首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献,搜索用时 31 毫秒
1.
Attapulgite modified with 2-hydroxy-1-naphthaldehyde was prepared and applied to the separation, preconcentration and determination of Cu(II) in aqueous solutions by inductively coupled plasma optical emission spectrometry. Experimental conditions for effective adsorption of trace levels of Cu(II) were optimized using batch and column procedures. The optimum pH value for the separation of Cu(II) on the newly sorbent was 4.0 and complete elution of Cu(II) from the sorbent surface was carried out using 2 mL of 0.01 mol L?1 HCl. The adsorption capacity for Cu(II) was 25.13 mg g?1. The detection limits of the method defined by IUPAC were found to be 0.24 μg L?1 with enrichment factor of 150. The method has been applied to the determination of Cu(II) in certified reference materials and natural water samples with satisfactory results.  相似文献   

2.
A procedure for the pre-concentration of Cu(II), Fe(III), Mn(II) and Zn(II) is described utilising a minicolumn of natural cellulose (almond bark) modified with fungus (Rhizopus oryzae) prior to their determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). The optimum pre-concentration conditions such as pH and flow rate for the analytes have been investigated. The analytes were quantitatively retained on the column between pH 6 and 8. Elution was made with 10 mL 1 M HCl solution. Under the optimum conditions, recoveries were found as 97 ± 3%, 96 ± 3%, 98 ± 3% and 94 ± 2% for Cu(II), Fe(III), Mn(II) and Zn(II), respectively, at 95% confidence level. The detection limits obtained from preconcentration of 50 mL of blank solutions (n = 11) were 1.6, 1.8, 2.8 and 1.2 µg L?1 for Cu(II), Fe(III), Mn(II) and Zn(II), respectively. Relative standard deviations (RSD) of the recoveries for five replicate analyses were lower than 3%. The proposed method was validated by analysing certified reference materials (Peach Leaves SRM 1547 and Fish Tissue IAEA-407). Determination of the Cu(II), Fe(III), Mn(II) and Zn(II) in K?z?l?rmak River water, green beans, beans leave and tomato leaves and fish (Tinca tinca) tissue samples was performed by the proposed method.  相似文献   

3.
A new Cu(II) ion-imprinted sorbent was synthesized by a surface imprinting technique and characterized by FT-IR and SEM. Compared to the non-imprinted sorbent, the Cu(II) ion-imprinted sorbent had a higher adsorption capacity and selectivity for Cu(II). The static adsorption capacity of the Cu(II) ion-imprinted sorbent and non-imprinted sorbent for Cu(II) were 84.5 and 46.5 μmol?g?1, respectively. The best selectivity coefficient over Zn(II) or Cd(II) ion was over 12. The relative selectivity coefficients of the sorbent for Cu(II) in the presence of Zn(II) and Cd(II) were 13 and 35, respectively. Furthermore, the new sorbent possessed a fast kinetics for Cu(II) sorption from aqueous solution with saturation time of <30 min, and could be used repeatedly. The standard deviation for 11 replicate determinations of 0.5 mg?L?1 Cu(II) was 0.8%. This new Cu(II) ion-imprinted sorbent can be used as an effective solid-phase extraction material for the selective preconcentration and separation of Cu(II).  相似文献   

4.
A novel on-line flow injection solid phase extraction method for the preconcentration of trace toxic metals prior determination by flame atomic absorption spectrometry (FI-SPE-FAAS) was developed. The potential application of the hydrophobic reversed phase co-polymer sorbent StrataTM-X packed into an on-line microcolumn for the quantification of Cd(II), Pb(II), Cu(II) and Cr(VI) was demonstrated for the first time. The method was based on the on-line formation of metal complexes using sodium diethyl-dithiocarbamate (DDTC) and on the subsequent retention of them onto the sorbent material. The target analytes were completely eluted by methanol and, subsequently, directed to FAAS for quantification. All chemical and flow variables affecting the performance of the developed method were thoroughly studied and optimised. For a preconcentration time of 90 s and a sampling frequency of 28 h?1, enhancement factors of 72, 140, 185, 63 and detection limits of 0.18, 1.6, 0.20 and 1.2 μg L ?1 were obtained for Cd(II), Pb(II), Cu(II) and Cr(VI), respectively. The accuracy of the FI-SPE-FAAS method was evaluated by analysing certified reference materials as well as spiked environmental water samples. Furthermore, a comparative study of the analytical characteristics, the properties as well as the chemical structures of commercial polymeric based sorbent materials was employed. Strata-X sorbent was compared against HypersepTM SCX, Bond Elut® PlexaTM PCX, Oasis-HLBTM and NobiasTM PA-1, regarding the adaptation in on-line FI-SPE-FAAS systems for metal determination, and herein presented.  相似文献   

5.
A new solid-phase extraction method utilising polyacrylonitrile activated carbon fibres (PAN-ACFs) as adsorbent was developed for the preconcentration of trace metal ions prior to their determination by inductively coupled plasma optical emission spectrometry (ICP-OES). The PAN-ACFs oxidised with nitric acid were characterised by FT-IR, XRD, SEM and BET analysis. Then the resulting PAN-ACFs were used as solid-phase adsorbent for simultaneously determination of trace Al(III), Be(II), Bi(III), Cr(III), Cu(II), Fe(III) and Pb(II) ions in aqueous solutions. The influences of the analytical parameters on the recoveries of the studied ions were investigated. The optimum experimental conditions of the proposed method were pH: 6.0; eluent concentration and volume: 3.0 mL of 1.5 mol L?1 nitric acid; flow rates of sample and eluent solution: 1.5 mL min?1. The preconcentration factors were found to be 67 for Al(III), Bi(III); 83 for Cr(III), Cu(II), Fe(III) and 50 for Be(II), Pb(II). The precision of this method was in range of 1.5%~3.5% and the detection limit of this metal ions was between 0.06~1.50 μg L?1. The developed method was validated by the analysis of a certified reference sample and successfully applied to the determination of trace metal ions in water samples with satisfactory results.  相似文献   

6.
A silica-based inorganic sorbent was synthesized by the thermal decomposition of ammonium heptamolybdate on silica and applied for the preconcentration and simultaneous determination of Cd, Co, Cr, Cu, Fe, Mn, Ni, and Pb in river water samples using a column system with flame atomic absorption spectrometry. Attenuated total reflection-Fourier transformation infrared spectroscopy, scanning electron microscopy, and electron dispersive spectroscopy were used for sorbent characterization. The effects of pH, sample volume, eluent type, eluent concentration, eluent volume, sample flow rate, and matrix ions (Al, Bi, Ca, Mg, and Zn) on the recovery of the metals in model solutions were investigated. The adsorption capacities (µmol g?1) of SiO2-MoO3 were 88.96 (Cd), 169.69 (Co), 153.85 (Cr), 188.88 (Cu), 179.05 (Fe), 163.81 (Mn), 136.31 (Ni), and 38.61 (Pb). The detection limits of the method were 9.09, 10.82, 10.77, 49.57, 31.64, 6.40, 8.86, 19.15?µg L?1 for Cd, Co, Cr, Cu, Fe, Mn, Ni, and Pb, respectively, with a preconcentration factor of 25. The developed method was used for the determination of the target metals in real samples and the recoveries for spiked samples were found to be from 91.2% to 102.9%.  相似文献   

7.
Copper(II)‐ion imprinted silica gel (Cu‐IISG) sorbent was synthesized by surface imprinting technique and was employed as a selective solid‐phase extraction material for on‐line preconcentration and separation, then coupled with atomic absorption spectrometry (AAS) determination of Cu(II). The higher selectivity coefficient of Cu‐IISG for Cu(II) in the presence of competitive ions such as Fe(III), Ni(II) and Zn(II) was above 411, which was 35 times of NISG. The static adsorption capacity and dynamic adsorption capacity were 41.11 mg g?1 and 16.20 mg g?1, respectively. The Cu‐IISG offered a fast kinetics for the adsorption and desorption of Cu(II), which can be used for on‐line preconcentration and detection. Two certified reference materials of GBW07301a sediment and GBW07401 soil were analyzed and the determined values were in a good agreement with the certified values. The developed method was also successfully applied to the determination of trace copper in tea leaf with satisfactory results (recovery between 96.3% and 102.3%).  相似文献   

8.
This paper describes our research on the synthesis of the sorbent with chemically bonded ketoimine groups, and, furthermore, using this sorbent in the SPE technique to extract and preconcentrate trace amounts of metal ions in water samples. Surface characteristics of the sorbent were determined by elemental analysis, NMR spectra for the solid phases (29Si CP MAS NMR), and analysis of pore size distribution of the sorbent and nitrogen adsorption-desorption. The newly proposed sorbent with ketoimine groups was applied for the extraction and preconcentration of trace amounts of Cu (II), Cr (III) and Zn (II) ions from the water from a lake, post-industrial water and purified water unburdened back to the lake. The determination of the transition-metal ions was performed on an emission spectroscope with inductively coupled plasma ICP-OES. For the batch method, the optimum pH range for Cu (II) and Cr (III) extraction was equal to 5, and Zn(II)–to 8. All the metal ions can be desorbed from SPE columns with 10?mL of 0.5?mol?HNO3. The detection limits of the method were found to be 0.7?µg?L?1 for Cu (II), 0.08?µg?L?1 for Cr (III), and 0.2?µg?L?1 for Zn (II), respectively.  相似文献   

9.
In the present study, the ?5-(4-dimethylaminobenzylidene)rhodanin-modified SBA-15? was applied as stable solid sorbent for the separation and preconcentration of trace amounts of cobalt ions in aqueous solution. SBA-15 was modified by ?5-(4-dimethylaminobenzylidene)rhodanin reagent. The sorption of Co2+ ions was done onto modified sorbent in the pH range of 6.8–7.9 and desorption occurred in 5.0 mL of 3.0 mol L?1 HNO3. The results exhibit a linear dynamic range from 0.01 to 6.0 mg L?1 for cobalt. Intra-day (repeatability) and inter-day (reproducibility) for 10 replicated determination of 0.06 mg L?1 of cobalt was ±1.82% and ?±1.97%?. Detection limit was 4.2 µg L?1 (3Sb, n = 5) and preconcentration factor was 80. The effects of the experimental parameters, including the sample pH, flow rates of sample and eluent solution, eluent type and interference ions were studied for the preconcentration of Co2+. The proposed method was applied for the determination of cobalt in standard samples, water samples and agricultural products.  相似文献   

10.
Determination of copper (Cu), zinc (Zn) and manganese (Mn) micronutrients in soil samples have been studied for an efficient fertiliser application. Plant-available micronutrients of soils were extracted with DTPA extraction procedure, then differential pulse stripping voltammetry (DPSV) and square wave stripping voltammetry (SWSV) methods were performed with inexpensive and disposable pencil graphite electrode for determination of Cu(II), Zn(II) and Mn(II). Parameters such as deposition potential, deposition time, pH and concentration of the supporting electrolyte were optimised for these ions. Under optimised conditions, the limits of detection were found as 0.01 mg L?1 for Cu(II) and 0.02 mg L?1 for Zn(II) and 0.25 mg L?1 for Mn(II). Relative standard deviation (%RSD) was 6.80, 8.86 and 3.29 for Cu(II), Zn(II) and Mn(II), respectively. The experimental study was conducted using a flame atomic absorption spectroscopy. The described stripping voltammetry methods were successfully applied for the determination of Mn(II), Cu(II) and Zn(II) in soil samples.  相似文献   

11.
《Analytical letters》2012,45(3):442-452
A procedure for the determination of trace levels of Cd, Co, Cr, Fe, Mn, Ni, and Pb by flame atomic absorption spectrometry using a column preconcentration system is described in which the metals were adsorbed on pulverized banana peel, an economically and environmentally acceptable sorbent. In the optimization procedure, five variables (sample pH, mass of biosorbent, type of eluent, sample flow rate, and volume) were optimized and the capacity of the biosorbent was established. Under the optimized conditions, the detection limits of the method were 2.4, 27.0, 49.4, 31.1, 6.7, 29.6, and 46.2 µg L?1 for Cd, Co, Cr, Fe, Mn, Ni, and Pb, respectively. The precision, expressed as relative standard deviation, was less than 4% based on twelve measurements. The recoveries were 81.1% (Cd), 91.4% (Co), 87.2% (Cr), 90.1% (Fe), 88.0% (Mn), 94.1% (Ni), and 93.2% (Pb) under the optimum conditions (pH; 9, sample flow rate; 3 mL min?1, mass of biosorbent; 200 mg; eluent; 1 mol L?1 nitric acid, preconcentration factor; 10). The sorption capacity of pulverized banana peel was 15.12, 28.85, 32.70, 30.44, 30.94, 28.97, and 8.21 µmol per gram of adsorbent for Cd, Co, Cr, Fe, Mn, Ni, and Pb, respectively.  相似文献   

12.
Silica gel surface was chemically functionalized by reaction the silanol from the silica surface with 3-chloropropyltrimethoxysilane followed by reaction with Sulfasalazine. This new sorbent has been used for the preconcentration of low levels of U(VI) ions from an aqueous phase. Parameters involved in extraction efficiency such as pH, weight of the sorbent, volume of sample and eluent were optimized in batch and column methods prior to determination by spectrophotometry using arsenazo(III) reagent. The results showed that U(VI) ions can be sorbed at pH range of 5.0–6.0 in a minicolumn and quantitative recovery of U(VI) (>98.0?±?1.6%) was achieved by stripping with 2.5 mL of 0.1 mol L?1 HCl. The sorption capacity of the functionalized silica gel was 1.15 mmol g?1 of U(VI). A linear calibration graph was obtained over the concentration range of 0.02–27.0 μg mL?1 with a limit of detection of 1 μg L?1 in treatment with 1000 mL of the U(VI) solution in which the preconcentration factor was as high as 400. The method was employed to the preconcentration of U(VI) ions from spiked ground water and synthetic sea water samples.  相似文献   

13.
《Analytical letters》2012,45(11):2285-2295
Abstract

Multi‐walled carbon nanotubes (MWNTs) were used as sorbent for flow injection (FI) on‐line microcolumn preconcentration coupled with flame atomic absorption spectrometry (FAAS) for determination of trace cadmium and copper in environmental and biological samples. Effective preconcentration of trace cadmium and copper was achieved in a pH range of 4.5–6.5 and 5.0–7.5, respectively. The retained cadmium and copper were efficiently eluted with 0.5 mol L?1 HCl for on‐line FAAS determination. The MWNTs packed microcolumn exhibited fairly fast kinetics for the adsorption of cadmium and copper, permitting the use of high sample flow rates up to at least 7.8 mL min?1 for the FI on‐line microcolumn preconcentration system without loss of the retention efficiency. With a preconcentration time of 60 sec at a sample loading flow rate of 4.3 mL min?1, the enhancement factor was 24 for cadmium and 25 for copper at a sample throughput of 45 h?1. The detection limits (3σ) were 0.30 and 0.11 µg L?1 for Cd and Cu, respectively. The precision (RSD) for 11 replicate measurements was 2.1% at the 10‐µg L?1 Cd level and 2.4% at the 10‐µg L?1 Cu level. The developed method was successfully applied to the determination of trace Cd and Cu in a variety of environmental and biological samples.  相似文献   

14.
Silica gel and nanometer SiO2 modified with 4-(2-aminoethylamino)-N-(2-(2-aminoethyl amino)ethyl)butanamide (SG-AAEB and nanometer SiO2-AAEB), which were prepared based on chemical immobilization, were used as sorbents for the solid phase extraction of Cu(II), Fe(III), and Pb(II) prior to their determination by inductively coupled plasma optical emission spectrometry. Adsorption efficiencies of the two sorbents towards metal ions were investigated by batch and column procedures. For both sorbents the preconcentration conditions of analytes including effects of pH, shaking time, sample flow rate and adsorption capacity, were investigated and compared. The differences of silica gel and nanometer SiO2 in sizes and surface structures resulted in distinct chemical activity and selectivity toward metals. At pH 4, the adsorption capacity of SG-AAEB was found to be 12.2, 14.5 and 9.8 mg g?1 for Cu(II), Fe(III), and Pb(II), respectively. In comparison, nanometer SiO2-AAEB showed a high selectivity toward Pb(II) and has a much larger adsorption capacity (22.3 mg g?1). Furthermore, the application of SG-AAEB and nanometer SiO2-AAEB for simultaneous preconcentration of trace Cu(II), Fe(III), and Pb(II) from natural samples was performed with satisfactory results.  相似文献   

15.
A simple and automated method involving in-capillary derivatization and in-capillary preconcentration was developed for the simultaneous determination of metal ions by capillary zone electrophoresis. Fe(II), Zn(II), Cu(II) and Cd(II) were derivatized using 1,10-phenanthroline as the derivatizing agent. The in-capillary derivatization and in-capillary preconcentration via large volume injection were performed sequentially as follows: 60 mmol L?1 1,10-phenanthroline was first hydrodynamically injected (0.2 psi) for 2 s; metal ions were introduced by hydrodynamic injection (0.5 psi) for 60 s; 0.2 mol L?1 acetate pH 5.5 containing 20 % methanol was used as the running buffer. Four metal ions can be determined within 8 min using 16 kV. The resulting preconcentration factors were in the range 12–21. Good linearity was obtained for concentrations of 0.1–8.0 mg L?1 (r 2 > 0.990). The mean recoveries of the metal ions evaluated by fortification of wine samples were in the range 90–102 %. The limits of detection ranged from 0.05 to 0.2 mg L?1. The proposed method can be applied for directly determining metal ions in wine samples.  相似文献   

16.
In the present work, a simple procedure is presented for the extraction and determination of pre-concentrated trace amounts of palladium ions through solid phase extraction (SPE) and flame atomic absorption spectrophotometry. This process was performed using Nylon-66/5-(4-dimethylaminobenzylidene) rhodanine composite nanofibres. These nanofibres were produced under optimised conditions via two-axial electrospinning technique and characterised by scanning electron microscopy and Fourier-transform infrared spectroscopy. The effect of experimental parameters including solution pH, the type and volume of eluent and contact time was investigated in extraction and desorption process. Under the optimised conditions, good linearity in the range of 0.07–8 μg L?1 and low detection limit of 0.015 μg L?1 were obtained. High enrichment factor of 187.5 and good relative standard deviation of ±2.2% at 5 μg L?1 of palladium had been achieved. The sorbent capacity for palladium adsorption was obtained 27 mg palladium per gram of nanofibres. So, the SPE was successfully applied to pre-concentrate and determine Pd(II) ions with flame atomic absorption spectrophotometer in real samples.  相似文献   

17.
A new solid phase extraction method for the separation and preconcentration of Pd(II) was developed. As solid phase material, a new chelating polymer, poly [N-(4-bromophenyl)-2-methacrylamide-co-2-acrylamido-2-methyl-1-propanesulfonic acid - co-divinylbenzene] was synthesized. The parameters such as the effect of pH, eluent type, volume and concentration, flow rate of sample solution, sample volume and effect of interfering ions for the preconcentration of Pd(II) were investigated. The optimum pH was found to be 9. Eluent for quantitative elution was 10 mL of 1 mol L?1 HCl. The preconcentration factor of the method was 75. At optimum conditions, the recovery for Pd(II) was found to be 101?±?4%. The limit of detection (3σ) was 1.1?µg L?1. The method was applied to the determination of palladium in tap water and converter samples with satisfactory results.  相似文献   

18.
A solid phase extraction method for simultaneous preconcentration and separation of trace amounts of copper, cobalt and silver in different samples, using a column packed with modified Amberlyst®15 resin is developed. Amberlyst®15 resin was modified with 5-(4-dimethylaminobenzylidene)rhodanine and then the modified resin was used as a support material for the solid phase extraction and preconcentration of Cu(II), Co(II) and Ag(I) ions from aqueous solution in the pH range 3.5–4.5. The adsorbed metal ions on the column were quantitatively eluted with a 7% thiourea solution prepared in 2?mol?L?1 HNO3, which were detected by flame atomic absorption spectrometry. The effects of analytical parameters including pH of the solution, eluent type, flow rate of samples, eluent and matrix ions were investigated for optimization of the presented procedure. The detection limits were 2.1, 0.9 and 0.9?ng?mL?1 for Cu(II), Co(II) and Ag(I) ions, respectively based on the three times the standard deviations of the blanks. The preconcentration factor was 112.5. The calibration graphs were obtained in the ranges of 0.05 to 10.0, 0.03 to 13.0 and 0.04 to 9.0?µg?mL?1 for Cu(II), Co(II) and Ag(I) ions concentrations, respectively. Relative standard deviations (n?=?7) for Cu(II), Co(II) and Ag(I) ions were found ±2.5 %, ±0.84% and ±3.8% respectively. The method was applied to the determination of mentioned ions in well water, waste water and lettuce sample.  相似文献   

19.
《Analytical letters》2012,45(12):1987-1998
Abstract

The present work describes a novel method for cadmium preconcentration and separation with microcrystalline phenolphthalein. Phenolphthalein as an extractant modified by crystal violet was originally applied to cadmium extraction from aqueous solution. Cadmium(II) as CdI3 ? and CdI4 2? can associate with the cationic crystal violet (CV+) forming water‐insoluble ion‐association complexes (CdI3 ?) · (CV+) and (CdI4 2?) · (CV+)2, which are quantitatively adsorbed on microcrystalline phenolphthalein over the pH range from 1.0 to 6.0. All experimental parameters necessary for successful preconcentration and separation have been investigated and optimized. The study shows that common metal ions, such as Zn(II), Fe(II), Co(II), Ni(II), Mn(II), Cr(III) and Al(III), cannot interfere with cadmium extraction in this microcrystalline system by controlling acidity. The extraction can be accomplished in 15 min. The interaction between CdI3 ?and CdI4 2? and CV+ plays an important role in the extraction process. The reported method was successfully applied to the preconcentration and separation of cadmium in synthetic samples and real samples with satisfactory results. The results proved that it is an efficient and attractive technique for cadmium preconcentration and separation at trace level.  相似文献   

20.
Graphene, a novel class of carbon nanostructures, has great promise for use as sorbent materials because of its ultrahigh specific surface area. A new method using reduced graphene oxide (RGO) as sorbent was developed for the preconcentration of trace amounts of zinc (Zn) to its determination by flame atomic absorption spectrometry. Zinc could be adsorbed quantitatively on RGO in the pH range of 1–9, and then eluted completely with 0.5 mL of 0.1 mol L?1 HCl. Some effective parameters on the extraction were selected and optimized. Under optimum conditions, the calibration graph was linear in the concentration range of 0.2–15 μg L?1 with a detection limit of 0.14 μg L?1 with an enrichment factor of 100.12. The relative standard deviation for ten replicate measurements of 10 μg L?1 of Zn was 0.58 %, respectively. The proposed method was successfully applied in the analysis of rock and vegetable samples. Good spiked recoveries over the range of 99.9–100 % were obtained. This work not only proposes a useful method for sample preconcentration, but also reveals the great potential of graphene as an excellent sorbent material in analytical processes.  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号