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1.
THREEPROM  Jirasak  SOM-AUM  Waraporn  林金明 《中国化学》2006,24(12):1747-1753
A new separation system of capillary electrophoresis for the simultaneous determination of metals by using ethylenediamine tetraacetic acid (EDTA) as complexing agent and employing vancomycin as complex selector was described. The Z-shape cell capillary electrophoresis was used to enhance the sensitivity for the determination of the complexes of Cu(Ⅱ), Ni(Ⅱ), Co(Ⅱ) and Fe(Ⅲ) with EDTA. The partial filling method (co-current mode) was used in order to increase the selectivity of the electrophoretic method, meanwhile vancomycin was not present at the detector path during the detection of metal-EDTA complexes. The vancomycin concentration, phosphate concentration and pH of the buffer strongly influenced mobility, resolution and selectivity of the studied analytes. Under the optimal condition, the relative standard deviations (n=5) of the migration time and the peak area were less than 3.14% and 7.35%, respectively. Application of the Z-shape cell capillary electrophoresis method with UV detection and vancomycin loading led to the reliable determination of these metal ions in tap water and the recoveries were 97%-101%. The detection limits based on a signal to noise ratio of 3 : 1 were found in the range of 2-10 μg·L^-1.  相似文献   

2.
Mudasir  Yoshioka N  Inoue H 《Talanta》1997,44(7):1195-1202
A reversed phase ion-paired chromatographic method that can be used to determine trace amounts of iron (II,III), nickel (II) and copper (II) was developed and applied to the determination of iron (II) and iron (III) levels in natural water. The separation of these metal ions as their 4,7-diphenyl-1,10-phenanthroline (bathophenanthroline) chelates on an Inertsil ODS column was investigated by using acetonitrile-water (80/20, v/v) containing 0.06 M perchloric acid as mobile phase and diode array spectrophotometric detection at 250-650 nm. Chromatographic parameters such as composition of mobile phase and concentration of perchloric acid in mobile phase were optimized. The calibration graphs of iron (II), nickel (II) and copper (II) ions were linear (r > 0.991) in the concentration range 0-0.5, 0-2.0 and 0-4.0 mug ml(-1), respectively. The detection limit of iron (II), nickel (II) and copper (II) were 2.67, 5.42 and 18.2 ng ml(-1) with relative standard deviation (n = 5) of 3.11, 5.81 and 7.16% at a concentration level of 10 ng ml(-1) for iron (II) and nickel (II) and 25 ng ml(-1) for copper (II), respectively. The proposed method was applied to the determination of iron(II) and iron(III) in tap water and sea water samples without any interference from other common metal ions.  相似文献   

3.
A simple, rapid, accurate, and selective complexometric method is proposed for the determination of palladium(II). Palladium(II), with associated diverse metal ions, is first complexed by adding a known excess of EDTA, and the uncomplexed EDTA is back titrated with lead nitrate solution in acetic acid-sodium acetate buffer (pH 5.0–6.0) until the end-point. Thiosemicarbazide (1%) solution in water is added to displace EDTA from the Pd-EDTA complex. The released EDTA is then titrated with the lead nitrate solution. Reproducible and accurate results are obtained in the concentration range of 1–10 mg of palladium with a relative error of less than 0.4% and a standard deviation of less than 0.02. The interference of many commonly associated metal ions was also studied. Advantages of this method over other complexometric methods of palladium determination are high-lighted.  相似文献   

4.
Goswami A  Singh AK 《Talanta》2002,58(4):669-678
A new chelating matrix has been prepared by immobilizing 1,8-dihydroxyanthraquinone (DHAQ) on silica gel modified with (3-aminopropyl)triethoxysilane. After characterizing the matrix with thermogravimetric analysis (TGA), cross polarization magic angle spinning (CPMAS) NMR and diffuse reflectance infrared fourier transformation (DRIFT) spectroscopy, it has been used to preconcentrate Pb(II), Cd(II) and Zn(II) prior to their determination by flame atomic absorption spectrometry. The optimum pH ranges for quantitative sorption are 6.0-7.5, 7.0-8.0 and 6.0-8.0 for Pb, Zn, and Cd, respectively. All the metal ions can be desorbed with 2 mol l(-1) HCl/HNO(3). The sorption capacity of the matrix has been found to be 76.0, 180.0 and 70.2 mumol g(-1) for Pb, Zn and Cd, respectively, with the preconcentration factor of approximately 200. The limits upto which electrolytes NaNO(3), NaCl, NaBr, Na(2)SO(4), Na(3)PO(4) sodium citrate, EDTA, glycine and humic acid and cations Ca(II), Mg(II), Cu(II), Co(II), Ni(II), Mn(II) Al(III), Cr(III) and Fe(III) can co-exist with the metal ions during their sorption without any adverse effect are reported. The lowest concentration of metal ions for quantitative recovery is 5.0 ng ml(-1) The simultaneous enrichment and determination of all the metals is possible if total load of metal ions is less than sorption capacity. The flame AAS was used to determine these metal ions in underground, tap and river water samples (relative standard deviation (R.S.D.)相似文献   

5.
A simple, rapid and accurate complexometric method for the determination of palladium(II) is proposed, based on the selective masking property of thioacetamide towards palladium(II). In the presence of diverse metal ions, palladium(II) is complexed with excess of EDTA and the surplus EDTA is back titrated at pH 5-5.5 (acetic acid-sodium acetate buffer) with standard lead nitrate solution using xylenol orange as indicator. An excess of a 0.5% aqueous solution of thioacetamide is then added to displace EDTA from Pd(II)-EDTA complex. The released EDTA is titrated with the same standard lead nitrate solution as before. Reproducible and accurate results are obtained in the concentration range 0.5 mg - 17.80 mg of palladium with relative error of +/- 0.16% and coefficient of variation not exceeding 0.26%. The effect of diverse ions is studied. The method is used for the determination of palladium in its complexes, catalysts and synthetic alloy mixtures.  相似文献   

6.
Two novel azocalix[4]pyrrole Amberlite XAD-2 polymeric chelating resins were synthesized by covalently linking diazotized Amberlite XAD-2 with calix[4]pyrrole macrocycles. The chelating resins were used for extraction, preconcentration and sequential separation of metal ions such as Cu(II), Zn(II) and Cd(II) by column chromatography prior to their determination by UV/vis spectrophotometry or flame atomic absorption spectrophotometry (FAAS) or inductively coupled plasma atomic emission spectroscopy (ICP-AES). Various parameters such as effect of pH on absorption, concentration of eluting agents, flow rate, total sorption capacity, exchange kinetics, preconcentration factor, distribution coefficient, breakthrough capacity and resin stability, were optimized for effective separation and preconcentration. The resin showed good ability for the separation of metal ions from binary and ternary mixture on the basis of pH of absorption and concentration of eluting agents. The newly synthesized resins showed good potential for trace enrichment of Cu(II), Zn(II) and Cd(II) metal ions, especially for Cu(II), as compared to the earlier reported resins. The synthesized resins were recycled at least 8-10 times without much affecting column sorption capacity. The presented method was successfully applied for determination of Cu(II), Zn(II) and Cd(II) in natural and ground water samples.  相似文献   

7.
The potential removal and preconcentration of lead(II), cadmium(II), and chromium(III) ions from wastewaters were investigated and explored. Magnetite nanoparticles were chemically modified with p-nitro aniline. The aniline-coated magnetite nanoparticles (ANMNPs) were fully characterized by FT-IR, XRD, SEM, and TEM measurements. Batch studies were performed to address various experimental parameters for the removal and determination of these ions. ANMNPs showed high tendency to investigated metal ions, in this order: Cr(III) > Cd(II) > Pb(II), owing to the strong contribution of surface loaded aniline. The potential applications of ANMNPs adsorbent for removal and preconcentration of Pb(II), Cr(III), and Cd(II) from wastewaters as well as drinking tap water samples were successfully accomplished giving recovery values of (98–101 %), without any noticeable interference of the wastewater or drinking tap water matrices.  相似文献   

8.
Mahmoud ME  Gohar GA 《Talanta》2000,51(1):77-87
Dithioacetal derivatives with different para-substituents, XH, CH(3), OCH(3), Cl and NO(2) were synthesized and chemically immobilized on the surface of silica gel for the formation of five newly synthesized silica gel phases (I-V). Characterization of the silica gel surface modification by the organic compounds was accomplished by both the surface coverage determination as well as the infrared spectroscopic analysis. The metal sorption properties of the silica gel phases were studied to evaluate their performance toward metal-uptake, extraction and selective extraction processes of different metal ions from aqueous solutions based on examination of the various controlling factors. The studied and evaluated factors are the pH effect of metal ion solution on the metal capacity values (mmol g(-1)), equilibration shaking time on the percent extraction as well as the structure and substituent (X) effects on the determined mmol g(-1) values. The results of these studies revealed a general rule of excellent affinity of these silica gel phases-immobilized-dithioacetal derivatives for selective extraction of mercury(II) in presence of other interfering metal ions giving rise to a range of 94-100% extraction of the spiked mercury(II) in the metal ions mixture. The potential application of the newly synthesized silica gel phases (I-V) for selective extraction of mercury(II) from two different natural water samples, namely sea and drinking tap water, spiked with 1.0 and 10.0 ng ml(-1) mercury(II) were also studied by column technique followed by cold vapour atomic absorption analysis of the unretained mercury(II). The results indicated a good percent extraction and removal (90-100+/-3%) of the spiked mercury(II) by all the five silica gel phases. In addition, insignificant contribution by the matrix effect on the processes of selective solid phase extraction of mercury(II) from natural water samples was also evident.  相似文献   

9.
A simple and reliable solid-phase extraction (SPE) method has been developed to synthesise two new sorbents: 6-propyl-2-thiouracil and 5,6-diamino-2-thiouracil physically loaded onto alumina surface, phases I and II, respectively. The synthesis of these new phases has been confirmed by IR-spectroscopy. The surface concentrations of the organic moieties were determined to be 0.182 and 0.562 mmol g?1 for phases I and II, respectively. The evaluation of the selectivity and metal uptake properties incorporated in these two alumina phases were also studied and discussed for 10 different metal ions: Ca(II), Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Cd(II), Hg(II), Pb(II) and Ag(I) under different controlling factors. The data obtained clearly indicated that the new SP-extractors have the highest affinity for retention of Hg(II) ions. Selective separation of Hg(II) from Ag(I) as one of the most interfering ion, in addition to the other eight coexisting metal ions under investigation, was achieved successfully using the new sorbents at pH = 9.0 under static conditions. Therefore, Hg(II) exhibits major retention percentage (100.0%) using phase I or II. However, Ag(I) exhibits minor retention percentage equal to 1.33% using phase I and 0.67% using phase II. On the other hand, the retention percentage of the other eight metal ions ranged (0.0–3.08%) using phase I and (0.0–1.54%) using phase II at the same pH. The new phases were applied for separation and determination of trace amounts of Hg(II) and Ag(I) spiked natural water samples using cold vapour atomic absorption spectroscopy and atomic absorption spectroscopy with no matrix interference. The high recovery values of Hg(II) and Ag(I) obtained using phases I and II were ranged 98.9 ± 0.1–99.2 ± 0.05% along with a good precision (RSD% 0.01–0.502%, N = 3) demonstrate the accuracy and validity of the new sorbents for separation and determination of Hg(II) and Ag(I).  相似文献   

10.
We have developed a fast method for sensitive extraction and determination of the metal ions silver(I), gold(III), copper(II) and palladium(II). Fe3O4 magnetic nanoparticles were modified with polythiophene and used for extraction the metal ions without a chelating agent. Following extraction, the ions were determined by flow injection inductively coupled plasma optical emission spectrometry. The influence of sample pH, type and volume of eluent, amount of adsorbent, sample volume and time of adsorption and desorption were optimized. Under the optimum conditions, the calibration plots are linear in the 0.75 to 100 μg L?1 concentration range (R2?>?0.998), limits of detection in the range from 0.2 to 2.0 μg L?1, and enhancement factors in the range from 70 to 129. Precisions, expressed as relative standard deviations, are lower than 4.2 %. The applicability of the method was demonstrated by the successful analysis of tap water, mineral water, and river water.
Figure
In the present work, polythiophene-coated Fe3O4 nanoparticles have been successfully synthesized and were applied as adsorbent for magnetic solid-phase extraction of some precious metal ions.  相似文献   

11.
Poly(p-chloromethylstyrene-ethyleneglycoldimethacrylate) polymeric microbeads, poly(p-CMS-EGDMA), were synthesized and 1,5,9,13-tetrathiacyclohexadecane-3,11-diol (S4HD) was attached chemically onto the polymeric microbeads. Characterization of all microbeads was done by Fourier transform-infrared spectrometry (FT-IR) and elemental analyzer. The amount of attached 1,5,9,13-tetrathiacyclohexadecane-3,11-diol to the polymer was found to be 2.23 mmol g−1 polymers. The ligand attached microbeads, poly(p-CMS-EGDMA-S4HD), were used to examine the adsorption capacity of Pb(II), Cd(II), Hg(II) and Cr(II) ions for recovery, pre-concentration and the matrix elimination by changing the pH and the initial metal ion concentrations and also adsorption kinetics of the studied metal ions was determined. Pre-concentration factors for the studied toxic metal ions were found to be more than 500-fold and recovery was between 92 and 106%. In the drinking, lake, tap and sea-water samples from water lands, ultra-trace toxic metal ion concentrations were determined easily by using ligand modified microbeads after pre-concentration because of the high pre-concentration factor and easily matrix elimination using ligand modified microbeads. Reference sea-water material was used for the validation of the method and it was found that recovery, pre-concentration and the matrix elimination were performed perfectly. For the desorption of the toxic metal ions, 3 M HCl containing 0.8 M thiourea was used and desorption ratio was obtained more than 96%.  相似文献   

12.
Soylak M  Divrikli U  Elci L  Dogan M 《Talanta》2002,56(3):565-570
A method for the preconcentration and determination of Cr(III), Co(II), Cu(II), Fe(III) and Pb(II) ions by atomic absorption spectrometry has been described. The method was based the collection of metal-calmagite complexes on a soluble cellulose nitrate membrane filter. The detection of the solution was obtained by flame atomic absorption spectrometry (FAAS) after completely dissolving the membrane with 0.5 ml of nitric acid at 80 degrees C. The metal ions were recovered quantitatively at pH 8. Various factors which affect the collection and determination of metal ions such as, type and size of the membrane filter, solvent for dissolution of the species retained on the filter were investigated. The detection limits were varying 0.06 mug l(-1) for Cu to 2.5 mug l(-1) for Cr. An application of the proposed method for analyte ions in mineral and tap water samples was also described with satisfactory results (recoveries >95%, relative standard deviations <10%).  相似文献   

13.
Silica gel was firstly functionalized with aminopropyltrimethoxysilane obtaining the aminopropylsilica gel (APSG). The APSG was reacted subsequently with curcumin yielding curcumin-bonded silica gel (curcumin-APSG). This new bonded silica gel was used for separation, pre-concentration and determination of Cu(II), Fe(III), Zn(II) in biological and natural water samples by inductively coupled plasma optical emission spectrometry (ICP-OES). Experimental conditions for effective adsorption of trace levels of metal ions were optimized with respect to different experimental parameters using batch and column procedures in detail. The optimum pH value for the separation of metal ions simultaneously on the newly sorbent was 4.0. Complete elution of the adsorbed metal ions from the sorbent surface was carried out using 2.0 mL of 0.1 mol L− 1 of HCl. Common coexisting ions did not interfere with the separation and determination at pH 4.0. The maximum static adsorption capacity of the sorbent at optimum conditions was found to be 0.63, 0.46 and 0.37 mmol g− 1 for Cu(II), Fe(III) and Zn(II) respectively. The time for 95% sorption for Cu(II) Fe(III) and Zn(II) was less than 2 min. The detection limits of the method defined by IUPAC was found to be 0.12, 0.15 and 0.40 ng mL− 1 for Cu(II), Fe(III) and Zn(II), respectively. The relative standard deviation (RSD) of the method under optimum conditions was lower 3.0% (n = 5). The procedure was validated by analyzing the certified reference river sediment material (GBW 08301, China), the results obtained were in good agreement with standard values. This sorbent was successfully employed in the separation and pre-concentration of trace Cu(II), Fe(III) and Zn(II) from the biological and natural water samples yielding 75-fold concentration factor.  相似文献   

14.
The bismuth‐coated electrode is known to be prone to errors caused by copper(II). This study investigates copper(II) interference at bismuth film electrode for the detection of lead(II) and cadmium(II). It was conducted using glassy carbon electrode, while the bismuth film was plated in situ simultaneously with the target metal ions at ? 1200 mV. Copper(II) presented in solution significantly reduced the sensitivity of the electrode, for example there was an approximately 70 % and 90 % decrease in peak signals for lead(II) and cadmium(II), respectively, at a 10‐fold molar excess of copper(II). The decrease in sensitivity was ascribed to the competition between copper and bismuth or the metal ions for surface active sites. Scanning electron microscopy (SEM) and energy dispersive X‐ray (EDX) analysis suggested a large decrease in the amount of bismuth nanoparticles formed on the electrode surface in the presence of copper(II) occurred, validating the competition between copper and bismuth ions for surface active sites. Recovery of the stripping signal of lead(II) and cadmium(II) was obtained by adding ferrocyanide ion to the solution. Finally, the proposed method was successfully applied to determine lead(II) and cadmium(II) in water samples and the method was validated by ICP‐MS technique.  相似文献   

15.
The cloud point extraction behavior of Sn(II) and Sn(IV) using alpha-polyoxometalate and mixed surfactants solution was investigated. The mixture of a nonionic surfactant (Triton X-100) and a cationic surfactant (CTAB) was utilized as a suitable micellar medium for preconcentration and extraction of tin complexes. Sn(II) in the presence of Sn(IV) was extracted with alpha-polyoxometalate, 0.3% (w/v) Triton X-100 and 3.5x10(-5) mol L(-1) CTAB at pH 1.2. Whereas the pH value of 3.7 were used for the individual determination of Sn(II) and Sn(IV) and also for total tin determination at the same conditions. Enrichment factors of 100 were obtained for the preconcentration of both metal ions. Under the optimal conditions, linearity was obeyed in the ranges of 55-670 microg L(-1) of Sn(II) and 46-750 microg L(-1) of Sn(IV) ion concentration. The detection limit of the method was also found to be 12.6 microg L(-1) for Sn(IV) and 8.4 microg L(-1) for Sn(II). The relative standard deviation of seven replicate determination of 100 microg L(-1) both metal ions were obtained about 2.4%. The diverse ion effect of some anions and cations on the extraction efficiency of target ions were tested. Finally, the optimized conditions developed were successfully utilized for the determination of each metal ion in various alloy, juice fruit, tape and waste water samples with satisfactory results.  相似文献   

16.
Lucifer yellow CH is shown to be a highly selective fluorescent reagent for the determination of Cu(III) in the microg L(-1) concentration range. The fluorophore is statically quenched by Cu(II); the carbohydrazide group was assigned as the complexing part of the dye molecule. A total range of Cu(II) determination from 0.06 mg L(-1) (1 micromol L(-1)) to 6.3 mg L(-2) (100 micromol L(-1)) with a limit of detection of 0.019 mg L(-1) (0.3 micromol L(-1)) was obtained, along with surprisingly high selectivity. There was no interference from alkaline and earth alkaline metal ions. The cross sensitivity to heavy metal ions was evaluated by the separate solution method and by competitive binding experiments. Calibration plots are shown for Cu(II) determination at different pH and the dissociation constant was determined. The application of the reagent was demonstrated by the determination of the Cu(II) content of tap water samples.  相似文献   

17.
Highly sensitive and interference-free sensitized spectrophotometric method for the determination of Ni(II) ions is described. The method is based on the reaction between Ni(II) ion and benzyl dioxime in micellar media in the presence of sodium dodecyl sulfate (SDS). The absorbance is linear from 0.1 up to 25.0 microg mL-1 in aqueous solution with repeatability (RSD) of 1.0% at a concentration of 1 microg mL-1 and a detection limit of 0.12 ng mL-1 and molar absorption coefficient of 68,600L mol-1 cm-1. The influence of reaction variables including type and amount of surfactant, pH, and amount of ligand and complexation time and the effect of interfering ions are investigated. The proposed procedure was applied to the determination of trace amounts of Ni(II) ion in tap water, river water, chocolate and vegetable without separation or organic solvent extraction.  相似文献   

18.
Mahmoud ME 《Talanta》1997,45(2):309-315
The immobilization of silica gel surface with Eriochrome black-T indicator (ERT) for the formation of silica-ERT phase is described. The surface coverage of silica gel, based on carbon and nitrogen analysis of the modified silica gel phase, is 0.38 mmol g(-1). The stability towards hydrolysis of silica-ERT phase in different buffer solutions (pH 1-10) is studied and evaluated. The applicability of silica-ERT as a solid phase extractor for Zn(II), Mg(II) and Ca(II) is studied by the batch equilibrium technique and found to show an order similar to the formation constant values of these three metal ions with the indicator. The selectivity of silica-ERT phase towards the extraction of a certain metal ion from a mixture containing only two metal ions is studied by the batch equilibrium technique and exhibited good discrimination orders for Zn(II) and Mg(II) in presence of Ca(II). The results of the column separation and preconcentration studies are consistent with the selectivity behaviour of silica-ERT phase, thus affording reasonable separation of the three studied metal ions.  相似文献   

19.
A chelating matrix prepared by immobilizing 1,8-dihydroxyanthraquinone on silica gel modified with 3-aminopropyltriethoxysilane has been characterized by use of cross-polarization magic angle spinning (CPMAS) NMR, diffuse reflectance infrared Fourier transformation (DRIFT) spectroscopy, and thermogravimetric analysis and used to preconcentrate Fe(III), Co(II), Ni(II), and Cu(II) before their determination by flame atomic absorption spectrometry. The optimum pH ranges for quantitative sorption are 6.5-8.0, 6.0-7.0, 6.0-8.0, and 7.0-8.5 for Cu, Fe, Co, and Ni, respectively. All the metal ions can be desorbed with 2 mol L(-1) HCl or HNO3. The sorption capacity ( micromol g(-1) matrix) and preconcentration factor were 226.6, 250; 365.6, 300; 101.8, 150; and 109.0, 250 for Cu, Fe, Co, and Ni, respectively. The lowest concentration for quantitative recovery was 4.0, 3.3, 6.6, and 4.0 ng mL(-1), respectively for the four metal ions. The limits up to which electrolytes NaNO3, NaCl, NaBr, Na2SO4, and Na3PO4 and cations Ca(II) and Mg(II) can coexist with the four metal ions during their sorption without adverse effect are reported. The simultaneous enrichment and determination of all the four metals is possible if the total load of metal ions is less than the sorption capacity. Flame AAS was used to determine the metal ions in underground, tap, and river water samples (RSD相似文献   

20.
The performances of a PVA/PEI complexing membrane for the removal of Hg(II) from aqueous solutions were investigated by performing sorption and filtration experiments. This membrane, that was previously shown to ensure efficient sorption of the heavy metal ions Pb(II), Cd(II) and Cu(II) at pH 5, presented a higher affinity for Hg(II) at pH 2.5. The sorption equilibrium was satisfactorily represented by the Langmuir model. In view of possible application to the treatment of industrial wastewaters, the effects of parameters such as pH, temperature, water hardness, and the presence of complexing chloride anions were investigated. The effect of increasing temperature was not straightforward: the complexation equilibrium constant decreased, but the mass of mercury sorbed increased, probably due to the higher mobility of the polymer chains that made internal sites available for complexing mercury. The maximum retention capacity of the membrane was 311 mg Hg g−1. Also, operating at large calcium or chloride concentrations was not detrimental to the membrane performances. For regeneration of the membrane, a 0.05 M solution of EDTA is recommended on the basis of limited performance loss. When used in the filtration mode, the elimination ratio of Hg(II) was close to 99%.  相似文献   

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