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1.
A multi-responsive Cd metal–organic framework {[Cd (ttpe)(H2O)(ip)]•4H2O•DMAC}n ( 1•4H 2 O•DMAC ) was synthesized using hydrothermal method (ttpe = 1,1,2,2-tetra(4-(1H-1,2,4-triazol-1-yl)phenyl)ethylene, ip = isophthalate, DMAC = N,N-dimethylacetamide), and characterized. 1 exhibits a 2D (4,4) network. The luminescent sensing experimrnts showed that 1•4H 2 O•DMAC as a new MOF luminescent sensor can detect Cr2O72−, CrO42−, MnO4, Cu2+, Ag+ and Fe3+ in aqueous solution with simultaneously high efficiency and high sensitivity. The quenching constants Ksv for Cr2O72−, CrO42−, MnO4, Cu2+, Ag+ and Fe3+ are 4.231 × 104 M−1, 2.471 × 104 M−1, 6.459 × 103 M−1, 7.617 × 103 M−1, 1.563 × 104 M−1 and 3.574 × 104 M−1, respectively. The detection limits are 0.094 μM for Cr2O72−, 0.108 μM for CrO42 − , 0.346 μM for MnO4, 0.302 μM for Cu2+, 0.221 μM for Ag + , and 0.100 μM for Fe3+. 1•4H 2 O•DMAC exhibits high photocatalytic efficiency for degradation of methylene blue under visible light irradiation.  相似文献   

2.
Composite of polyacrylamide-bentonite (PAA-B) was prepared by direct polymerization in a suspension of bentonite (B), the composite was then modified by phytic acid (PAA-B-Phy). The parameters related to adsorption of UO2 2+ in absence and presence of 0.01M CaCl2 and of natural radionuclides (Tl+, Pb2+, Ra2+ and Ac3+ in a leaching solution) onto PAA-B and PAA-B-Phy, and thermodynamics of the adsorption were investigated. Adsorption isotherms were of L and H types for the adsorption of UO2 2+ onto PAA-B and PAA-B-Phy, whilst for Tl+, Pb2+, Ra2+ and Ac3+ they were of C type for both adsorbents. Langmuir equilibrium constants for the adsorption of all studied ions onto PAA-B-Phy were significantly higher than those found for PAA-B. The thermodynamic parameters indicated that adsorption reactions are spontaneous in terms of adsorption free enthalpy. The composite of PAA-B and its modification by Phy have been used for the first time in this study. It is concluded that the composites can be practically used for adsorption and applied as adsorbent of radionuclides.  相似文献   

3.
New quaternary selenides M2Sb5Bi5Se17 (M = Sn, Pb) were synthesized using solid-state sintering reactions that crystallize in the monoclinic system with C2/m (No. 12) space group with lattice parameters a = 27.914(7) Å, b = 4.0804(11) Å, c = 15.512(4) Å, and β = 114.881(9)° for M = Sn, and a = 27.987(3) Å, b = 4.1062(5) Å, c = 15.6372(19) Å, and β = 115.318(3)° for M = Pb, respectively. The crystal structure is related to a homologous series [A+22x−4B+34 Se−22x−2][B+32y−2Se−23y−3] with (x, y) = (3, 4) that contains building units of two-dimensional slabs of NaCl111-type [Sb2Bi4Se11] separated by 1D ribbons NaCl100-type [Pb2Sb3BiSe6]. The NaCl111 unit contains edge-shared octahedra filled with Sb3+ and Bi3+ cations, which are parallel and overlapped to form a step-layer 2D network stacking alone [001]. The NaCl100 type ribbons containing Pb2+ and Sb3+ in square or trigonal pyramidal environments with the general formula [M6Se6] filled in the space between 2D layers of NaCl111 units. The conductivity measurement revealed semiconducting property with band gaps of ~0.1 eV. Pb2Sb5Bi5Se17 exhibits low thermal conductivity 3,000 μW cm−1 K−1 in a temperature range of 300–480 K.  相似文献   

4.
A new class of solid‐phase extraction column prepared with grafted mercapto‐silica polymerized high internal phase emulsion particles was used for the preconcentration of trace lead. First, mercapto‐silica polymerized high internal phase emulsion particles were synthesized by using high internal phase emulsion polymerization and carefully assembled in a polyethylene syringe column. The influences of various parameters including adsorption pH value, adsorption and desorption solvents, flow rate of the adsorption and desorption procedure were optimized, respectively, and the suitable uploading sample volumes, adsorption capacity, and reusability of solid phase extraction column were also investigated. Under the optimum conditions, Pb2+ could be preconcentrated quantitatively over a wide pH range (2.0–5.0). In the presence of foreign ions, such as Na+, K+, Ca2+, Zn2+, Mg2+, Cu2+, Fe2+, Cd2+, Cl? and NO3?, Pb2+ could be recovered successfully. The prepared solid‐phase extraction column performed with high stability and desirable durability, which allowed more than 100 replicate extractions without measurable changes of performance. The feasibility of the developed method was further validated by the extraction of Pb2+ in rice samples. At three spiked levels of 40.0, 200 and 800 μg/kg, the average recoveries for Pb2+ in rice samples ranged from 87.3 to 105.2%.  相似文献   

5.
6.
SiO2‐PAN nanoparticles has been synthesized by reacting silica nanoparticles with 3‐aminopropyltriethoxysilane, formaldehyde and 1‐(2‐pyridylazo)‐2‐naphthol and characterized by FT‐IR and SEM which were used as new sorbent for the preconcentration of trace amount of Pb2+ from various samples. Conditions of the analysis such as preconcentration factor, effect of pH, sample volume, shaking time, elution conditions and effects of interfering ions for the recovery of analyte were investigated. The adsorption capacity of the nanometer SiO2‐PAN was found to be 168.34 μmol/g at optimum pH and the detection limit (3δ) was 0.63 µg/L. The extractant showed rapid kinetic sorption. The adsorption equilibrium of Pb2+ on the nanometer SiO2‐PAN was achieved within 15 min. Adsorbed Pb2+ was easily eluted with 6 mL of 4 mol·L?1 hydrochloric acid. The maximum preconcentration factor was 50. The method was applied to determine trace amounts of Pb2+ in different samples (water and food samples).  相似文献   

7.
《Electroanalysis》2018,30(3):533-542
A simple and highly sensitive electrochemical sensor COOH−C4 derived from dicarboxyl‐calix[4]arene modified on a screen printed gold electrode (Au) was developed for the determination of lead ions in water samples. A 3‐mercaptopropionic acid (MPA) monolayer was used as a template on the gold electrode for the surface modification with dicarboxyl‐calixarene. The modified electrodes were surface‐characterized using Fourier Transform infrared spectroscopy (FTIR). The data obtained proved the confirmation of each stage of the electrode modification. The electrochemical analyses of the COOH−C4 electrode showed an enhanced electrocatalytic activity and higher current towards Pb2+ ions as compared to the bare Au and MPA/Au electrodes. Under optimum conditions, the differential pulse voltammetry response of COOH−C4 displayed a wide linear response ranging from 280–2500 μg/L for Pb2+ with a detection limit of 6.2 μg/L. In addition, the fabricated electrode showed a high selectivity and stability towards the Pb2+ ions in presence of possible interfering species. The present method was successfully applied to determine Pb2+ ions in real samples with satisfactory precision, with a relative standard deviation of 3.12 % and an acceptable recovery of 92 %, which demonstrated the potential application of dicarboxyl‐calix[4]arene modified on electrodes for heavy‐metal sensing.  相似文献   

8.
A highly specific lead-binding peptide ThrAsnThrLeuSerAsnAsn was displayed on Escherichia coli, and lead adsorption characteristics of the recombinant bacteria were investigated. Cell surface-displayed peptide was expressed under the control of an arabinose promoter using outer membrane protein C (OmpCt) as an anchoring motif. The optimal induction period and arabinose concentration for the expression of peptide-fused OmpCt were determined to be 2 h and 0.001 g/L, respectively. Selective adsorption of Pb2+ onto recombinant cells was verified with individual or combinatory use of four metal ions, Pb2+, Ni2+, Co2+, and Cu2+; the amount of bound Pb2+ onto the biosorbents was significantly higher than the other metal ions. The adsorption isotherm of recombinant cells for Pb2+ followed the Langmuir isotherm with a maximum adsorption loading (q max) of 526 μmol/g dry cell weight.  相似文献   

9.
The anodic stripping peak current of lead on the glassy carbon electrode surface was greatly increased in the presence of high concentration of copper ion. The effects of supporting electrolyte, concentration of Cu2+, accumulation potential and accumulation time were studied on the stripping peak current of Pb2+. As a result, a sensitive, simple and rapid electrochemical method was developed for the detection of lead. In 0.01 M HNO3 solution containing 800 g,g L?1 Cu2+, the stripping peak current of Pb2+ increases linearly with its concentration over the range from 2 to 100 μg L?1. The detection limit is 1 μg L?1 after 4-min accumulation at ?0.8 V. It was used to detect the concentration of lead in blood samples, and the results consisted with the values that obtained by atomic absorption spectrometry.  相似文献   

10.
In this study, optimum conditions for adsorption of heavy metals such as Cu2+, Cd2+ and Pb2+ onto a low-cost, magnetically modified-alkali conditioned anaerobically digested sludge (MADS) adsorbent were obtained. Response Surface Methodology (RSM) incorporating Central Composite Design (CCD) of experiments was applied to optimize four independent process variables. Statistical analysis was executed by ANOVA and the quadratic model developed had regression coefficients of 0.959, 0.957 and 0.95 for Cu2+, Cd2+ and Pb2+, respectively. The independent variables such as pH, time and initial concentration positively influenced adsorption capacity, qe, whereas the value of qe decreased with an increase in MADS dosage. Model validation experiments for optimization of adsorption process showed comparable results with predicted values. The adsorption capacity of MADS adsorbent at optimum conditions found through RSM analysis was 29.721 mg L?1, 28.551 mg L?1 and 28.601 mg L?1 for Cu2+, Cd2+ and Pb2+ respectively.  相似文献   

11.
Facile synthesis of two 2-anthracene ammonium-based magnetic ionic liquids (MILs), 2-anthracene ammonium tetrachloroferrate (III) ([2A-A]FeCl4) and 2-anthracene ammonium trichlorocobaltate (II) ([2A-A]CoCl3) was performed by protonation of 2-aminoanthracene, followed complexation with FeCl3/CoCl2. The MILs were tested in the adsorptive removal of Cd2+, As3+, Pb2+ and Cr3+ from water sources. Upon treatment with 10 mg dosage of MILs in 10 mL aqueous solution of 50 ppm each of Cd2+, As3+, Pb2+ and Cr3+, adsorption capacity (mg/g) in the range of 5.73–55.5 and 23.6–56.8 for [2A-A]FeCl4 and [2A-A]CoCl3 respectively were recorded. Thus, the optimization, kinetic and isotherms studies were conducted using the [2A-A]CoCl3 adsorbent. The [2A-A]CoCl3 was more effective in pH 7–9, and equilibrium adsorption was achieved after 60 min contact time. The adsorption process proceeded via the Pseudo-second order pathway and the Langmuir isotherm model is the best fit for the adsorption process (with qmax = 227 – 357 mg/g) of all the targeted metal ions. The [2A-A]CoCl3 adsorbent demonstrated practicality with large distribution and selectivity coefficients of the targeted ions, and up to six times regeneration.  相似文献   

12.
基于铜纳米簇的聚集诱导发光检测铅离子   总被引:1,自引:0,他引:1  
基于谷胱甘肽保护的非贵金属铜纳米簇(Cu NCs@GSH)的聚集诱导发光现象,建立了快速检测铅离子(Pb2+)的“Turn on”型荧光分析方法.Cu NCs@GSH溶液荧光强度很弱,当存在pb2+时,荧光强度可显著增强,溶液显示明亮的橙黄色.基于此原理建立了检测pb2+的荧光方法,线性范围为200~700 μmol/L,检出限为106 μmol/L,常见金属离子不干扰pb2+的测定.本方法简单快速、选择性高,可实现对pb2+的可视化定性检测.  相似文献   

13.
In this study, the ion-imprinting method has been integrated to develop a novel composite material for the selective separation of Pb2+ ions. Also, Pb2+ ion binding ability of the organosmectite based inorganic-organic composite incorporation of bicyclic C18 organic compound into smectite layers was conducted to draw a projection its potential use as a solid phase exchanger which is quite selective toward Pb2+ ions. The ion-imprinted nanocomposites were characterized by Fourier transform infrared (FTIR), X-ray diffraction (XRD), swelling tests, and elemental analyses. After that, maximum binding capacity, pH, and equilibrium binding time were also been optimized. In order to show the selectivity of the composite synthesized, non-imprinted composites were also synthesized in absence of Pb2+ ions during polymerization. In this step, Ni2+, Co2+, Al3+, Zn2+, and Cu2+ ions were used as competitors under batch adsorption conditions. The relative selectivity coefficients of imprinted composite were calculated as 28.5, 156.5, 69.3, 24.8 and 131.6 for Pb2+/Co2+, Pb2+/Cu2+, Pb2+/Al3+, Pb2+/Zn2+, Pb2+/Ni2+ binary solutions, respectively. Finally, reusability of the composites was evaluated to show its cost-efficiency by repeating adsorption-desorption experiments ten-times. The adsorption capacity of the imprinted composites did not change significantly whereas that of non-imprinted version reduced dramatically.  相似文献   

14.
A novel ion imprinted polyvinylimidazole-silica hybrid copolymer (IIHC) was synthesized and used as a selective solid sorbent for Pb2+ ions preconcentration using an on-line solid phase extraction (SPE) system coupled to TS-FF-AAS. The ionic hybrid sorbent was prepared using 1-vinylimidazole and 3-(trimethoxysilyl)propylmethacrylate as monomers, Pb2+ ions as template, tetraethoxysilane as reticulating agent and 2,2′-azobis-isobutyronitrile as initiator. The best on-line SPE conditions concerning sorption behavior, including sample pH (6.46), buffer concentration (9.0 mmol L−1), eluent (HNO3) concentration (0.5 mol L−1) and preconcentration flow rate (4.0 mL min−1), were optimized by means of full factorial design and Doehlert matrix. The analytical curve ranged from 2.5 to 65.0 μg L−1 (r = 0.999) with limit of detection of 0.75 μg L−1; the precision (repeatability) calculated as relative standard deviation (n = 10) was 5.0 and 3.6% for Pb2+ concentration of 10.0 and 60.0 μg L−1, respectively. From on-line breakthrough curve, column capacity was 3.5 mg g−1. Preconcentration factor (PF), consumptive index (CI) and concentration efficiency (CE) were 128.0, 0.16 mL and 25.6 min−1, respectively. The selective performance of the sorbent, based on relative selectivity coefficient, was compared to NIC (non imprinted copolymer) for the binary mixture Pb2+/Cd2+, Pb2+/Cu2+ and Pb2+/Zn2+. The results showed that ion imprinted polyvinylimidazole-silica hybrid polymer had higher selectivity for Pb2+ than NIC at 64.9, 16.0 and 8.8 folds. The developed method was successfully applied for highly sensitive and selective Pb2+ determination in different kinds of water samples, parenteral solutions and urine. Accuracy was also assessed by analyzing certified reference fish protein (DORM-3) and marine sediment (MESS-3 and PACS-2) with satisfactory results.  相似文献   

15.
In order to explore the reuse properties of oxidized chelating resin containing sulfur after adsorption, two kinds of novel chelating resins, poly[4-vinylbenzyl-(2-hydroxyethyl)] sulfoxide (PVBSO) and poly[4-vinylbenzyl-(2-hydroxyethyl)] sulfone (PVBSO2), were synthesized using poly[4-vinylbenzyl-(2-hydroxyethyl)] sulfide (PVBS) as material. Their structures were confirmed by FTIR and XPS. The adsorption properties and mechanism for metal ions such as Au3+, Pt4+, Pd2+, Hg2+, Cu2+, Ni2+, Fe3+, Pb2+, Cd2+, and Zn2+ were investigated. Experimental results showed that PVBSO had good adsorption and selective properties for Au3+, Pd2+ and Cu2+ when the coexisting ion was Pt4+, Ni2+, Pb2+ or Cd2+. In the aqueous system containing Cu2+ and Pb2+ or Cu2+ and Cd2+, PVBSO2 only adsorbed Cu2+. The selective coefficients of PVBSO and PVBSO2 were αAu/Pt = 4.8, αAu/Pd = 11.8, αPd/Pt = 10.9, αCu/Ni = 2.5, αCu/Cd = 41.2, αCu/Pb = ∞, αCu/Ni = 3.0, αCu/Cd = ∞, αCu/Pb = ∞, respectively.  相似文献   

16.
Zirconium (IV) 4-amino, 3-hydroxy naphthalene sulfonate ion-exchanger has been synthesized by mixing equimolar solutions of zirconium oxychloride and ammonium hydroxide in molar ratio 1:1.66 to get a gelatinous material. To this were added varying amounts of 4-amino, 3-hydroxynaphthalene sulphonic acid (ANSA) with constant stiring in order to ensure a complete adsorption of organic molecules to the surface of the gel. The ion exchange material shows a dual character possessing both cation and anion exchange capacities. The former is attributed to the dissociation of strong sulphonic groups from ANSA and acidic sites of hydrous oxide gel, the later one is due to the formation of a positive charge on the nitrogen atom ; in addition, the material may have a sorption capacity. A preliminary investigation to characterize the material has been carried out which includes IR, TGA, DTA and X-ray diffraction. On the basis of distribution coefficients the separation of Hg+2 from Zn2+, Al2+, Ni2+, Ce4+, Mg2+, Pb2+, Mn2+, Cu2+, has been achieved. The decreasing sequence of Kd values for different anionic species are found to be PO43− > Fe (CN)63− > MnO4 > VO3 > AsO43− > C2O42− and for halides Cl > Br > I.  相似文献   

17.
Li M  Li DW  Li YT  Xu DK  Long YT 《Analytica chimica acta》2011,701(2):157-163
A novel and facile hybrid analytical method coupling electrochemical “adsorption–desorption” and colorimetric analyses was developed to detect heavy metal ions in turbid water samples. The target metal ions were deposited onto an electrode inserted into the original sample, which was referred to as the “adsorption” process. After changing the medium, the concentrated target metal ions were dissolved in a new, clean buffer (blank buffer), which was referred to as the “desorption” process. The concentrations of the target metal ions were measured by colorimetric analyses after the addition of specific indicator amounts. We demonstrated the applicability of this method by detecting Cd2+, Pb2+ and Cu2+ with co-depositing Bi3+ on portable screen-printed electrodes (SPEs). A good correlation (correlation coefficient of R = 0.997) was observed between concentrations ranging from 1 to 200 μM and absorbance values. After the multiple “desorption” process, the even better detection limits as low as 10, 10 and 100 nM were achieved for Cd2+, Pb2+ and Cu2+, respectively. The practicality of this hybrid method was confirmed by the detection of Cd2+, Pb2+ and Cu2+ in wastewater samples, and these results were in agreement with inductively coupled plasma atomic emission spectroscopy (ICP-AES). Overall, this hybrid method provides a simple, selective and effective technique for environmental pollutant analyses.  相似文献   

18.
The presented study investigates the application of MnO2/3MgO nanocomposite, as a new sorbent for solid phase extraction and determination of trace amounts of Pb2+ and Cu2+ from various samples using flame atomic absorption spectrometry. After extraction, the analytes were desorbed using 0.01 M ethylenediaminetetraacetic acid. The effects of various parameters were studied and optimized. Under optimized experimental conditions the linear dynamic ranges for Cu2+ and Pb2+ were 10?900 and 30?900 μg/L, respectively, with a preconcentration factor of 20. The detection limits of Cu2+ and Pb2+ were 4 and 11 μg/L, respectively, and relative standard deviations for eight determinations of 100 μg/L were 3.6 and 3.8% for Cu2+ and Pb2+, respectively. The method was successfully applied for determination of copper and lead in mushrooms, rice, tap water and refinery wastewater with good spike recoveries ranging between 95?106%.  相似文献   

19.
We fabricated a new MnO2-loaded biocomposite based on microcrystalline cellulose (MCC–MnO2) by an in situ synthesis method and investigated its adsorption behavior and mechanism for Pb2+ removal from aqueous medium. As-prepared MCC–MnO2 was characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), Fourier-transform infrared (FTIR) spectroscopy, and X-ray diffraction (XRD) analyses. The effects of pH value, initial Pb2+ concentration, contact time, and solution temperature on the uptake of Pb2+ onto MCC–MnO2 were investigated using a batch system. Adsorption equilibrium could be achieved in 3 h for various studied initial concentrations, and a pseudo-second-order model could fit the adsorption behavior well. The equilibrium data could be well described by the Langmuir isotherm model, and the maximum monolayer adsorption capacity of MCC–MnO2 (with 7.98% MnO2 loading) for Pb2+ was estimated to be 247.5 mg/g at 313 K. Thermodynamic studies indicated a spontaneous and endothermic adsorption process. X-ray photoelectron spectroscopy (XPS) was used to analyze the adsorption mechanism, revealing that the chemical speciation of Pb2+ on MCC–MnO2 was similar to the compound PbO. Moreover, no variations in the valence of Mn were observed after adsorbing Pb2+. The regeneration study showed that the adsorption capacity retained about 89.6% of its initial value at the fifth sequential regeneration cycle, indicating that this material is an efficient and renewable hybrid adsorbent for Pb2+ removal.  相似文献   

20.
The present paper has focused on the potential application of the bifunctional polydopamine@Fe3O4 core–shell nanoparticles for development of a simple, stable and highly selective electrochemical method for metal ions monitoring in real samples. The electrochemical method is based on electrochemical preconcentration/reduction of metal ions onto a polydopamine@Fe3O4 modified magnetic glassy carbon electrode at −1.1 V (versus SCE) in 0.1 M pH 5.0 acetate solution containing Pb2+ and Cd2+ during 160 s, followed by subsequent anodic stripping. The proposed method has been demonstrated highly selective and sensitive detection of Pb2+ and Cd2+, with the calculated detection limits of 1.4 × 10−11 M and 9.2 × 10−11 M. Under the optimized conditions, the square wave anodic stripping voltammetry response of the modified electrode to Pb2+ (or Cd2+) shows a linear concentration range of 5.0–600 nM (or 20–590 nM) with a correlation coefficient of 0.997 (or 0.994). Further, the proposed method has been performed to successfully detect Pb2+ and Cd2+ in aqueous effluent.  相似文献   

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