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 46 毫秒
1.
A solid phase extraction system for separation and preconcentration of trace amounts of Pb(II), Ni(II), Cd(II) and Cu(II) is proposed. The procedure is based on the adsorption of Pb2+, Ni2+, Cd2+ and Cu2+ ions on a column of 1-(2-pyridylazo)-2-naphthol (PAN) immobilised on surfactant-coated clinoptilolite prior to their determinations by Flame Atomic Absorption Spectroscopy (FAAS). The effective parameters including pH, sample volume, sample flow rate and eluent flow rate were also studied. The analytes collected on the column were eluted with 5 mL of 1 mol L?1 nitric acid. A concentration factor of 180 can be achieved by passing 900 mL of sample through the column. The detection limits (3 s) for Cd, Cu, Pb and Ni were found to be 0.28, 0.12, 0.44 and 0.46 µg L?1, respectively. The relative SDs at 10 µg L?1 (n = 10) for analytes were in the range of 1.2–1.4%. The method was applied to the determination of Pb, Ni, Cd and Cu in water samples.  相似文献   

2.
1,2-Bis(salicylidenamino)ethane loaded onto sodium dodecyl sulfate-coated alumina was used as a new chelating sorbent for the preconcentration of traces of Pb(Ⅱ) and Cu(Ⅱ) prior to atomic absorption spectrometric determination. The influence of pH, flow rates of sample and eluent solutions, and foreign ions on the recovery of Pb(Ⅱ) and Cu(Ⅱ) by this sorbent has been studied. The retained ions were eluted with 4 mol·L nitric acid and determined by electrothermal atomic absorption spectrometry (ETAAS). The data of limit of detection (3σ) for Pb(Ⅱ) and Cu(Ⅱ) were found to be 8.57 and 2.69 ng·L^-1 respectively, while the enrichment factor for both ions was 100. The proposed method was successfully applied to determination of lead and copper in different water samples.  相似文献   

3.
We describe a novel magnetic metal-organic framework (MOF) for the preconcentration of Cd(II) and Pb(II) ions. The MOF was prepared from the Fe3O4-pyridine conjugate and the copper(II) complex of trimesic acid. The MOF was characterized by IR spectroscopy, elemental analysis, SEM and XRD. A Box-Behnken design through response surface methodology and experimental design was used to identify the optimal parameters for preconcentration. Extraction time, amount of magnetic MOF and pH value were found to be critical factors for uptake, while type, volume, concentration of eluent, and elution time are critical in the elution step. The ions were then determined by FAAS. The limits of detection are 0.2 and 1.1 μg?L?1 for Cd(II), and Pb(II) ions, respectively, relative standard deviations are <4.5% (for five replicates at 50 μg?L?1 of Cd(II) and Pb(II) ions), and the enrichment capacity of the MOF is at around 190 mg?g?1 for both ions which is higher than the conventional Fe3O4-pyridine material. The magnetic MOF was successfully applied to the rapid extraction of trace quantities of Cd(II) and Pb(II) ions in fish, sediment, and water samples.
Figure
Schematic illustration of synthesized magnetic MOF-pyridine nanocomposite  相似文献   

4.
A sensitive and simple method has been established for simultaneous preconcentration of trace amounts of Pb (II) and Ni (II) ions in water samples prior to their determination by flame atomic absorption spectrometry. This method was based on the using of a micro-column filled with graphene oxide as an adsorbent. The influences of various analytical parameters such as solution pH, adsorbent amount, eluent type and volume, flow rates of sample and eluent, and matrix ions on the recoveries of the metal ions were investigated. Using the optimum conditions, the calibration graphs were linear in the range of 7–260 and 5–85 μg L?1 with detection limits (3Sb) of 2.1 and 1.4 μg L?1 for lead and nickel ions, respectively. The relative standard deviation for 10 replicate determinations of 50 μg L?1 of lead and nickel ions were 4.1% and 3.8%, respectively. The preconcentration factors were 102.5 and 95 for lead and nickel ions, respectively. The adsorption capacity of the adsorbent was also determined. The method was successfully applied to determine the trace amounts of Pb (II) and Ni (II) ions in real water samples. The validation of the method was also performed by the standard reference material.  相似文献   

5.
A novel UV-VIS spectrophotometric method was developed in this study by using solid phase extraction procedure for the simultaneous preconcentration, separation and determination of trace levels of Pb (II), Cd (II) and Zn (II) ions in various water samples by using Amberlite N,N-bis(salicylidene)cyclohexanediamine (SCHD) resin. This study presents the results of experimental procedures carried out like the adsorption of analytes to the resin, influences of some analytical parameters that effect the recovery such as pH, sample volume, sample flow rate, eluent type and concentration, eluent volume, eluent flow rate and the effects of alkaline metals, earth alkaline metals and some other transition metals. The analytes in the samples with the adjusted pH range of 4–7 were adsorbed on XAD-4-SCHD resin and eluted by using 1.0 mol L?1 nitric acid. The amounts of ions were determined by using UV-VIS spectrometer. The limits of detection were 0.03, 0.07 and 0.05 µg mL?1 for Pb (II), Cd (II) and Zn (II), respectively. The accuracy of the method was assured by the analysis of the certified standard water sample NW-TMDA-70.2 and the observed recoveries were above 93%. Different environmental water samples that contain trace amounts of Pb (II), Cd (II) and Zn (II) were analysed by using the method developed in this study. Same samples were also analysed by ICP-MS for comparison and almost the similar results were observed. The method developed in this study was successfully applied to the various environmental water samples to determine the trace levels of Pb (II), Cd (II) and Zn (II) ions.  相似文献   

6.
Graphene nanosheets were modified with amino groups and the resulting material was used as a sorbent for the extraction of cadmium and lead ions. The nanosheets were characterized by IR spectroscopy, transmission electron microscopy, thermal gravimetric analysis and elemental analysis. The effects of sample pH, eluent parameters (type, concentration and volume of eluent), flow rates (of both sample and eluent), and of a variety of other ions on the efficiency of the extraction of Cd(II) and Pb(II) were optimized. Following solid phase extraction, the elements were determined by FAAS. The limits of detection are <0.9 μg L?1 for Pb(II) and <5 ng L?1 for Cd(II). The relative standard deviations are <2.2 %. The method was validated by analyzing several certified reference materials and was then used for Pb(II) and Cd(II) determination in natural waters and vegetables.
Figure
In this work, grapheme oxide nanosheets were modified with amino and tri-amino groups and their application were investigated in Cd(II) and Pb(II) determination in food sample. The results show high preconcentration factor and adsorption capacities for these nanosheets.  相似文献   

7.
A new solid phase extractant, sinapinaldehyde (SA) modified SBA-15 mesoporous silica, was developed for selective extraction and preconcentration of trace Pb(II) from aqueous solutions. The successful immobilization of SA on SBA-15 and the strong interaction between SA-SBA-15 and Pb(II) were characterized and confirmed by FTIR spectroscopy and scanning electron microscopy. Parameters such as solution pH, shaking time, eluent condition and sample volume were optimized so that the maximum removal of Pb(II) from solution could be achieved. At pH 4.0, the maximum adsorption capacity of the sorbent for Pb(II) was found to be 33.6?mg?g?1 and the adsorbed Pb(II) could be completely eluted using a mixed solution of 2?M HCl and 5% CS(NH2)2. Some common metal ions such as K(I), Na(I), Mg(II), Ca(II), Cr(III), Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Hg(II) did not interfere with the adsorption of trace Pb(II). The detection limit of the present method was found to be 1.3?ng?mL?1 and the relative standard deviation was less than 2.0% (n?=?8). These results suggested that this new sorbent is very efficient and selective for the removal of trace Pb(II) in water samples.  相似文献   

8.
A new solid-phase extraction sorbent was used for the preconcentration of Pb(II) and Cr(III) ions prior to their determination by flame atomic absorption spectrometry. It was prepared by immobilization of 2,4-dinitrophenylhydrazine on nano-alumina coated with sodium dodecyl sulfate. The sorbent was characterized by scanning electron microscopy, N2 adsorption and Fourier transform infrared spectrometry, and used for preconcentration and separation of Pb(II) and Cr(III) from aqueous solutions. The ions on the sorbent were eluted with a mixture of nitric acid and methanol. The effects of sample pH, flow rates of samples and eluent, type of eluent, breakthrough volume and potentially interfering ions were studied. Linearity is maintained between 1.2 and 350???g?L-1 of Pb(II), and between 2.4 and 520???g?L-1 of Cr(III) for an 800-mL sample. The detection limit (3?s, N?=?10) for Pb(II) and Cr(III) ions is 0.43 and 0.55???g?L-1, respectively, and the maximum preconcentration factor is 267. The method was successfully applied to the evaluation of these trace and toxic metals in various water, food, industrial effluent and urine samples.
Figure
Recovery percentage of Pb(II) and Cr(III) ions at different solution volumes.  相似文献   

9.
A new polychelatogen, AXAD-16-1,2-diphenylethanolamine, was developed by chemically modifying Amberlite XAD-16 with 1,2-diphenylethanolamine to produce an effective metal-chelating functionality for the preconcentration of Mn(II), Ni(II), Cu(II), Zn(II), Cd(II), and Pb(II) and their determination by flame atomic absorption spectrometry. Various physiochemical parameters that influence the quantitative preconcentration and recovery of metal were optimized by both static and dynamic techniques. The resin showed superior extraction efficiency with high-metal loading capacity values of 0.73, 0.80, 0.77, 0.87, 0.74, and 0.81 mmol/g for Mn(II), Ni(II), Cu(II), Zn(II), Cd(II), and Pb(II), respectively. The system also showed rapid metal-ion extraction and stripping, with complete saturation in the sorbent phase within 15 min for all the metal ions. The optimum condition for effective metal-ion extraction was found to be a neutral pH, which is a great advantage in the preconcentration of trace metal ions from natural water samples without any chemical pretreatment of the sample. The resin also demonstrated exclusive ion selectivity toward targeted metal ions by showing greater resistivity to various complexing species and more common metal ions during analyte concentration, which ultimately led to high preconcentration factors of 700 for Cu(II); 600 for Mn(II), Ni(II), and Zn(II); and 500 for Cd(II) and Pb(II), arising from a larger sample breakthrough volume. The lower limits of metal-ion detection were 7 ng/mL for Mn(II) and Ni(II); 5 ng/mL for Cu(II), Zn(II), and Cd(II), and 10 ng/mL for Pb(II). The developed resin was successful in preconcentrating metal ions from synthetic and real water samples, multivitamin-multimineral tablets, and curry leaves (Murraya koenigii) with relative standard deviations of < or = 3.0% for all analytical measurements, which demonstrated its practical utility.  相似文献   

10.
We have synthesized two ditopic ligands for selective extraction of copper(II) nitrate. We also synthesized one cation-only binding analog for comparison. All three ligands were characterized by conventional techniques. Competitive two-phase metal ion solvent extraction experiments were performed at 25 °C over a period of 24 h. These ligands showed significant selectivity for Cu(II) ions, having the ditopic ligands extract 81 and 73% of the Cu(II) ions in a solution of different metal ions {Ni(II), Co(II), Cu(II), Zn(II), Cd(II), Pb(II)} at pH 5.09. Competitive transport experiments (water/chloroform/water) were undertaken employing each ligand separately as the ionophore in the membrane (chloroform) phase. No metal ion transport was observed, but a large concentration of Cu(II) was present in the membrane phase. Competitive anion extraction and transport were carried out with the ditopic ligands, yielding selective extraction and transport of nitrate. Furthermore, a pH isotherm of the best ditopic ligand (H2L2) with Cu(II) was determined from pH 1.0 to 6.0, producing a pH½ value of approximately 2.6. Finally, crystal structures of the ditopic ligands complexed with Cu(II) were determined and refined. The coordination geometry around the metal centers are distorted square planar and the Cu(II)-donor bond lengths fall within the normal range.  相似文献   

11.
A solid phase extraction method is presented for the preconcentration of trace lead ions on oxidized multiwalled carbon nanotubes (ox-MWCNTs). In the first step, the cationic Pb(II) complex of 2,2-bipyridyl is formed which, in a second step, is adsorbed on ox-MWCNTs mainly due to electrostatic and van der Waals interactions. The Pb(II) ions were then eluted with dilute nitric acid and quantified by FAAS. The effects of pH value, mass of sorbent, concentration of 2,2-bipyridyl, stirring time, of type, concentration and volume of eluent, of eluent flow rate and sample volume were examined. Most other ions do not affect the recovery of Pb(II). The limits of detection are 240 and 60 ng L?1 for sample volumes of 100 and 400 mL, respectively. The recovery and relative standard deviation are >95 % and 2.4 %, respectively. Other figures of merit include a preconcentration factor of 160 and a maximum adsorption capacity of 165 mg g?1. The method was successfully applied to the determination of Pb(II) in spiked tap water samples. The accuracy of the method was verified by correctly analyzing a certified reference material (NCS ZC85006; lead in tomatoes).
Figure
A solid phase extraction method is presented for the preconcentration of trace lead ions on oxidized multiwalled carbon nanotubes (ox-MWCNTs). Most other ions do not affect the recovery of Pb(II).  相似文献   

12.
A simple and rapid solid phase extraction?Cflow injection procedure is developed for on-line trace determination of Cu(II) and Pb(II) by flame atomic absorption spectrometry (FAAS). Multi-walled carbon nanotubes modified with a new Schiff??s base, 2,2??-(1E, 1E??)-(4-Methyl-1, 2-phenylene) bis (azen-1-yl-1-ylidine) bis (Methane-1-yl-1-ylidene) diphenol was used as a novel adsorbent material. Quantitative simultaneous extraction was obtained at pH 7.0. The retained metal ions were then eluted efficiently with 1.0?M HNO3 into the nebulizer of FAAS for on-line determination. Different variables affecting the preconcentration efficiency, including pH, eluent concentration, sample and eluent flow rates and sample loading time, were optimized. Using 3?min preconcentration of sample solution at flow rate of 5?mL?min?1 provided the enrichment factors of 20 and 21.5 for Cu(II) and Pb(II), respectively, at a sampling frequency of 17?h?1. The detection limits (3??) were found to be 0.80 and 1.80???g?L?1 for Cu(II) and Pb(II), respectively; and the relative standard deviations at 0.05???g?mL?1 of these metal ions were 1.7 and 1.8% (n?=?8), respectively. The accuracy was assessed by analysis of a certified reference material NKK-916 and the obtained results are in good agreement with certified amounts of Cu(II) and Pb(II). The proposed method was successfully applied to the determination of target analytes in different real samples.  相似文献   

13.
Multi-walled carbon nanotubes (MWCNTs) were chemically functionalized by glutaric dihydrazide (GDH) and characterized with FT-IR technique. This new sorbent was used for enrichment and preconcentration of Co(II), Cd(II), Pb(II), and Pd(II) ions. The adsorption was achieved quantitatively on MWCNTs at pH 4.0, and then the retained metal ions on the adsorbent were eluted with 1.5 mol L?1 HNO3. The effects of analytical parameters including pH of the solution, eluent type, sample volume, and matrix ions were investigated for optimization of the presented procedure. The adsorption capacity of the adsorbent at optimum conditions was found to be 33.6, 29.2, 22.1, and 36.0 mg g?1 for Co(II), Cd(II), Pb(II), and Pd(II), respectively. The LOD values of the method were 0.16, 0.19, 0.17, and 0.12 ng mL?1 (3Sb, n = 10) for Co(II), Cd(II), Pb(II), and Pd(II), respectively. The RSDs values of the method were 0.75, 0.85, 1.16, and 1.30 ng mL?1 for Co(II), Cd(II), Pb(II), and Pd(II), respectively. The method was applied for the determination of analytes in soil, well water, and wastewater samples with satisfactory results.  相似文献   

14.
A new solid-phase extraction method utilising polyacrylonitrile activated carbon fibres (PAN-ACFs) as adsorbent was developed for the preconcentration of trace metal ions prior to their determination by inductively coupled plasma optical emission spectrometry (ICP-OES). The PAN-ACFs oxidised with nitric acid were characterised by FT-IR, XRD, SEM and BET analysis. Then the resulting PAN-ACFs were used as solid-phase adsorbent for simultaneously determination of trace Al(III), Be(II), Bi(III), Cr(III), Cu(II), Fe(III) and Pb(II) ions in aqueous solutions. The influences of the analytical parameters on the recoveries of the studied ions were investigated. The optimum experimental conditions of the proposed method were pH: 6.0; eluent concentration and volume: 3.0 mL of 1.5 mol L?1 nitric acid; flow rates of sample and eluent solution: 1.5 mL min?1. The preconcentration factors were found to be 67 for Al(III), Bi(III); 83 for Cr(III), Cu(II), Fe(III) and 50 for Be(II), Pb(II). The precision of this method was in range of 1.5%~3.5% and the detection limit of this metal ions was between 0.06~1.50 μg L?1. The developed method was validated by the analysis of a certified reference sample and successfully applied to the determination of trace metal ions in water samples with satisfactory results.  相似文献   

15.
A new, simple, fast and reliable solid-phase extraction method has been developed for separation/preconcentration of trace amounts of Pb(II) using dithizone/sodium dodecyl sulfate-immobilized on alumina-coated magnetite nanoparticles, and its determination by flame atomic absorption spectrometry (FAAS) and graphite furnace atomic absorption spectrometry (GFAAS) after eluting with 4.0?mol?L?1 HNO3. Optimal experimental conditions including pH, sample volume, eluent concentration and volume, and co-existing ions have been studied and established. Under the optimal experimental conditions, the preconcentration factor, detection limit, linear range and relative standard deviation of Pb(II) using FAAS technique were 280 (for 560?mL of sample solution), 0.28?ng?mL?1, 1.4?C70?ng?mL?1 and 4.6% (for 10?ng?mL?1, n?=?10), respectively. These analytical parameters using GFAAS technique were 300 (for 600?mL of sample solution), 0.002?ng?mL?1, 0.006?C13.2?ng?mL?1 and 3.1% (for 5?ng?mL?1, n?=?10), respectively. The presented procedure was successfully applied for determination of Pb(II) content in opium, heroin, lipstick, plants and water samples.  相似文献   

16.
A silica-based inorganic sorbent was synthesized by the thermal decomposition of ammonium heptamolybdate on silica and applied for the preconcentration and simultaneous determination of Cd, Co, Cr, Cu, Fe, Mn, Ni, and Pb in river water samples using a column system with flame atomic absorption spectrometry. Attenuated total reflection-Fourier transformation infrared spectroscopy, scanning electron microscopy, and electron dispersive spectroscopy were used for sorbent characterization. The effects of pH, sample volume, eluent type, eluent concentration, eluent volume, sample flow rate, and matrix ions (Al, Bi, Ca, Mg, and Zn) on the recovery of the metals in model solutions were investigated. The adsorption capacities (µmol g?1) of SiO2-MoO3 were 88.96 (Cd), 169.69 (Co), 153.85 (Cr), 188.88 (Cu), 179.05 (Fe), 163.81 (Mn), 136.31 (Ni), and 38.61 (Pb). The detection limits of the method were 9.09, 10.82, 10.77, 49.57, 31.64, 6.40, 8.86, 19.15?µg L?1 for Cd, Co, Cr, Cu, Fe, Mn, Ni, and Pb, respectively, with a preconcentration factor of 25. The developed method was used for the determination of the target metals in real samples and the recoveries for spiked samples were found to be from 91.2% to 102.9%.  相似文献   

17.
Porous solid insoluble polysiloxane-immobilized ligand system bearing propylamine of the general formula P-(CH2)3-NH2 (where P represents [Si–O]n siloxane network) was prepared and evaluated for the separation and preconcentration of copper(II) from aqueous solution. The ligand system retained Cu(II) effectively when used as a metal ion extractant. The ligand system also showed high selectivity to separate copper(II) from a mixture of metal ions (Co(II), Ni(II), Cu(II)) when used as chromatographic stationary phase. The optimum pH appeared to be pH = 5.5 using acetate buffer as an eluent. Thermal analysis showed that the ligand system is very stable at relatively high temperatures.  相似文献   

18.
Silica gel chemically bonded with aminothioamidoanthraquinone was synthesized and characterized. The metal sorption properties of modified silica were studied towards Pb(II), Cu(II), Ni(II), Co(II) and Cd(II). The determination of metal ions was carried out on FAAS. For batch method, the optimum pH ranges for Pb(II), Cu(II) and Cd(II) extraction were ≥3 but for Ni(II) and Co(II) extraction were ≥4. The contact times to reach the equilibrium were less than 10 min. The adsorption isotherm fitted the Langmuir's model showed the maximum sorption capacities of 0.56, 0.30, 0.15, 0.12 and 0.067 mmol/g for Pb(II), Cu(II), Ni(II), Co(II) and Cd(II), respectively. In the flow system, a column packed modified silica at 20 mg for Pb(II) and Cu(II), 50 mg for Cd(II), 60 mg for Co(II), Ni(II) was studied at a flow rate of 4 and 2.5 mL/min for Ni(II). The sorbed metals were quantitatively eluted by 1% HNO3. No interference from Na+, K+, Mg2+, Ca2+, Cl and SO42− at 10, 100 and 1000 mg/L was observed. The application of this modified silica gel to preconcentration of pond water, tap water and drinking water gave high accuracy and precision (%R.S.D. ≤ 9). The method detection limits were 22.5, 1.0, 2.9, 0.95, 1.1 μg/L for Pb(II), Cu(II), Ni(II), Co(II) and Cd(II), respectively.  相似文献   

19.
Amberlite XAD-4 modified with N-para-anisidine-3,5-di-tert-butylsalicylaldimine was investigated as a new chealting sorbent for the selective separation and preconcentration of Cu(II). The metal ion was retained by chemical sorption on the modified resin, eluted by hydrochloric acid, and determined by high-resolution continuum source flame atomic absorption spectrometry. The prepared resin was characterized for the solid-phase extraction of Cd2+, Co2+, Cr3+, Cu2+, Fe3+, Mn2+, Ni2+, Pb2+, and Zn2+ in a column. The influence of the pH, the mass of solid phase, eluent, flow rate, and sample volume was optimized. Using the optimum conditions, only Cu(II) showed quantitative sorption at the 95% confidence level, and the recoveries of the other metal ions were below 80%. A preconcentration factor 125 was obtained for Cu(II) with a limit of detection of 0.56?µg?L?1. The method was used for the determination of Cu(II) in tap water, river water, tomato leaves, and fish. The relative standard deviation and the relative error were lower than 7%.  相似文献   

20.
The coupled transport of Cu(II), Cd(II) and Ni(II) ions through a bulk liquid membrane (BLM) containing pyridine-2-acetaldehyde benzoylhydrazone (2-APBH) as carrier dissolved in toluene has been studied. Once the optimal conditions of extraction of each metal were established, a comparative study of the transport kinetics for these metals was performed by means of a kinetic model involving two consecutive irreversible first-order reactions. The kinetic parameters (apparent rate constants of the metal extraction and re-extraction reactions (k 1, k 2), the maximum reduced concentration of the metal in the liquid membrane (), the time of the maximum value of R o ( t max) and the maximum entry and exit fluxes of the metal through the liquid membrane ( and ) of the extraction and stripping reactions were evaluated and results showed good agreement between experimental data and theoretical predictions. Complete transport through the membrane took place according to the following order: Cd(II)>Cu(II)>Ni(II), with similar kinetic parameters obtained for Cu(II) and Cd(III). The transport behaviour of Ni(II) was different to that of Cu(II) and Cd(III), probably due to the different stoichiometry of the nickel complex compared to those of the other metal ions and the different chemical conditions required for its formation. The influence of the sample salinity on the transport kinetics was studied. k 1 values decreased slightly when the feed solution salinity was increased for Cu(II) and Ni(II), but not for Cd(II). Values of k 2 were practically unaffected. The proposed BLM was applied to the preconcentration and separation of metal ions (prior to their determination) in water samples with different saline matrices (CRM, river water and seawater), and good agreement with the certified values was obtained.  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