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1.
A sulphide selective colorimetric metal complexing indicator-displacement assay has been developed using an immobilized copper(II) complex of the azo dye 1-(2-pyridylazo)-2-naphthol printed by inkjetting on a nylon support. The change in colour measured from the image of the disposable membrane acquired by a digital camera using the H coordinate of the HSV colour space as the analytical parameter is able to sense sulphide in aqueous solution at pH 7.4 with a dynamic range up to 145 μM, a detection limit of 0.10 μM and a precision between 2 and 11%.  相似文献   

2.
A disposable sensor has been developed for the measurement of copper(II) concentration in aqueous solution based on a change in the fluorescence of porphyrazine 2,7,12,17-tetra-tert-butyl-5,10,15,20-tetraaza-21H,23H-porphine (TP). The sensor was constructed by spin-coating a polyester support with a PVC solution containing TP, a plasticizer, the chelating agent Zincon and the ion-pairing benzetonium chloride. The measurement principle is based on the radiationless resonance energy transfer (RET) from TP immobilized in membrane, and acting as fluorescence donor, to Zincon acting as an acceptor induced by copper(II). The absorption spectrum of the Zincon-Cu(II) complex presents adequate overlapping with the emission spectrum of TP, producing a useful analytical signal by the RET process.The disposable sensor responds to copper(II) irreversibly over a dynamic range from 0.039 to 14 μmol L−1 (2.5-890 μg L−1) with a sensor-to-sensor reproducibility (relative standard deviation RSD) of 1.9%, as log aCu2+, at the medium level of the range and a response time of 10 min. The performance of the optical disposable sensor was tested for the analysis of copper in different types of natural waters (river, well, spring and swimming pool), validating results against a reference procedure.  相似文献   

3.
A new chelating resin based on chitosan biopolymer modified with 5-sulphonic acid 8-hydroxyquinoline using the spray drying technique for immobilization is proposed. The chelating resin was characterized by thermogravimetric analysis (TGA) and X-ray diffraction (XRD) and surface area by nitrogen sorption. The efficiency of the chelating resin was evaluated by the preconcentration of metal ions Cu(II) and Cd(II) present in aqueous samples in trace amounts. The metal ions were previously enriched in a minicolumn and the concentrations of the analytes were determined on-line by flame atomic absorption spectrometry (FAAS). The maximum retention for Cu(II) occurred in the pH range 8-10, and for Cd(II) at pH 7. The optimum flow rate for sorption was found to be 7.2 ml min−1 for the preconcentration of the metal ions. The analytes gave relative standard deviations (R.S.D.) of 0.7 and 0.6% for solutions containing 20 μg l−1 of Cu(II) and 15 μg l−1 of Cd (II), respectively (n=7). The enrichment factors for Cu(II) and Cd (II) were 19.1 and 13.9, respectively, and the limits of detection (LOD) were 0.2 μg l−1 for Cd(II) and 0.3 μg l−1 for Cu(II), using a preconcentration time of 90 s (n=11). The accuracy of the proposed method was evaluated by the metal ion recovery technique, in the analysis of potable water and water from a lake, with recoveries being between 97.2 and 107.3%.  相似文献   

4.
The aim of this study was to investigate the possibility to synthesize new chelating polymeric microspheres owing immobilized biocompatible agent as chelating functional groups and to evaluate their performance in metal ions removal from aqueous solution.The microparticles were synthesized via precipitation polymerization of 4-O-(4-vinylbenzyl)-myo-inositol 1,3,5-orthoformate with ethylene glycol dimethacrylate (EGDMA) and subsequent exhaustive phosphorylation of myo-inositol groups using phosphoric acid.Spherical geometry with monodisperse nature of the polymeric microparticles was confirmed by scanning electron micrographs (SEM) and dimensional analysis. A large surface area of the microspheres provided a maximum interaction of metal ions and the chelating functional groups on the surface. Absorption capacity of the beads for the selected metal ions, i.e., Cu(II), Ni(II), Fe(III), was investigated in detail in aqueous solution at pH 5.0 utilizing UV/Vis spectroscopy. This study showed that the macromolecular systems are very effective in chelating these metal ions and the affinity order of the microbeads toward metal ions is: Fe(III) > Ni(II) > Cu(II).The chelating beads can be easily regenerated by 1.0 M HNO3 with high effectiveness. These features make the synthesized beads a potential candidate for metal ions removal at high capacity.  相似文献   

5.
Alireza Mohadesi 《Talanta》2007,72(1):95-100
An electrochemical sensor for the detection of copper(II) ions is described using a meso-2,3-dimercaptosuccinic acid (DMSA) self-assembled gold electrode. First in ammonia buffer pH 8, copper(II) ions complex with self-assembled monolayer (SAM) via the free carboxyl groups on immobilized meso-2,3-dimercaptosuccinic acid (accumulation step). Then, the medium is exchanged to acetate buffer pH 4.6 and the complexed Cu(II) ions are reduced in negative potential of −0.3 V (reduction step). Following this, reduced coppers are oxidized and detected by differential pulse (DP) voltammetric scans from −0.3 to +0.7 V (stripping step). The effective parameters in sensor response were examined. The detection limit of copper(II) was 1.29 μg L−1 and R.S.D. for 200 μg L−1 was 1.06%. The calibration curve was linear for 3-225 μg L−1 copper(II). The procedure was applied for determination of Cu(II) to natural waters and human hairs. The accuracy and precision of results were comparable to those obtained by flame atomic absorption spectroscopy (FAAS).  相似文献   

6.
A new simple and reliable method has been developed to selectively separate and concentrate ultra trace amounts of copper ion in aqueous samples for subsequent measurement by atomic absorption spectrometry (AAS). The Cu2+ ions are adsorbed selectively and quantitatively during passage of aqueous solutions through octadecyl silica membrane disks modified with bis(2-hydroxyphenylamino) glyoxime. The retained copper ions then stripped from the disk with a minimal amount of 0.2 M nitric acid solution as eluent, and determined by AAS. The proposed method permitted large enrichment factors of about 100 or higher.The limit of detection of the proposed method is 0.004 ng ml−1. The maximum capacity of the membrane disks modified with 25 mg of ligand was found to be 280±32 μg of copper(II). The effects of various cationic interferences on the percent recovery of copper in binary mixtures were studied.The method was successfully applied to the recovery and determination of copper in several water samples.  相似文献   

7.
A procedure for the determination of trace level of copper(II) and cadmium(II) by FAAS using an on-line preconcentration system has been proposed. In this system, copper and cadmium ions were adsorbed onto a minicolumn packed with silica gel modified with niobium(V) oxide (Nb2O5-SiO2), followed by nitric acid elution in reverse mode and determination on-line by flame atomic absorption spectrometry (AAS) without interference of the matrix. Chemical and flow variables as well as concomitant ions were studied in the developed procedure. The enrichment factor for copper(II) and cadmium(II) was 34.2 and 33.0, respectively, using a preconcentration time of 2 min. The limit of detection for copper(II) and cadmium(II) was 0.4, and 0.1 μg l−1, respectively. The precision of the method, evaluated as the relative standard deviation in solutions containing 15 μg l−1 of copper and 10 μg l−1 of cadmium, by analyzing a series of seven replicates, was 1.8 and 1.6%, respectively. The accuracy was assessed through recovery experiments of certified material and water samples.  相似文献   

8.
A procedure involving bead-injection concept and sequential determination of copper and mercury ions in river-water samples is proposed. The method is based on the solid-phase extraction of both metal ions on the same beads surface (Chelex 100 resin) and in their subsequent reaction with the colorimetric reagents (APDC and Dithizone for copper and mercury ions, respectively). For this task, a resin mini-column is established in the optical path by the selection, introduction and trapping of a defined volume of the Chelex-100 resin beads suspension in the flow system. The passage of the sample solution through the resin mini-column promotes the sorption of Cu(II) ions and, making the APDC colorimetric reagent flows through the beads, the formation of the coloured complex on the solid phase surface occurs. The absorbance of the formed APDC-Cu complex is then monitored at 436 nm and the spent beads are discarded. Packing another resin mini-column in the flow cell and repeating the concentration step it is possible to carried out the mercury determination by using Dithizone as reagent. The absorbance of the Dithizone-Hg complex is monitored at 500 nm. After each measurement, the spent beads are wasted and a new portion of fresh one is trapped in the system, letting it ready for the next measurement. The bead injection system is versatile and can be used to concentrate different sample volumes, which permits the determination of a wide range of copper and mercury ions concentrations. When the sample-selected volumes are 100 and 1000 μl the analytical ranges were 5.0 up to 500.0 μg l−1 and 2.5 up to 30.0 μg l−1 for Cu(II) and Hg(II) ions, respectively. Under these conditions, the detection limit was estimated as 0.63 and 0.25 μg l−1 for copper and mercury ions determination. The system consumes 2 mg of Chelex 100 resin beads, 0.20 mg of APDC or 1.25 mg of Dithizone per determination and the traditional organic solvent extraction methodology, normally used in connection with APDC and Dithizone reagents, is not used here which permits to classify the present method as green.  相似文献   

9.
In this work, urea detection techniques based on the pH sensitivity of CdSe/ZnS QDs were developed using three types of sol-gel membranes: a QD-entrapped membrane, urease-immobilized membrane and double layer consisting of a QD-entrapped membrane and urease-immobilized membrane. The surface morphology of the sol-gel membranes deposited on the wells in a 24-well microtiter plate was investigated. The linear detection range of urea was in the range of 0-10 mM with the three types of sol-gel membranes. The urea detection technique based on the double layer consisting of the QD-entrapped membrane and urease-immobilized membrane resulted in the highest sensitivity to urea due to the Michaelis-Menten kinetic parameters. That is, the Michaelis-Menten constant (Km =2.0745 mM) of the free urease in the QD-entrapped membrane was about 4-fold higher than that (Km =0.549 mM) of the immobilized urease in the urease-immobilized membrane and about 12-fold higher than that (Km =0.1698 mM) of the immobilized urease in the double layer. The good stability of the three sol-gel membranes for urea sensing over 2 months showed that the use of sol-gel membranes immobilized with QDs or an enzyme is suitable for biomedical and environmental applications.  相似文献   

10.
This study describes the functionalization of biopolymer chitosan, using the complexing agent 8-hydroxyquinoline (oxine) by reaction of diazotization. The chelating resin was characterized by degree of deacetylation, infrared, Raman spectroscopy. The efficiency of the chelating resin and accuracy of the proposed method was evaluated by the metal ion recovery technique in the analysis of potable water, lake water, seawater and a certified sample of oyster tissue. The metal ions Cd(II) and Cu(II) in the samples were previously enriched in a minicolumn and flow injection flame atomic absorption spectrometry (FI-FAAS) determined the concentrations of the analytes. The chelating resin exhibited high selectivity for Cd(II) at pH 7 and for Cu(II) at pH 10. The eluent concentration was tested by the use of HNO3 in concentrations of 0.1-3 mol l−1 maximum response was obtained at 0.5 mol l−1 for Cd(II) and Cu(II), with R.S.D. values of 0.4%. The analytes gave relative standard deviations (R.S.D.) of 1.5 and 0.7% for solutions of Cd(II) and Cu(II), respectively (n = 7) containing 20 μg l−1 of the metal ions, defining a high reproducibility. The limits of detection (LOD) were 0.1 μg l−1 for Cd(II) and 0.4 μg l−1 for Cu(II). The analytical properties of merit were obtained using the parameters previously optimized with preconcentration time of 90 s. The chelating resin showed chemical stability within a wide range of pH and the efficiency was not altered for the preconcentration of the metal ions during all the experiments.  相似文献   

11.
Kagaya S  Araki Y  Hirai N  Hasegawa K 《Talanta》2005,67(1):90-97
The coprecipitation behavior of 44 elements (47 ions because of chromium(III,VI), arsenic(III,V), and antimony(III,V)) with yttrium phosphate was investigated at various pHs. Yttrium phosphate could quantitatively coprecipitate iron(III), lead, bismuth, and indium over a wide pH range; however, 18 ions, including alkali metals and oxo anions, such as vanadium(V), chromium(VI), molybdenum(VI), tungsten(VI), germanium(IV), arsenic(III,V), selenium(IV), and tellurium(VI), were scarcely collected. In addition, 19 ions, including cobalt, nickel, and copper(II), were hardly coprecipitated at pHs below about 3. Based on these results, the separation of iron(III), lead, and bismuth from cobalt, nickel, and copper(II) matrices was investigated. Iron(III), lead, and bismuth ranging from 0.5 to 25 μg could be separated effectively from a solution containing 0.5 g of cobalt, nickel, or copper at pH 3.0. The separated iron(III), lead, and bismuth could be determined by inductively coupled plasma atomic emission spectrometry using internal standardization. The detection limits (3σ, n = 7) of iron(III), lead, and bismuth were 0.008, 0.137, and 0.073 μg, respectively. The proposed method was applied to the analyses of metals and chlorides of cobalt, nickel, and copper.  相似文献   

12.
Sawula GM 《Talanta》2004,64(1):80-86
Microcolumns containing 8-hydroxyquinoline azo-immobilized on controlled pore glass were incorporated in a field sampler for on-site collection, isolation and preconcentration of trace metal ions in waters of the Okavango Delta, Botswana. Sequestered trace metal ions were recovered by elution with 0.5 ml of 1.5 M nitric acid, and determined by graphite furnace atomic absorption spectrometry (GFAAS). This sampling and enrichment method minimizes sample contamination, and collection of large volumes of water samples for transporting, over long distances, to analytical laboratories is avoided.Data reported comprise one of the initial surveys on trace metal ion concentrations in waters of the Okavango Delta, Botswana. In waters with more efficient mixing, dissolved metal ion concentrations found were generally low with slightly elevated levels of manganese (7-19 μg l−1), zinc (2.7-4.8 μg l−1), nickel (0.2-2.5 μg l−1) and copper (0.3-2.1 μg l−1). For each trace metal ion, concentration levels seem to reflect zones of varying water conveyance, and show no obvious temporal and spatial variations apart from a slight increment from the inlet in the upper Delta to the outlets in the lower Delta.  相似文献   

13.
A novel optical fibre reflectance sensor coupled to a multisyringe flow injection system (MSFIA) for the determination and speciation analysis of iron at trace level using chelating disks (iminodiacetic groups) is proposed. Once iron(III) has been retained onto a chelating disk, an ammonium thiocyanate stream is injected in order to form the iron(III)-thiocyanate complex which is spectrophotometrically detected at 480 nm. Iron(III) is eluted with 2 M hydrochloric acid so that the chelating disk is regenerated for subsequent experiments. The determination of total iron is achieved by the on-line oxidation of iron(II) to iron(III) with a suitable hydrogen peroxide stream.A mass calibration was feasible in the range from 0.001 to 0.25 μg. The detection limit (3sb/S) was 0.001 μg. The repeatability (RSD), calculated from nine replicates using 1 ml injections of a 0.1 mg/l concentration, was 2.2%. The repeatability between five chelating disks was 3.6%. The applicability of the proposed methodology in fresh and seawater samples has been proved.The proposed technique has been validated by replicate analysis (n = 4) of certified reference materials of water with satisfactory results.  相似文献   

14.
Thiacalix[4]arenetetrasulfonate (TCAS) has been examined as a pre-column chelating reagent for the determination of trace metal ions by kinetic differentiation mode (KD) ion-pair reversed-phase high-performance liquid chromatography (HPLC) with spectrophotometric detection. Among 14 kinds of common metal ions tested here, viz. Al(III), Ca(II), Cd(II), Co(II), Cr(III), Cu(II), Fe(III), Hg(II), Mg(II), Mn(II), Ni(II), Pb(II), V(V), and Zn(II) ion, only Ni(II) ion was detected as the TCAS chelate in the HPLC separation stage in spite of TCAS forming the chelates with various metal ions except for Al(III), Ca(II), and Mg(II) at the pre-column chelation stage. The undetected metal-TCAS chelates seemed to be dissociated on an HPLC column where no added TCAS was present in the mobile phase because of their kinetic unstability. The calibration graph for Ni(II) ion gave a wide linear dynamic range (40-20,000 nM) with the very low detection limit (DL) (3σ base-line fluctuation) to be 5.4 nM (0.32 ng ml−1). The practical applicability of the KD-HPLC method with TCAS was demonstrated with the determination of trace Ni in coal fly ash.  相似文献   

15.
For the first time, the formation of a luminescent hexanuclear cluster has been used for the selective determination of copper. In aqueous solutions, the non-luminescent ligand N-ethyl-N′-methylsulfonylthiourea (EMT) forms an intensely red luminescent hexanuclear Cu(I)-cluster with an emission maximum at 663 nm only with Cu(II) ions. The intensity of the luminescence is proportional to the Cu(II) concentration and allows for selective Cu determinations in the μg l−1-range. Ubiquitous metal ions such as Fe(III), Al(III), Ca(II), Mg(II), and alkaline metal ions, as well as other heavy metal ions, e.g. Co(II), Ni(II), Zn(II), Cd(II), Hg(II), and Pb(II) are tolerated in concentrations up to 50 mg l−1. The detection limit for Cu(II) in aqueous solution, calculated according to Funk et al. [Qualitätssicherung in der Analytischen Chemie, Verlag Chemie, Weinheim, 1992], is 113 μg l−1. The cluster formation has been used for the quantitative analysis of copper in tap water and in industrial water, as well as for the localization of copper adsorbed by activated-sludge flocs.  相似文献   

16.
A stable chelating sorbent was synthesized by covalently linking 4-hydroxytoluene or 4-hydroxyacetophenone with the polyurethane foam (PUF) through -NN- group. The synthesized chelating sorbents were characterized by IR and UV/vis measurements. The modified foams show excellent stability towards various solvents. Factors influencing the extraction process of Zn(II), Pb(II), Cd(II) and Hg(II) were studied and evaluated as a function of pH of metal ion solution and equilibration shaking time. The values of sorption capacity of metal ions (μg g−1) were determined with the two types of bonded foams. The two phenolic bonded foams were studied comparatively. The potential applications of the two newly synthesized foams for the removal and separation of the examined metal ions from two natural water samples (drinking tap water and Qaroun lake water at Fayoum City, Egypt) were investigated. Precision (assessed as a relative standard deviation, R.S.D.) was also evaluated and found to be ≤7.3% (N = 5) with a detection limit under 0.46 μg L−1.  相似文献   

17.
A simple, long life, rapid response and sensitive barium(II)-PVC membrane sensor that typically follows Nernstian behavior has been developed for the assay of barium(II) ions. The developed sensor has been made by incorporating the complex ion associate of barium(II)-Rose Bengal (Ba-RB) as an ionophore into a plasticized PVC matrix. The sensor is stable and exhibited fast potential response of 20 s and gave a good linear response with a Nernstian slope of 28.5 ± 0.4 mV/decade of activity within the concentration range 5 × 10−5 to 10−1 M over a wide range of pH 4.5-10.0 for barium(II) ions. The developed sensor showed comparatively good selectivity for barium(II) ions with respect to other alkali, alkaline earth, transition and heavy metal ions. The plasticizer o-nitrophenyloctyl ether controlled significantly the calibration slope and the lifetime of the fabricated sensor. The proposed sensor was used successfully for the analysis of barium(II) ions in wastewater samples and in lithophone pigment with excellent recovery percentages in the range 98.9-99.8 ± 1.6%. The determination of sulphate in fresh and potable water samples with the developed sensor has been also achieved successfully. The described sensor provides a reliable means with good correlation with the data obtained by atomic absorption spectrometry (AAS) and other spectrophotometric methods for the analysis of trace amounts of barium(II) and/or sulphate ions in different matrices.  相似文献   

18.
A simple, sensitive and powerful on-line sequential injection (SI) dispersive liquid-liquid microextraction (DLLME) system was developed as an alternative approach for on-line metal preconcentration and separation, using extraction solvent at microlitre volume. The potentials of this novel schema, coupled to flame atomic absorption spectrometry (FAAS), were demonstrated for trace copper and lead determination in water samples. The stream of methanol (disperser solvent) containing 2.0% (v/v) xylene (extraction solvent) and 0.3% (m/v) ammonium diethyldithiophosphate (chelating agent) was merged on-line with the stream of sample (aqueous phase), resulting a cloudy mixture, which was consisted of fine droplets of the extraction solvent dispersed entirely into the aqueous phase. By this continuous process, metal chelating complexes were formed and extracted into the fine droplets of the extraction solvent. The hydrophobic droplets of organic phase were retained into a microcolumn packed with PTFE-turnings. A portion of 300 μL isobutylmethylketone was used for quantitative elution of the analytes, which transported directly to the nebulizer of FAAS. All the critical parameters of the system such as type of extraction solvent, flow-rate of disperser and sample, extraction time as well as the chemical parameters were studied. Under the optimum conditions the enhancement factor for copper and lead was 560 and 265, respectively. For copper, the detection limit and the precision (R.S.D.) were 0.04 μg L−1 and 2.1% at 2.0 μg L−1 Cu(II), respectively, while for lead were 0.54 μg L−1 and 1.9% at 30.0 μg L−1 Pb(II), respectively. The developed method was evaluated by analyzing certified reference material and applied successfully to the analysis of environmental water samples.  相似文献   

19.
A new chelating polymeric sorbent is developed using Merrifield chloromethylated resin anchored with calix[4]arene-o-vanillinsemicarbazone for simultaneous separation and solid phase extractive preconcentration of U(VI) and Th(IV). The “upper-rim” functionalized calix[4]arene-o-vanillinsemicarbazone was covalently linked to Merrifield resin and characterized by FT-IR and elemental analysis. The synthesized chelating polymeric sorbent shows superior binding affinity towards U(VI) and Th(IV) under selective pH conditions. Various physico-chemical parameters that influence the quantitative extraction of metal ions were optimized. The optimum pH range and flow rates for U(VI) and Th(IV) were 6.0-7.0 and 1.0-4.0 ml min−1 and 3.5-4.5 and 1.5-4.0 ml min−1, respectively. The total sorption capacity found for U(VI) and Th(IV) was 48734 and 41175 μg g−1, respectively. Interference studies carried out in the presence of diverse ions and electrolyte species showed quantitative analyte recovery (98-98.5%) with lower limits of detection, 6.14 and 4.29 μg l−1 and high preconcentration factors, 143 and 153 for U(VI) and Th(IV), respectively. The uptake and stripping of these metal ions on the resin were fast, indicating a better accessibility of the metal ions towards the chelating sites. The analytical applicability of the synthesized polymeric sorbent was tested with some synthetic mixtures for the separation of U(VI) and Th(IV) from each other and also from La(III), Cu(II) and Pb(II) by varying the pH and sequential acidic elution. The validity of the proposed method was checked by analyzing these metal ions in natural water samples, monazite sand and standard geological materials.  相似文献   

20.
A method is presented for the cloud-point extraction and separation of copper and lanthanoid ions. A water-soluble calixarene, p-sulfonatocalix[4]arene (C4AS), is used as the chelating agent and Triton X-100 is chosen as the surfactant. The factors affecting the extraction efficiency, such as pH, the concentrations of Triton X-100 and C4AS, equilibration time and centrifugation time, were evaluated. The results demonstrate that there are different extraction behaviors for Cu(II) and Ln(III). Cu(II) can be separated from Ln(III) using C4AS as the chelating agent under weakly acidic conditions. The method may be used to remove trace copper from the lanthanoids.  相似文献   

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