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1.
Aminopropyl-functionalized mesoporous silicas, NH2-MCM-41 and NH2-SBA-15, as absorbents were utilized for rapid extraction, preconcentration and determination of trace amounts of silver. Flow rates of sample and eluent, pH, eluent solution, type, concentration and the least amount of eluent for desorption of silver ions were optimized; moreover, break through volume and the effect of various cationic interferences on the sorption of silver were evaluated. The extraction efficiency of silver ions was greater than 95% for MCM-41-NH2 and 85% for SBA-15-NH2 and the limit of detection (LOD) was less than 4 ng mL?1 for both functionalized mesoporous silicas. The preconcentration factor was greater than 210 and the relative standard deviation (RSD) was <2%. The adsorption capacity of the mesoporous silicas is higher than 143 mg g?1 for NH2-MCM-41 and 137 mg g?1 for NH2-SBA-15. Under similar experimental conditions the results for these solid phases were compared with each other. NH2-SBA-15, in spite of larger pore size diameter and adsorption of silver ions in higher flow rates has lower recovery and a higher RSD compared to MCM-41. This method has been applied to determine silver in photographic emulsions and real samples.  相似文献   

2.
This paper described a facile and direct electrochemical method for the determination of ultra-trace Cu2+ by employing amino-functionalized mesoporous silica (NH2-MCM-41) as enhanced sensing platform. NH2-MCM-41 was prepared by using a post-grafting process and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and fourier transform infrared (FTIR) spectroscopy. NH2-MCM-41 modified glassy carbon (GC) electrode showed higher sensitivity for anodic stripping voltammetric (ASV) detection of Cu2+ than that of MCM-41 modified one. The high sensitivity was attributed to synergistic effect between MCM-41 and amino-group, in which the high surface area and special mesoporous morphology of MCM-41 can cause strong physical absorption, and amino-groups are able to chelate copper ions. Some important parameters influencing the sensor response were optimized. Under optimum experimental conditions the sensor linearly responded to Cu2+ concentration in the range from 5 to 1000 ng L−1 with a detection limit of 0.9 ng L−1 (S/N = 3). Moreover, the sensor possessed good stability and electrode renewability. In the end, the proposed sensor was applied for determining Cu2+ in real samples and the accuracy of the results were comparable to those obtained by inductively coupled plasma optical emission spectrometry (ICP-OES) method.  相似文献   

3.
Abstract

In this study the effect of the dose and particle size of the adsorbent, initial dye concentration, initial pH, contact time and temperature were investigated for the removal of by means of fly ash (FA) methylene blue (MB) from an aqueous solution. The FA dose was found to be 2.0?g and the under 270 mesh sized particles were found to be effective particles for adsorption. The adsorption process reached its maximum value at 0.5?mg/L dye concentration and attained equilibrium within 10?minutes. The adsorption isotherm was found to follow the Langmuir model. The estimated adsorption free energy (ΔGo), enthalpy change (ΔHo), and entropy change (ΔSo) for the adsorption process were ?37.77?kJ mol?1, ?13.44?kJ mol?1 and 122 J mol?1 K?1 respectively at 298 K. The maximum adsorption capacity is 0,12?mg g?1 at 298 K and 0,07?mg g?1 at 398 K. The adsorption process was exothermic, feasible and spontaneous. The positive value of ΔSo shows the affinity of FA for MB while the low value of ΔGo suggests a physical adsorption process.  相似文献   

4.
The spherical mesoporous MCM-41 coated with a novel Ca2MoO5:Eu3+ phosphor layer was prepared for the first time. The obtained Ca2MoO5:Eu3+-MCM-41 was characterized via XRD and FT-IR. The crystal system of the Ca2MoO5 phase was determined to be orthorhombic, and its space group was found to be Ima2 (46), and its cell parameters were a = 16.175, b = 5.1514, c = 5.6977 A°; α = β = γ = 90°. The particle dimensions of MCM-41 and Ca2MoO5:Eu3+-MCM-41 nanoparticles were determined to be 260 nm and 229 nm via scanning electron microscopy analysis. Bortezomib was loaded into the Ca2MoO5:Eu3+-MCM-41 nanoparticles under scCO2 at 200 bars and 40 °C. The results of the TG analysis showed that the amount of drug-loaded to MCM-41 and Ca2MoO5:Eu3+-MCM-41 nanoparticles were determined to be 14.02% and 3.02%, respectively. The BET analysis showed that while the specific surface area and pore volume of MCM-41 and Ca2MoO5:Eu3+ before Bortezomib (BTZ) loading were 1,506 m2/g and 267 m2/g, respectively, after drug loading these values were found to decrease to 488 m2/g and 7.883 m2/g. It was determined that BTZ was released from the nanoparticles in a sustained manner over 66 h. The R2 value, which was calculated to be 0.9739, indicated that the release kinetic of BTZ followed the Korsmeyer–Peppas model.  相似文献   

5.
A series of vanadoaluminosilicate MCM-41 mesoporous molecular sieves with various compositions have been hydrothermally synthesized. Hexadecyltrimethylammonium bromide was used as a surfactant in the synthesis. The samples were characterized with nitrogen sorption, X-ray diffraction, differential thermal analysis, thermogravimetric analysis, Fourier transform-Infrared spectroscopy, UV-visible spectroscopy, scanning electron microscopy, transmission electron microscopy, and solid state NMR. The solid products had the MCM-41 structure and contained only atomically dispersed vanadium and aluminum consistent with framework vanadium and aluminum. The samples were hydrophobic and contained large amount of surfactant in the as-synthesized samples. The surfactant could be removed upon calcination at 450°C. N2 sorption measurements and TEM demonstrate the high mesoporosity of [V, Al]-MCM-41. The incorporation of vanadium and aluminum into MCM-41 decreased the surface area to some extent. The morphologies of all the samples were the agglomerate of plates. 29Si MAS NMR shows that the pore wall is amorphous. 27Al MAS NMR shows that all of aluminum species were tetrahedrally coordinated even after calcination at 550°C.  相似文献   

6.
The adsorption of the antibiotic amoxicillin at low concentration levels (µg?L?1 order) from aqueous solution on almond shell ashes has been investigated, either by kinetic or equilibrium assays. The effect of the adsorbent amount, initial concentration of the antibiotic, particle diameter (dp) and temperature were considered to evaluate the adsorption capacity of the adsorbent. The results showed that amoxicillin sorption is dependent on these four factors. The adsorption process was relatively fast and equilibrium was established in about 12 hours. The optimum parameters for an initial concentration of 450?µg?L?1 were 50?mg of adsorbent, 303?K and dp?<?600?µm. A comparison of kinetic models showed that pseudo-second order kinetics provides the best correlation of the experimental data. Isotherm data adjusted better to Langmuir equation, with an adsorption capacity of 2.5?±?0.1?mg?g?1 at 303?K. The desorption process was also evaluated (maximum efficiency of 5%). Thermodynamic parameters were calculated and the negative value of ΔH0 and ΔG0 showed that adsorption was exothermic and a spontaneous process.  相似文献   

7.
Polyoxometalates K7[α-PW11O39]·14H2O (PW11) modified mesoporous silica (MCM-48) with cubic structure, was prepared by impregnation and calcination methods. The modified mesoporous silica sorbent (PW11/MCM-48) was studied as a potential adsorbent for U(VI) from aqueous solutions. MCM-48 and PW11/MCM-48 were confirmed by X-ray diffraction and nitrogen physisorption techniques. The results indicate the original keggin structure of PW11 and mesoporous structure of MCM-48 are maintained after supporting PW11 on mesoporous silica MCM-48. The effects of contact time, solid-to-liquid ratio (m/V), solution pH and ionic strength on U(VI) sorption behaviors of the pure and modified mesoporous silicas were also studied. Typical sorption isotherms such as Langmuir and Freundlich isotherms were determined for sorption process. The results suggest that the sorption of U(VI) on MCM-48 or PW11/MCM-48 are strongly dependent on pH values but independent of ionic strength. The sorption capacity of PW11/MCM-48 for U(VI) is about ten times more than that of MCM-48.  相似文献   

8.
The adsorption of Cr(VI) and Ni(II) using ethylenediaminetetraacetic acid‐modified diatomite waste (EDTA‐DW) as an adsorbent in single and binary systems was investigated. The EDTA‐DW was characterized using various analytical techniques, including Fourier transform infrared spectroscopy, thermogravimetric analysis, Brunauer–Emmett–Teller measurements, X‐ray diffraction, scanning electron microscopy and energy‐dispersive spectrometry. The adsorption experiment was conducted by varying pH, adsorbent dosage, initial concentration and temperature. In the single system, the sorption data for Cr(VI) fitted the Langmuir isotherm, but the Ni(II) adsorption data fitted well the Freundlich isotherm. The maximum sorption capacity of Cr(VI) and Ni(II) was 2.9 mg g?1 at pH = 3 and 3.64 mg g?1 at pH = 8, respectively. The kinetic data for both Cr(VI) and Ni(II) followed well the pseudo‐second‐order kinetic model in single and binary systems. Meanwhile, the extended Langmuir and extended Freundlich multicomponent isotherm models were found to fit the competitive adsorption data for Cr(VI) and Ni(II). In addition, in the binary system, the existence of Ni(II) hindered the adsorption of Cr(VI), but the presence of Cr(VI) enhanced the removal of Ni(II). This study provides some realistic and valid data about the usage of modified diatomite waste for the removal of metal ions.  相似文献   

9.
Experiments on the removal and recovery of U(VI) from aqueous solution by tea waste were conducted. The adsorbent was characterized by scanning electron microscope and energy dispersive spectrometer before and after the adsorption treatment. The removal of U(VI) amounts to 86.80?% at optimum pH 6. The adsorption process reaches its equilibrium in 12?h at 308?K, and the kinetic characteristic can be described by the pseudo-second-order kinetic equation. The amount of adsorption increases from 22.92 to 142.21?mg?g?1 with the decrease of tea waste dosage from 100 to 10?mg for solution with an initial uranium concentration of 50?mg?L?1. Desorption for the four strippants is higher than 80?%. The equilibrium data are more agreeable with Freundlich isotherm than Langmuir isotherm.  相似文献   

10.
An indigenously prepared zinc chloride activated Ipomoea carnea (morning glory), a low-cost and abundant adsorbent, was used for removal of Cu(II) ions from aqueous solutions in a batch adsorption system. The chemical activating agent ZnCl2 was dissolved in deionised water and then added to the adsorbent in two different ratios 1:1 and 1:0.5 adsorbent to activating agent ratio by weight. Studies were conducted as a function of contact time, initial metal concentration, dose of adsorbent, and pH. Activated Ipomoea carnea (AIC) were characterised using scanning electron microscopy (SEM), iodine number and methylene blue number. High iodine numbers indicates development of micro pores with zinc chloride activation. Maximum adsorption was noted within pH range 6.0(±0.05). Adsorption process is fast initially and reaches equilibrium after about 4 hours. The kinetic data were analysed using pseudo-first-order and pseudo-second-order models. The pseudo-second-order kinetic model was found to agree well with the experimental data. Adsorption equilibrium data were analyzed using Langmuir and Freundlich isotherm models. The Langmuir model represented the sorption process better than the Freundlich model. Based on the Langmuir isotherm, the monolayer adsorption capacity of Cu(II) ions was 7.855 mg?g?1 for AIC (1:1) and 6.934 mg?g?1 for AIC (1:0.5).  相似文献   

11.
A new synthesized modified mesoporous silica (MCM-41) using 5-nitro-2-furaldehyde (fural) was applied as an effective sorbent for the solid phase extraction of uranium(VI) and thorium(IV) ions from aqueous solution for the measurement by inductively coupled plasma optical emission spectrometry (ICP OES). The influences of some analytical parameters on the quantitative recoveries of the analyte ions were investigated in batch method. Under optimal conditions, the analyte ions were sorbed by the sorbent at pH 5.5 and then eluted with 1.0 mL of 1.0 mol L−1 HNO3. The preconcentration factor was 100 for a 100 mL sample volume. The limits of detection (LOD) obtained for uranium(VI) and thorium(IV) were 0.3 μg L−1. The maximum sorption capacity of the modified MCM-41 was found to be 47 and 49 mg g−1 for uranium(VI) and thorium(IV), respectively. The sorbent exhibited good stability, reusability, high adsorption capacity and fast rate of equilibrium for sorption/desorption of uranium and thorium ions. The applicability of the synthesized sorbent was examined using CRM and real water samples.  相似文献   

12.
The adsorption of uranium (VI) using tetraphenylimidodiphosphinate (Htpip) was studied. Factors of affecting sorption efficiency have been investigated and results showed the adsorption of uranium (VI) was equilibrium at pH 4.5, time 20 min, adsorbent dosage 0.005 g and initial concentration 50 mg L?1 reaching 99.86 mg g?1 of adsorption capacity and 99.86% of removal efficiency. Additionally, the interfering ions studies showed that the adsorbent possessed excellent adsorption selectivity of uranium (VI). The surface morphology of Htpip was investigated by SEM. The adsorption process of uranium (VI) onto Htpip fit the pseudo-second-order kinetic model and the Freundlich isotherm model very well.  相似文献   

13.
Uranium (VI)-containing water has been recognized as a potential longer-term radiological health hazard. In this work, the sorptive potential of sunflower straw for U (VI) from aqueous solution was investigated in detail, including the effect of initial solution pH, adsorbent dosage, temperature, contact time and initial U (VI) concentration. A dose of 2.0 g L?1 of sunflower straw in an initial U (VI) concentration of 20 mg L?1 with an initial pH of 5.0 and a contact time of 10 h resulted in the maximum U (VI) uptake (about 6.96 mg g?1) at 298 K. The isotherm adsorption data was modeled best by the nonlinear Langmuir–Freundlich equation. The equilibrium sorption capacity of sunflower straw was observed to be approximately seven times higher than that of coconut-shell activated carbon as 251.52 and 32.37 mg g?1 under optimal conditions, respectively. The positive enthalpy and negative free energy suggested the endothermic and spontaneous nature of sorption, respectively. The kinetic data conformed successfully to the pseudo-second-order equation. Furthermore, energy dispersive X-ray, fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy demonstrated that U (VI) adsorption onto sunflower straw was predominantly controlled by ion exchange as well as complexation mechanism. The study revealed that sunflower straw could be exploited for uranium remediation of aqueous streams as a promising adsorbent.  相似文献   

14.
A new magnetic nanocomposite material, magnetic 18-crown-6/Fe3O4 nanocomposite (MCFN), was prepared for the removal of U(VI) from aqueous solution. The MCFN was composed of Fe3O4 nanoparticales modified by covalent attachment of 18-crown-6, which can help the material to be removed easily from solution by magnetic force. As a new adsorbent for U(VI) removal, MCFN was characterized by infrared radiation, scanning electron microscopy with energy dispersive X-ray spectroscopy, vibrating sample magnetometer and thermal gravimetric analysis. Those factors affecting the sorption behavior of U(VI), such as acidity, temperature, initial concentration of U(VI) and the amount of crown ethers were studied by orthogonal experiments. A maximum U(VI) sorption capacity of 91.12 mg g?1 was achieved at 45 °C, pH 5.5 for 30 min. The experimental results showed that MCFN had great sorption capacity, high selectivity and strong potentiality of enrichment and recovery for U(VI). In summary, MCFN is a promising candidate for U(VI) separation in future practical applications.  相似文献   

15.
A novel nanospheres adsorbent was successfully prepared using functionalized 1H-Pyrrole-1-ethanamine by homopolymerization. It could be easily protonated to form double-charged repeating structural units on the surface of nanospheres. The physic-chemical properties were characterized by SEM, TGA, XPS and Zeta potential. The effects of initial pH, adsorbent dosage, contact time, initial concentration, and ionic strength were studied in detail. The maximum adsorption capacity of Chromium(VI) was about 729.09?mg?g?1 at room temperature. Electrostatic attraction played an important role in the adsorption process and the size of the ion group had a greater effect on the adsorption performance than the charge.  相似文献   

16.
A new functionalized nanometer mesoporous silica (MCM-41) using 2,4-dihydroxybenzaldehyde (4-OHsal) was applied as an effective sorbent for solid phase extraction (SPE) of beryllium ions from aqueous solution followed by inductively coupled plasma optical emission spectrometric detection (ICP OES). The influences of some analytical parameters on the quantitative recoveries of the analyte ion were investigated in batch method. In order to perform the batch mode of SPE, known amount of sorbent was added to a test tube containing sample solution buffered at pH 7.2. After manual shaking and centrifugation the aqueous phase was decanted and beryllium was desorbed by adding 1.0 mL of 1.0 mol L?1 HNO3 to the sedimented sorbent. The sorbent was separated by centrifugation and the concentration of beryllium in the supernatant was determined by ICP OES. The maximum sorption capacity of the modified MCM-41 was found to be 34 mg g?1. The sorbent exhibited good stability, reusability and fast rate of equilibrium for sorption/desorption of beryllium ions. The present method was used for preconcentration and determination of beryllium for water samples. Under optimal conditions, the limit of detection (LOD) obtained was 0.3 ng L?1. The accuracy of the procedure was evaluated by analysis of the certified reference material (NIST 1640).  相似文献   

17.
Poly[aniline(AN)‐co‐5‐sulfo‐2‐anisidine(SA)] nanograins with rough and porous structure demonstrate ultrastrong adsorption and highly efficient recovery of silver ions. The effects of five key factors—AN/SA ratio, AgI concentration, sorption time, ultrasonic treatment, and coexisting ions—on AgI adsorbability were optimized, and AN/SA (50/50) copolymer nanograins were found to exhibit much stronger AgI adsorption than polyaniline and all other reported sorbents. The maximal AgI sorption capacity of up to 2034 mg g?1 (18.86 mmol g?1) is the highest thus far and also much higher than the maximal Hg‐ion sorption capacity (10.28 mmol g?1). Especially at ≤2 mM AgI, the nanosorbents exhibit ≥99.98 % adsorptivity, and thus achieve almost complete AgI sorption. The sorption fits the Langmuir isotherm well and follows pseudo‐second‐order kinetics. Studies by IR, UV/Vis, X‐ray diffraction, polarizing microscopy, centrifugation, thermogravimetry, and conductivity techniques showed that AgI sorption occurs by a redox mechanism mainly involving reduction of AgI to separable silver nanocrystals, chelation between AgI and ? NH? /? N?/? NH2/ ? SO3H/? OCH3, and ion exchange between AgI and H+ on ? SO3?H+. Competitive sorption of AgI with coexisting Hg, Pb, Cu, Fe, Al, K, and Na ions was systematically investigated. In particular, the copolymer nanoparticles bearing many functional groups on their rough and porous surface can be directly used to recover and separate precious silver nanocrystals from practical AgI wastewaters containing Fe, Al, K, and Na ions from Kodak Studio. The nanograins have great application potential in the noble metals industry, resource reuse, wastewater treatment, and functional hybrid nanocomposites.  相似文献   

18.
Abstract

Fly ash and soil mixtures with a range of fly ash content from 1 to 100% were used to study adsorption and desorption of four organophosphorus insecticides, ethyl parathion, methyl parathion, fenitrothion and fenthion, in batch experiments. The object of the study was to develop a treatment process using fly ash as sorbent material to isolate/immobilize organic contaminants from aqueous solutions. The adsorption isotherms fit the Freundlich equation x/m=KdC1/n. The Kd values increase with the increase of the fly ash content. The isotherms seem to fit the S type, in mixtures of soil with a fly ash content from 0 to 10%, which implies that adsorption becomes easier as the concentration in the liquid phase increases. In mixtures of soil with a fly ash content from 25 to 50% the isotherms become L type and correspond to a decrease of site availability as the solution concentration increases. Finally in mixtures of soil with a fly ash content over 50%, C type adsorption was observed which correspond to a constant partition of the insecticides between the bulk solution and the adsorbent. Mass balance estimations show that the mean percent amounts of insecticides for a range of concentration 0.5–15 mg/l, removed by adsorption in the soil sample are 81.56 % for ethyl parathion, 48.97 % for methyl parathion, 67.06 % for fenitrothion and 86.65 % for fenthion. The adsorption increases as the fly ash content increased and reach the 100% in the “pure” fly ash. The adsorbed amounts of insecticides in mixtures of soils with >50% fly ash content, are up to 99%. In contrast, the amounts of desorption in water decrease as the fly ash content increase.

The results of this research demonstrate that the fly ash shows a significant capacity for adsorption of organophosphorus compounds from aqueous solution and can be used for pesticide removal process.  相似文献   

19.
A modified SBA-15 mesoporous silica was developed, as an adsorbent, for the removal of Cr(VI) ions from natural-water samples. The effects of experimental parameters, including pH of solution, sample and eluent flow rate, the eluent composition, the eluent volume, and the effect of coexisting ions on the separation and determination of Cr(VI), were investigated. It was shown that Cr(VI) was selectively adsorbed from aqueous solution at pH 3, but Cr(III) could be adsorbed from solution at alkaline pH range. The retained Cr(VI) was eluted with 0.5?mol?L?1 KCl solution in 0.1?mol?L?1 Na2CO3 subsequently. Under the optimum conditions, the modified mesoporous silica (py-SBA-15) with a high pore diameter exhibited an adsorption capacity of 136?mg?g?1 and a lower limit of detection than 2.3?µg?L?1 by using diphenylcarbazide as a chromophorous reagent for the determination of Cr(VI) ions. A preconcentration factor as high as 200 was calculated for Cr(VI). The loaded py-SBA-15 can be reactivated with recovery of more than 98.5% over at least eight cycles. The relative standard deviation (RSD) for Cr(VI) ion recovery was less than 1.8%. Validation of the outlined method was performed by analysing a certified reference material (BCR 544). The proposed method was applied to determine Cr(VI) value in natural and waste water samples successfully.  相似文献   

20.
In the current study tea waste and rice husk biochars were used for the elimination of Cr(VI) from wastewater with the objectives to study the effect of pH (3–10), shaking time (0.016–24 h), sorbent dose (0.1–1.3 g L−1) and initial concentration of Cr(VI) (10–250 mg L−1). The Cr(VI) sorption was studied under various factors in which solution pH played a main role and at pH 5.2, maximum 99.3% and 96.8% Cr(VI) were removed by tea waste biochar (TWB) and rice husk biochar (RHB), respectively. In comparison, 197.5 mg g−1 and 195.24 mg g−1 Cr(VI) were sorbed by TWB and RHB, respectively with 120 mg L−1 initial Cr(VI) concentration. In contact time study, after 2 h, equilibrium was achieved for both biochars which indicated that the Cr(VI) elimination from aqueous medium is a fast process. Kinetic and isotherm modeling data showed that pseudo-second order model and Langmuir (monolayer sorption) models provided the best fit for sorption of Cr(VI) onto both biochars. The –OH, COO– and –NH2 functional groups were involved in the sorption of Cr(VI) onto biochars according to FTIR. Biochars produced from both biomass effectively removed Cr(VI) from polluted water, however in comparison sorption capacity of TWB was slightly higher than RHB. It was concluded that TWB and RHB could provide a cost-effective and viable option for elimination of Cr(VI) from wastewater.  相似文献   

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