A micro-flow injection sorbent extraction preconcentration system was combined with a graphite furnace atomic absorption spectrometry that formed an integrated system for the determination of trace amounts of elements...A micro-flow injection sorbent extraction preconcentration system was combined with a graphite furnace atomic absorption spectrometry that formed an integrated system for the determination of trace amounts of elements. The analytical performances of the prospsed method for determining Cd, Cu and Mn were studied. The analytes were preconcentrated with a thiol resin(Type 190, produced by Nankai University, China) whose active group is -SH. The elements to be determined were preconcentrated onto the column for 60 s and then rinsed with deionized water and eluted with 30 μL of 1 mol/L HCl. The graphite furnace atomic absorption spectrometry(GFAAS) determination of the concentrated analyte was carried out in parallel with the next preconcentration cycle. Enrichment factors 41, 22 and 20 and detection limits(3 σ , n =10) 0.36, 3.8 and 7.0 ng/L for Cd, Cu and Mn, respectively, along with a sampling frequency of 20 h -1 , were obtained with a 60 s loading time at a sample flow rate of 3.5 mL/min. The analytical results for a number of water samples show that the flow-injection semi-online column preconcentration can not only eliminate the effect of some concomitant elements, such as Li, Na, K, Ca and Mg, on the determination of the analyte, but also enhance the sensitivity.展开更多
A rapid and sensitive on-line preconcentration method for spectrophotometric determination of chromium (VI) in nature water is described. Preconcentration and determination are based on (i) the quantitative and fast a...A rapid and sensitive on-line preconcentration method for spectrophotometric determination of chromium (VI) in nature water is described. Preconcentration and determination are based on (i) the quantitative and fast adsorption of chromium (VI) on the high surface area nanometer-size TiO2 (anatase) powders, which prepared by a sol-gel method from hydrolysis of TiCI4 and (ii) the quantitative and reproducible elution of Cr (VI) by 2. 0 mol. L-1 HCI. A mini-column system for preconcentration is developed, Cr(VI)on the mini-column is eluted and merged with a stream water and DPCB (1, 5-diphenylcarbazide ) as the chromogenic reagent. The Proposed system permits throughputs of 6 sample h--l (0. 001 μg mL-1 Cr(VI) ) or 20 sample h-1 (0. 1 μg mL-1Cr (VI) . The preconcentration factor is 55. The detection limit is 0. 8 ng·mL-1 Cr(VI). The reproducibility is satisfactory with a relative standard deviation of less than 3. 35% (0. Of μg’mL-1Cr (VI), n = 5).展开更多
A new method is proposed for the preconcentration of vanadium(Ⅴ) with crosslinked chitosan (CCTS) and determination by graphite furnace atomic absorption spectrometry (GFAAS). The adsorption rate of vanadium(Ⅴ) by C...A new method is proposed for the preconcentration of vanadium(Ⅴ) with crosslinked chitosan (CCTS) and determination by graphite furnace atomic absorption spectrometry (GFAAS). The adsorption rate of vanadium(Ⅴ) by CCTS was 97% at pH 4.0, and vanadium(Ⅴ) was eluted from crosslinked chitosan with 2 mL 2.0 mol·L -1 chlorhydric acid and determined by GFAAS. The detection limit (3σ,n=7) for vanadium(Ⅴ) was 4.8×1 0 -12g and the relative standard deviation (R.S.D) at concentration level of 2.6 μg·L -1 is less than 3.6%. The method shows a good selectivity and high sensitivity, and it was applied to determination of vanadium(Ⅴ) in oyster and water samples. The analytic recoveries are (97±5)%.展开更多
2-(pyridine-2-yl)-N-p-chlorohydrazinecarbothioamide (HCPTS) was synthesized, characterized and successfully applied for the preconcentration of Cu(II), Ni(II), Zn(II), Cd(II), Co(II), Pb(II), Fe(II), and Hg(II) in wat...2-(pyridine-2-yl)-N-p-chlorohydrazinecarbothioamide (HCPTS) was synthesized, characterized and successfully applied for the preconcentration of Cu(II), Ni(II), Zn(II), Cd(II), Co(II), Pb(II), Fe(II), and Hg(II) in water, blood, and urine samples prior to graphite furnace atomic absorption determination (GFAAS);Hg was determined by cold vapor technique. Under the optimum experimental conditions (i.e. pH = 8, 10–4 M of HCPTS, 0.05% w/v of Triton X-114), calibration graphs were linear in the range of 0.02 to 200 ng?mL–1 for Co(II), Cd(II), Pb(II) and Ni(II);0.03 to 200 ng?mL–1 for Cu(II);0.07 to 200 ng?mL–1 for Fe(II) and Zn(II) and 0.02 to 150 ng?mL–1 for Hg(II). The enrichment factors were 43, 51, 41, 46, 54, 40, 45 and 52 for Cu(II), Ni(II),Zn (II), Cd(II), Co(II), Pb(II), Fe(II), and Hg(II), respectively. The limit of detection were found to be 0.019, 0.094, 0.0514, 0.052, 0.0165, 0.047, 0.068 and 0.041 ng?mL–1 for Cu(II), Ni(II), Zn(II), Cd(II), Co(II), Pb(II), Fe(II), and Hg(II), respectively. The developed method was applied to the determination of these metal ions in water, blood and urine samples with satisfactory results.展开更多
Hydroxyquinoline 5 sulfonic acid, covalently bound to filter cellulose, was used for preconcentrating trace rare earth element(REE) ions from complex matrices and matrix separation, respectively. Multi REE ions were p...Hydroxyquinoline 5 sulfonic acid, covalently bound to filter cellulose, was used for preconcentrating trace rare earth element(REE) ions from complex matrices and matrix separation, respectively. Multi REE ions were preconcentrated on the column filled with 8 hydroxyquinoline 5 sulfonic acid cellulose filter and analysed by ICP AES after being eluted with dilute HNO 3. In the given pH range, alkali and alkaline earth metal ions can be separated as matrix elements; a high concentration factor is obtained and the eluates can be measured without interference. The usefulness of the method is shown by the control analyses of standard reference materials. [WT5FZ]展开更多
Trace copper (II) in water can be preconcentrated using silica gel modified with 1-(2-pyridylazo)-2-naphthol (PAN) and be determined spectrophotometri-cally. The conditions for the preconcentration were studied. The m...Trace copper (II) in water can be preconcentrated using silica gel modified with 1-(2-pyridylazo)-2-naphthol (PAN) and be determined spectrophotometri-cally. The conditions for the preconcentration were studied. The method was applied to both artificial and natural water samples and the results suggest that copper (II) of ppb level in water can be measured accurately after the preconcentration.展开更多
The suitability of 1-nitroso-2-naphthol(NN) as a complexing agent for on-line preconcen tration of cobalt eluted on the C18 microcolumn by means of the FI-FAAS system was tested.Various parameters affecting the comple...The suitability of 1-nitroso-2-naphthol(NN) as a complexing agent for on-line preconcen tration of cobalt eluted on the C18 microcolumn by means of the FI-FAAS system was tested.Various parameters affecting the complex formation and its elution were optimized. A 2.3 × 10-3 mol/L reagent solution and the aqueous sample solution acidified with 0. 1 % (volume fraction) nitric acid were on-line mixed (6.4 mL/ min) on a reaction coil set at (65 ±1) ℃ and flowed through the microcolumn for 30 s. The pH of the mixed solution was adjusted to 3-4 with HNO3(1 mol/L) or NaOH(1 mol/L). The adsorbed complexes in the microcolumn were eluted into the nebulizer of FAAS in 10 s with ethanol acidified with 1 % HNO3(3.0 mL/min). A good precision(1.6 % for 100 μg/L Co( Ⅱ ), n=10), a high enrichment factor 17.2, with detection limit (3σ) 3.2 μg/L, and sample throughput (90 h-1) were obtained. The method was applied to the certified reference materials(CRMs), NBS-362 and NBS-364, for the determination of cobalt and the results were in good agreement with the certified values.展开更多
Preconcentration of catecholamines by the modified monolithic silica in the capillary was investigated in this study. In order to achieve a microchip-based method for determining catecholamines in the saliva,the monol...Preconcentration of catecholamines by the modified monolithic silica in the capillary was investigated in this study. In order to achieve a microchip-based method for determining catecholamines in the saliva,the monolithic silica was fabricated in the capillary and the monolithic silica was chemically modified by on-column reaction with phenylboronate. Different modified methods were compared. The concentration conditions were optimized. This study indicates the applicability of the modified monolithic silica capillary when it was used to concentrate catecholamines.展开更多
Synthetic resin, Amberlite XAD-4 was linked covalently with the third generation supramolecule, octa-O-methoxy resorcin [4] arene through -N=N-group to form chelating resin, which has been characterized and effectivel...Synthetic resin, Amberlite XAD-4 was linked covalently with the third generation supramolecule, octa-O-methoxy resorcin [4] arene through -N=N-group to form chelating resin, which has been characterized and effectively used for the separation and preconcentration of metal ions such as Ni(II), Cu(II), Zn(II) and Cd(II). Critical parameters such as pH, flow rate, sorption capacity, breakthrough studies, distribution coefficient, preconcentration factor, concentration of eluting agents responsible for quantitative extraction of metal ions were optimized. The synthesized resin showed good binding affinity towards Ni(II), Cu(II), Zn(II) and Cd(II) under selective pH conditions. Good breakthrough capacity and fast exchange kinetics of the resin lead to effective separation of metal ions from their binary and ternary mixture by column method on the basis of pH and eluting agents. The resin could be reused for about 8 -10 cycles. The proposed method having the analytical data with the relative standard deviation (RSD) 2% and with recoveries of analytes higher than 98%, reflects upon the reproducibility and reliability of the method which has been successfully applied in the separation and determination of Ni(II), Cu(II), Zn(II) and Cd(II) ions in synthetic, natural and ground water samples.展开更多
A direct analysis method combining an iminodiacetate extraction disk (IED) with graphite furnace atomic absorption spectrometry was developed for the determination of Co, Ni, Cu, Cd, Sn, Pb, and Bi at sub-ppb levels i...A direct analysis method combining an iminodiacetate extraction disk (IED) with graphite furnace atomic absorption spectrometry was developed for the determination of Co, Ni, Cu, Cd, Sn, Pb, and Bi at sub-ppb levels in water. A 100 mL water sample was adjusted to pH 5.6 with nitric acid and a 1 mol?L–1 ammonium acetate solution, and then passed through an IED (diameter, 47 mm;effective filtering diameter, 35 mm) at a flow rate of 80 - 100 mL?min–1 to preconcentrate seven analytes. The IED was dried at 100?C for 20 min in an electric oven, and 110 - 145 small disks, each 2 mm in diameter, were punched out from the IED. A small disk was introduced into the graphite furnace and atomized according to a heating program. For Cd, Sn, Pb, and Bi measurements, Pd was used as a chemical modifier to enhance the absorbances. Calibration was performed using aqueous standard solutions. The detection limits, corresponding to three times the standard deviation (n = 5) of the blank values, were 0.092 μg·L–1 for Co, 0.12 μg·L–1 for Ni, 0.40 μg·L–1 for Cu, 0.077 μg·L–1 for Cd, 0.92 μg·L–1 for Sn, 0.61 μg·L–1 for Pb, and 0.80 μg·L–1 for Bi with an enrichment factor of 140 using a 100-mL water sample. A spike test for the seven analytes in tap water, rainwater, river water, and mineral drinking water showed quantitative recoveries (93% - 108%).展开更多
The styrene-maleic anhydride copolymer was chemically modi?ed, in the presence of formaldehyde, with 4-amino-2-hydroxybenzoic acid or 4-aminobenzoic acid giving sorbents S1 and S2, respectively. The specific sorption ...The styrene-maleic anhydride copolymer was chemically modi?ed, in the presence of formaldehyde, with 4-amino-2-hydroxybenzoic acid or 4-aminobenzoic acid giving sorbents S1 and S2, respectively. The specific sorption behaviour of S1 and S2 towards germanium(IV) was examined and optimized, the preconcentrated germanium(IV) after desorption being spectrophotometrically quantified with bis(2,3,4-trihydroxyphenylazo)benzidine in the presence of hexamethylenetetramine, phenanthroline and 2,2’-bipyridine. The dynamic sorption capacity and detection limits (3σ, n = 17) of germanium were found to be 152.2 and 127.1 mg·g–1, and 0.9 and 1.1 ng·mL–1, for S1 and S2, accordingly. The application of S1 and S2 was demonstrated for the selective preconcentration/determination of germanium in seawater and water obtained after oil pumping.展开更多
The copolymer of the maleic anhydride-styrene is modified at the presence of 4-amino-2-thiouracil and formaldehyde and the new polymeric sorbate with spatial structure is received. The received sorbate is identified b...The copolymer of the maleic anhydride-styrene is modified at the presence of 4-amino-2-thiouracil and formaldehyde and the new polymeric sorbate with spatial structure is received. The received sorbate is identified by the IR-spectroscopy method. The complete static sorption capacitance was studied (CSSC<sup>+</sup>K</sub>= 7.8 mmol/g) and the ionization constants of ionic groups in a sorbate link was defined by electrometric method. Ionization constants were determined by potentiometric titration of the sorbent (). Sorption and desorption of the received sorbent with a lead ion (II) are investigated and optimum concentration conditions are defined: рН<sub>opt.</sub> = 5, ionic force μ = 0.8 pier/l, full sorption balance 4 hours, optimum eluent 5 ml of 0.5 M HCl.展开更多
In this work, a flow injection analysis (FIA) method for the trace determination of lead, cadmium, nickel and cobalt in natural waters by formation of neutral chelates with ammonium pyrrolidine dithiocarbamate (APDC) ...In this work, a flow injection analysis (FIA) method for the trace determination of lead, cadmium, nickel and cobalt in natural waters by formation of neutral chelates with ammonium pyrrolidine dithiocarbamate (APDC) was developed. The neutral chelates formed was retained in a mini-column packed with Linde type A zeolite (LTA) and type Y Faujasite zeolite (FAU) and then eluted with methyl isobutyl ketone (MIBK) to flame atomic absorption spectrometry (EAA) for its detection. Physicochemical characterization of this zeolite was carried out by Fourier Transform infrared spectroscopy and attenuated total reflectance (FTIR and IR-ATR), scanning electron microscopy and energy dispersive X-ray microanalysis (SEM-EDX) and X-ray power diffraction (XRD). Then, a FIA configuration was used with a column preconcentration system coupled to the detection system at room temperature (22?C). The detection limit and the relative standard deviation for 5 determinations of different solutions of Pb2+, Co2+, Ni2+ and Cd2+ for FAU and LTA zeolite were calculated. The sampling frequency ranged from 18-35 h-1 and preconcentration factors from 21-250 were achieved, for a sample volume of 6 mL using 20 mg of sorbents, indicating a high retention of the analytes on the zeolites material. The recoveries obtained in natural waters samples were close to 100% for all ions metal using synthetic zeolites, confirming the applicability of the method. The isotherm models of Langmuir, Scatchard, Freundlich and Dubinin-Radushkevich were used to study the equilibrium data, indicating that successfully followed the Freundlich and Dubinin-Radushkevich (D-R) isotherms at low metal ion concentration. The Freundlich parameter n varied between 0.35-1.01, whereas D-R isotherm yields the sorption free energy E 8 kJ.mol-1 indicating psysisorption.展开更多
A flow injection preconcentration system for the flame atomic absorption spectrometric determination of hexavalent chromium has been developed. The method employs on-line preconcentration of Cr(VI) on a minicolumn pac...A flow injection preconcentration system for the flame atomic absorption spectrometric determination of hexavalent chromium has been developed. The method employs on-line preconcentration of Cr(VI) on a minicolumn packed with Cr(VI)-imprinted poly(4-vinyl pyridineco-2-hydroxyethyl methacrylate) placed into a flow injection system. Hexava-lent chromium was eluted with a small volume of diluted hydrochloric acid into the nebulizer-burner system of a flame atomic absorption spectrometer. An enrichment factor of 550 and a 3σ detection limit of 0.04 μg·L-1 along a sampling frequency of 4 h-1 at a sample flow rate of 3.5 mL·min-1. The relative standard deviation is 2.9% for 1 μg·L-1 Cr(VI) (n = 11). The flow injection system proposed has the advantage of being simpler because the use of expensive and sophisticated instruments is avoided. Ease of use, continuous process and selectivity make this method suitable for Cr(VI) determination in different environmental samples such as sea and river waters, soils and sediments.展开更多
This paper reports a simple and highly selective method for preconcentrating and separating of trace Pd(II) and Pt(IV) with silica gel bonded by aminopropyl-benzoylazo-4-(2-pyridy-lazo)-resorcinol (ABPR-SG). ABPR-SG i...This paper reports a simple and highly selective method for preconcentrating and separating of trace Pd(II) and Pt(IV) with silica gel bonded by aminopropyl-benzoylazo-4-(2-pyridy-lazo)-resorcinol (ABPR-SG). ABPR-SG is stable in solution from 6 mol/L HCl to pH 7.0 and in common organic solvents. The maximum adsorptive capacity of Pd(n) on ABPR-SG is 362 μmol/g. After preconcentration and separation by using ABPR-SG column, Pd(II) and Pt(IV) of μg/L level in artificial water samples can be measured reliably by common spedrophotometry. The maximum concentration factors of Pd(II) and Pt(IV) on ABPR-SG column are 143 and 125 respectively. The chromatographic column packed with ABPR-SG can be reused. The method is simple and efficient.展开更多
Solidified floating organic drop microextraction(SFODME)in combination with high performance liquid chromatography was used for separation/preconcentration and determination of carbamazepine(CBZ)in human plasma and ur...Solidified floating organic drop microextraction(SFODME)in combination with high performance liquid chromatography was used for separation/preconcentration and determination of carbamazepine(CBZ)in human plasma and urine samples.Parameters that affect the extraction efficiency such as the type and volume of extraction solvent,ionic strength,sodium hydroxide concentration,stirring rate,sample volume and extraction time,were investigated and optimized.Under the optimum conditions(extraction solvent,40μL of 1-undecanol;sodium hydroxide concentration,1 mol/L;temperature,50℃;stirring speed,400 r/min;sample volume,8 mL;sodium chloride concentration,3%(w/v)and extraction time,60 min)the calibration curve was found to be linear in the mass concentration range of 0.4-700.0μg/L.The limit of detection(LOD)was 0.1μg/L and the relative standard deviation(RSD)for six replicate extraction and determination of carbamazepine at 100μg/L level was found to be 4.1%.The method was successfully applied to the determination of CBZ in human plasma and urine samples.展开更多
A novel electroanalytical method. oscillographic chronopotentiometry with high and low frequency current. is presented in this paper. With this method. the sensitivity of almost all kinds of oscillographic chronopoten...A novel electroanalytical method. oscillographic chronopotentiometry with high and low frequency current. is presented in this paper. With this method. the sensitivity of almost all kinds of oscillographic chronopotentiometry can be enhanced about one order.展开更多
The liquid phase microextraction (LPME) was combined with the modified Graphite furnace atomic absorption spectrometry (GF-AAS) for determination of lead in the water and solid samples. In a preconcentration step, lea...The liquid phase microextraction (LPME) was combined with the modified Graphite furnace atomic absorption spectrometry (GF-AAS) for determination of lead in the water and solid samples. In a preconcentration step, lead was extracted from a 2 ml of its aqueous sample in the pH = 5 as lead-Pyrimidine-2-thiol cationic complex into a 4 μl drop of 1,2 dichloroethane and ammonium tetraphenylborate as counter ion immersed in the solution. In the drop, the lead-Pyrimidine-2-thiol ammonium tetraphenylborate ion associated complex was formed. After extraction, the microdrop was retracted and directly transferred into a graphite tube modified by [W.Pd.Mg] (c). Some effective parameters on extraction and complex formation, such as type and volume of organic solvent, pH, concentration of chelating agent and counter ion, extraction time, stirring rate and effect of salt were optimized. Under the optimum conditions, the enrichment factor and recovery were 525% and 94%, respectively. The calibration graph was linear in the range of 0.01 - 12 μg?L–1 with correlation coefficient of 0.9975 under the optimum conditions of the recommended procedure. The detection limit based on the 3Sb criterion was 0.0072 μg?L–1 and relative standard deviation (RSD) for ten replicate measurement of 0.1 μg?L–1 and 0.4 μg?L–1 lead was 4.5% and 3.8% respectively. The characteristic concentration was 0.0065 μg?L–1 equivalent to a characteristic mass of 26 fg. The results for determination of lead in reference materials, spiked tap water and seawater demonstrated the accuracy, recovery and applicability of the presented method.展开更多
A simple on-line sonodigestion system was successfully used for breakdown organic nickel complexes in environmental waters acidified with diluted nitric acid prior to flow injection total dissolved nickel preconcentra...A simple on-line sonodigestion system was successfully used for breakdown organic nickel complexes in environmental waters acidified with diluted nitric acid prior to flow injection total dissolved nickel preconcentration in a microcolumn containing a chelating resin (Chelite Che with iminodiacetic acid groups) and determination by flame atomic absorption spectrometry. For the determination of the dissolved labile nickel fraction, microcolumns packed with the chelating resin were loaded in-situ with the sample without sample pH modification, and once in the laboratory were inserted in the flow injection device where nickel elution-detection was carried out. The performance of the chelating resin was investigated in order to elucidate its behavior in the presence of dissolved nickel species. The results obtained reveal that the resin, at the experimental employed conditions, retained only dissolved free nickel ions and nickel bound to weak complexes (labile fraction). The figures of merit for determinations in both nickel fractions are given and the obtained values are discussed. The speciation scheme is applied to the analysis of nickel in river and seawater samples collected in Galicia (Northwest, Spain). The results of fractionation showed that Ni are mainly in the dissolved labile fraction in river water, while in seawater samples analyzed was mainly present in the organic fraction.展开更多
文摘A micro-flow injection sorbent extraction preconcentration system was combined with a graphite furnace atomic absorption spectrometry that formed an integrated system for the determination of trace amounts of elements. The analytical performances of the prospsed method for determining Cd, Cu and Mn were studied. The analytes were preconcentrated with a thiol resin(Type 190, produced by Nankai University, China) whose active group is -SH. The elements to be determined were preconcentrated onto the column for 60 s and then rinsed with deionized water and eluted with 30 μL of 1 mol/L HCl. The graphite furnace atomic absorption spectrometry(GFAAS) determination of the concentrated analyte was carried out in parallel with the next preconcentration cycle. Enrichment factors 41, 22 and 20 and detection limits(3 σ , n =10) 0.36, 3.8 and 7.0 ng/L for Cd, Cu and Mn, respectively, along with a sampling frequency of 20 h -1 , were obtained with a 60 s loading time at a sample flow rate of 3.5 mL/min. The analytical results for a number of water samples show that the flow-injection semi-online column preconcentration can not only eliminate the effect of some concomitant elements, such as Li, Na, K, Ca and Mg, on the determination of the analyte, but also enhance the sensitivity.
文摘A rapid and sensitive on-line preconcentration method for spectrophotometric determination of chromium (VI) in nature water is described. Preconcentration and determination are based on (i) the quantitative and fast adsorption of chromium (VI) on the high surface area nanometer-size TiO2 (anatase) powders, which prepared by a sol-gel method from hydrolysis of TiCI4 and (ii) the quantitative and reproducible elution of Cr (VI) by 2. 0 mol. L-1 HCI. A mini-column system for preconcentration is developed, Cr(VI)on the mini-column is eluted and merged with a stream water and DPCB (1, 5-diphenylcarbazide ) as the chromogenic reagent. The Proposed system permits throughputs of 6 sample h--l (0. 001 μg mL-1 Cr(VI) ) or 20 sample h-1 (0. 1 μg mL-1Cr (VI) . The preconcentration factor is 55. The detection limit is 0. 8 ng·mL-1 Cr(VI). The reproducibility is satisfactory with a relative standard deviation of less than 3. 35% (0. Of μg’mL-1Cr (VI), n = 5).
文摘A new method is proposed for the preconcentration of vanadium(Ⅴ) with crosslinked chitosan (CCTS) and determination by graphite furnace atomic absorption spectrometry (GFAAS). The adsorption rate of vanadium(Ⅴ) by CCTS was 97% at pH 4.0, and vanadium(Ⅴ) was eluted from crosslinked chitosan with 2 mL 2.0 mol·L -1 chlorhydric acid and determined by GFAAS. The detection limit (3σ,n=7) for vanadium(Ⅴ) was 4.8×1 0 -12g and the relative standard deviation (R.S.D) at concentration level of 2.6 μg·L -1 is less than 3.6%. The method shows a good selectivity and high sensitivity, and it was applied to determination of vanadium(Ⅴ) in oyster and water samples. The analytic recoveries are (97±5)%.
文摘2-(pyridine-2-yl)-N-p-chlorohydrazinecarbothioamide (HCPTS) was synthesized, characterized and successfully applied for the preconcentration of Cu(II), Ni(II), Zn(II), Cd(II), Co(II), Pb(II), Fe(II), and Hg(II) in water, blood, and urine samples prior to graphite furnace atomic absorption determination (GFAAS);Hg was determined by cold vapor technique. Under the optimum experimental conditions (i.e. pH = 8, 10–4 M of HCPTS, 0.05% w/v of Triton X-114), calibration graphs were linear in the range of 0.02 to 200 ng?mL–1 for Co(II), Cd(II), Pb(II) and Ni(II);0.03 to 200 ng?mL–1 for Cu(II);0.07 to 200 ng?mL–1 for Fe(II) and Zn(II) and 0.02 to 150 ng?mL–1 for Hg(II). The enrichment factors were 43, 51, 41, 46, 54, 40, 45 and 52 for Cu(II), Ni(II),Zn (II), Cd(II), Co(II), Pb(II), Fe(II), and Hg(II), respectively. The limit of detection were found to be 0.019, 0.094, 0.0514, 0.052, 0.0165, 0.047, 0.068 and 0.041 ng?mL–1 for Cu(II), Ni(II), Zn(II), Cd(II), Co(II), Pb(II), Fe(II), and Hg(II), respectively. The developed method was applied to the determination of these metal ions in water, blood and urine samples with satisfactory results.
基金Supported by the National Natural Science Foundation of China
文摘Hydroxyquinoline 5 sulfonic acid, covalently bound to filter cellulose, was used for preconcentrating trace rare earth element(REE) ions from complex matrices and matrix separation, respectively. Multi REE ions were preconcentrated on the column filled with 8 hydroxyquinoline 5 sulfonic acid cellulose filter and analysed by ICP AES after being eluted with dilute HNO 3. In the given pH range, alkali and alkaline earth metal ions can be separated as matrix elements; a high concentration factor is obtained and the eluates can be measured without interference. The usefulness of the method is shown by the control analyses of standard reference materials. [WT5FZ]
文摘Trace copper (II) in water can be preconcentrated using silica gel modified with 1-(2-pyridylazo)-2-naphthol (PAN) and be determined spectrophotometri-cally. The conditions for the preconcentration were studied. The method was applied to both artificial and natural water samples and the results suggest that copper (II) of ppb level in water can be measured accurately after the preconcentration.
基金Supported by Zhejiang Natural Science Foundation of China.
文摘The suitability of 1-nitroso-2-naphthol(NN) as a complexing agent for on-line preconcen tration of cobalt eluted on the C18 microcolumn by means of the FI-FAAS system was tested.Various parameters affecting the complex formation and its elution were optimized. A 2.3 × 10-3 mol/L reagent solution and the aqueous sample solution acidified with 0. 1 % (volume fraction) nitric acid were on-line mixed (6.4 mL/ min) on a reaction coil set at (65 ±1) ℃ and flowed through the microcolumn for 30 s. The pH of the mixed solution was adjusted to 3-4 with HNO3(1 mol/L) or NaOH(1 mol/L). The adsorbed complexes in the microcolumn were eluted into the nebulizer of FAAS in 10 s with ethanol acidified with 1 % HNO3(3.0 mL/min). A good precision(1.6 % for 100 μg/L Co( Ⅱ ), n=10), a high enrichment factor 17.2, with detection limit (3σ) 3.2 μg/L, and sample throughput (90 h-1) were obtained. The method was applied to the certified reference materials(CRMs), NBS-362 and NBS-364, for the determination of cobalt and the results were in good agreement with the certified values.
基金supported by the Fundamental Research Foundation of Xi’an Polytechnic University ( XGJ07001)
文摘Preconcentration of catecholamines by the modified monolithic silica in the capillary was investigated in this study. In order to achieve a microchip-based method for determining catecholamines in the saliva,the monolithic silica was fabricated in the capillary and the monolithic silica was chemically modified by on-column reaction with phenylboronate. Different modified methods were compared. The concentration conditions were optimized. This study indicates the applicability of the modified monolithic silica capillary when it was used to concentrate catecholamines.
文摘Synthetic resin, Amberlite XAD-4 was linked covalently with the third generation supramolecule, octa-O-methoxy resorcin [4] arene through -N=N-group to form chelating resin, which has been characterized and effectively used for the separation and preconcentration of metal ions such as Ni(II), Cu(II), Zn(II) and Cd(II). Critical parameters such as pH, flow rate, sorption capacity, breakthrough studies, distribution coefficient, preconcentration factor, concentration of eluting agents responsible for quantitative extraction of metal ions were optimized. The synthesized resin showed good binding affinity towards Ni(II), Cu(II), Zn(II) and Cd(II) under selective pH conditions. Good breakthrough capacity and fast exchange kinetics of the resin lead to effective separation of metal ions from their binary and ternary mixture by column method on the basis of pH and eluting agents. The resin could be reused for about 8 -10 cycles. The proposed method having the analytical data with the relative standard deviation (RSD) 2% and with recoveries of analytes higher than 98%, reflects upon the reproducibility and reliability of the method which has been successfully applied in the separation and determination of Ni(II), Cu(II), Zn(II) and Cd(II) ions in synthetic, natural and ground water samples.
文摘A direct analysis method combining an iminodiacetate extraction disk (IED) with graphite furnace atomic absorption spectrometry was developed for the determination of Co, Ni, Cu, Cd, Sn, Pb, and Bi at sub-ppb levels in water. A 100 mL water sample was adjusted to pH 5.6 with nitric acid and a 1 mol?L–1 ammonium acetate solution, and then passed through an IED (diameter, 47 mm;effective filtering diameter, 35 mm) at a flow rate of 80 - 100 mL?min–1 to preconcentrate seven analytes. The IED was dried at 100?C for 20 min in an electric oven, and 110 - 145 small disks, each 2 mm in diameter, were punched out from the IED. A small disk was introduced into the graphite furnace and atomized according to a heating program. For Cd, Sn, Pb, and Bi measurements, Pd was used as a chemical modifier to enhance the absorbances. Calibration was performed using aqueous standard solutions. The detection limits, corresponding to three times the standard deviation (n = 5) of the blank values, were 0.092 μg·L–1 for Co, 0.12 μg·L–1 for Ni, 0.40 μg·L–1 for Cu, 0.077 μg·L–1 for Cd, 0.92 μg·L–1 for Sn, 0.61 μg·L–1 for Pb, and 0.80 μg·L–1 for Bi with an enrichment factor of 140 using a 100-mL water sample. A spike test for the seven analytes in tap water, rainwater, river water, and mineral drinking water showed quantitative recoveries (93% - 108%).
文摘The styrene-maleic anhydride copolymer was chemically modi?ed, in the presence of formaldehyde, with 4-amino-2-hydroxybenzoic acid or 4-aminobenzoic acid giving sorbents S1 and S2, respectively. The specific sorption behaviour of S1 and S2 towards germanium(IV) was examined and optimized, the preconcentrated germanium(IV) after desorption being spectrophotometrically quantified with bis(2,3,4-trihydroxyphenylazo)benzidine in the presence of hexamethylenetetramine, phenanthroline and 2,2’-bipyridine. The dynamic sorption capacity and detection limits (3σ, n = 17) of germanium were found to be 152.2 and 127.1 mg·g–1, and 0.9 and 1.1 ng·mL–1, for S1 and S2, accordingly. The application of S1 and S2 was demonstrated for the selective preconcentration/determination of germanium in seawater and water obtained after oil pumping.
文摘The copolymer of the maleic anhydride-styrene is modified at the presence of 4-amino-2-thiouracil and formaldehyde and the new polymeric sorbate with spatial structure is received. The received sorbate is identified by the IR-spectroscopy method. The complete static sorption capacitance was studied (CSSC<sup>+</sup>K</sub>= 7.8 mmol/g) and the ionization constants of ionic groups in a sorbate link was defined by electrometric method. Ionization constants were determined by potentiometric titration of the sorbent (). Sorption and desorption of the received sorbent with a lead ion (II) are investigated and optimum concentration conditions are defined: рН<sub>opt.</sub> = 5, ionic force μ = 0.8 pier/l, full sorption balance 4 hours, optimum eluent 5 ml of 0.5 M HCl.
基金The authors are grateful to the FondoNacional de Ciencia y Tecnología(FONACIT)and Consejo de Desarrol-loCientífico,Humanístico,Tecnológico y de lasArtes(CDCHTA)for financial support,Proyects S1-97001192 and C-133105-08B respectively,Laboratorio de Análisis Químico Estructural de Materiales(LAQUEM)and La-boratorio de Cristalografía of the Universidad de Los Andes(ULA)Mérida-Venezuela.
文摘In this work, a flow injection analysis (FIA) method for the trace determination of lead, cadmium, nickel and cobalt in natural waters by formation of neutral chelates with ammonium pyrrolidine dithiocarbamate (APDC) was developed. The neutral chelates formed was retained in a mini-column packed with Linde type A zeolite (LTA) and type Y Faujasite zeolite (FAU) and then eluted with methyl isobutyl ketone (MIBK) to flame atomic absorption spectrometry (EAA) for its detection. Physicochemical characterization of this zeolite was carried out by Fourier Transform infrared spectroscopy and attenuated total reflectance (FTIR and IR-ATR), scanning electron microscopy and energy dispersive X-ray microanalysis (SEM-EDX) and X-ray power diffraction (XRD). Then, a FIA configuration was used with a column preconcentration system coupled to the detection system at room temperature (22?C). The detection limit and the relative standard deviation for 5 determinations of different solutions of Pb2+, Co2+, Ni2+ and Cd2+ for FAU and LTA zeolite were calculated. The sampling frequency ranged from 18-35 h-1 and preconcentration factors from 21-250 were achieved, for a sample volume of 6 mL using 20 mg of sorbents, indicating a high retention of the analytes on the zeolites material. The recoveries obtained in natural waters samples were close to 100% for all ions metal using synthetic zeolites, confirming the applicability of the method. The isotherm models of Langmuir, Scatchard, Freundlich and Dubinin-Radushkevich were used to study the equilibrium data, indicating that successfully followed the Freundlich and Dubinin-Radushkevich (D-R) isotherms at low metal ion concentration. The Freundlich parameter n varied between 0.35-1.01, whereas D-R isotherm yields the sorption free energy E 8 kJ.mol-1 indicating psysisorption.
基金This work has been funded by the Spain’s Ministry of Science and Innovation,within the framework of Project CTQ2009-12282.
文摘A flow injection preconcentration system for the flame atomic absorption spectrometric determination of hexavalent chromium has been developed. The method employs on-line preconcentration of Cr(VI) on a minicolumn packed with Cr(VI)-imprinted poly(4-vinyl pyridineco-2-hydroxyethyl methacrylate) placed into a flow injection system. Hexava-lent chromium was eluted with a small volume of diluted hydrochloric acid into the nebulizer-burner system of a flame atomic absorption spectrometer. An enrichment factor of 550 and a 3σ detection limit of 0.04 μg·L-1 along a sampling frequency of 4 h-1 at a sample flow rate of 3.5 mL·min-1. The relative standard deviation is 2.9% for 1 μg·L-1 Cr(VI) (n = 11). The flow injection system proposed has the advantage of being simpler because the use of expensive and sophisticated instruments is avoided. Ease of use, continuous process and selectivity make this method suitable for Cr(VI) determination in different environmental samples such as sea and river waters, soils and sediments.
基金Project (No. 2932009) supported by the Natural Science Foundation of Beijing.
文摘This paper reports a simple and highly selective method for preconcentrating and separating of trace Pd(II) and Pt(IV) with silica gel bonded by aminopropyl-benzoylazo-4-(2-pyridy-lazo)-resorcinol (ABPR-SG). ABPR-SG is stable in solution from 6 mol/L HCl to pH 7.0 and in common organic solvents. The maximum adsorptive capacity of Pd(n) on ABPR-SG is 362 μmol/g. After preconcentration and separation by using ABPR-SG column, Pd(II) and Pt(IV) of μg/L level in artificial water samples can be measured reliably by common spedrophotometry. The maximum concentration factors of Pd(II) and Pt(IV) on ABPR-SG column are 143 and 125 respectively. The chromatographic column packed with ABPR-SG can be reused. The method is simple and efficient.
文摘Solidified floating organic drop microextraction(SFODME)in combination with high performance liquid chromatography was used for separation/preconcentration and determination of carbamazepine(CBZ)in human plasma and urine samples.Parameters that affect the extraction efficiency such as the type and volume of extraction solvent,ionic strength,sodium hydroxide concentration,stirring rate,sample volume and extraction time,were investigated and optimized.Under the optimum conditions(extraction solvent,40μL of 1-undecanol;sodium hydroxide concentration,1 mol/L;temperature,50℃;stirring speed,400 r/min;sample volume,8 mL;sodium chloride concentration,3%(w/v)and extraction time,60 min)the calibration curve was found to be linear in the mass concentration range of 0.4-700.0μg/L.The limit of detection(LOD)was 0.1μg/L and the relative standard deviation(RSD)for six replicate extraction and determination of carbamazepine at 100μg/L level was found to be 4.1%.The method was successfully applied to the determination of CBZ in human plasma and urine samples.
基金The authors gratefully acknowedge the financial support from the National Natural Scicllcc Foundation of China Nat
文摘A novel electroanalytical method. oscillographic chronopotentiometry with high and low frequency current. is presented in this paper. With this method. the sensitivity of almost all kinds of oscillographic chronopotentiometry can be enhanced about one order.
文摘The liquid phase microextraction (LPME) was combined with the modified Graphite furnace atomic absorption spectrometry (GF-AAS) for determination of lead in the water and solid samples. In a preconcentration step, lead was extracted from a 2 ml of its aqueous sample in the pH = 5 as lead-Pyrimidine-2-thiol cationic complex into a 4 μl drop of 1,2 dichloroethane and ammonium tetraphenylborate as counter ion immersed in the solution. In the drop, the lead-Pyrimidine-2-thiol ammonium tetraphenylborate ion associated complex was formed. After extraction, the microdrop was retracted and directly transferred into a graphite tube modified by [W.Pd.Mg] (c). Some effective parameters on extraction and complex formation, such as type and volume of organic solvent, pH, concentration of chelating agent and counter ion, extraction time, stirring rate and effect of salt were optimized. Under the optimum conditions, the enrichment factor and recovery were 525% and 94%, respectively. The calibration graph was linear in the range of 0.01 - 12 μg?L–1 with correlation coefficient of 0.9975 under the optimum conditions of the recommended procedure. The detection limit based on the 3Sb criterion was 0.0072 μg?L–1 and relative standard deviation (RSD) for ten replicate measurement of 0.1 μg?L–1 and 0.4 μg?L–1 lead was 4.5% and 3.8% respectively. The characteristic concentration was 0.0065 μg?L–1 equivalent to a characteristic mass of 26 fg. The results for determination of lead in reference materials, spiked tap water and seawater demonstrated the accuracy, recovery and applicability of the presented method.
文摘A simple on-line sonodigestion system was successfully used for breakdown organic nickel complexes in environmental waters acidified with diluted nitric acid prior to flow injection total dissolved nickel preconcentration in a microcolumn containing a chelating resin (Chelite Che with iminodiacetic acid groups) and determination by flame atomic absorption spectrometry. For the determination of the dissolved labile nickel fraction, microcolumns packed with the chelating resin were loaded in-situ with the sample without sample pH modification, and once in the laboratory were inserted in the flow injection device where nickel elution-detection was carried out. The performance of the chelating resin was investigated in order to elucidate its behavior in the presence of dissolved nickel species. The results obtained reveal that the resin, at the experimental employed conditions, retained only dissolved free nickel ions and nickel bound to weak complexes (labile fraction). The figures of merit for determinations in both nickel fractions are given and the obtained values are discussed. The speciation scheme is applied to the analysis of nickel in river and seawater samples collected in Galicia (Northwest, Spain). The results of fractionation showed that Ni are mainly in the dissolved labile fraction in river water, while in seawater samples analyzed was mainly present in the organic fraction.
