through a com-bination of 1,3‐indandione, propiophenone or acetophenone derivatives, aromatic aldehydes, and ammonium acetate in ethanol/H2 O at room temperature. The methodology is mild, efficient and high to excellent yielding.     

Extraction optimization of polycyclic aromatic hydrocarbons by alcoholic-assisted dispersive liquid-liquid microextraction and their determination by HPLC

A sensitive method for the extraction and determination of polycyclic aromatic hydrocarbons (PAHs) using alcoholic-assisted dispersive liquid-liquid microextraction (AA-DLLME) and HPLC was developed. The extraction procedure was based on alcoholic solvents for both extraction and dispersive solvents. The effective parameters (type and volume of extraction and dispersive solvents, amount of salt and stirring time) on the extraction recovery were studied and optimized utilizing factorial design (FD) and central composite design (CCD). The best recovery was achieved by FD using 2-ethyl-1-hexanol as the extraction solvent and methanol as the dispersive solvent. The results showed that volume of dispersive solvent and stirring time had no effect on the recovery of PAHs. The optimized conditions were 145 μL of 2-ethyl-1-hexanol as the extraction solvent and 4.2% w/v of salt (NaCl) in sample solution. The enrichment factors of PAHs were in the range of 310-325 with limits of detection of 0.002-0.8 ng/mL. The linearity was 0.01-800 ng/mL for different PAHs. The relative standard deviation (RSD) for intra- and inter-day of extraction of PAHs were in the range of 1.7-7.0 and 5.6-7.3, respectively, for five measurements. The method was also successfully applied for the determination of PAHs in environmental water samples.     

Determination of aliphatic amines using fluorescence intensity of 4-methyl umbelliferone

Effect of aliphatic amines and their concentration on fluorescence intensity of 4-methyl umbelliferone (4-MU) one of coumarin derivative were investigated. This compound has blue light emission under UV lamp in methanolic solution. Spectral investigation of 4-MU solution containing amine compounds showed lower intensity at 350-410 nm (quenching region) and higher intensity at 430-500 nm (enhancing region) as compared to pure methanolic solution of 4-MU. Fluorescence intensity at isoemitting point was independent from concentration of amines. The variation of fluorescence intensity could be used for determination of aliphatic amines in both quenching and enhancing region. Linear ranges for determination of amines in the quenching region were obtained from Stern-Volmer diagram of 4-MU. Determination of amines at fluorescence enhancing region using inverse fluorescence intensity against inverse amine concentration (bireciprocal plot) were investigated and related equations was also proposed.     

Comparison of C18 silica and multi‐walled carbon nanotubes as the adsorbents for the solid‐phase extraction of Chlorpyrifos and Phosalone in water samples using HPLC

A comparison between C₁₈ silica and multi‐walled carbon nanotubes (MWCNTs) in the extraction of Chlorpyrifos and Phosalone in environmental water samples was carried out using HPLC. Parameters affecting the extraction were type and volume of elution solvent, pH and flow rate of sample through the adsorbent. The optimum conditions obtained by C₁₈ cartridge for adsorption of these pesticides were 4 mL dichloromethane as elution solvent, sample pH of 5, flow rate of 1 mL/min, and those for MWCNT cartridge were 3 mL dichloromethane, pH of 5 and flow rate of 10 mL/min, respectively. Optimized mobile phase for separation and determination of these compounds by HPLC was methanol/water (80:20 v/v) with pH=5 (adjusted with phosphate buffer). Under optimal chromatographic and SPE conditions, LOD, linear range and precision (RSD n=8) were 3.03×10^?3, 0.01–5.00 μg/mL and 2.7% for Chlorpyrifos and 4.03×10^?4, 0.01–5.00 μg/mL and 2.3% for Phosalone, in C₁₈ cartridge, respectively. These values for MWCNT were 4.02×10^?6, 0.001–0.500 μg/mL and 1.8% for Chlorpyrifos and 1.02×10^?6, 0.001–0.500 μg/mL and 1.5% for Phosalone, respectively.