首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献，搜索用时 578 毫秒
1.
Dispersive liquid–liquid microextraction based on solidification of floating organic droplet (DLLME‐SFO) technique was successfully applied for simultaneous assay of eight polychlorinated biphenyls, two organochlorine, and four pyrethroid pesticides multi‐residue in aqueous samples by using GC‐electron capture detection. The effects of various parameters such as kind of extractant and dispersant and volume of them, extraction time, effect of salt addition, and pH were optimized. As a result, 5.0 µL 1‐dodecanol was chosen as extraction solvent, 600 µL methanol were used as dispersive solvent without salt addition, pH was adjusted to 7. Under the optimized conditions, the limits of detection (LOD) were ranged from 1.4 to 8.3 ng L?1. Satisfactory linear range was observed from 5.0 to 2000 ng L?1 with correlation coefficient better than 0.9909. Good precisions were also acquired with RSD better than 13.6% for all target analytes. The enrichment factors of the method were ranged from 786 to 1427. The method can be successfully applied to simultaneous separation and determination of three class residues in real water samples and good recoveries were obtained ranging from 76 to 130, 73 to 129, and 78 to 130% for tap water, lake water, and industrial waste water, respectively.  相似文献   

2.
In the present work, experiments have been carried out with a focus to reduce the volume requirement of solvent by mixing with imidazolium based ionic liquids (ILs) for the solvent extraction of phenol, p‐chlorophenol, 2,4‐dichlorophenol, 2,4,6‐trichlorophenol, and pentachlorophenol from aqueous solutions. The effect of aqueous phase pH (2–12), agitation speed (100–450 rpm), solute concentration in feed (2–50 mg/L), temperature (303–333 K), treat ratio (1–11), and 1‐butyl‐3‐methyl imidazolium tetrafluoroborate [Bmim]+[BF4]? volume in tributyl phosphate (TBP; 0–0.7% v/v) on extraction of phenols has been studied and optimized. Parameters like strip phase pH (3–13) and stripping agent concentration (0.001–0.009 N) have also been studied for stripping of phenols from solvent phase. It has been found that 0.5% v/v of ionic liquid [Bmim]+[BF4]? in solvent TBP extracts more than 97.5% of phenol and chlorophenols from aqueous solutions with a treat ratio (aqueous to solvent phase ratio) of 5. Transport mechanism for extraction and stripping of phenol and chlorophenols using ionic liquid [Bmim]+[BF4]? has been discussed. The results show that by appropriate selection of extraction and stripping conditions, it is possible to remove nearly all phenols with a treat ratio of 5.  相似文献   

3.
A method for the determination of nickel in water was developed. The procedure involves preconcentration of nickel by using dispersive liquid–liquid microextraction. The Ni(II) ions were extracted in chloroform in the form of complex with the reagent 2‐(2′‐benzothiazolylazo)‐p‐cresol. Ethanol was used as the disperser solvent. After injection of the extracting mixture in a solution of nickel, a cloudy mixture was observed. A quick centrifugation induces phase separation and thus the settling of rich phase. The nickel content in the rich phase is measured by flame atomic absorption spectrometry. Under optimal conditions, the limit of detection and quantification obtained were 1.4 and 4.7 µg L?1, respectively. Some parameters used to characterize preconcentration systems, such as enrichment factor and consumption index were calculated and resulted in 29 and 0.34 mL, respectively. After optimization of variables and determination of analytical characteristics, the method was used for the analysis of certified reference materials (BCR‐713: wastewater, effluent and BCR‐414: plankton) and real water samples.  相似文献   

4.
DyeLIF? is a new version of laser‐induced fluorescence (LIF) for high‐resolution three‐dimensional subsurface mapping of nonaqueous phase liquids (NAPLs) in the subsurface. DyeLIF eliminates the requirement that the NAPL contains native fluorophores (such as those that occur in compounds like polynuclear aromatic hydrocarbons [PAHs]) and can therefore be used to detect chlorinated solvents and other nonfluorescing NAPLs that had previously been undetectable with conventional LIF tools. With DyeLIF, an aqueous solution of water and nontoxic hydrophobic dye is continuously injected ahead of the sapphire detection window while the LIF probe is being advanced in the subsurface. If soil containing NAPL is penetrated, the injected dye solvates into the NAPL within a few milliseconds, creating strong fluorescence that is transmitted via fiber‐optic filaments to aboveground optical sensors. A detailed field evaluation of the novel DyeLIF technology was performed at a contaminated industrial site in Lowell, Massachusetts, USA where chlorinated solvent dense nonaqueous phase liquid (DNAPL) persists below the water table in sandy sediments. Continuously cored boreholes were drilled adjacent to 5 of 30 DyeLIF probes that were advanced at that site. The cores were subsampled in high resolution to generate discrete‐depth soil samples as splits at the same depths where DNAPL was detected in the colocated DyeLIF probes. The cores were analyzed above ground using (1) colorimetric screening using hydrophobic dye tests, (2) laboratory extraction and quantitative chemical analysis, (3) “Benchtop” DyeLIF, and (4) volumetric moisture content. Correlation between DyeLIF and aboveground analyses of the soil cores was excellent: 98% agreement with positive DNAPL detections in samples where DNAPL pore saturations were >0.7% (based on quantitative soil analyses) and the ex situ tests. DyeLIF produced the equivalent of one aboveground colorimetric dye test every 0.2 inch (0.5 cm) of probing. With average daily probing of 395 linear feet (120.4 m), this was the equivalent of 12,039 discrete‐depth colorimetric dye tests/day. Because DyeLIF is an in situ measurement, there are no issues with soil core recovery like there would be for conventional ex situ colorimetric dye tests and 100% characterization of the probed intervals is achieved. Tracking the injection rate and pressure of the dye solution provides simultaneous data regarding relative soil permeability, similar to other direct push (DP) hydraulic profiling tools. Conventional LIF is considered the premier DP tool to identify and map NAPL containing PAHs in the subsurface or confirm its absence. While chlorinated solvent DNAPLs at some field sites contain impurities (e.g., solvated greases or oils) that make them detectable with conventional LIF techniques, at other sites, the DNAPL cannot be detected with conventional LIF. At such sites, the injection of a hydrophobic dye ahead of the sapphire window with the DyeLIF system now makes the LIF technology applicable to the many types of NAPLs that were previously invisible using conventional LIF techniques.  相似文献   

5.
This study investigates structural and adsorption properties of the powdered waste shells of Rapana gastropod and their use as a new cheap adsorbent to remove reactive dye Brilliant Red HE‐3B from aqueous solutions under batch conditions. For the powder shells characterization, solubility tests in acidic solutions and X‐ray diffraction (XRD), scanning electron microscopy (SEM), energy‐dispersive X‐ray spectroscopy (EDX), Fourier transform IR spectroscopy (FT‐IR) and thermogravimetric analyses were performed. The results revealed that the adsorbent surface is heterogeneous consisting mainly from calcium carbonate layers (either calcite or aragonite) and a small amount of organic macromolecules (proteins and polysaccharides). The dye adsorptive potential of gastropod shells powder was evaluated as function of initial solution pH (1–5), adsorbent dose (6–40 g L?1), dye concentration (50–300 mg L?1), temperature (5–60°C), and contact time (0–24 h). It was observed that the maximum values of dye percentage removal were obtained at the initial pH of solution 1.2, shells dose of 40 g L?1, dye initial concentration of 50–50 mg L?1 and higher temperatures; the equilibrium time decreases with increasing of dye concentration. It is proved that the waste seashell powder can be used as low cost bioinorganic adsorbent for dyes removal from textile wastewaters.  相似文献   

6.
A simple and reliable method for rapid and selective extraction and determination of trace levels of Ni2+ and Mn2+ was developed by ionic liquid (IL) based dispersive liquid–liquid microextraction coupled to flame atomic absorption spectrometry (FAAS) detection. The proposed method was successfully applied to the preconcentration and determination of nickel and manganese in soil, vegetable, and water samples. After preconcentration, the settled IL‐phase was dissolved in 100 µL of ethanol and aspirated into the FAAS using a home‐made microsample introduction system. Injection of 50 µL of each analyte into an air–acetylene flame provided very sensitive spike‐like and reproducible signals. Effective parameters such as pH, amount of IL, volume of the disperser solvent, concentration of the chelating agent, and effect of salt concentration were inspected by a (25‐1) fractional factorial design to identify the most important parameters and their interactions. Under optimum conditions, preconcentration of 10 mL sample solution permitted the detection of 0.93 µg L?1 Ni2+ and 0.52 µg L?1 Mn2+ with enrichment factors 77.2 and 82.6 for Ni2+ and Mn2+, respectively. The accuracy of the procedure was evaluated by analysis of a certified reference material (CRM TMDW‐500, drinking water).  相似文献   

7.
  相似文献   

8.
Malachite green (MG), a traditional agent used in aquaculture although is not approved; its low cost and high efficacy make illicit use likely. We developed a small‐scale, simple, and sensitive dispersive liquid–liquid microextraction procedure for the assay of trace amounts of MG in aquatic environment of Trout fish. Fiber optic‐linear array detection spectrophotometry with charge‐coupled device detector benefiting from a microcell was used for this purpose. The method is based on enhancement effect of an anionic surfactant on the extraction of MG in to very fine multidroplets of microextraction solvent which made assisted by disperser solvent. Under the optimum conditions, the enrichment factor 77.5 was obtained from a 5‐mL water sample. The calibration graph was linear up to 5 × 10?7 mol L?1 with detection limit of 1 × 10?8 mol L?1. The relative standard deviation for seven replicate measurements of 4 × 10?7 and 5 × 10?8 mol L?1 of MG were 3.3 and 4.5%, respectively.  相似文献   

9.
Batch sorption technique was carried out for the removal of anionic dye Congo red (CR) from aqueous solution using raw rectorite (R‐REC) and organified rectorite (CTA+‐REC) modified by cetyltrimethylammonium bromide (CTAB) as adsorbents. The effects of organification degree of CTA+‐REC as well as the process parameters including the pH of dye solution, sorption time, and initial dye concentration on adsorption capacity for CR were investigated and the sorption kinetics was also evaluated. The results showed that the sorption behaviors of R‐REC and CTA+‐REC for CR followed pseudo‐second‐order kinetic model and the sorption equilibrium data perfectly obeyed the Langmuir isotherm. The thermodynamic parameters including entropy of sorption (ΔS0), enthalpy of sorption (ΔH0), and Gibbs free energy of sorption (ΔG0) were obtained and analyzed. Fourier transform infrared study revealed that a chemisorption process occurred between CR and CTA+‐REC. REC modified by cationic surfactants showed the higher adsorption capacities for CR compared to R‐REC and in theory would be used as an efficient and promising adsorbent for the removal of anionic dyes in wastewater treatment.  相似文献   

10.
Highly sensitive and selective methods for the determination of trace elements in waters and solutions are made possible by the combination of flotation and spectrophotometry (flotation spectrophotometry). The basis for it are multiply charged anion complexes of the analyte, which form sparingly soluble ion association complexes with singly charged basic dye cations in aqueous solution. Intense shaking of the aqueous solution with an organic solvent (having a low dielectric constant) results in the accumulation of these ion association complexes at the interface or on the vessel walls (flotation step). After separating the ion association complexes from the liquid phases, they are dissolved and dissociated in a polar organic solvent and the absorbance of the basic dye ions is measured as a function of the concentration of the analyte. By the example of the trace determination of arsenic in natural water, the possibilities of analytical chemistry by combination of flotation steps and spectrophotometry are demonstrated. According to the arsenic content, its determination can be performed by flotation spectrophotometry with crystal violet (detection limit 50 ng/ml As), by an indirect determination of arsenic via flotation spectrophotometry of molybdenum in the dodecamolybdoarsenic acid (detection limit 1 ng/ml As) or by the combination of collector precipitation of arsenic with zirconium hydroxide followed by froth flotation and flotation spectrophotometry as the determination technique (detection limit 0.05 ng/ml As). The reproducibilities of these variants are indicated and their accuracy is checked by comparison of methods.  相似文献   

11.
An innovative micro‐extraction of aqueous samples coupled with gas chromatography/mass spectrometry in selected ion‐monitoring mode (GC/MS‐SIM) was developed to selectively analyze for 1,4‐dioxane with low part‐per‐billion detection sensitivity. Recoveries of 1,4‐dioxane ranged from 93% to 117% for both spiked laboratory reagent water and natural groundwater matrices, the later having elevated organic carbon content (8.34 ± 0.31 mg/L as total organic carbon). We observed that freezing the aqueous sample along with the extraction solvent enhanced the extraction efficiency, minimized physical interferences, and improved sensitivity resulting in a limit of detection for 1,4‐dioxane to approximately 1.6 μg/L. This method substantially reduces the labor, time, reagents and cost, and uses instruments that are commonly found in analytical laboratories. This method requires a relatively small sample volume (200 μL), and can be considered a green analytical method as it minimizes the use of toxic solvents and the associated laboratory wastes.  相似文献   

12.
Photooxidation degradation of Reactive Brilliant Red K‐2BP (K‐2BP) aqueous solution by ultraviolet irradiation/sodium hypochlorite (UV/NaClO) was investigated. The effects of NaClO dosage, pH, temperature and initial dye concentrations were studied. A possible degradation pathway of K‐2BP was investigated. Acidic or neutral conditions were beneficial to the decolorization of K‐2BP aqueous solution. However, alkaline conditions facilitated chemical oxygen demand (COD) removal. Increasing the solution temperature from 20 to 50°C increased the removal of color and COD. However, at 60°C, the final percentage color and COD removal decreased by approximately 17 and 10%, respectively. Based on the products indentified and theoretical analysis, N=N cleavage and C‐N cleavage were possible initial steps in the degradation of K‐2BP. From the results of this work, we conclude that treatment of UV/NaClO is an efficient method to degrade K‐2BP in aqueous solution.  相似文献   

13.
The removal of Malachite green (MG) from aqueous solutions by cross‐linked chitosan coated bentonite (CCB) beads was investigated and the CCB beads were characterized by Fourier Transform Infrared (FTIR) spectroscopy, scanning electron microscopy (SEM) coupled with energy dispersive spectroscopy (EDS) and X‐ray diffraction (XRD) analysis. Solubility and swelling tests were performed in order to determine the stability of the CCB beads in acidic solution, basic solution and distilled water. The amount of MG adsorbed was shown to be influenced by the initial pH of the solution, contact time and the initial MG concentration. A kinetic study indicated that a pseudo‐second‐order model agreed well with the experimental data. From the Langmuir isotherm model, the maximum adsorption capacity of MG was found to be 435.0 mg g–1. Desorption tests were carried out at different concentrations of EDTA, H2SO4 and NaOH. However, all desorbing solutions showed zero recovery of MG at all concentrations.  相似文献   

14.
In this study, 5,17‐bis‐[(4‐benzylpiperidine)methyl]‐25,26,27,28‐tetrahydroxy‐calix[4]arene ( 3 ) has been prepared by the treatment of calix[4]arene with a secondary amine (4‐benzylpiperidine) and formaldehyde by means of Mannich reaction. The prepared Mannich base ( 3 ) has been grafted onto [3‐(2,3‐epoxypropoxy)‐propyl]‐trimethoxysilane‐modified Fe3O4 magnetite nanoparticles (EPPTMS‐MN) in order to obtain 5,17‐bis‐[(4‐benzylpiperidine)methyl]‐25,26,27,28‐tetrahydroxy calix[4]arene‐grafted EPPTMS‐MN (BP‐calix[4]arene‐grafted Fe3O4). All new compounds were characterized by a combination of FTIR and 1H‐NMR analyses. The morphology of the magnetic nanoparticles was examined by transmission electron microscopy. Moreover, the studies regarding the removal of arsenate and dichromate ions from the aqueous solutions were also carried out by using 5,17‐bis‐[(4‐benzylpiperidine)methyl]‐25,26,27,28‐tetrahydroxy‐calix[4]arene in liquid–liquid extraction and BP‐calix[4]arene‐grafted Fe3O4 ( 4 ) in solid–liquid extraction experiments. The extraction results indicated that 3 is protonated at proton‐switchable binding sites in acidic conditions. Hence, facilitating binding of arsenate and dichromate is resulted from both electrostatic interactions and hydrogen bonding. To understand the selectivity of 3 , the retention of dichromate anions in the presence of Cl−, NO, and SO anions at pH 1.5 was also examined.  相似文献   

15.
A novel, simple method based on magnetic separation was developed for analytical purposes. In this method, N‐methyl‐D‐glucamine (NMDG) modified magnetic microparticles that were synthesized by using the sol‐gel method were used for the selective extraction and preconcentration of boron from aqueous solutions. This method combines the simplicity and selectivity of solvent extraction with the easy separation of magnetic microparticles from a solution with a magnet without any preliminary filtration step. The structure of the prepared γ‐Fe2O3‐SiO2‐NMDG (magnetic sorbent) composites were characterized by using X‐ray diffraction (XRD), Transmission Electron Microscopy (TEM), and Fourier Transform Infrared Spectroscopy (FTIR). The influence of different parameters on the sorbent capacity, such as the sorption/desorption of boron, magnetic sorbent dosage, pH, equilibrium time, type, and amount of stripping solution, were evaluated by using the magnetic sorbent. Any equilibrium pH greater than 6 can be used for sorption. Desorption from the sorbent was carried out by using 1.0 M HCl. The sorption and desorption efficiency of the γ‐Fe2O3‐SiO2‐NMDG was found as 92.5 ± 0.5% and 99.8 ± 6%, respectively.  相似文献   

16.
Zero‐valent, iron‐encapsulated alginate beads were synthesized and were applied for the removal of Cr(VI) from aqueous solutions. The effects of several important parameters including solution pH, contact time, initial concentration and reaction temperature on Cr(VI) removal levels were investigated in batch studies. An initial solution pH of 1.0 was seen to be most favorable for Cr(VI) removal. The removal process was quick and almost 80% of the removal was attained within 60 min. The kinetic data followed the second‐order equation well. The Cr(VI) removal was almost reaction temperature‐independent and decreased with an increase in Cr(VI) initial concentration. The removal of Cr(VI) by iron‐encapsulated alginate beads was found to be significantly higher than that of non‐encapsulated alginate beads.  相似文献   

17.
The removal of three basic dyes by adsorption onto bentonite was investigated for single, binary, and ternary solutions in a batch system. Before and after dye adsorption, bentonite samples were analyzed by using X‐ray fluorescence spectrometer, SEM, and Fourier transform IR spectrometry. The D‐optimal design and response surface methodology were applied in designing the experiments for evaluating the interactive effects of each initial concentrations variable of the dyes in binary systems. Predicted values were found to be in good agreement with experimental values, which defined propriety of the model and the achievement of D‐optimal in optimization of adsorption of binary dye systems. The competitive adsorption results showed that the adsorption amount of a dye was suppressed in the presence and increasing concentrations of second or third dye. For mono‐component isotherm modeling, Langmuir and Freundlich models were applied to equilibrium data of single, binary, and ternary dye solutions, while modified Langmuir, Sheindrof–Rebhun–Sheintuch and modified extended Freundlich models were also applied to equilibrium data of binary dye solutions for multi‐component isotherm modeling. The results showed that the Langmuir was the more suitable model for single dye systems while extended Freundlich model fitted best to the experimental data with the lowest error values for multi‐dye systems.  相似文献   

18.
Electrical resistance heating (ERH) experiments were performed in a two‐dimensional water‐saturated porous medium comprising an electrically conductive, low‐permeability clay lens embedded within a less electrically conductive, higher permeability silica sand. These were compared to experiments performed in homogeneous silica sand. All experiments were performed in the absence of a non‐aqueous phase liquid (NAPL) or dissolved volatile organic compound (VOC). Temperature monitoring showed preferential heating in the clay lens and higher overall heating rates throughout the test cell compared to the homogeneous case. Gas production was localized around the sand–clay interface due to high temperature and low capillary displacement pressure. Above the clay lens, unexpected temperature plateaus were observed, similar to those observed in previous experiments during NAPL–water co‐boiling. A conceptual model based on the consumption of thermal energy as latent heat of vaporization in the highly localized heating and gas production region adjacent to the clay lens is proposed to explain the temperature plateaus. Supporting data is drawn from images of the gas phase and electric current measurements. These results show that the use of co‐boiling plateaus as an indicator of NAPL–water co‐boiling could be misleading during applications of ERH at sites containing electrically conductive, low‐permeability clay lenses embedded within less electrically conductive, higher‐permeability sands.  相似文献   

19.
Adsorption is of significant importance for effluent treatment, especially for the treatment of colored effluent generated from the dyeing and bleaching industries. Low cost adsorbents have gained attention over the decades as a means of achieving very high removal efficiencies to meet effluent discharge standards. The present article reports on batch investigations for color removal from aqueous solutions of Methylene Blue (MB) and Congo Red (CR) using Rice Husk Ash (RHA) as an alternative low cost adsorbent. The performance analysis was carried out as a function of various operating parameters, such as initial concentration of dye, adsorbent dose, contact time, shaker speed, interruption of shaking and ionic concentration. Performance studies revealed that a very high percentage removal of color was achievable for both dyes. The maximum percentage removal of MB was 99.939%, while 98.835% removal was observed for CR. These percentage removals were better than existing systems. Detailed data analysis indicated that adsorption of MB followed the Temkin isotherm, while CR followed the Freundlich isotherm. These isotherms were feasible within the framework of experimentation. Batch kinetic data, on the other hand, indicated that pseudo second order kinetics governed adsorption in both cases. Sensitivity analysis further indicated that the effects of initial dye concentration, shaker speed, pH and ionic strength had no noticeable effect on the percentage dye removal at equilibrium. Batch desorption studies revealed that 50% acetone solution was optimum for CR, while desorption of MB varied directly with acetone concentration.  相似文献   

20.
A miniaturized ultrasonic extraction procedure was developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in soil by gas chromatography‐mass spectrometry. After determination of the most suitable extraction solvent with 5 min sonication time, several other parameters (sample amount, solvent volume and number of extraction times) were optimized using a 23 factorial experimental design. Recoveries of PAHs from spiked soil samples were over 90% for three different fortification levels between 50 and 300 μg/kg, and relative standard deviations of the recoveries were in the range of < 1–15%. The limits of detection ranged from 0.002 to 1.87 μg/kg. The performance of the developed procedure was also compared with other traditional Soxhlet, shake flask and large scale ultrasonic extraction procedures on real soil samples, and extraction methods showed comparable efficiencies. The proposed procedure required small volumes of solvent and sample. It was practicable, rapid and easy to use for analysis of PAHs in soils.  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号