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1.
Polyurethane foams (PUFs) loaded with the chromogenic reagent 4,4′-dichlorodithizone (Cl2H2DZ) have been investigated for the quantitative retention, chemical speciation and sequential determination of traces of inorganic selenium(IV) and (VI) from aqueous media containing bromide ions. The retention profile of selenium(IV) onto the reagent loaded foam followed a dual-mode sorption mechanism involving both absorption related to “solvent extraction” and an added component for surface adsorption. The kinetics and thermodynamic characteristics of selenium(IV) uptake onto PUFs have been studied. The kinetics of selenium(IV) sorption onto PUFs was found fast, reached equilibrium in few minutes and followed a first-order rate constant in presence of bromide ions in the extraction media. The thermodynamic parameters, ΔH, ΔS and ΔG, indicated the exothermic and spontaneous nature of the sorption process. The sorption and the recovery percentages of inorganic selenium(IV) from fresh water by the proposed loaded foam columns were achieved quantitatively. The height equivalent to theoretical plate (HETP), the number of layers (N), breakthrough capacity and the critical capacity for selenium(IV) uptake onto Cl2H2DZ loaded foams columns were found to be 1.3, 103, 8.6 and 7.2 mg/g, respectively. The method was successfully applied for the chemical speciation and sequential determination of inorganic selenium(IV) and/or (VI) species spiked to fresh and industrial wastewaters.  相似文献   

2.
The influence of different parameters on the sorption profiles of trace and ultra traces of gold (I) species from the aqueous cyanide media onto the solid sorbents ion exchange polyurethane foams (IEPUFs) and commercial unloaded polyurethane foams (PUFs) based polyether type has been investigated. The retention of gold (I) species onto the investigated solid sorbents followed a first-order rate equation with an overall rate constant k in the range 2.2-2.8 ± 0.2 s−1. The sorption data of gold (I) followed Freundlich and Langmuir isotherm models. Thus, the a dual-mode of sorption mechanism involving absorption related to “weak base anion exchanger” and an added component for “surface adsorption” seems the most likely proposed dual mechanism for retention profile of gold (I) by the IEPUFs and PUFs solid sorbents. The capacity of the IEPUFs and PUFs towards gold (I) sorption calculated from the sorption isotherms was found to be 11.21 ± 1.8 and 5.29 ± 0.9 mg g−1, respectively. The chromatographic separation of the spiked inorganic gold (I) from de ionized water at concentrations 5-15 μg mL−1 onto the developed IEPUFs and PUFs packed columns at 10 mL min−1 flow rate was successfully achieved. The retained gold (I) species were then recovered quantitatively from the IEPUFs (98.4 ± 2.4%, n = 5) and PUFs (95.4 ± 3.4%, n = 5) packed columns using perchloric acid (60 mL, 1.0 mol L−1) as a proper eluating agent. Thiourea (1.0 mol L−1)-H2SO4 (0.1 mol L−1) system was also used as eluating agent for the recovery of gold (I) from IEPUFS (95.4 ± 5.4%, n = 3) and also PUFs (93.4 ± 4.4%, n = 3) packed columns. The performance of the IEPUFs and PUFs packed columns in terms of the height equivalent to the theoretical plates (HETP), number of plates (N), and critical and breakthrough capacities towards gold (I) species were evaluated. The developed IEPUFs packed column was applied successfully for complete retention and recovery (98.5 ± 2.7) of gold (III) species spiked onto tap- and industrial wastewater samples at <10 μg Au mL−1 after reduction to gold (I). The IEPUFs packed column was applied satisfactorily for complete retention and recovery (98.5 ± 2.7) of total inorganic gold (I) and/or gold (III) species spiked to tap- and industrial wastewater samples at <10 μg mL−1 gold. Chromatographic separation of gold (I) from silver (I) and base metal ions (Fe, Ni, Cu and Zn) using IEPUFS packed columns was satisfactorily achieved. The proposed method was applied successfully for the pre-concentration and separation from anodic slime and subsequent FAAS determination of analyte with satisfactory results (recoveries >95%, relative standard deviations <4.0%).  相似文献   

3.
El-Shahawi MS  Kiwan AM  Al-Daheri SM  Saleh MH 《Talanta》1995,42(10):1471-1478
This paper reports the concentration of some dissolved organic phosphorus insecticides in water by open-cell polyurethane foam. The results of preliminary screening tests on the retention of the tested insecticides (Diazinon, Malathion and Chloropyrifos) by polyester foams indicated that a very high percent removal of the insecticides was obtained. The retention rate was fast and reaches equilibrium in a few minutes. The various parameters affecting the preconcentration of the tested insecticides by unloaded foam, e.g. pH, extraction media, shaking time, salt effect, flow rate, temperature and sample volumes have been optimized via the static mode of separation. The unloaded foams were employed in columns for the retention and recovery of the tested species. The sorption efficiency and the recovery of the tested compounds by the unloaded foam column were found to be up to 95.5%. The equivalent to a theoretical plate by the unloaded foam was found in the range 1.12 - 1.32 +/- 0.2 mm. The sorption mechanism of the tested species by the foam is discussed. The separation of some of the tested species in a mixture was achieved. The foam membrane offers unique advantages over conventional bulk-type granular sorbents and solvent extraction in offering high flow rates, rapid, versatile, effective separation and preconcentration of different species from aqueous samples. The foam provides the advantages of being, insoluble, easily separable and non-polluting, as well as inexpensive.  相似文献   

4.
This paper reports the preconcentration of some dissolved organic phosphorous and chlorinated acaricides in water by porous polyether based polyurethane foam. Preliminary screening tests on the retention of the tested compounds, i.e., dicofol and bromopropylate, by polyether foams indicated that a very high percent removal of the tested species was obtained. The retention rate was found fast and reaches equilibrium in a few minutes. The various parameters, e.g., pH, extraction media, shaking time, salt effect, temperature and sample volumes affecting the preconcentration of the tested species by the unloaded foam, trioctylamine and trimethylphosphate treated foam have been optimized via batch modes of separation. The unloaded foams were employed in column modes for the retention and recovery of the tested species. The sorption efficiency and recovery of the compounds by the unloaded foams column were found to be up to 97.5%. The height equivalent to a theoretical plate (HETP) obtained by the unloaded foam was found to be in the range 1.1-1.3 ± 0.2 mm. The sorption mechanism of the tested compounds by the foams was discussed.  相似文献   

5.
The retention of chromium (VI) from aqueous media onto tetraphenylarsonium chloride (TPAs+Cl) or tetraphenylphosphonium bromide (TPP+Br) immobilized polyurethane foams (PUFs) was fast and followed first order reaction. The kinetic data of the retention step were subjected to Weber-Morris, Lagergren, Bhattacharya and Venkobachar and Bt kinetic models. The results revealed that, film and intraparticle transport might be the two steps controlling the rate of chromium (VI) sorption from the aqueous acid solutions of pH ∼ zero. The positive values of the Δ H of chromium (VI) retention by the reagents loaded PUFs were interpreted as an endothermic process. Under the optimum pH (pH ∼ zero ) of the aqueous solution, the proposed TPAs+Cl or TPP+Br immobilized PUFs was successfully used in a series of medical syringe (30, 50 mL capacity) as pulse columns for complete collection of chromium (VI) species present in fresh and industrial wastewater samples at ultra trace low level of chromium (VI) (≤ 0.05 μg mL− 1). The collected chromium (VI) species onto TPAs+Cl or TPP+Br-PUFs was then stripped quantitatively (98-102 ± 2.6%) from the pulse columns with NaOH (2.0 mol L− 1) and subsequently analyzed photometrically. The chromium (VI) ions could be pre concentrated up to 100-fold from large volume of water samples. The proposed pulse foam columns were applied successfully for complete collection, recovery (97.5 ± 2.6%, n = 5) and subsequent chemical speciation of chromium (III) and (VI) in wastewater samples. The results are in good agreement with the reported and standard methods at 95% confidence.  相似文献   

6.
This work deals with the preconcentration of some water soluble pesticides, pyrethroids and acaricides by polyurethane foams. The retention profiles of the tested species were found quickly and reached equilibrium in a few min. Various parameters — e.g. pH, extraction media, shaking time, salt effect, temperature and sample volume — affecting the preconcentration of the tested species by the unloaded foams and tri-n-octylamine and tri-n-methylphosphate treated foams were optimized. The unloaded foams were employed in a column mode to study the quantitative retention and recovery of the tested species. The sorption efficiency and recovery of the compounds by the unloaded foam column were found to be up to 99.5%±2.1. The height equivalent of a theoretical plate for the unloaded foam column was found to be in the range 1.9–2±0.2 mm. The sorption mechanisms of the tested compounds by the foams are discussed. Analysis of N, P, Na, K, Cu, Zn, Mn, Fe, humidity, wet and dry mass of tomato and parsley untreated and sprayed for different time intervals — i.e. 24, 72 and 120 h — with Chlorpyrifos, was carried out.  相似文献   

7.
El-Shahawi MS 《Talanta》1994,41(9):1481-1488
The analytical utility of unloaded and polyester-based polyurethane loaded foams with tri-n-octylamine (TOA) in the removal of some phenols from water were carried out. In static mode, the TOA-loaded foams showed a good affinity of extraction towards the tested compounds as compared to the untreated foams. The various parameters affecting the retention efficiency of the tested compounds from aqueous media by the foam were examined via batch technique. The TOA-loaded foams were employed in column modes for the extraction and recovery of the tested phenols. The retention efficiency and the recovery of the tested compounds from the loaded foam column were up to 98.5%. Sorption of the compounds by the foam were brought by solvent extraction mechanism. The molecular weight and the pK(a) of the compounds play an important role in the extraction process. The height equivalent to a theoretical plate (HETP) of the TOA-foam column was found in the range 1.8-2.05 +/- 0.1 mm at flow-rates up to 10 cm(3)/min. Separation of some of the tested phenols was also carried out by the TOA-foam columns. The membrane properties of the polyester foam sorbents give unique advantages over conventional granular sorbents in rapid, versatile and effective separations and preconcentrations of the tested compounds.  相似文献   

8.
The retention profile of uranyl ions from aqueous thiocyanate media by polyether-type based polyurethane foams (PUFs) has been studied to gain more information regarding the mechanism of extraction. The effect of pH, shaking time, surfactant type, extraction media, temperature and analyte concentration on the retention of uranyl ions onto PUFs has been studied. It has been found that, the sorption of uranyl ions involved in the formation of a ternary complex ion associate of uranyl ion, thiocyanate and PUFs is highly dependent on these parameters. The kinetics and thermodynamics of the uranyl ions sorption have been studied in more detail. The dependency of the extraction on the parameters can be explained via a “solvent extraction,” mechanism. However, owing to the complex nature of the PUFs a dual-mode sorption mechanism involving both absorptions related to “solvent extraction” and an added component for “surface adsorption” may be operated simultaneously. Attempts for quantitative retention and recovery of the uranyl ions in tap and industrial waste water samples by the proposed PUFs columns has been carried out and satisfactory results have been obtained. The cellular structure of the PUF sorbent offer unique advantages over a conventional bulk type sorbents in rapid, versatile effective separation and/or preconcentration of uranyl ions.  相似文献   

9.
Strongly polar phenolic acids are weakly retained and often poorly separated in reversed-phase (RP) liquid chromatography. We prepared zwitterionic polymethacrylate monolithic columns for micro-HPLC by in situ co-polymerization in fused-silica capillaries. The capillary monolithic columns prepared under optimized polymerization conditions show some similarities with the conventional particulate commercial ZIC-HILIC silica-based columns, however have higher retention and better separation selectivity under reversed-phase conditions, so that they can be employed for dual-mode HILIC-RP separations of phenolic acids on a single column. The capillary polymethacrylate monolithic sulfobetaine columns show excellent thermal stability and improved performance at temperatures 60–80 °C. The effects of the operation conditions on separation were investigated, including the type and the concentration of the organic solvent in the aqueous-organic mobile phase (acetonitrile and methanol), the ionic strength of the acetate buffer and temperature. While the retention in the RP mode decreases at higher temperatures in mobile phases with relatively low concentrations of acetonitrile, it is almost independent of temperature at HILIC conditions in highly organic mobile phases. The best separation efficiency can be achieved using relatively high acetate buffer ionic strength (20–30 mmol L−1) and gradient elution with alternately increasing (HILIC mode) and decreasing (RP mode) concentration of aqueous buffer in aqueous acetonitrile. Applications of the monolithic sulfobetaine capillary columns in alternating HILIC-RP modes are demonstrated on the analysis of phenolic acids in a beer sample.  相似文献   

10.
Werbowesky R  Chow A 《Talanta》1996,43(2):263-274
The extraction of 12 closely related mono-azo dyes by polyester and polyether-type polyurethane foams was studied to gain more information regarding the mechanism of the extraction of organic compounds. The effects on extraction of solution pH, dye concentration and salt concentration were investigated. It was found that the extraction of the dyes involved a neutral zwitterionic species and is highly dependent on the parameters studied. The dependency of the extraction on these parameters can be explained in a manner consistent with solvent extraction; however, the dual-mode sorption mechanism seems a more likely model. This mechanism involves both absorption related to solvent extraction, and an added component for surface adsorption. While the dual-mode sorption model explains the observed extraction behaviour, the data suggest that surface adsorption plays a much larger role than previously considered.  相似文献   

11.
Zhang L  Zhang M  Guo X  Liu X  Kang P  Chen X 《Talanta》2010,83(2):344-350
Titanium dioxide nanoparticles (nano-TiO2) were employed for the sorption of Te(IV) ions from aqueous solution. A detailed study of the process was performed by varying the sorption time, pH, and temperature. The sorption was found to be fast, equilibrium was reached within 8 min. When the concentration of Te(IV) was below 40 mg L−1, at least 97% of tellurium was adsorbed by nano-TiO2 in the pH range of 1-2 and 8-9. The sorbed Te(IV) ions were desorbed with 2.0 mL of 0.5 mol L−1 NaOH. The sorption data could be well interpreted by the Langmuir model with the maximum adsorption capacity of 32.75 mg g−1 (20 ± 0.1 °C) of Te(IV) on nano-TiO2. The kinetics and thermodynamics of the sorption of Te(IV) onto nano-TiO2 were also studied. The kinetic experimental data properly correlated with the second-order kinetic model (k2 = 0.0368 g mg−1 min−1, 293 K). The overall rate process appeared to be influenced by both boundary layer diffusion and intra-particle diffusion. The mean energy of adsorption was calculated to be 17.41 kJ mol−1 from the Dubinin-Radushkevich (D-R) adsorption isotherm at room temperature. Moreover, the thermodynamic parameters for the sorption were estimated, and the ΔH0 and ΔG0 values indicated the exothermic and spontaneous nature of the sorption process, respectively. Finally, Nano-TiO2 as sorbent was successfully applied to the separation of Te(IV) from the environmental samples with satisfactory results (recoveries >95%, relative standard deviations was 2.0%).  相似文献   

12.
M.F. El-Shahat  A.B. Farag 《Talanta》2007,71(1):236-241
The new type of the grafted polyurethane foam sorbents were prepared by coupling polyether polyol, toluene diisocyanate and basic dyestuff (Methylene blue, Rhodamine B and Brilliant green). The Me.B-PUF, Rh.B-PUF and Br.G-PUF were characterized using UV/vis, IR and TGA. The adsorption properties and chromatographic behaviour of these new adsorbents for preconcentration and separation of uranium(VI) ions at low concentrations from aqueous thiocyanate media were investigated by a batch process. The maximum sorption of U(VI) was in the pH ranges 1-4. The kinetics of sorption of the U(VI) by the Grafted-PUF were found to be fast with half life of sorption (t1/2) in 2.43 min. The average sorption capacity of different sorbents 0.124 meq g−1 for uranyl ions, enrichment factors ≈40 and the recovery 98-100% were achieved (R.S.D. ≈ 0.73%). The basic dyestuff Grafted-PUF could be used many times without decreasing their capacities significantly. The value of the Gibbs free energy (ΔG) for the sorbents is −7.3 kJ mol−1, which reflects the spontaneous nature of sorption process. The sorption mechanism of the metal ion onto Grafted-PUF was also discussed.  相似文献   

13.
A stable chelating sorbent was synthesized by covalently linking 4-hydroxytoluene or 4-hydroxyacetophenone with the polyurethane foam (PUF) through -NN- group. The synthesized chelating sorbents were characterized by IR and UV/vis measurements. The modified foams show excellent stability towards various solvents. Factors influencing the extraction process of Zn(II), Pb(II), Cd(II) and Hg(II) were studied and evaluated as a function of pH of metal ion solution and equilibration shaking time. The values of sorption capacity of metal ions (μg g−1) were determined with the two types of bonded foams. The two phenolic bonded foams were studied comparatively. The potential applications of the two newly synthesized foams for the removal and separation of the examined metal ions from two natural water samples (drinking tap water and Qaroun lake water at Fayoum City, Egypt) were investigated. Precision (assessed as a relative standard deviation, R.S.D.) was also evaluated and found to be ≤7.3% (N = 5) with a detection limit under 0.46 μg L−1.  相似文献   

14.
The sorption behaviour of 2.5 × 10−5 M solution of Cd(II) on polyurethane foam (PUF) from iodide medium have been investigated. The conditions were optimized from aqueous solutions of different pH (1-10) and of acids of varied concentration (0.01-1.0 M). The maximum concentration of KI was found to be 0.24 M and equilibration time was established to be 20 min. The data successfully followed the Freundlich and Dubinin-Radushkevich (D-R) isotherms at low metal ion concentration while Langmuir isotherm followed at higher metal ion concentration. The Freundlich parameter 1/n = 0.66 ± 0.02 have been evaluated whereas D-R isotherm yields the sorption free energy E = 10.5 ± 0.1 kJ mol−1 indicating ion exchange type chemisorption. The monolayer coverage (XL) constant of Langmuir isotherm was found to be 23.7 ± 0.4 mg g−1. The numerical values of thermodynamics parameters enthalpy (ΔH), entropy (ΔS) and Gibbs free energy (ΔG) indicated the endothermic and spontaneous nature of sorption. The Scatchard plot analysis was tested to evaluate the binding sites of the PUF and stability constants of sorption were determined. On the basis of these parameters, the sorption mechanism was discussed. Among the foreign ions tested, Pb(II), Hg(II), cyanide and nitrite should be absent. The clean separation of Cd(II) from Zn(II) ions in the ratio 1:250, respectively, was achieved by column chromatography.  相似文献   

15.
The recovery of the gold-thiourea complex from aqueous solutions with TBP-loaded and unloaded polyurethane foams was investigated in batch experiments. The rates of adsorption of the gold complex on various types of loaded and unloaded foams were studied in detail and compared with the rate of adsorption on active carbon. Loaded and unloaded polyurethane foams of the polyether or polyester type behaved similarly to active carbon. The adsorption capacity of the foams was lower than that of active carbon but the use of foam simplifies the procedure by eliminating the filtration process which is necessary with carbon.  相似文献   

16.
《Analytical letters》2012,45(4):703-717
Abstract

The formation of blue perchromic acid represents one of the most sensitive and selective tests for the identification of chromium. The sorption of perchromic acid on TBP loaded foam has been investigated for the detection, semiquantitative and quantitative determinations of chromium (VI). In foam batch method, it was possible to detect as los as 0.6, 0.4 and 0.2 ppm of chromium (VI) with unloaded or tricaprylylamine loaded foams, TBP-amine-loaded foams and TBP loaded foams, respectively.  相似文献   

17.
Malik UR  Hasany SM  Subhani MS 《Talanta》2005,66(1):166-173
The sorptive potential of sunflower stem (180-300 μm) for Cr(III) ions has been investigated in detail. The maximum sorption (≥85%) of Cr(III) ions (70.2 μM) has been accomplished using 30 mg of high density sunflower stem in 10 min from 0.001 M nitric and 0.0001 M hydrochloric acid solutions. The accumulation of Cr(III) ions on the sorbent follows Dubinin-Radushkevich (D-R), Freundlich and Langmuir isotherms. The isotherm yields D-R saturation capacity Xm = 1.60 ± 0.23 mmol g−1, β = −0.00654 ± 0.00017 kJ2 mol−2, mean free energy E = 8.74 ± 0.12 kJ mol−1, Freundlich sorption capacity KF = 0.24 ± 0.11 mol g−1, 1/n = 0.90 ± 0.04 and of Langmuir constant KL = 6800 ± 600 dm3 mol−1 and Cm = 120 ± 18 μmol g−1. The variation of sorption with temperature (283-323 K) gives ΔH = −23.3 ± 0.8 kJ mol−1, ΔS = −64.0 ± 2.7 J mol−1 K−1 and ΔG298k = −4.04 ± 0.09 kJ mol−1. The negative enthalpy and free energy envisage exothermic and spontaneous nature of sorption, respectively. Bisulphate, Fe(III), molybdate, citrate, Fe(II), Y(III) suppress the sorption significantly. The selectivity studies indicate that Cr(III), Eu(III) and Tb(III) ions can be separated from Tc(VII) and I(I). Sunflower stem can be used for the preconcentration and removal of Cr(III) ions from aqueous medium. This cheaper and novel sorbent has potential applications in analytical and environmental chemistry, in water decontamination, industrial waste treatment and in pollution abatement. A possible mechanism of biosorption of Cr(III) ions onto the sunflower stem has been proposed.  相似文献   

18.
In vitro degradation of porous 50/50, 70/30 and 90/10 PLGA (poly(dl-lactide-co-glycolide)) foams and PLGA/bioactive glass (20 wt%) composite foams was studied up to 16 weeks in TRIS (pH 7.4; 37 °C). Polar PLGA/bioactive glass composite films were prepared by applying the bioactive glass (S53P4) on one side of the composite. Porous foams were made by solvent casting and pressure quenching with CO2. The fabricated foams had an initial pore size of 50-500 μm and thickness of 2-2.5 mm. In vitro degradation of the prepared foams was evaluated after 1, 2, 4, 6, 8, 12 and 16 weeks. Weight loss, water uptake, molecular mass and the amount of dissolved bioactive glass were measured after each time period. Changes in pore morphology were analysed with SEM. The present in vitro results will be evaluated and compared with the results from ongoing animal studies where comparable implants are used for bone defect treatment under non-load-bearing conditions.  相似文献   

19.
Low sample recovery may represent an important drawback in liquid chromatography at the critical adsorption point (LC-CAP) if the critical eluent is not carefully fitted to the system. So far, this problem was often overlooked and only few experimental examples can be found in literature. We showed that in the case of polystyrene (PS) in a tetrahydrofuran (THF)/n-hexane critical mixed eluent, PS with molar masses higher than 100 kg mol−1 were not eluted from a tandem of two columns packed by bare silica gels with 30 nm and 100 nm pore size, respectively. The polymer trapped within the columns was well recovered after injection of a small volume of pure THF as demonstrated using 2D chromatography. We studied PS conformations by means of small angle neutron scattering and found that the THF/n-hexane critical eluent is in fact a theta solvent for PS. By replacing it by a CH2Cl2/n-hexane critical mixture, which is a good solvent for PS, the limits of reduced sample recovery was displaced towards far higher molar masses. Thus, thermodynamic quality of eluent - theta or good solvent - plays an important role on the phenomenon of sample recovery.  相似文献   

20.
Farag AB  El-Shahawi MS  Farrag S 《Talanta》1994,41(4):617-623
The preliminary screening tests on the preconcentration of lanthanum(III), aluminium(III), molybdenum(VI), gallium(III) and tungsten(VI) thiocyanate complexes in aqueous media by unloaded foam indicated a reasonable percentage of metal ions were retained on the foam. The influence of various parameters affecting the retention of these complex species from the aqueous media by the foam were critically studied and the possible mechanisms of the sorption of the compounds were suggested. However, owing to the complex chemical nature of the polyether-polyurethane foam, several mechanisms may be involved simultaneously. Attempts for the quantitative retention and recovery of the tested complexes by the foam columns were also made and satisfactory results were obtained. The height equivalent to theoretical plates (HETP) of the foam columns were calculated from the chromatograms and break through capacity curve and were found in the range 1.8-2.3 mm at flow rates up to 15 cm(3)/min. The proposed foam column method has been successfully used for the separation of a series of complex mixtures of the tested metal thiocyanate complexes in aqueous media. The membrane properties of the foam sorbents offer unique advantages over conventional bulk type granular sorbents in rapid, versatile effective separations and preconcentrations of different complexes from fluid samples.  相似文献   

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