Flow Injection Flame Atomic Absorption Research Articles

Preparation of a hydrogel sorbent based on agar-polyethylene glycol stabilized with iminodiacetic acid using electron irradiation method and its use for dispersive micro-solid phase extraction of Mn(II)

An agar/polyethylene glycol hydrogel was synthesized and modified with iminodiacetic acid (IDA-agar/PEG), and its ability as a biocompatible sorbent for extraction of manganese (II) ions from different environmental and food samples was investigated. The prepared IDA-agar/PEG hydrogel was characterized by scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, energy dispersive X-ray (EDX) spectroscopy, thermogravimetric analysis (TGA), and X-ray diffraction (XRD). The crucial parameters of manganese (II) extraction before its determination by flow injection flame atomic absorption spectrometry were optimized. At optimized conditions, a detection limit of 0.12 μg L−1, a limit of quantification of 0.41 μg L−1, and the relative standard deviations of 3.5 % (intra-day) and 5.5 % (inter-day) for six replicate quantifications of Mn (5.0 μg L−1) were obtained. The linearity range (LR) and preconcentration factor (PF) were determined as 0.4–50.0 µg/L and 187.5, respectively. The IDA-agar/PEG hydrogel sorbent was successfully employed for the dispersive micro-solid phase extraction (DMSPE) of Mn(II) in waters, soil, vegetables, and nuts with good recoveries (97.2–101.0 %).

Novel determination of copper(II) in natural waters by solid-phase extraction (SPE) flow-injection (FI) flame atomic absorption spectrometry (FAAS)

A novel functionalized silica gel with the Schiff base of N-{[3-[(3-aminopropyl)amino]propyl}-2-hydroxy-benzaldimine was fabricated and utilized for flow-injection (FI) solid-phase extraction (SPE) of Cu(II) ions with flame atomic absorption spectrometric determination in environmental water samples. The practical factors on the FI-SPE of Cu(II) ions, including flow rates and volumes of sample and eluent solutions, eluent type and concentration, sample pH, and matrix ions, were studied. The maximum absorbance of Cu(II) ions was obtained using sample solutions at pH 7.0 at 5.0 mL min−1 with elution by 500 µL of 1.0 M HCl. Batch adsorption capacity of the functionalized silica gel for Cu(II) ions was 24.7 ± 0.3 mg g−1. The developed FI-SPE method was successfully validated by the determination of Cu(II) in water certified reference materials, including water-trace elements (NWTM-15.2) and Ontario Lake water (NWTMDA-54.4). Cu(II) levels in environmental samples such as tap, river, and sea water were successfully determined using the reported FI-SPE method.

Chemometric design-based optimization of a green, selective and inexpensive switchable hydrophilicity solvent-based liquid phase microextraction procedure for pre-concentration and extraction of sulfadiazine in milk, honey and water samples

In this research, a green, selective and inexpensive switchable hydrophilicity solvent-based liquid phase microextraction (SHS-LPME) procedure has been optimized for the extraction and preconcentration of sulfadiazine (SDZ) in milk, honey and water samples prior to spectrophotometric analysis. Five variables affecting the SHS-LPME procedure were optimized using chemometric-based central composite design. For the SHS-LPME procedure, analytical parameters such as linearity, limit of detection, extraction recovery and enrichment factor were 15–300 μg L−1, 4.5 μg L−1, 96 ± 3% and 113, respectively. The precision of the method was investigated by repeatability and reproducibility studies. The relative standard deviation from these studies was found in the range of 2.4–4.5%. The recovery of the SDZ in the samples was in the range of 94 ± 4–99 ± 2%. Collected samples were analyzed by both the SHS-LPME procedure and the reference method using flow injection-flame atomic absorption technique, and the results were compared. There was no statistically significant difference between the two methods. This showed that the SHS-LPME procedure can be safely applied to the analysis of real samples.

An automatic on-line sorptive extraction platform for palladium determination in automobile exhaust catalysts based on a PTFE-turnings packed column, flow injection analysis and flame atomic absorption spectrometry

ABSTRACT A novel simple sensitive and effective on-line flow injection column preconcentration platform using poly-tetrafluoroethylene turnings as sorbent was developed prior to flame atomic absorption spectrometric (FAAS) determination of palladium in vehicle exhaust catalysts, hydrogenation catalysts and environmental water samples. The method is based on the sorption of palladium(II)-diethyldithiophosphate, which was found to be more effective than dithiocarbamate ones. Methyl isobutyl ketone (MIBK) was used as eluent prior atomisation and quantification. All parameters like pH, DDPA concentration, flow rates, preconcentration time that affect the sensitivity of the method as well as interferences of other metals were investigated in detail. The enhancement factor calculated as 114 for 60 s preconcentration time while the sampling frequency as 40 h−1. The detection limit was 0.9 μg L−1 and the relative standard deviation (RSD) was 2.8% at 20.0 μg L−1 concentration level. The accuracy of the proposed method was estimated by analysing certified reference material and spiked environmental samples. The analytical features of the method were compared with other on-line column preconcentration methods reported in the literature.

Efficient lead preconcentration using two chemically functionalized carbon nanotubes in hyphenated flow injection-flame atomic absorption spectrometry system

Lead contamination in drinking and natural water has reached alarming concentrations, thus necessitating the development of accurate and rapid determination systems for Pb(II) in aqueous systems. Two hyphenated flow injection-solid phase extraction- FAAS (FI-SPE-FAAS) systems using oxidized and m-phenylenediamine functionalized multiwalled carbon nanotubes for Pb(II) preconcentration from industrially contaminated real water samples have been proposed. The chemical and hydrodynamic parameters affecting Pb(II) sorption/desorption were optimized. The effect of common interfering ions in water was also studied. Different figures of merit such as preconcentration factor (> 70), detection limit (≤ 1.5 µg L−1), and relative standard deviation (≤ 1.3%) were achieved at the preconcentration time of 120 s for both the preconcentration systems. The method was applied to industrially contaminated real water samples and the spike recovery tests were carried out using standard Pb(II) solution traceable to NIST. The proposed method was validated using standard reference material 1640a supplied by NIST Gaithersburg, MD, USA.

Deep eutectic solvent containing 2-(3-hydroxy-1-methylbut-2-enylideneamino)pyridine-3-ol immobilized on magnetic graphene oxide as a selective sorbent for dispersive micro-solid phase extraction of cadmium ions

A sorbent with high selectivity and capacity for cadmium ions was prepared through immobilization of deep eutectic solvent (DES) of ChCl- glycerol containing the ligand 2-(3-hydroxy-1-methylbut-2-enylideneamino)pyridine-3-ol (acacapyrH2) on the magnetic graphene oxide. A dispersive micro-solid phase extraction was designed, and the separated/preconcentrated cadmium ion was determined by flow injection flame atomic absorption spectrometry. After the optimization of effective parameters, the method showed linearity in the concentration range of 0.25–15 µg L−1 with the coefficient of determination (r2) of 0.9991 and enhancement factor of 195 for cadmium. The method was very sensitive with the detection limit (defined as 3Sb/m) of 0.06 µg L−1. The method was successfully applied to the determination of Cd(II) in water (drinking and river), fruit (lemon, apricot, and peach) and meat (fish, chicken, and cow meat) samples.

Solidified floating organic drop microextraction for pre-concentration and trace monitoring of cadmium ions in environmental food and water samples

In this research, solidified floating organic drop microextraction as an efficient sample preparation method was used for trace monitoring of cadmium ions in environmental samples. In this method, a free microdroplet of 1-undecanol is floated on the surface of aqueous solution and agitated by a stirring bar placed on the bottom of the sample vial. Cadmium ions were complexed with neocuproine to obtain hydrophobic complex and extracted to extraction solvent. The extracted target ions were determined by flow injection–flame atomic absorption spectrometry. The effect of important factors on the extraction of target ions by the proposed sample preparation method was evaluated and optimized. The limit of detection, relative standard deviation (%) and enrichment factor of the method were 0.02, 3.7 and 98.5%, respectively. The validation of the method was examined by the analysis of cadmium ions in the certified reference material (sea food mix), and the obtained data can proof the reliability of the method for trace detection of cadmium ions. The method was successfully applied for determination of cadmium in the real food and water samples, and satisfactory relative recoveries (97–102%) were achieved.

Application of Deep Eutectic Solvent Modified Cotton as a Sorbent for Online Solid-Phase Extraction and Determination of Trace Amounts of Copper and Nickel in Water and Biological Samples.

Deep eutectic solvent (DES) was used as the extractant to improve the extraction properties of cotton. DES of choline chloride-urea (ChCl-urea) was prepared and immobilized on the surface of cotton fibers. The resulting sorbent was packed on a microcolumn, and a flow injection flame atomic absorption spectrometry was designed for the online separation and determination of trace amounts of copper and nickel. Various parameters affecting the extraction recovery of analytes such as pH, sample volume, sample loading rate, nature, volume, concentration, and flow rate of eluent were investigated and optimized. Under the optimum conditions, the method showed good linearity in the concentration range of 0.25-50.0 and 4.0-125.0μgL-1 with the coefficient of determination (r 2) of 0.9991 and 0.9990 for copper and nickel, respectively. The method was very sensitive with the detection limits (defined as 3Sb/m) of 0.05 and 0.60μgL-1 for Cu and Ni, respectively. It was successfully applied for the determination of Cu and Ni in water and biological samples. The accuracy of the method was evaluated through the recovery experiments and independent analysis by electrothermal atomic absorption spectrometry.

Application of supramolecular solvent-based dispersive liquid–liquid microextraction for trace monitoring of lead in food samples

An efficient sample treatment method based on supramolecular solvent-based dispersive liquid–liquid microextraction was applied for trace monitoring of lead by flow injection flame atomic absorption spectrometry.

Determination of copper in industrial water by innovative flow injection flame atomic absorption spectrometry

ABSTRACTAn online flow injection procedure for the preconcentration of copper at µg L−1 levels was developed using a novel chelating resin and flame atomic absorption spectrometry for the analysis of industrial water. Amberlite XAD-2 functionalized with dithizone resin was packed in a minicolumn for flow injection. The pH, sample and eluent flow rates, and eluent concentration were optimized to ensure maximum recovery of Cu(II). The effect of concomittant ions on Cu (II) sorption was also investigated. The limit of detection and enrichment factor for a 180 s preconcentration time were 76 and 0.6 µg L−1, respectively. The resin offered precision of 1.0% for seven successive determinations of 100 µg L−1 Cu(II). The resin was used for more than 300 sorption and desorption cycles without appreciable loss of efficiency. The accuracy of the preconcentration procedure was confirmed by fortified recovery studies in industrial water with NIST certified copper nitrate with recovery exceeding 96%. Validation was performed by the analysis of a standard reference material.

Dispersive solid phase microextraction with magnetic graphene oxide as the sorbent for separation and preconcentration of ultra-trace amounts of gold ions

A selective, simple and rapid dispersive solid phase microextraction was developed using magnetic graphene oxide (MGO) as an efficient sorbent for the separation and preconcentration of gold ions. The MGO was synthesized by means of the simple one step chemical coprecipitation method, characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM). Gold ions retained by the sorbent were eluted using 0.5molL−1 thiourea in 0.1molL−1 HCl solution and determined by the flow injection flame atomic absorption spectrometry (FI-FAAS). The factors affecting the separation and preconcentration of gold were investigated and optimized. Under the optimized conditions, the method exhibited a linear dynamic range of 0.02–100.0µgL−1 with a detection limit of 4ngL−1 and an enrichment factor of 500. The relative standard deviations of 3.2% and 4.7% (n=6) were obtained at 20µgL−1 level of gold ions for the intra and the inter day analysis, respectively. The method was successfully applied to the determination of gold ions in water and waste water samples as well as a certified reference material (CCU-1b, copper flotation concentrate).

Development and evaluation of selective coating for stir bar sorptive extraction of silver using sol–gel technique in combination with double-imprinting concept

The flexibility and simplicity of stir bar sorption extraction (SBSE) have been combined with the selectivity of ion imprinted polymers (IIP) and a selective and fast extraction and preconcentration method for Ag(I) has been developed. The stir bar was coated with silver imprinted polymer using sol–gel technique in combination with double-imprinting concept. The retained silver was eluted with 250 µL thiourea solution (0.5 mol L−1) at a pH of 3.0–4.0 and was determined by flow injection-flame atomic absorption spectrometry. The factors affecting the separation and preconcentration of Ag(I) were optimized. Under the optimized conditions, the method exhibited a linear dynamic range of 0.5–50 µg L−1 with a detection limit of 0.04 µg L−1 and an enhancement factor of 196. A relative standard deviation of 3.2 % (n = 6) was obtained at the level of 20 µg L−1. The proposed method was successfully applied to the determination of silver in hair, nail and different water samples. The accuracy of the proposed procedure was verified by recovery experiments, independent analysis by electrothermal atomic absorption spectrometry (ET–AAS) and application of the method to the determination of silver in a certified reference material.

Separation/Preconcentration System Based on Emulsion-Induced Breaking Procedure for Determination of Cadmium in Edible Oil Samples by Flow Injection-Flame Atomic Absorption Spectrometry

In this work, a new procedure using extraction induced by emulsion breaking (EIEB) procedure has been developed for extraction/preconcentration of cadmium in various edible oils (canola, corn, hazelnut, olive, and sunflower oil) prior to its determination by flow injection (FI) flame atomic absorption spectrometry (FAAS). Five chemical variables (surfactant type, concentration of the surfactant, concentration of the nitric acid, emulsion breaking time, and temperature) were selected as the main factors affecting extraction efficiency, and two variables (sample flow rate and sample volume) were studied for optimizing flow injection conditions. The limits of detection of 1.53 and 1.55 μg L−1 were observed for cadmium when aqueous standard and oil-based standards were added to the samples for calibration, respectively. The linear range of cadmium in aqueous standard was varied in the range of 5.9–94 μg L−1. The precision of the EIEB procedure was obtained as 4.1 % by determination of ten replicates of 2.5 μg L−1 of cadmium, and the preconcentration factor 13.8 was obtained from only 4 mL of edible oil samples. The accuracy of the procedure was performed by comparison with the reference method based on the digestion of samples in a closed-vessel microwave oven and by spiking the samples with the known amounts of the cadmium in the form of oil-based standards. There were no statistical differences between the results obtained with the EIEB procedure and the reference microwave digestion method, and the recoveries were in the range of 97–104 %.

Homogeneous Liquid–Liquid Microextraction via Flotation Assistance with Thiol Group Chelating Reagents for Rapid and Efficient Determination of Cadmium(II) and Copper(II) Ions in Water Samples

In the present study, facile and competent homogeneous liquid–liquid microextraction via flotation assistance (HLLME-FA) method combined with flow injection flame atomic absorption spectrometry (FI-FAAS) was proposed for simultaneous separation/preconcentration and determination of trace amounts of cadmium and copper in water samples. The efficient 2-(3,4-dihydroxyphenyl)-1,3-dithiolane (DHPDTO) with thiol groups was used as chelating reagent. The predominant parameters influencing the HLLME-FA, such as solution pH, concentration of DHPDTO, extraction and homogeneous solvent types and volumes, ionic strength, and extraction time were studied. Applying all the optimum conditions in the process, the detection limits of 0.008 and 0.01 μg L−1, linear ranges of 0.08–40 and 0.1–45 μg L−1, and the precision (RSD%, n = 7) of 3.4 and 3.9 % were obtained, respectively, for cadmium and copper. The proposed procedure showed satisfactory results for analysis of tap water, river water, well water, and seawater.

Crosslinked poly (4-vinylpyridine-ethylene glycol dimethacrylate) used for preconcentration of Cd(II) and its determination by flow injection flame atomic absorption spectrometry.

The main purpose of this research was to synthesize crosslinked poly(4-vinylpyridine-ethylene glycol dimethacrylate) and evaluate its feasibility for highly sensitive and selective determination of Cd in water samples by using flow injection flame atomic absorption spectrometry. The crosslinked polymer, prepared by bulk polymerization, was characterized by FTIR spectrometry and scanning electron microscopy. The flow injection solid-phase method was based on preconcentration of 20.0 mL of sample through 100 mg of the polymer packed into a minicolumn at pH 8.25 using a flow rate of 6.0 mL/min, followed by elution with 1.0 M HNO3. The sample solution parameters influencing the preconcentration behavior of Cd ions, such as pH, buffer concentration, and flow rate, were simultaneously studied and optimized using a Doehlert matrix. Values of 0.10 microg/L, 2.0-210 microg/L, 32.3, 18/h, 9.7/min, and 0.62 mL were obtained for LOD, linear range, preconcentration factor, sample throughput, concentration efficiency, and consumption index, respectively. The effect of the presence of the inorganic cations Pb(II), U(IV), Co(II), Hg(II), Cu(II), As(II), Mg(II), Sb(III), Ni(II), Th(IV), Ba(II), and Ca(II) on the method was studied, and the preconcentration of Cd was observed to have no interference. The accuracy of the method was assessed by analysis of natural water samples using addition and recovery tests and inductively coupled plasma/MS as a reference technique, as well as by analysis of a standard reference material of trace elements in water.

Epichlorohydrin crosslinked chitosan–clay composite beads for on-line preconcentration and determination of chromium(iii) by flow injection flame atomic absorption spectrometry

Download options Please wait... Article information DOI https://doi.org/10.1039/C4AY00638K Article type Paper Submitted 13 Mar 2014 Accepted 13 May 2014 First published 13 May 2014 Download Citation Anal. Methods, 2014,6, 5298-5303 BibTex EndNote MEDLINE ProCite ReferenceManager RefWorks RIS Permissions Request permissions Epichlorohydrin crosslinked chitosan–clay composite beads for on-line preconcentration and determination of chromium(III) by flow injection flame atomic absorption spectrometry M. Cittan, V. N. Tirtom, A. Dinçer and A. Çelik, Anal. Methods, 2014, 6, 5298 DOI: 10.1039/C4AY00638K To request permission to reproduce material from this article, please go to the Copyright Clearance Center request page. If you are an author contributing to an RSC publication, you do not need to request permission provided correct acknowledgement is given. If you are the author of this article, you do not need to request permission to reproduce figures and diagrams provided correct acknowledgement is given. If you want to reproduce the whole article in a third-party publication (excluding your thesis/dissertation for which permission is not required) please go to the Copyright Clearance Center request page. Read more about how to correctly acknowledge RSC content. Social activity Tweet Share Search articles by author Mustafa Cittan V. Nüket Tirtom Ayşe Dinçer Ali Çelik

Preconcentration and Determination of Trace Silver Ion Using Benzothiazole Calix[4]arene Modified Silica by Flow Injection Flame Atomic Absorption Spectrometry

The silica gel modified with benzothiazole calix[4]arene (APS-L1) via Schiff's base reaction was applied as a sorbent in an online system for preconcentration and determination of silver ion by flame atomic absorption spectrometry (FAAS). APS-L1 was used as an effective sorbent for solid phase extraction (SPE) of silver(I) ion in both batch and column methods. The optimum experimental parameters such as pH, eluent type, sample flow rate, eluent volume and eluent flow rate including the effect of interfering ions were investigated. Silver(I) ion was determined at pH 6-7. The capacity of APS-L1 sorbent was found to be 12.2 mg/g of sorbent. The high affinity was obtained without interference from the interfering ions. The optimum conditions of the online flow injection preconcentration coupled with the FAAS (FI-FAAS system) were evaluated. The sample flow rate was 3.0 mL min(-1) using sample volume of 5-10 mL. Elution was performed with 250 μL of 0.1 mol L(-1) thiosulfate at the flow rate of 1.5 mL min(-1). The analytical characteristics and performance of the FI-FAAS system were studied under optimum conditions using a solution spiked with standard silver(I) ion at 20 and 50 μg L(-1). The detection limit of 0.44 μg L(-1) was obtained. The accuracy of the proposed method was evaluated and percentages of recovery at 20 and 50 μg L(-1) were 100.2 and 99.5%, respectively. The percent relative standard deviations (%RSD) at 20 and 50 μg L(-1) were 6.1 and 3.3%, respectively. The developed method was successfully applied to determine trace silver(I) ion in drinking and tap water samples.

Determination of zinc in edible oils by flow injection FAAS after extraction induced by emulsion breaking procedure

A new procedure using extraction induced by emulsion breaking (EIEB) procedure has been developed for extraction/preconcentration of zinc in various edible oils (canola oil, corn oil, hazelnut oil, olive oil, and sunflower oil) prior to its determination by the single line flow injection (FI) flame atomic absorption spectrometry (FAAS). Several parameters affecting the extraction efficiency of the procedure were investigated including the type and concentrations of surfactant, the concentration of HNO3, and the other operational conditions (emulsion breaking time and temperature). The limits of detection of 1.1 and 1.0μgL−1 were observed for zinc when aqueous standard and oil-based standards were added to the emulsions for calibration, respectively. The proposed procedure of combining EIEB and single line FI-FAAS can be regarded as a new procedure for the determination of zinc in edible oil samples.

On-line Preconcentration and Determination of Cd(II) in Water by Flow Injection-Flame Atomic Absorption Spectrometry (FI-FAAS) Using Salicylic Acid Functionalized Amberlite XAD-2 Resin-Packed Minicolumn

On-line Preconcentration and Determination of Cd(II) in Water by Flow Injection-Flame Atomic Absorption Spectrometry (FI-FAAS) Using Salicylic Acid Functionalized Amberlite XAD-2 Resin-Packed Minicolumn

A novel solidified floating organic drop microextraction method for preconcentration and determination of copper ions by flow injection flame atomic absorption spectrometry in water samples

A simple, rapid and inexpensive solidified floating organic drop microextraction (SFODME) and flow injection flame atomic absorption spectrometric determination (FI-FAAS) method for copper was developed. 3-amino-7-dimethylamino-2-methylphenazine (Neutral red, NR) was used as the complexing agent. Several factors affecting the microextraction efficiency, such as, pH, NR and sodium dodecylbenzenesulfonate (SDBS) concentration, extraction time, stirring rate, and temperature were investigated and optimized. Under optimized experimental conditions an enrichment factor of 541 was obtained for 100 mL of sample solution. The calibration graph was linear in the range of 0.5 - 20.0 ng mL -1 and the limit of detection (3s) was 0.18 ng mL -1 , the limit of quantification (10s) was 0.58 ng mL -1 . The relative standard deviation (RSD) for 10 replicate measurements of 10 ng mL -1 copper was 2.7%. The developed method was successfully applied to the extraction and determination of copper in different certified reference materials (Estuarine water, Slew 3 and fortified water, TM 23.2) and real water samples and satisfactory results were obtained.