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1.
HPLC was coupled with sequential injection (SI) for simultaneous analyses of some heavy metals, including Co(II), Ni(II), Cu(II), and Fe(II). 2-(5-Nitro-2-pyridylazo)-5-[N-propyl-N-(3-sulfopropyl)amino]phenol (nitro-PAPS) was employed as a derivatizing reagent for sensitive spectrophotometric detection by online precolumn derivatization. The SI system offers an automated handling of sample and reagent, online precolumn derivatization, and propulsion of derivatives to the HPLC injection loop. The metal-nitro-PAPS complexes were separated on a C(18)-muBondapak column (3.9x300 mm(2)). Using the proposed SI-HPLC system, determination of four metal ions by means of nitro-PAPS complexes was achieved within 13 min in which the parallel of derivatization and separation were processed at the same time. Linear calibration graphs were obtained in the ranges of 0.005-0.250 mg/L for Cu(II), 0.007-1.000 mg/L for Co(II), 0.005-0.075 mg/L for Ni(II), and 0.005-0.100 mg/L for Fe(II). The system provides means for automation with good precision and minimizing error in solution handling with the RSD of less than 6%. The detection limits obtained were 2 microg/L for Cu(II) and Co(II), and 1 microg/L for Ni(II) and Fe(II). The method was successfully applied for the determination of metal ions in various samples, including milk powder for infant, mineral supplements, local wines, and drinking water.  相似文献   

2.
Amberlite XAD-2 has been functionalized by coupling it to quinalizarin [1,2,5,8-tetrahydroxyanthraquinone] by means of an -N = N- spacer. Elemental analysis, thermogravimetric analysis, and infrared spectra were used to characterize the resulting new polymer matrix. The matrix has been used to preconcentrate Cu(II), Cd(II), Co(II), Pb(II), Zn(II), and Mn(II) before their determination by flame atomic absorption spectrometry (FAAS). UO2(II) has been preconcentrated for fluorimetric determination. The optimum pH values for maximum adsorption of the metals are between 5.0 and 7.0. All these metal ions are desorbed (recovery 91-99%) with 4 mol L(-1) HNO3. The adsorptive capacity of the resin was found to be in the range 0.94-5.28 mg metal g(-1) resin and loading half-life (t1/2) between 5.3 and 15.0 min. The effects of NaF, NaCl, NaNO3, Na2SO4, Na3PO4, Ca(II), and Mg(II) on the adsorption of these metal ions (0.2 microg mL(-1)) are reported. The lower limits of detection for these metal ions are between 1 and 15.0 microg L(-1). After enrichment on this matrix flame AAS has been used to determine these metal ions (except the uranyl ion) in river water samples (RSD < or = 6.5%); fluorimetry was used to determine uranyl ion in well water samples (RSD < or = 6.3%). Cobalt from pharmaceutical vitamin tablets was preconcentrated by use of this chelating resin and estimated by FAAS (RSD approximately 4%).  相似文献   

3.
Araujo L  Wild J  Villa N  Camargo N  Cubillan D  Prieto A 《Talanta》2008,76(1):111-115
In this work, the reactions of various copper ions with 1,3,3-trimethyl-2-[5-(1,3,3-trimethyl-1,3-dihydro-indol-2-ylidene)-penta-1,3-dienyl]-3H-indolium--more commonly known as dimethylindodicarbocyanine polymethyne dye (DIDC)--as well as the application of the results obtained for the development of a spectrophotometric method for the determination of Cu(I), Cu(II) and Cu(III) are described. Cu(I) and Cu(II) in the presence of chloride ions and DIDC reagent are extractable by a variety of organic solvents. It is important to emphasize that Cu(I) was extracted under considerably different experimental conditions than Cu(II). The optimum conditions for the extraction of the Cu ion associates with DIDC by amyl acetate and the determination of Cu(I) and Cu(II) were found to be: pH 3-5 and pH 3-6 and chloride concentrations of 0.5-0.8 mol L(-1) and 3-6 mol L(-1) for Cu(I) and Cu(II), respectively. The molar absorptivities for Cu(I) and Cu(II) are 1.8x10(5) L mol(-1) cm(-1) and 1.2x10(5) L mol(-1) cm(-1), respectively. A reaction mechanism is suggested. Cu(III) does not extract in the presence of chloride ions. However, Cu(III) is a strong oxidative agent which can cause the decolourisation of the DIDC reagent. The optimum conditions for Cu(III) determination were found to be: 2x10(-5) mol L(-1) DIDC; pH 8; water:acetone 4:1 medium. The developed procedures were tested for the determination of Cu(I), Cu(II) and Cu(III) in semiconductor samples.  相似文献   

4.
This work describes the synthesis and characterization of 2-aminothiazole-modified silica gel (SiAT), as well as its application for preconcentration (in batch and column technique) of Cu(II), Ni(II) and Zn(II) in ethanol medium. The adsorption capacities of SiAT determined for each metal ion were (mmol g(-1)): Cu(II)=1.20, Ni(II)=1.10 and Zn(II)=0.90. In addition, results obtained in flow experiments, showed a recovery of ca. 100% of the metal ions adsorbed in a column packed with 500 mg of SiAT. The eluent was 2.0 mol L(-1) HCl. The sorption-desorption of the studied metal ions made possible the development of a preconcentration method for metal ions at trace level in fuel ethanol using flame AAS for their quantification.  相似文献   

5.
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   

6.
Gholivand MB  Nozari N 《Talanta》2001,54(4):597-602
Poly(vinyl chloride) membrane electrode, that is highly selective and sensitive to Cu(II) ions, was developed by using 2,2'-dithiodianiline and dibutyl phthalate as carrier and plasticizer, respectively. The electrode exhibits good potentiometric response for Cu(II) over a wide concentration range (5.0x10(-2)-7.0x10(-7) mol l(-1)) with Nernstian slope of 30+/-1 mV per decade. The response time of the electrode is 10 s and it has been used for a period of one month and exhibits good selectivity towards Cu(2+) in comparison to alkali, alkaline earth, transition and heavy metal ions, with no interference caused by Pb(2+), Cd(2+) and Fe(+2) which are known to interfere with many other copper electrodes.  相似文献   

7.
A new highly sensitive and selective chromogenic reagent, p-carboxyphenylfluorone (p-CPF), was studied for spectrophotometric determination of trace molybdenum. In 0.36 mol L(-1)phosphoric acid medium, p-CPF reacts with molybdenum(VI) to form a 1:3 red complex, which has a sensitive absorption peak at 531 nm. Under optimal conditions, the reaction of molybdenum(VI) with p-CPF completed rapidly and absorbance remains almost constant for at least 24 h. Molybdenum(VI) obeyed Beer's law in the range 0-2.0 microg mL(-1); the apparent molar absorption coefficient, Sandell's sensitivity and the limit of detection were found to be 1.03 x 10(5) L mol(-1) cm(-1), 1.028 ng cm(-2)and 0.73 ng mL(-1) respectively; the effect of various foreign ions were examined in detail. It was found that most coexisting ions can be tolerated in considerable amounts, especially 800 mg of Mn(II), 200 mg of Mg(II), Fe(II), Co(III), Ni(II) and Cd(II), 50 mg of Ca(II) and Al(III), 25 mg of Cu(II) and Fe(III), 10 mg of Hg (II), La(III), Bi(III), Pb(II) and Zn(II) don't interfere with the determination of molybdenum(VI). The proposed method is very simple, sensitive and selective, it has been applied to determine molybdenum in vegetable and food samples with a very high precision and accuracy. Moreover, the synthesis of the reagent and the conditions of the colour reaction were also studied in detail.  相似文献   

8.
Ihara K  Hasegawa S  Naito K 《Talanta》2008,75(4):944-949
The membrane filtration was examined as an effective and selective method for collection of Al(III) ions from aqueous solutions using Alizarin Yellow R, one of a pH-indicator, as a precipitating reagent. For preparation of aqueous solutions without precipitate or turbidity, a non-ionic surfactant, Triton X-100, was used as a solubilizing reagent for insoluble materials. Three metal ions, Al(III), V(III) and Cu(II) ions, were able to be collected as yellow-orange precipitates from aqueous solutions controlled in a range of pH 4-7, pH 4-9, and pH 5.5-12, respectively, on a membrane filter by filtration under suction. Hydrogen peroxide and o-phenanthroline were found to be capable of masking V(III) and Cu(II) ions in a range of pH 5.5-8 in which Al(III) ions were collected. This membrane filtration was applied to selective separation and determination of Al(III) ions in tap water.  相似文献   

9.
A new preconcentration method was developed for the determination of trace amounts of Cu(II), Fe(III), Pb(II), Ni(II), and Cd(II) on a double-walled carbon nanotube disk. 4-(2-Thiazolylazo) resorcinol was used as a complexing reagent. The effects of parameters, including pH of the solutions, amounts of complexing reagent, eluent type, sample volume, flow rates of solutions, and matrix ions were examined for quantitative recoveries of the studied analyte ions. The retained metal ions were eluted by 2 M HNO3. The LOD values for the analytes were in the range of 0.7-4.4 microg/mL. Natural water samples and standard reference materials were analyzed by the presented method.  相似文献   

10.
Abbaspour A  Moosavi SM 《Talanta》2002,56(1):91-96
The utility of carbon paste electrode modified with DTPT (3,4-dihydro-4,4,6-trimethyl-2(1H)-pyrimidine thione) for the potentiometric determination of Cu(II) in aqueous medium is demonstrated. The electrode exhibits linear response to Cu(II) over a wide concentration range (9.77x10(-7)-7.6x10(-2)) with Nernstian slope of 30+/-2 mV per decade. It has a response time of about 45 s and can be used for a period of two months with good reproducibility. The detection limit of this electrode was 7.0x10(-7) M. The proposed electrode shows a very good selectivity for Cu(II) over a wide variety of metal ions. This chemically modified carbon paste electrode was successfully used for the determination of Cu(II) in electronics waste sample solution.  相似文献   

11.
Tewari PK  Singh AK 《Talanta》2001,53(4):823-833
A new chelating resin is prepared by coupling Amberlite XAD-2 with pyrocatechol through an azo spacer, characterized (by elemental analysis, IR and TGA) and studied for preconcentrating Cd(II), Co(II), Cu(II), Fe(III), Ni(II) and Zn(II) using flame atomic absorption spectrometry (FAAS) for metal monitoring. The sorption is quantitative in the pH range 3.0-6.5, whereas quantitative desorption occurs instantaneously with 2 M HCl or HNO(3) The sorption capacity has been found to be in the range 0.023-0.092 mmol g(-1) of resin. The loading half time (t(1/2)) is 1.4, 4.8, 1.6, 3.2, 2.3 and 1.8 min, respectively for Cd, Co, Cu, Fe, Ni and Zn. The tolerance limits of electrolytes NaCl, NaBr, NaNO(3), Na(2)SO(4) and Na(3)PO(4) in the sorption of all the six metal ions (0.2 mug ml(-1)) are reported. The Mg(II) and Ca(II) are tolerable with each of them (0.2 mug ml(-1)) up to a concentration level of 0.01-1.0 M. The enrichment factor has been found to be 200 except for Fe and Cu for which the values are 80 and 100, respectively. The lowest concentration of metal ion for quantitative recovery is 5, 10, 20, 25, 10 and 10 mug l(-1) for Cd, Co, Cu, Fe, Ni and Zn, respectively. The simultaneous determination of all these metal ions is possible and the method has been applied to determine all the six metal ions in tap and river water samples (RSD相似文献   

12.
A new Cu(II)-imprinted polymer (Cu-IIP) for preconcentration of copper by liquid-solid extraction via flow injection technique has been proposed. Cu-IIP was obtained by copolymerization of salen-Cu(II) complex with styrene and divinylbenzene using suspension polymerization technique. Granules fraction of 60-80 microm in diameter was used as a microcolumn packing. Cu(II) sorption was proved to be the most effective from solutions of pH 7, whereas similar elution effectiveness was observed when applying as eluents hydrochloric or nitric acid in the concentration range of 0.5-10% (v/v). The system exhibited good long-term stability and acid resistance. Batch sorbent capacity was found to be 0.11 mmol g(-1) of a dry polymer. Enrichment factor (EF) for 30 s loading time was 16. Preconcentration of Cu(II) and potentially interfering metal ions is strongly pH dependent. Examination of Cu(II) sorption in the presence of Pb(II), Cd(II), Zn(II) and Ag(I) showed significant influence of cadmium and zinc ions only and that was for the interferent concentrations above 0.5 mg L(-1) (Cu-IIP mass of ca. 35 mg). The interference effect was reduced with the sorbent mass increase. Fe(III) and Mn(II) ions, present in treated tap water in relatively high concentrations, did not interfere. Effective pH adjusting of the loaded solution in on-line mode, when applying diluted Clark-Lubs buffering solution, allowed accurate copper determination in tap water (compared to graphite furnace atomic absorption spectrometry, GFAAS) using standard addition or combination calibration method.  相似文献   

13.
The use of the chemically modified silica gel N-(3-propyl)-O-phenylenediamine (SiG-NPPDA) adsorbent, for the preconcentration and separation of trace heavy metals, was described. SiG-NPPDA sorbs quantitatively (90-100% recovery) trace amounts of nine heavy metals, viz., Cd(II), Zn(II), Fe(III), Cu(II), Pb(II), Mn(II), Cr(III), Co(II) and Ni(II) at pH 7-8. The sorption capacity varies from 350 to 450 micromol g(-1). Desorption was found to be quantitative with 1-2 M HNO3 or 0.05 M Na2EDTA. The distribution coefficient, Kd and the percentage concentration of the investigated metal ions on the adsorbent at equilibrium, C(M,eqm)% (Recovery, R%), were studied as a function of experimental parameters. The logarithmic values of the distribution coefficient, log Kd, ranges between 4.0 and 6.4. Some foreign ions caused little interference in the preconcentration and determination of the investigated nine metals by flame atomic absorption spectrometry (AAS). The adsorbent and its formed metal chelates were characterized by IR (absorbance and/or reflectance), potentiometric titrations and thermogravimetric analysis (TGA and DTG). The mode of chelation between the SiG-NPPDA adsorbent and the investigated metal ions is proposed to be due to the reaction of the investigated metal ions with the two nitrogen atoms of the SiG-NPPDA adsorbent. The present adsorbent coupled with flame AAS has been used to enrich and determine the nine metal ions in natural aqueous systems and in certified reference materials (RSD < or = 5%). The copper, iron, manganese and zinc present in some pharmaceutical vitamin samples were also preconcentrated on SiG-NPPDA adsorbent and determined by flame AAS (RSD < or = 4.2%). Nanogram concentrations (0.07-0.14 ng ml(-1)) of Cd(II), Zn(II), Fe(III), Pb(II), Cr(III), Mn(II), Cu(II), Co(II) and Ni(II) can be determined reliably with a preconcentration factor of 100.  相似文献   

14.
Sugrue E  Nesterenko P  Paull B 《The Analyst》2003,128(5):417-420
Iminodiacetic acid has been covalently bonded to a bare silica monolith to produce the first reported high-performance monolithic chelating ion exchange column. Using the new column, separation and determination of traces of alkaline earth metal ions (low ppm) in high ionic strength samples (up to 2 M NaCl and KCl brines), could be achieved in under 40 s. At an eluent flow rate of 4 mL min(-1) retention time precision was < 1.2% (n = 9) for Mg(II) and Ca(II), with detector linearity (n = 5) over the range 2-10 mg L(-1) of between R2 = 0.985 and R2 = 0.995. In 1 M KCl and NaCl brine samples, detection limits of 0.2 mg L(-1) were possible.  相似文献   

15.
Ethylenediaminetetraacetic acid (EDTA) in the background electrolyte (BGE) of capillary zone electrophoresis coupled to an electrospray ionization mass spectrometer is presented as an approach for the determination of metal ions. Significant signals for the metal-ligand complexes were observed even when EDTA was continually eluted from the capillary during the entire electrophoretic run. The signal-to-noise ratio was improved by the addition of ammonia to the sheath liquid and by using an acquisition m/z range above the m/z of EDTA. The LODs for the test metal ions (i.e. calcium(II), manganese(II), and zinc(II)) with conventional injection were around 1-2 mg/L with corrected peak areas that are linear from 8 to 100 mg/L. The presence of EDTA in the BGE was critical not only for the separation but also for sweeping via complexation as an on-line sample concentration technique. The peak height of the test metal ions was improved at least tenfold with sweeping via EDTA complexation and yielded LODs in the μg/L range.  相似文献   

16.
Bingol D  Kulcu M 《The Analyst》2011,136(19):4036-4044
A solid-phase extraction method was proposed for the preconcentration of Cu(II) in different samples in a mini-column packed with functionalized multi-walled carbon nanotubes (MWCNTs-COOH) as an effective sorbent, without using any complexing reagent, prior to its determination by flame atomic absorption spectrometry using response surface methodology. The experimental optimization step was performed by both a two-level full factorial design, with a center point, and a Box-Behnken design combined with response surface methodology. Three variables (pH, amount of Cu(II), and sample volume) were regarded as factors in the optimization. It was found that pH is the most significant factor affecting the preconcentration of Cu(II). The preconcentration factor was obtained as 100. The linear range was 1-5 mg L(-1) (R(2) = 0.999). Under the optimized experimental conditions, the detection limit (3s) of the proposed method followed by FAAS was found to be 0.27 μg L(-1). The relative standard deviation for 10 replicate measurements of 50 and 100 μg L(-1) Cu(II) was 2.39% and 0.98%, respectively. The response surface methodology was successfully applied to the determination of Cu(II) in water samples and mussel samples, and in a certified standard reference material (BCR-320R, Channel sediment).  相似文献   

17.
Two new mixed aza-thia crowns 5-aza-2,8-dithia[9]-(2,9)-1,10-phenanthrolinophane (L(4)) and 2,8-diaza-5-thia[9]-(2,9)-1,10-phenanthrolinophane (L(7)) have been synthesized and characterized. The coordination behavior of L(4) and L(7) toward the metal ions Cu(II), Zn(II), Pb(II), Cd(II), Hg(II), and Ag(I) was studied in aqueous solution by potentiometric methods, in CD3CN/D2O 4:1 (v/v) by (1)H NMR titrations and in the solid state. The data obtained were compared with those available for the coordination behavior toward the same metal ions of structurally analogous mixed donor macrocyclic ligands L(1)-L(3), L(5), L(6): all these contain a phenanthroline subunit but have only S/O/N(aromatic) donor groups in the remaining portion of the ring and are, therefore, less water-soluble than L(4) and L(7). The complexes [Cd(NO3)2(L(5))], [Pb(L(7))](ClO4)2 x 1/2MeCN, [Pb(L(4))](ClO4)2 x MeCN, and [Cu(L(7))](ClO4)2 x 3/2MeNO2 were characterized by X-ray crystallography. The efficacy of L(1)-L(7) in competitive liquid-liquid metal ion extraction of Cu(II), Zn(II), Cd(II), Pb(II), Ag(I), and Hg(II) was assessed. In the absence of Hg(II), a clear extraction selectivity for Ag(I) was observed in all systems investigated.  相似文献   

18.
A coated-wire ion-selective electrode (ISE) based on cyclam (1,4,8,11-tetraazacyclotetradecane) as a neutral carrier in a polyvinyl chloride (PVC) matrix was fabricated for the determination of Ag(I) ions. The coated-wire ISE exhibited a linear Nernstian response over the range 1 x 10(-1) to 1 x 10(-7) M with a slope of 59 +/- 2 mV per decade change and a detection limit of 5 x 10(-8) M. The ISE shows a greater preference for Ag over other cations with good precision. The electrode was selective towards Ag(I) ions in the presence of 13 different metal ions tested. The selectivity coefficients (K(ij)) were determined for Na(I), K(I), Mg(II), Ca(II), Ba(II), Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II), Pb(II) and Hg(II). The selectivity coefficients of these cations are in the range of 10(-4) to 10(-2). This ISE was used for the determination of free silver and total silver in electroplating bath solutions, additives and brighteners.  相似文献   

19.
A sorbent extraction procedure for Pb(II), Cu(II), Ni(II), and Fe(III) ions on single-walled carbon nanotube disks has been established. Analyte ions were converted to 2-(5-bromo-2-pyridylazo)-5-diethylamino-phenol chelates, then adsorbed on the disk. Adsorbed chelates were easily desorbed from the disk by using 10 mL 2 M HNO3. The various analytical parameters, including pH and reagent amounts that were effective for the recoveries of the analytes on nanotube disks, were optimized. The influence of matrix ions was also studied. The LOD values based on 3sigma were in the 0.3-4.6 microg/L range. Validation of the proposed SPE procedure was carried out by the determination of analytes in certified reference materials (TMDA-54.4 fortified lake water and HR-1 Humber River sediment). Spiking and recovery experiments for the analyte ions in real samples gave good results. Application of the procedure was illustrated by the determination of analyte contents in some animal feeds and water samples from Turkey.  相似文献   

20.
A copper(II) ion-selective electrode based on a recently synthesized 2-quinolyl-2-phenylglyoxal-2-oxime (phenylglyoxal-alpha-monoxime) has been developed. The PVC-based membrane containing phenylglyoxal-alpha-monoxime, dibutyl phthalate as plasticizer, and sodium tetraphenylborate as anion excluder and membrane modifier, was directly coated on the surface of a platinum-wire electrode. The response of the electrode was linear with a near-Nernstian slope of 28.2 mV decade(-1) within the Cu2+ ion concentration range 1x10(-6)-1x10(-1) mol x L(-1). The response time for the proposed electrode to achieve a 95% steady potential for Cu2+ concentrations ranging from 1x10(-1) to 1x10(-6) mol x L(-1) is between 10 and 50 s, and the electrode is suitable for use within the pH range of 3 to 6.5. The electrode has a detection limit of 5x10(-7) mol x L(-1) Cu2+ and its selectivity relative to several alkali, alkaline earth, transition, and heavy metal ions was good. The coated-wire electrode could be used for at least two months without a considerable alteration of its potential. Applications of the electrode for determination of copper in milk powder samples and as an indicator electrode for potentiometric titration of Cu2+ ion using EDTA are reported.  相似文献   

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