Solid phase extraction and determination of ultra trace amounts of copper(II) using octadecyl silica membrane disks modified by 11-hydroxynaphthacene-5,12-quinone and flame atomic absorption spectrometry

A simple and selective method for rapid extraction and determination of trace amounts of copper(II) ions using octadecyl-bonded silica membrane disks modified with 11-hydroxynaphthacene-5,12-quinone and flame atomic absorption spectrometry is presented. Extraction efficiency and the influence of pH, flow rates, amount of ligand and type and least amount of stripping acid were evaluated. Maximum capacity of the membrane disks modified by 5 mg of the ligand was found to be 360 mug of Cu(2+) ion. The break through volume is larger than 2000 ml. The limit of detection of the proposed method is 0.2 ng ml(-1). The effects of various cationic interferences on the percent recovery of copper in binary mixtures were studied. The method was applied to the recovery of Cu(2+) ions from four different water samples and a synthetic sample.     

Solid phase extraction and flame atomic absorption spectroscopic determination of trace amounts of iron(III) using octadecyl silica membrane disks modified with 2-mercaptopyridine-1-oxide

A simple and selective method for rapid extraction and determination of trace amounts of iron(III) using octadecyl-bonded silica membrane disks modified with 2-mercaptopyridine-1-oxide and flame atomic absorption spectroscopy is presented. The factors influencing extraction efficiency were evaluated, including the nature of the counter anion, pH of the sample solution, amount of ligand, flow rate of the sample and type of stripping solution. The maximum capacity of the membrane disk, modified by 10 mg of the ligand, was found to be 926 ± 6 μg of iron(III). The breakthrough volume was greater than 2500 ml. Iron(III) was completely recovered (>99%) from water with a preconcentration factor of more than 166. The limit of detection of the proposed method was 0.63 ng ml^?1. The various cationic interferences had no effect on the recovery of iron(III) from the binary mixtures. The proposed method was applied to the determination of iron(III) from three different water samples.     

Determination of copper in water and plant samples by flame atomic absorption spectrometry after preconcentration on octadecyl silica membrane disks modified with a recently synthesized Schiff's base

A simple, selective, reliable, and sensitive method for the determination of trace amounts of CU2+ ions in aqueous samples is proposed. The Cu2+ ions are adsorbed quantitatively during the passage of aqueous samples through an octadecyl (C18) silica membrane disk modified by a symmetrical tetradentate Schiff base ligand, N,N'-bis(4-phenylazo salicylaldimine) 3-chloro-1,2-phenylenediamine (H2L). The retained Cu2+ ions were then stripped from the disk by elution with the minimal amount of nitric acid solution and determined by flame atomic absorption spectrometry. Various parameters, such as the effect of pH, flow rate, type and amount of eluent, and the effects of various cationic interferences on the recovery of ions were studied. The proposed method permitted large enrichment factors (about 550 and higher). The limit of detection of the method was 1.5 x 10(-2) microg/L. The use of the same disk modified with 6 mg H2L for at least 30 times showed no change in the recovery of Cu2+ ions. The accuracy of the method was confirmed by determination of Cu2+ ions in standard samples [National Institute of Environmental Studies (NIES) No. 2 and Nippon Keikinzoku Kogyo (NKK) No. 920]. The results demonstrated good agreement with certified values.     

Solid phase extraction of trace cadmium and lead in food samples using modified peanut shell prior to determination by flame atomic absorption spectrometry

Microchimica Acta - Peanut shell was chemically modified with phosphoric acid and used as a solid phase extraction material for the determination of trace amounts of Pb2+ and Cd2+ in food samples...     

Solid-phase extraction and determination of ultra trace amounts of lead,mercury and cadmium in water samples using octadecyl silica membrane disks modified with 5,5′-dithiobis(2-nitrobenzoic acid) and atomic absorption spectrometry

A simple and fast method for preconcentration and determination of ultra trace amounts of lead(II), mercury(II) and cadmium(II) in water samples is presented. Lead, mercury and cadmium adsorbed quantitatively during passage of water samples (pH?=?7, flow rate?=?20 mL min^?1) through octadecyl silica membrane disks modified with 5,5′-dithiobis(2-nitrobenzoic acid). The retained lead, mercury and cadmium are then stripped from the disk with a minimal amount of 1 M hydrochloric acid solution as eluent, and determined by atomic absorption spectrometry. The influence of flow rates of the eluent and sample solution, the amount of ligand, type and least amount of eluent, pH of sample, effect of other ions and breakthrough volume are determined. The breakthrough volume of the method is greater than 2000 mL for lead and greater than 1500 mL for mercury and cadmium, which results in an enrichment factor of 200 for lead and an enrichment factor of 150 for both mercury and cadmium. The limit of detection of the proposed method is 177, 2 and 13 ng l^?1 for lead, mercury and cadmium, respectively.     

Solid phase extraction of copper (II) by sorption on octadecyl silica membrane disk modified with a new Schiff base and determination with atomic absorption spectrometry

A simple, selective and reliable method for rapid extraction and determination of trace amounts of Cu (II) ions from aqueous samples using octadecyl-bonded silica membrane disks modified with bis-(3-methoxy salicylaldehyde)-1,6-diaminohexane and flame atomic absorption spectrometry (FAAS) is presented. Extraction efficiency, the influence of pH, flow rates, amount of ligand, and type and least amount of eluant were investigated. The linear dynamic range of the proposed method for Cu (II) ions was found in a wide concentration range of 1.0 (± 0.2)–150 (± 2) μg l^− 1. The detection limit and preconcentration factor of this method were found 30.0 (± 0.7) ng l^− 1 and 100 respectively. The reproducibility of the procedure is at the most 2.0%. The effects of various cationic interferences on the percent recovery of copper ion were studied. The method was used to the recovery of copper ion from different synthetic, alloys and biological samples.     

Solid phase extraction and flame atomic absorption spectrometric determination of trace amounts of cadmium and lead in water and biological samples using modified TiO2 nanoparticles

A solid phase extraction procedure for the separation and preconcentration of trace amounts of Cd(II) and Pb(II) using the alizarin red S modified TiO₂ nanoparticles prior to their determination by flame atomic absorption spectrometry has been proposed. The influences of some analytical parameters such as pH, flow rates of sample and eluent, type and concentration of the eluent, and interfering ions on the recovery of Cd(II) and Pb(II) by the sorbent were investigated. The analytes were quantitatively sorbed from the aqueous solution at pH 5.5 onto a microcolumn packed with the sorbent and recovered with 2.0?mL of 1.5?mol?L^?1 hydrochloric acid. Under the optimum experimental conditions, the detection limits for Cd(II) and Pb(II) were 0.11 and 0.30?ng?mL^?1 and the relative standard deviations for ten replicate measurements of 5.0 and 50.0?ng?mL^?1 of Cd(II) and Pb(II) were 2.1 and 1.9%, respectively. A sample volume of 200?mL resulted in a preconcentration factor of 100. The method was successfully applied to the determination of Cd(II) and Pb(II) in water and biological samples, and accuracy was examined by the recovery experiments, independent analysis using electrothermal atomic absorption spectrometry, and analysis of a water standard reference material (SRM 1643e).     

Solid phase extraction of gold by sorption on octadecyl silica membrane disks modified with pentathia-15-crown-5 and determination by AAS

A simple and selective method for rapid and efficient concentration and determination of μg l⁻¹ levels of Au(III) ions in aqueous solution using octadecyl silica membrane disks modified by pentathia-15-crown-5 and flame atomic absorption spectrometry is presented. The influence of flow rates of eluent and sample solution, amount of ligand, types and least amount of eluent for elution of Au from disks were investigated. Break through volume and limit of detection of the membrane disks modified by 5 mg of the thiacrown ether was found to be 2.0 l and 1.0 μg l⁻¹, respectively. The effects of various cationic interferences on percent recovery of gold were studied. The method was successfully applied for the determinations of gold in some pharmaceutical samples and for the recovery of trace Au³⁺ ions from synthetic and water samples.     

Preconcentration of trace amounts of silver ion in aqueous samples on octadecyl silica membrane disks modified with hexathia-18-crown-6 and its determination by atomic absorption spectrometry

A simple and reliable method has been developed to selectively separate and concentrate trace amounts of silver ion from aqueous samples for the subsequent measurement by atomic absorption spectrometry. Ag⁺ ions are absorbed quantitatively during passage of aqueous samples through an octadecyl-bonded silica membrane disk modified by hexathia-18-crown-6. Almost all matrix elements will pass through the disk to drain. The retained Ag⁺ ions are then stripped from the disk with a minimal amount of thiosulfate solution as eluent. The proposed method permitted large enrichment factors of about 200 and higher. The limit of detection of the proposed method is 50 ng Ag⁺ per 1000 mL. The effects of various cationic interferences on the recovery of silver in binary mixtures were studied. The method was applied to the recovery of Ag⁺ ions from different synthetic and water samples. Received: 28 September 1999 / Revised: 2 December 1999 / Accepted: 8 December 1999     

Preconcentration of trace amounts of silver ion in aqueous samples on octadecyl silica membrane disks modified with hexathia-18-crown-6 and its determination by atomic absorption spectrometry

A simple and reliable method has been developed to selectively separate and concentrate trace amounts of silver ion from aqueous samples for the subsequent measurement by atomic absorption spectrometry. Ag+ ions are absorbed quantitatively during passage of aqueous samples through an octadecyl-bonded silica membrane disk modified by hexathia-18-crown-6. Almost all matrix elements will pass through the disk to drain. The retained Ag+ ions are then stripped from the disk with a minimal amount of thiosulfate solution as eluent. The proposed method permitted large enrichment factors of about 200 and higher. The limit of detection of the proposed method is 50 ng Ag+ per 1,000 mL. The effects of various cationic interferences on the recovery of silver in binary mixtures were studied. The method was applied to the recovery of Ag+ ions from different synthetic and water samples.     

Flame atomic absorption determination of palladium in solutions after preconcentration using octadecyl silica membrane disks modified by thioridazine.HCl

A new simple and reliable method for rapid and selective extraction and determination of trace level of Pd(II) ion is developed. Palladium ions are adsorbed quantitatively during passage of aqueous samples through octadecyl silica membrane disks modified with thioridazine·HCl (TRH). The influence of flow rates of eluent and sample solution, amount of ligand, types and least amount of eluent, and pH of samples were studied. Almost all matrix elements were found to pass through the disk to drain. Break through volume and limit of detection of the membrane disks modified by 5 mg of TRH was found to be 1.0 l and 12 μg l⁻¹, respectively. The retained Pd(II) ions are then stripped from the disk with a minimal amount of sulfite solution as eluent and subsequently measured by atomic absorption spectrometry. The proposed method permitted large enrichment factors of about 100 and higher. The method was applied to the recovery of Pd(II) ions from different industrial samples and waters.     

New anion-exchange solid-phase extraction support used for preconcentration and determination of lead in water samples by flame atomic absorption spectrometry

A new chelating resin was prepared by coupling Amberlite XAD-2 with Brilliant Green through an azo spacer. The resulting resin has been characterized by FTIR spectrometry, elemental analysis, and thermogravimetric analysis and studied for the preconcentration and determination of trace Pb(II) ions from solution samples. The anionic complex of Pb(II) and iodide was retained on the resin by the formation of an ion associate with Brilliant Green on Amberlite XAD-2 in weak acidic medium. The optimum pH value for sorption of the metal ion was 5.5. The sorption capacity of the functionalized resin is 53.8 mg/g. The chelating resin can be reused for 20 cycles of sorption-desorption without any significant change in sorption capacity. A recovery of 103% was obtained for the metal ion with 0.1 M EDTA as the eluting agent. Scatchard analysis revealed that the homogeneous binding sites were formed in the polymers. The resin was subjected to evaluation through batch binding and column chromatography of Pb(II). The equilibrium adsorption data of Pb(II) on modified resin were analyzed by Langmuir, Freundlich, and Temkin models. Based on equilibrium adsorption data, the Langmuir, Freundlich, and Temkin constants were determined to be 0.192, 13.189, and 3.418 at pH 5.5 and 25 degrees C. The method was applied for lead ion determination in tap water samples.     

Preconcentration of trace amounts of beryllium in water samples on octadecyl silica cartridges modified by quinalizarine and its determination with atomic absorption spectrometry

A simple method has been developed for rapid and selective extraction, preconcentration and determination of trace amounts of beryllium. The extraction is carried out by octadecyl silica cartridge, modified with quinalizarine as a chelating agent. The effect of different parameters, such as sample matrix, flowrates of sample solution and eluent, pH, type and least amount of eluent for elution of Be(+2) ions from cartridge, breakthrough volume and limit of detection, were evaluated. Also, the effects of various cationic and anionic interferences on percent recovery of Be(+2) were studied. Be(+2) was extracted from solution at pH 6-6.6 and was eluted from modified cartridge with 5 ml of 0.5 M HNO(3). Extraction efficiencies >99% were obtained by elution of the cartridges with minimal amount of eluent. A preconcentration factor of 200 and a detection limit of 200 ng per 1000 ml were obtained. The method was applied to the recovery and determination of Be(+2) in different water and alloy samples.     

Ultratrace determination of lead,cadmium and copper in environmental and biological samples by atomic absorption spectrometry after their separation and preconcentration using octadecyl silica membrane disks modified with a new n–s schiff base

Pb(II), Cd(II) and Cu(II) ions were separated and preconcentrated by solid-phase extraction on octadecyl-bonded silica membrane disks modified with a new S–N-containing Schiff base (bis-2-thiophenal propandiamine) (BTPD) followed by elution and atomic absorption spectrometric detection. The method was applied as a separation and detection method for lead(II), cadmium(II) and copper(II) in environmental and biological samples. Extraction efficiency and the influence of sample matrix, flow rate, pH, and type and minimum amount of stripping acid were investigated. The maximum capacity of the membrane disks modified by 4?mg of BTPD was found to be 668 ± 10, 480 ± 8 and 454 ± 7?µg of lead, cadmium and copper, respectively. The limit of detection of the proposed method is 0.25, 0.01 and 0.02?ng/mL for lead, cadmium and copper, respectively.     

Solid-phase extraction and atomic absorption spectrometric determination of cobalt using an octadecyl bonded silica membrane disk modified with Cyanex 272

A simple SPE method for determination of cobalt(II) using a C18 bonded silica membrane disk impregnated with Cyanex 272 has been developed. Cobalt(II) was quantitatively sorbed at pH 6.0 from a sample solution and eluted using 10.0 mL 1.0 M HNO3 prior to its flame atomic absorption spectrometric determination. The influence of eluting agents, the minimum volume and maximum flow rate of the eluent, and interfering ions on cobalt(II) was studied. The method developed for cobalt(II) had an LOD of 1.4 microg/L, and a preconcentration factor > 200 with an RSD of 0.6%. The reusability of the modified disk was for 40 cycles. The method was applied for the determination of cobalt in certified samples, urine, and industrial sludge samples.     

Application of modified multiwalled carbon nanotubes for palladium preconcentration and determination in water and soil samples by flame atomic absorption spectrometry

A new solid-phase extraction method for determination of palladium by atomic absorption spectrometry is described. Multiwalled carbon nanotube (MWCNT) modified with 1-butyl 3-methyl imidazolium hexafluorophosphate (MWCNT-[BMIM]PF₆) and supported on sawdust was used as an adsorbent for preconcentration of palladium. Palladium ions are retained on (MWCNT-[BMIM]PF₆) adsorbent as [PdI₄]^2? and eluted from the column with a thiosulfate–ammonia mixture. The optimum conditions for the adsorption were evaluated by changing various parameters such as pH, sample volume, concentration and volume of eluent, iodide concentration and interfering ions to achieve highest sensitivity and selectivity. The calibration graph was linear in the range of 2–120 ng mL^?1 of palladium in the initial solution and the limit of detection based on 3S_b was 0.41 ng mL^?1. The method was applied to the determination of palladium in water, wastewater and soil samples.     

Micelle mediated extraction of magnesium from water samples with trizma-chloranilate and determination by flame atomic absorption spectrometry

This article describes an analytical method for the determination of magnesium taking advantage of the cloud point phenomenon employing a suitable chelating agent (chloranilate) for Mg analysis. The method encompasses pre-concentration of the metal chelate followed by flame atomic absorption spectrometry (FAAS) analysis. The chelating agent chosen for this task is a newly synthesised salt of chloranilic acid, trizma-chloranilate, which reacts with Mg but at the same time has a very low affinity for other metallic cations like silicon, aluminium and sodium, which interfere with the determination of Mg in FAAS. The condensed surfactant phase with the metal chelate(s) is introduced into the flame of an atomic absorption spectrometer after its treatment with an acidified methanolic solution. In this way, complex and time-consuming steps for sample treatment are avoided while increased sensitivity is achieved by the presence of both methanol and surfactant in the aspirated sample. The analytical curve was rectilinear in the range of 5-220 mugl(-1) and the limit of detection was as low as 0.75 mugl(-1) with a standard deviation of 5.2%. The method was applied for the determination of Mg in natural and mineral waters with satisfactory results and recoveries in the range of 97-102%.     

Solid phase extraction of ultra-trace amounts of Ag+ by using octadecyl silica membrane disks modified with a new fulvalen derivative.

A simple method for the rapid extraction and determination of ultra-trace amounts of Ag+ ions using octadecyl-bonded silica membrane disks modified with a recently synthesized fulvalen (tetramethyltetrathiafulvalen) (TMTTF) and graphite furnace atomic absorption spectrometry is presented. The extraction efficiency and influence of the flow rate, pH, nature of the counter ion and type and the least amount of eluent for the stripping of Ag+ from disks and breakthrough volume were evaluated. The maximum capacity of the membrane disks modified by 5 mg of TMTTF used was found to be 482 +/- 6 micrograms Ag+. The detection limit of the proposed method is 1.0 ng/dm3. The method was applied to the recovery of Ag+ ions from different synthetic and water samples.     

Evaluation of polychlorotrifluoroethylene as sorbent material for on-line solid phase extraction systems: determination of copper and lead by flame atomic absorption spectrometry in water samples

Polychlorotrifluoroethylene (PCTFE) in the form of beads was applied, as packing material for flow injection on-line column preconcentration and separation systems coupled with flame atomic absorption spectrometry (FAAS). Its performance characteristics were evaluated for trace copper determination in environmental samples. The on-line formed complex of metal with diethyldithiophosphate (DDPA) was sorbed on the PCTFE surface. Isobutyl methyl ketone (IBMK) at a flow rate of 2.8 mL min⁻¹ was used to elute the analyte complex directly into the nebulizer-burner system of spectrophotometer. The proposed sorbent material reveal, excellent chemical and mechanical resistance, fast adsorption kinetics permitting the use of high sample flow rates up to 15 mL min⁻¹ without loss of retention efficiency. For copper determination, with 90 s preconcentration time the sample frequency was 30 h⁻¹, the enhancement factor was 250, which could be further improved by increasing the loading (preconcentration) time. The detection limit (3s) was c_L = 0.07 μg L⁻¹, and the precision (R.S.D.) was 1.8%, at the 2.0 μg L⁻¹ Cu(II) level. For lead determination, the detection limit was c_L = 2.7 μg L⁻¹, and the precision (R.S.D.) 2.2%, at the 40.0 μg L⁻¹ Pb(II) level. The accuracy of the developed method was evaluated by analyzing certified reference materials and by recovery measurements on spiked natural water samples.