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 15 毫秒
1.
A 2,2′‐azinobis (3‐ethylbenzothiazoline‐6‐sulfonate) diammonium salt (ABTS)‐multiwalled carbon nanotubes (MWCNTs) nanocomposite/Bi film modified glassy carbon (GC) electrode was constructed for the differential pulse stripping voltammetric determination of trace Pb2+ and Cd2+. This electrode was more sensitive than ABTS‐free Bi/GC and Bi/MWCNTs/GC electrodes. Linear responses were obtained in the range from 0.5 to 35 μg L?1 for Cd2+ and 0.2 to 50 μg L?1 Pb(II), with detection limits of 0.2 μg L?1 for Cd2+ and 0.1 μg L?1 for Pb2+, respectively. This sensor was applied to the simultaneous detection of Cd2+ and Pb2+ in water samples with satisfactory recovery.  相似文献   

2.
《Electroanalysis》2017,29(8):1903-1910
This paper describes the electrochemical behaviors of Cd2+ and Pb2+ on the proposed mesoporous carbon microspheres/mefenamic acid/nafion modified glassy carbon electrode (MC/MA/Nafion/GC) studied by square wave anodic stripping voltammetry (SWASV). The prepared material is characterized by XRD, SEM, FTIR, RAMAN and BET analysis. Experimental parameters, such as the deposition potential and time, the pH value of buffer solution were optimized. Under the optimized conditions, the electrode responded linearly to Cd2+ and Pb2+ in the concentration range from 50 to 300 nM, and the detection limits were 24.2 and 11.26 nM respectively. The sensitivity determined was 0.0623 μA/nM (Cd2+) and 0.192 μA/nM (Pb2+). Multiple metal ion detection with clear demarcation of peaks was produced by the electrode. Moreover, the modified electrode has possessed good selectivity and reproducibility of Cd2+ and Pb2+ detection. We also investigated the interference of various anions and surfactants for the detection of Cd2+ and Pb2+ ions. Finally the modified electrode was used to detect the presence of metal ions in practical samples and the results obtained are comparatively good with respect to AAS.  相似文献   

3.
Summary The separation of trace metals from solutions of electrolytes by electrodeposition in a 30 l electrolytical flow-through cell was studied. The working electrode of the flow cell was made from powdered spectral or glassy carbon. The electrodeposition is complete for Cu2+, Cd2+, Mn2+ and Pb2+, partial for Zn2+, Fe3+ and Ni2+. Mn2+ and Pb2+ can also be deposited by anodic oxidation on the working electrode. The deposition is complete up to sample flow rates of 3–4 ml/min. The deposited elements are dissolved by short-circuiting the electrodes and flushing the cell with diluted acid. The dissolved elements are determined on-line by flame AAS. Data evaluation through peak area measurement is discussed.  相似文献   

4.
The aim of this study was to investigate the performance of monoliths composed of hydroxyethyl methacrylate (HEMA) to which N-methacryloyl-(L)-cysteine methyl ester (MAC) was polymerized for removal of heavy metal ions. Poly(HEMA-MAC) monolith was produced by bulk polymerization. Poly(HEMA-MAC) monolith was characterized by FTIR and scanning electron microscopy (SEM). The poly(HEMA-MAC) monolith with a swelling ratio of 89%, and containing 69.4 μmol MAC/g were used in the adsorption studies. Adsorption capacity of the monolith for the metal ions, i.e., Cu2+, Cd2+, Zn2+, Hg2+, and Pb2+ were investigated in aqueous media containing different amounts of the ions (10–750 mg/L) and at different pH values (3.0–7.0). The maximum adsorption capacities of the poly(HEMA-MAC) monolith were 68.2 mg/g for Zn2+, 129.2 mg/g for Cu2+, 245.8 mg/g for Pb2+, 270.2 mg/g for Hg2+, and 284.0 mg/g for Cd2+. pH significantly affected the adsorption capacity of MAC incorporated monolith. The competitive adsorption capacities were 587 μmol/g for Zn2+, 1646 μmol/g for Cu2+, 687 μmol/g for Pb2+, 929 μmol/g for Hg2+, and 1993 μmol/g for Cd2+. The chelating monolith exhibited the following metal ion affinity sequence on molar basis: Cd2+ > Cu2+ > Hg2+ > Pb2+ > Zn2+. The formation constants of MAC–metal ion complexes have been investigated applying the method of Ruzic. The calculated values of stability constants were 5.28 × 104 L/mol for Cd2+, 4.16 × 104 L/mol for Cu2+, 2.27 × 104 L/mol for Hg2+, 1.98 × 104 L/mol for Pb2+, and 1.25 × 104 L/mol for Zn2+. Stability constants were increased with increasing binding affinity. The chelating monoliths can be easily regenerated by 0.1 M HNO3 with higher effectiveness. These features make poly(HEMA-MAC) monolith a potential adsorbent for heavy metal removal.  相似文献   

5.
A multi-wall carbon nanotube (MWNT) modified glassy carbon electrode (GCE) was described for the simultaneous determination of trace levels of cadmium and lead by anodic stripping voltammetry (ASV). In pH 4.5 NaAc-HAc buffer containing 0.02 mol/l KI, Cd2+ and Pb2+ first adsorb onto the surface of a MWNT film coated GCE and then reduce at −1.20 V. During the positive potential sweep, reduced cadmium and lead were oxidized, and two well-defined stripping peaks appeared at −0.88 and −0.62 V. Compared with a bare GCE, a MWNT film coated GCE greatly improves the sensitivity of determining cadmium and lead. Low concentration of I significantly enhances the stripping peak currents since it induces Cd2+ and Pb2+ to adsorb at the electrode surface. The striping peak currents change linearly with the concentration of Cd2+ from 2.5×10−8 to 1×10−5 mol/l and with that of Pb2+ from 2×10−8 to 1×10−5 mol/l. The lowest detectable concentrations of Cd2+ and Pb2+ are estimated to be 6×10−9 and 4×10−9 mol/l, respectively. The high sensitivity, selectivity, and stability of this MWNT film coated electrode demonstrated its practical application for a simple, rapid and economical determination of trace levels of Cd2+ and Pb2+ in water samples.  相似文献   

6.
《Comptes Rendus Chimie》2016,19(7):789-797
A smectite-based inorganic-organic hybrid material was prepared by a one-step intercalation of cetyltrimethylammonium ions and thiourea within the interlayer space of montmorillonite (MT). The surface and textural properties of the resulting material were examined using several techniques (X-ray diffraction, elementary analysis and N2 adsorption-desorption experiments (BET method)) that demonstrated the presence of both modifiers in the clay mineral structure. The presence of thiourea molecules in the modified MT greatly improved its ability towards the fixation of Pb2+ and Cd2+ ions when the organoclay material was used for sensing purposes as a glassy carbon electrode modifier. The electro-analytical procedure was based on the chemical accumulation of both analytes under open-circuit conditions, followed by the detection of the preconcentrated species using square wave voltammetry. Upon optimization of different parameters likely to influence the electrode response, linear calibration graphs were obtained in the concentration ranges from 0.1 to 1 μM and 0.01 to 0.1 μM for Cd2+ and Pb2+, respectively, leading to low limits of detection (4.2 × 10−10 M for Pb2+and 1.2 × 10−9 M for Cd2+).  相似文献   

7.
Graphene nanosheets, dispersed in Nafion (Nafion-G) solution, were used in combination with in situ plated bismuth film electrode for fabricating the enhanced electrochemical sensing platform to determine the lead (Pb2+) and cadmium (Cd2+) by differential pulse anodic stripping voltammetry (DPASV). The electrochemical properties of the composite film modified glassy carbon electrode were investigated. It is found that the prepared Nafion-G composite film not only exhibited improved sensitivity for the metal ion detections, but also alleviated the interferences due to the synergistic effect of graphene nanosheets and Nafion. The linear calibration curves ranged from 0.5 μg L−1 to 50 μg L−1 for Pb2+ and 1.5 μg L−1 to 30 μg L−1 for Cd2+, respectively. The detection limits (S/N = 3) were estimated to be around 0.02 μg L−1 for Pb2+ and Cd2+. The practical application of the proposed method was verified in the water sample determination.  相似文献   

8.
《中国化学快报》2019,30(12):2211-2215
An electrochemical sensor based on self-made nano-porous pseudo carbon paste electrode (nano-PPCPE) has been successfully developed, and used to detect Cd2+ and Pb2+. The experimental results showed that the electrochemical performance of nanoPPCPE is evidently better than both glassy carbon electrode (GCE) and pure carbon paste electrode (CPE). Then the prepared nano-PPCPE was applied to detect Cd2+ and Pb2+ in standard solution, the results showed that the electrodes can quantitatively detect trace Cd2+ and Pb2+, which has great significance in electrochemical analysis and detection. The linear ranges between the target ions concentration and the DPASV current were from 0.1–3.0 μmol/L, 0.05–4.0 μmol/L for Cd2+ and Pb2+, respectively. And the detection limits were 0.0780 μmol/L and 0.0292 μmol/L, respectively. Moreover, the preparation of the nano-PPCPE is cheap, simple and has important practical value.  相似文献   

9.
Hu C  Wu K  Dai X  Hu S 《Talanta》2003,60(1):17-24
A simple and effective chemically modified carbon paste electrode (CMCPE) for the simultaneous determination of lead(II) and cadmium(II) was developed in this work. The electrode was prepared by the addition of diacetyldioxime into a carbon paste mixture. Pb2+ and Cd2+ were preconcentrated on the surface of the modified electrode by complexing with diacetyldioxime and reduced at a negative potential (−1.10 V). Then the reduced products were oxidized by differential pulse stripping. The fact that two stripping peaks appeared on the voltammograms at the potentials of −0.65 V (Cd2+) and −0.91 V (Pb2+) demonstrates the possibility of simultaneous determination of Pb2+ and Cd2+. Under the optimized working conditions, calibration graphs were linear in the concentration ranges of 1.0×10−7-1.5×10−5 mol l−1 (Pb2+) and 2.5×10−7-2.5×10−5 mol l−1 (Cd2+), respectively. For 5 min preconcentration, detection limits of 1×10−8 mol l−1 (Pb2+) and 4×10−8 mol l−1 (Cd2+) were obtained at the signal noise ratio (SNR) of 3. To evaluate the reproducibility of the newly developed electrode, the measurements of 5×10−7 mol l−1 Pb2+ and Cd2+ were parallel carried out for six times at different electrodes and the relative standard deviations were 2.9% (Pb2+) and 3.2% (Cd2+), respectively. Interferences by some metals were investigated. Only Ni2+ and Hg2+ apparently affected the peak currents of Pb2+ and Cd2+. The diacetyldioxime modified carbon paste electrode was applied to the determination of Pb2+ and Cd2+ in water samples. The results indicate that this electrode is sensitive and effective for the simultaneous determination of Pb2+ and Cd2+.  相似文献   

10.
The fabrication and evaluation of a glassy carbon electrode (GCE) modified with ordered mesoporous carbon (OMC), 2‐mercaptoethanesulfonate (MES)‐tethered polyaniline (PANI) and bismuth for simultaneous determination of trace Cd2+ and Pb2+ by differential pulse anodic stripping voltammetry (DPASV) are presented here. The morphology and electrochemical properties of the fabricated electrode were respectively characterized by scanning electron microscopy (SEM) and electrochemical impedance spectroscopy (EIS). Experimental parameters such as PANI disposition, preconcentration potential, preconcentration time and bismuth concentration were optimized. Under optimum conditions, the fabricated electrode exhibited linear calibration curves ranged from 1 to 120 nM for Cd2+ and Pb2+. The limits of detection (LOD) were 0.26 nM for Cd2+ and 0.16 nM for Pb2+ (S/N=3), respectively. Additionally, repeatability, reproducibility, interference and application were also investigated, and the proposed electrode exhibited excellent performance. The proposed method could be extended for the development of other new sensors for heavy metal determination.  相似文献   

11.
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   

12.
The development of nanostructured conducting polymers based materials for electrochemical applications has attracted intense attention due to their environmental stability, unique reversible redox properties, abundant electron active sites, rapid electron transfer and tunable conductivity. Here, a phytic acid doped polyaniline nanofibers based nanocomposite was synthesized using a simple and green method, the properties of the resulting nanomaterial was characterized by electrochemical impedance spectroscopy (EIS), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS). A glassy carbon electrode modified by the nanocomposite was evaluated as a new platform for the simultaneous detection of trace amounts of Cd2+ and Pb2+ using differential pulse anodic stripping voltammetry (DPASV). The synergistic contribution from PANI nanofibers and phytic acid enhances the accumulation efficiency and the charge transfer rate of metal ions during the DPASV analysis. Under the optimal conditions, good linear relationships were obtained for Cd2+ in a range of 0.05–60 μg L−1, with the detection limit (S/N = 3) of 0.02 μg L−1, and for Pb2+ in a range of 0.1–60 μg L−1, with the detection limit (S/N = 3) of 0.05 μg L−1. The new electrode was successfully applied to real water samples for simultaneous detection of Cd2+ and Pb2+ with good recovery rates. Therefore, the new electrode material may be a capable candidate for the detection of trace levels of heavy metal ions.  相似文献   

13.
A new type of covalent bulk modified glassy carbon composite electrode has been fabricated and utilized in the simultaneous determination of lead and cadmium ions in aqueous medium. The covalent bulk modification was achieved by the chemical reduction of 2-hydroxybenzoic acid diazonium tetrafluroborate in the presence of hypophosphorous acid as a chemical reducing agent. The covalent attachment of the modifier molecule was examined by studying Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and the surface morphology was examined by scanning electron microscopy images. The electrochemistry of modified glassy carbon spheres was studied by its cyclic voltammetry to decipher the complexing ability of the modifier molecules towards Pb2+ and Cd2+ ions. The developed sensor showed a linear response in the concentration range 1–10 μM with a detection limit of 0.18 and 0.20 μM for lead and cadmium, respectively. The applicability of the proposed sensor has been checked by measuring the lead and cadmium levels quantitatively from sewage water and battery effluent samples.  相似文献   

14.
A new chemically modified bismuth film electrode coated with an ionic liquid [(1‐ethyl‐3‐methylimidazolium tetracyanoborate (EMIM TCB)] and Nafion was developed for the simultaneous determination Pb2+ and Cd2+ by anodic stripping voltammetry. Compared with conventional bismuth film electrodes, this electrode exhibited greatly improved electrochemical activity for Pb2+ and Cd2+ detection due to the unique properties of Nafion polymer and ionic liquid. The key experimental parameters related to the fabrication of the electrode and the voltammetric measurements were optimized on the basis of the stripping signals, where the peak currents increased linearly with the metal concentrations in a range of 10–120 µg L?1 with a detect limit of 0.2 µg L?1 for Pb2+, and 0.5 µg L?1 for Cd2+ for 120s deposition. High reproducibility was indicated from the relative standard deviations (1.9 and 2.5 %) for nine repetitive measurements of 20 µg L?1 Pb2+ and Cd2+, respectively. In addition, the surface characteristics of the modified BiFE were investigated by scanning electron microscopy (SEM), and results showed that fibril‐like bismuth nanostructures were formed on the porous Nafion polymer matrix. Finally, the developed electrode was applied to determine Pb2+ and Cd2+ in water samples, indicating that this electrode was sensitive, reliable and effective for the simultaneous determination of Pb2+ and Cd2+.  相似文献   

15.
Kaolinite clay obtained from Ubulu-Ukwu, Delta state in Nigeria was modified with polyvinyl alcohol (PVA) reagent to obtain PVA-modified Kaolinite clay adsorbent. Scanning Electron Microscopy (SEM) of the PVA-modified adsorbent suggests that Kaolinite clay particles were made more compact in nature with no definite structure. Modification of Kaolinite clay with PVA increased its adsorption capacity for 300 mg/L Pb2+ and Cd2+ by a factor of at least 6, i.e., from 4.5 mg/g to 36.23 mg/g and from 4.38 mg/g to 29.85 mg/g, respectively, at 298 K. Binary mixtures of Pb2+ and Cd2+ decreased the adsorption capacity of Unmodified Kaolinite clay for Pb2+ by 26.3% and for Cd2+ by 0.07%, respectively. In contrast, for PVA-modified Kaolinite clay, the reductions were up to 50.9% and 58.5% for Pb2+ and Cd2+, respectively. The adsorption data of Pb2+ and Cd2+ onto both Unmodified and PVA-modified Kaolinite clay adsorbents were found to fit the Pseudo-Second Order Kinetic model (PSOM), indicating that adsorption on both surfaces was mainly by chemisorption and is concentration dependent. However, kinetic adsorption data from both adsorbent generally failed the Pseudo-First order Kinetic model (PFOM) test. Extents of desorption of 91% Pb2+ and 94% Cd2+ were obtained, using 0.1 M HCl, for the Unmodified Kaolinite clay adsorbent. It was found that 99% Pb2+ and 97% Cd2+, were desorbed, for PVA-modified Kaolinite clay adsorbents within 3 min for 60 mg/L of the metal ions adsorbed by the adsorbents.  相似文献   

16.
The sonochemically facilitated, mercury free detection of Pb2+ at a copper electrode has been investigated as a means of simplifying the quantification of this important analyte and to minimise the interference of copper ion. The procedure relies upon maximising the formation of Pb-Cu intermetallic compounds leading to the emergence of a single, easily quantifiable stripping signal. Linear responses to Pb2+ were obtained with a sensitivity comparable to that obtained at a bare glassy carbon electrode. Interference from Cu2+, Zn2+ and Cd2+ was assessed on the copper electrode with no appreciable change in the Pb2+ voltammetric profile observed. In contrast, bare glassy carbon showed a significant change in Pb2+ voltammetric profile as Cu2+ was added, due to the formation of intermetallic species.  相似文献   

17.
An 1-(pyridylazo)-2-naphthol modified glassy carbon electrode has been investigated as sensor for the measurement of trace levels of Cd2+. Cd2+ is deposited on the surface of a PAN modified glassy carbon electrode at –1.10 V (vs. SCE) via forming Cd2+–PAN and subsequent reduction at the electrode. In the following step, Cd-PAN is oxidized, and voltammograms are recorded by scanning the potential in a positive direction. Calibration plots were found to be linear in the range 2 × 10–8 mol/L to 8 × 10–7 mol/L. The detection limit was 5 × 10–10 mol/L, and the coefficient of variation, determined on one single electrode at a concentration of 5 × 10–7 mol/L, was calculated to be 3.2% (n = 5). Using this new kind of modified electrode, trace levels of Cd(II) in water samples were determined; the average recovery was calculated to be 98.78%. Received: 17 August 2000 / Revised: 19 December 2000 / Accepted: 27 December 2000  相似文献   

18.
We report the simultaneous electroanalytical determination of Pb2+ and Cd2+ by linear sweep anodic stripping voltammetry (LSASV) using an antimony nanoparticle modified boron doped diamond (Sb‐BDD) electrode. Sb deposition was performed in situ with the analytes, from a solution of 1 mg L?1 SbCl3 in 0.1 M HCl (pH 1). Pb2+ inhibited the detection of Cd2+ during simultaneous additions at the bare BDD electrode, whereas in the presence of antimony, both peaks were readily discernable and quantifiable over the linear range 50–500 μg L?1.  相似文献   

19.
A cost-efficient kaolinite-cellulose/cobalt oxide green nanocomposite (Kao-Cel/Co3O4 NC) was successfully synthesized, and utilized as a promising material for removing Pb2+ and Cd2+ from aqueous solution. The fabricated nanocomposite has been characterized by Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy-energy dispersive X-ray, high-resolution transmission electron microscopy, and Brunauer-Emmett-Teller analysis. The batch methodology was exploited for optimization of process parameters and the optimized conditions were found to be adsorbent dosage (2.0 g/L), extraction time (50 min), initial concentration (60 mg/L), and initial solution pH (6). Kao-Cel/Co3O4 NC displayed excellent adsorption properties and achieved maximum saturation capacity (Qm) of 293.68 mg Pb2+/g and 267.85 mg Cd2+/g, with an equilibration time of 50 min at 323 K. The Langmuir model best expressed the isotherm data recommending the adsorption onto energetically homogeneous NC surface, while the compatibility of kinetics data with pseudo-second-order model revealed the dependency of adsorption rate on adsorption capacity, and probable involvement of chemisorption in the rate-controlling step. Electrostatic interaction and ion exchange mechanism were responsible for the uptake of Pb2+ and Cd2+ by Kao-Cel/Co3O4 NC as demonstrated by Fourier transform infrared spectroscopy and pH studies. Thermodynamic parameters confirmed the physical, spontaneous, and endothermic sequestration processes. Real water investigation specified that the present adsorbent could be effectively used for liquid phase decontamination of Pb2+ and Cd2+. The nanocomposite exhibited high reusability, which could be utilized efficiently for five runs with sustainable results. In summary, this study portrayed the present nanocomposite as an emerging material for the adsorption of heavy metal ions particularly Pb2+ and Cd2+.  相似文献   

20.
Gold nanoparticles were deposited electrolessly on multiwalled carbon nanotubes (CNTs) via in situ reduction of HAuCl4 by NaBH4. The resulting gold covered nanotubes were immobilised onto the surface of a glassy carbon electrode via evaporation of a suspension in chloroform. Anodic stripping voltammetry was performed with the modified electrode in As(III) solutions. A limit of detection (LOD based on 3σ) of 0.1 μg L−1 was obtained but more importantly a sensitivity of 1985 μA μM−1 was obtained with square wave voltammetry (SWV) in an optimised system with a deposition time of 120 s. These values, particularly the high sensitivity compare favourably with previously reported methods in the area of electrochemical arsenic detection.  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