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1.
Complex formation between N,N,N′,N′‐tetrakis(2‐aminoethyl)ethane‐1,2‐diamine (penten) and the metal ions Mn2+, Co2+, Cu2+, Zn2+, Cd2+, Hg2+, Ag+, Pb2+, and Tl3+ (in 1.00M NaNO3 and 25°) was investigated by potentiometry and spectrophotometry. These are the first reported values of the stability constants for this ligand with Ag+, Pb2+, and Tl3+. The X‐ray crystal structure of [Tl(NO3)(penten)](NO3)2 was determined. In this structure, Tl3+ shows a coordination number of seven made up of the six N‐donors and one O‐atom of NO.  相似文献   

2.
The fast chemiluminescence (CL) arising from the reaction of bis(2,4,6-trichlorophenyl)oxalate (TCPO) with hydrogen peroxide in the presence of 1-(dansylamidopropyl)-1-aza-4,7,10-trithiacyclododecane (L) as a novel fluorophore, and imidazole as catalyst, has been studied in ethyl acetate solution. The relationships between the chemiluminescence intensity and concentrations of TCPO, imidazole, hydrogen peroxide and L are reported. In the presence of imidazole as catalyst, the entire CL signal was completed in less than 3 s. The quenching effect of Cu2+, Pb2+, Cd2+, Hg2+ and Ag+ ions on the chemiluminescent system was investigated, the resulting Stern–Volmer plots were obtained and the KQ values were calculated. It was found that the quenching effect of metal ions on the chemiluminescence of L decreases in the order Cu2+ > Pb2+ > Cd2+ > Hg2+ > Ag+.  相似文献   

3.
In our study, the single‐use & eco‐friendly electrochemical sensor platform based on herbal silver nanoparticles (AgNPs) was developed for detection of mercury (II) ion (Hg2+). For this purpose, the surface of pencil graphite electrode (PGE) was modified with AgNPs and folic acid (FA), respectively. The concentrations of AgNPs and FA were firstly optimized by differential pulse voltammetry (DPV) to obtain an effective surface modification of PGE. Each step at the surface modification process was characterized by using cyclic voltammetry (CV) and electrochemical impedence spectroscopy (EIS). The limit of detection (LOD) for Hg2+ was estimated and found to be 8.43 μM by CV technique. The sensor presented an excellent selectivity for Hg2+ against to other heavy metal ions such as Ca2+, Cd2+, Cr3+, Cu2+, Mg2+, Ni2+, Pb2+, Zn2+, Co2+ and Mn2+. Moreover, a rapid, selective and sensitive detection of Hg2+ was successfully performed in the samples of tap water within 1 min.  相似文献   

4.
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   

5.
Four metal‐organic frameworks (MOFs), {[Mn3.5L(OH)(HCOO)4(DMF)] · H2O} ( 1 ), {[In2.5L2O(OH)1.5(H2O)2] · DMF · CH3CN · 2H2O} ( 2 ), {[Pb4L3O(DMA)] · CH3CN} ( 3 ), and {[LaL(NO3)(DMF)2] · 2H2O} ( 4 ) were synthesized by utilizing the ligand 2,2′,6,6′‐tetramethoxy‐4,4′‐biphenyldicarboxylic acid (H2L) via solvothermal methods. All MOFs were characterized by single‐crystal X‐ray diffraction, powder X‐ray diffraction, thermogravimetric analysis, and infrared spectroscopy. In 1 , the Mn2+ ions are interconnected by formic groups in situ produced via DMF decomposition to form a rare 2D macrocyclic plane, which is further linked by L2– to construct the final 3D network. In 2 , 1D zip‐like infinite chain is formed and then interconnected to build the 3D framework. In 3 , a [Pb64‐O)2(O2C)10(DMA)2] cluster with a centrosymmetric [Pb64‐O)2]8+ octahedral core is formed in the 3D structure. In 4 , the La3+ ions are connected with each other through carboxylate groups of L2– to generate 1D zigzag chain, which is further linked by L2– to construct a 3D network with sra topology. Solid photoluminescence properties of 3 and 4 were also investigated.  相似文献   

6.
Stable ultra‐thin Langmuir monolayers of calix[4]resorcinarene derivatives, namely: C‐dec‐9‐enylcalix[4]resorcinarene‐O‐(R+)‐α‐methylbenzylamine (Ionophore I ), and C‐dec‐9‐enylcalix[4]resorcinarene‐O‐(S‐)‐α‐methylbenzylamine (Ionophore II ), were prepared at the air‐water interface. Their interactions with a series of heavy metals (HM) ions (Cu2+, Pb2+, Hg2+ and Cd2+) present in the aqueous subphase were investigated by measuring surface pressure‐area isotherms, at different concentrations. The surface pressure‐area (Π‐A) isotherms were stable and demonstrated the HM amounts influence on the limiting area (Alim) values, therefore confirming the examined macrocycles capability to host the metallic toxicants. Additionally, a HM concentration dependence was realized and interpreted by a selective tendency of both ionophores towards Cu2+ and Cd2+ ions over Pb2+ and Hg2+, especially at high concentrations. The HM ions interactions with the applied calix[4]resorcinarene Langmuir ultra‐thin monolayers were interpreted based on the Gibbs‐Shishkovsky adsorption equation. Moreover, quartz crystal microbalance with impedance measurement (QCM‐I), was applied for the detection of HM ions in solutions. The QCM‐I results showed the effectiveness of the coated QCM‐I crystals in detecting the ions at different concentrations. The detection limit values were in the order of 0.16, 0.3, 0.65, 1.1 ppm (Ionophore I), as well 0.11, 0.45, 0.2, 0.89 (Ionophore II) for the Cu2+, Pb2+, Hg2+ and Cd2+ cations, respectively. Additionally, a selective tendency of both ionophores towards copper ions was shown.  相似文献   

7.
8.
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   

9.
Rigid N‐(substituted)‐2‐aza‐[3]‐ferrocenophanes L1 and L2 were easily synthesized from 1,1 ‐dicarboxyaldehydeferrocene and the corresponding amines. Ligands L1 and L2 were characterized by 1H NMR, 13C NMR and single‐crystal X‐ray crystallography. The coordination abilities of L1 and L2 with metal ions such as Cu2+, Mg2+, Ni2+, Zn2+, Pb2+ and Cd2+ were evaluated by cyclic voltammetry. The electrochemical shift (ΔE1/2) of 125 mV was observed in the presence of Cu2+ ion, while no significant shift of the Fc/Fc + couple was observed when Mg2+, Ni2+, Zn2+, Pb2+, Cd2+ metal ions were added to the solution of L1 in the mixture of MeOH and H2O. Moreover, the extent of the anodic shift of redox potentials was approximately equal to that induced by Cu2+ alone when a mixture of Cu2+, Mg2+, Ni2+, Zn2+, Pb2+ and Cd2+ was added to a solution of L1. Ligand L1 was proved to selectively sense Cu2+ in the presence of large, excessive first‐row transition and late‐transition metal cations. The coordination model was proposed from the results of controlled experiments and quantum calculations. Copyright © 2012 John Wiley & Sons, Ltd.  相似文献   

10.
A novel cadmium(II) coordination polymer, poly[[[bis­(4,4′‐bipyridine)cadmium(II)]‐μ3‐4,4′‐dicarboxy­biphenyl‐3,3′‐di­carboxyl­ato] 0.35‐hydrate], {[Cd(C16H8O8)(C10H8N2)2]·0.35H2O}n, was obtained by reaction of Cd(CH3COO)2·3H2O, 4,4′‐bipyridine (4,4′‐bpy) and biphenyl‐3,3′,4,4′‐tetra­car­boxylic acid (H4L) under hydro­thermal conditions. Each CdII atom lies at the centre of a distorted octa­hedron, coordinated by four O atoms from three H2L2− ligands and N atoms from two monodentate 4,4′‐bpy ligands. Each H2L2− ligand coordinates to three CdII atoms through two carboxyl­ate groups, one acting as a bridging bidentate ligand and the other in a chelating bidentate fashion. Two Cd atoms, two H2L2− anions and four 4,4′‐bpy ligands form a ring dimer node, which links into an extended broad zonal one‐dimensional chain along the c axis.  相似文献   

11.
In the title PbII coordination polymer, [Pb(C16H10O4)(C14H8N4)(C3H7NO)]n, each PbII atom is eight‐coordinated by two chelating N atoms from one pyrazino[2,3‐f][1,10]phenanthroline (L) ligand, one dimethylformamide (DMF) O atom and five carboxylate O atoms from three different 4,4′‐ethylenedibenzoate (eedb) ligands. The eedb dianions bridge neighbouring PbII centres through four typical Pb—O bonds and one longer Pb—O interaction to form a two‐dimensional structure. The C atoms from the L and eedb ligands form C—H...O hydrogen bonds with the O atoms of eedb and DMF ligands, which further stabilize the structure. The title compound is the first PbII coordination polymer incorporating the L ligand.  相似文献   

12.
A new chemically modified carbon paste electrode by 2,2?-((pyridine-2,6-diylbis(azanylylidene))bis(methanylylidene))diphenol (L) ligand has been made and used as a sensor for determination of trace mercury and cadmium ions with cyclic voltammetry (CV) and differential pulse voltammetry (DPV) methods. Complexation studies of the ligand with Cu2+, Zn2+, Hg2+, Ni2+ and Cd2+ ions by conductometric method in acetonitrile–ethanol mixture at 25°C show that the ML complexes have formed. The formation constants of complexes were calculated from the computer fitting of the molar conductance–mole ratio data, and the stability of the resulting complexes varied in order of Cd2+ > Hg2+ > Cu2+ > Zn2+ > Ni2+. Then a simple and effective chemically modified carbon paste electrode with L was prepared, and the electrochemical properties and applications of the modified electrode were investigated. Under the optimal conditions, the detection limit was 0.0494 μg L?1 and 0.0782 μg L?1 for cadmium and mercury ions, respectively, and the linear range for both metal ions were from 1 to 100 μg L?1. The electrode shows high sensitivity, reproducibility and low cost, and was successfully applied to determination of Cd2+ and Hg2+ ions in water samples with recovery in the range of 97–101%.  相似文献   

13.
Gao J  Chen H  Dai H  Lv D  Ren J  Wang L  Yang W 《Analytica chimica acta》2006,571(1):150-155
A highly sensitive method for the determination of trace amounts of transition metal ions by use of sulfide in the Belousov-Zhabotinskii (B-Z) oscillating chemical reaction is proposed. The use of sulfide increased strongly the sensitivity of the B-Z reaction for transition metal ions, such as Ag+, Pb2+, Hg2+, Cd2+, Cu2+,and Bi3+. Results showed that the variational ratio of oscillating period (PR) is linearly proportional to the negative logarithm of concentration of metal ions. The detection limit is down to 10−12 mol L−1. Various influencing factors on the determination were also examined.  相似文献   

14.
The influence of Li+, Na+, K+, Rb+, Cs+, Mg2+, Ca2+, Sr2+, Ba2+, Ag+, Cd2+, Co2+, Fe2+, Hg2+, Mn2+, Pb2+, Zn2+ and Fe3+ on the spectroscopic properties of two dansyl (1-dimethylaminonaphthalene-5-sulfonyl) groups linked to the lower rims of a series of three, structurally related, di-ionized calix[4]arenes is investigated by means of absorption and emission spectrophotometry. Di(tetramethylammonium) salts of the di-ionized ligands, L, L1, and L2, which differ in having no, two and four allyl groups, respectively, on the upper rim of the calix[4]arene scaffold, are utilized for the spectrofluorimetric titration experiments in MeCN. On complexation by alkaline earth metal cations, the emission spectra undergo marked red shifts and quenching of the dansyl fluorescence. These effects are weaker with alkali metal cations. Transition metal cations and Pb2+ interact strongly with the ligands. In particular, Fe3+, Hg2+ and Pb2+ cause greater than 99% quenching of the dansyl fluorescence.  相似文献   

15.
The new application of C-dec-9-enylcalix[4]resorcinarene (R1), as an ionophore to detect heavy metals (HMs) cations (Cd2+, Hg2+, Cu2+, and Pb2+) in the aqueous media has been investigated through the preparation of an effective mass-sensitive sensor via the exploitation of a flow-type QCM-I technique. By adjusting the ions’ amounts in model solutions over a wide range of concentrations, acquired changes in the oscillating frequency related to the loading of metal ions on the sensor’s surface were gained, and thus favorable metrological parameters displaying the lowest detection limit (LOD) associated with copper ions (10 ppb). Simultaneously, a novel voltammetric sensor was prepared by modifying gold screen-printed electrodes (SPEs) with R1. Electrochemical characterization employing CV, SWV, and EIS was carried out, showing the success of the electrode modification. Then, the experimental conditions of supporting electrolyte, pH, accumulation time, and accumulation potential were optimized to achieve an enhanced detection. The R1@SPE sensor simultaneously detected the HMs (Cd2+, Hg2+, Cu2+, Pb2+), and the lowest LOD was associated with Pb2+ (0.19 ppb). The selectivity evaluation of the electrochemical sensor was performed by studying the effect of interferences majorly present in water sources (Mg2+, Ni2+, Zn2+, Al3+, and K+) on the SWV detection signals, and it was revealed that the interfering ions did not affect the simultaneous detection of the studied HMs (RSD less than 5%), the voltammetric sensors also presented excellent repeatability and reproducibility (RSD less than 5%).  相似文献   

16.
Highly selective all solid state electrochemical sensor based on a synthesized compound i.e. 2‐(1‐(2‐((3‐(2‐hydroxyphenyl)‐1H‐pyrozol‐1‐yl)methyl)benzyl)‐1H‐pyrazol‐3‐yl)phenol (I) as an ionophore has been prepared and investigated for the selective quantification of chromium(III) ions. The effect of various plasticizers, viz. dibutyl phosphonate (DBP), dibutyl(butyl) phosphonate (DBBP), nitrophenyl octyl ether (NPOE), tris‐(2‐ethylhexyl)phosphonate (TEP), tri‐butyl phosphonate (TBP), dioctyl phthalate (DOP), dioctyl sebacate (DOS), benzyl acetate (BA) and acetophenone (AP) along with anion excluders NaTPB (sodium tetraphenyl borate) and KClTPB (potassium(tetrakis‐4‐chlorophenyl)borate was also studied. The optimum composition of the best performing membrane contained (I):KClTPB:NPOE:PVC in the ratio 15 : 3 : 40 : 42 w/w. The sensor exhibited near Nernstian slope of 20.1±0.2 mV/decade of activity in the working concentration range of 1.2×10?7–1.0×10?1 M, and in a pH range of 3.8–4.5. The sensor exhibited a fast response time of 10 s and could be used for about 5 months without any considerable divergence in potentials. The proposed sensor showed very good selectivity over most of the common cations including Na+, Li+, K+, Cu2+, Sr2+, Ni2+, Co2+, Ba2+, Hg2+, Pb2+, Zn2+, Cs+, Mg2+, Cd2+, Al3+, Fe3+and La3+. The activity of Cr(III) ions was successfully determined in the industrial waste samples by using this sensor.  相似文献   

17.
The competitive removal of Pb2+, Cu2+, and Cd2+ ions from aqueous solutions by the copolymer of 2‐acrylamido‐2‐methyl‐1‐propane sulfonic acid (AMPS) and itaconic acid (IA), P(AMPS‐co‐IA), was investigated. Homopolymer of AMPS (PAMPS) was also used to remove these ions from their aqueous solution. In the preparation of AMPS–IA copolymer, the molar percentages of AMPS and IA were 80 and 20, respectively. In order to observe the changes in the structures of polymers due to metal adsorption, FTIR spectra by attenuated total reflectancetechnique and scanning electron microscopy (SEM) pictures of the polymers were taken both before and after adsorption experiments. Total metal ion removal capacities of PAMPS and P(AMPS‐co‐IA) were 1.685 and 1.722 mmol Me2+/gpolymer, respectively. Experimental data were evaluated to determine the kinetic characteristics of the adsorption process. Competitive adsorption of Pb2+, Cu2+, and Cd2+ ions onto both PAMPS and P(AMPS‐co‐IA) was found to fit pseudo‐second‐order type kinetics. In addition, the removal orders in the competitive adsorption of these metal ions onto PAMPS and P(AMPS‐co‐IA) were found to be Cd2+ > Pb2+ > Cu2+ and Pb2+ > Cd2+ > Cu2+, respectively. Copyright © 2008 John Wiley & Sons, Ltd.  相似文献   

18.
In a search for environmentally friendly metal-chelating ligands for industrial applications, the protonation and complex formation equilibria of iminodisuccinic acid (IDS) and 3-hydroxy-2,2′-iminodisuccinic acid (HIDS) with Cd2+, Hg2+, and Pb2+ in aqueous 0.1?mol?L?1 NaNO3 solution were studied at 25°C by potentiometric titration. Models for complexation and stability constants of the different complexes were determined for each metal ion using the computer program SUPERQUAD. In all cases, complex formation was dominated by stable ML2? complexes.  相似文献   

19.
The influence of metal cations (Li+, Na+, K+, Rb+, Cs+, Mg2+, Ca2+, Sr2+, Ba2+, Ag+, Cd2+, Co2+, Fe2+, Hg2+, Mn2+, Pb2+, Zn2+ and Fe3+) on the spectroscopic properties of two dansyl (1-dimethylaminonaphthalene-5-sulfonyl) groups linked to the lower rims of a series of three, structurally related, di-ionized calix[4]arenes was investigated by means of absorption and emission spectrophotometry. Di(tetramethylammonium) salts of the di-ionized ligands, (TMA)2L1, (TMA)2L2 and (TMA)2L3, which differ in having zero, two and four tert-butyl groups, respectively, on the upper rim of the calix[4]arene scaffold were utilized for the spectrofluorimetric titration experiments in acetonitrile. On complexation by alkaline earth metal cations, both the absorption and emission spectra undergo marked red shifts and quenching of the dansyl fluorescence. These effects are weaker with alkali metal cations. Transition metal cations interact strongly with the ligands. In particular, Fe3+, Hg2+ and Pb2+ cause greater than 97% quenching of the dansyl fluorescence in the di-ionized ligands.  相似文献   

20.
The title coordination polymer, poly[[aqua(μ5‐1,1′‐biphenyl‐2,2′,5,5′‐tetracarboxylato)bis[μ2‐1,4‐bis(1H‐imidazol‐1‐yl)benzene]dicadmium(II)] dihydrate], {[Cd2(C16H6O8)(C12H10N4)2(H2O)]·2H2O}n, was crystallized from a mixture of 1,1′‐biphenyl‐2,2′,5,5′‐tetracarboxylic acid (H4bpta), 1,4‐bis(1H‐imidazol‐1‐yl)benzene (1,4‐bib) and cadmium nitrate in water–dimethylformamide. The crystal structure consists of two crystallographically independent CdII cations, with one of the CdII cations possessing a slightly distorted pentagonal bipyramidal geometry. The second CdII centre is coordinated by carboxylate O atoms and imidazole N atoms from two separate 1,4‐bib ligands, displaying a distorted octahedral CdN2O4 geometry. The completely deprotonated bpta4− ligand, exhibiting a new coordination mode, bridges five CdII cations to form one‐dimensional chains viaμ3‐η1212 and μ2‐η1100 modes, and these are further linked by 1,4‐bib ligands to form a three‐dimensional framework with a (42.64)(4.62)(43.65.72) topology. The structure of the coordination polymer is reinforced by intermolecular hydrogen bonding between carboxylate O atoms, aqua ligands and crystallization water molecules. The solid‐state photoluminescence properties were investigated and the complex might be a candidate for a thermally stable and solvent‐resistant blue fluorescent material.  相似文献   

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