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1.
A rapid and simple on-line method is described for the determination of Au(III) in various samples. The method is based on the sorption of gold(III) on Lewatit MonoPlus TP207 chelating resin including the iminodiacetate group, which is used as sorbent material and packed in a minicolumn. The chemical variables such as the pH of the sample solution, eluent type, interfering ions and concentrations of reagents, and instrumental variables such as sample loading volume, reagents flow rates, and tubing length, which affect the efficiency of the method were studied and optimised. Au(III) was sorbed on the chelating resin, from which it could be eluted with 3 mol L?1 HCl, and then introduced directly to the nebuliser-burner system of FAAS. The limit of detection of the method was 0.2 µg L?1 while the relative standard deviation was <4.0% for 20 µg L?1 Au(III) concentration. The preconcentration factor was found to be 106 while the optimised sample volume was 15.3 mL. The accuracy of the method was verified by analysing the certified reference material. The developed method was applied successfully for the determination of gold in different samples with satisfactory results.  相似文献   

2.
A selective, simple and fast dispersive micro solid phase extraction method using magnetic graphene oxide (GO) as an efficient sorbent has been developed for the extraction, separation and speciation analysis of chromium ions. The method is based on different adsorption behaviour of Cr(VI) and Cr(III) species onto magnetic GO in aqueous solutions which allowed the selective separation and extraction of Cr(VI) in the pH range of 2.0–3.0. The retained Cr(VI) ions by the sorbent were eluted using 0.5 mL of 0.5 mol L?1 nitric acid solution in methanol and determined by ?ame atomic absorption spectrometry. Total chromium content was determined after the oxidation of Cr(III) to Cr(VI) by potassium permanganate. All effective parameters on the performance of the extraction process were thoroughly investigated and optimised. Under the optimised conditions, the method exhibited a linear dynamic range of 0.5–50.0 µg L?1 with a detection limit of 0.1 µg L?1 and pre-concentration factor of 200. The relative standard deviations of 3.8% and 4.6% (n = 8) were obtained at 25.0 µg L?1 level of Cr(VI) for intra- and inter-day analysis, respectively. The method was successfully applied to the speciation and determination of Cr(VI) and Cr(III) in environmental water samples.  相似文献   

3.
A solid phase extraction (SPE) procedure based on Amberlite IRA 900 resin was developed for speciation and separation of inorganic arsenic species (III, V) and total As in water samples. The As species and total As in eluent solutions were determined by electrothermal atomic absorption spectrometry (ETAAS) using Ni chemical modifier with 1200°C pyrolysis temperature. Experimental parameters such as pH value, sample volume, flow rate, volume and concentration of eluent solution for As(V) were optimised and 98.0 ± 1.9% recovery was found at pH 4.0. Experimental adsorption capacity of the resin for As(V) was investigated and 229.9 mg g1 was found. Under optimised experimental conditions, instrumental parameters such as limit of detection (LOD) and limit of quantification (LOQ) found were 0.126 and 0.420 µg L1, respectively. Interference effects of coexisting ions in the sample matrix on the recovery of As(V) were investigated. Concentration of As(III) was obtained by subtracting As(V) concentration found at pH 4.0 from total As(III + V) found at pH 8.0. The accuracy of the method proposed by using the resin was tested for analysing As species in a waste water standard reference material (SRM, CWW-TM-D) and spiked real water samples with recovery above 95%. The method proposed was also applied to the determinations of As species and total As in underground hot waters and tap water with relative error below 3%.  相似文献   

4.
A novel adsorbent of multi-wall carbon nanotubes (MWCNTs) chemically modified silica (MWCNTs-silica) was synthesised and employed as the adsorbent material for solid-phase extraction (SPE) of trace Zn(II), Cu(II), Cd(II), Cr(III), V(V) and As(V) in environmental water samples followed by inductively coupled plasma optical emission spectrometry detection. This material inherits the advantages of nanomaterial MWCNTs and conventional silica with dual functional groups (–NH2 and –COOH), and avoid the problem of nanomaterial in SPE, such as high pressure. The factors affecting the separation and preconcentration of target elements such as pH, sample flow rate and volume, eluent concentration and volume were investigated. Under the optimised conditions, the detection limits for Zn(II), Cu(II), Cd(II), Cr(III), V(V) and As(V) were 0.27, 0.11, 0.45, 0.91, 0.55 and 0.67 μg L?1 with the relative standard deviations of 3.1, 5.9, 4.1, 4.0, 7.3 and 8.6% (c = 10 μg L?1, n = 7), respectively. The adsorption capacity of MWCNTs-silica was 26.6, 70.0, 13.8, 58.0, 20.0 and 20.0 mg g?1 for Zn(II), Cu(II), Cd(II), Cr(III), V(V) and As(V), respectively, and the prepared adsorbent could be reused more than 100 times. In order to validate the developed method, two certified reference materials of GSBZ50009-88 and GSBZ 50029-94 environmental waters were analysed and the determined values were in good agreement with the certified values. The developed method has been applied to the determination of trace elements in environmental water samples with satisfactory results.  相似文献   

5.
A liquid phase microextraction method-based conformation of supramolecular assembly was developed for the separation and preconcentration of trace levels of Sudan blue II. Various analytical parameters such as pH, supramolecular solvent type and volume, sample volume and matrix effect etc. were optimised. Sudan blue II concentration in the extraction phase was determined by UV-visible spectrophotometer. Under the optimised conditions, detection limit and preconcentration factor was found as 2.16 µg L?1 and 80, respectively. Relative standard deviation value was found 5%. The developed procedure was successfully applied for the determination of trace levels of Sudan blue II in environmental samples.  相似文献   

6.
The development of a solid-phase extraction (SPE) procedure for the pre-concentration of trace amounts of Pb2+ ion on 2-furan-2-yl-1-furan-2-ylmethyl-1H-benzoimidazole loaded on activated carbon modified with silver nanoparticles (L-AC-Ag-NP) was presented. The metal ion retained on the sorbent was quantitatively determined via complexation with the ligand. The complexed metal ion was efficiently eluted using 10 mL of 4 mol L?1 sulphuric acid in 10 w/v% acetone. The influences of the analytical parameters, including pH, amounts of the ligand and the solid phase, eluent conditions and sample volume, on the recoveries of the metal ion were optimised. Using the optimised parameters, the linear response of the SPE method for Pb2+ ion were in the ranges of 0.2–160 µg L?1, and the detection limit for Pb2+ ion was 0.034 µg L?1. The proposed method exhibits a pre-concentration factor (PF) of 80 and an enhancement factor of 30 for Pb2+ ion. The presented results demonstrate the successful application of the proposed method for the determination of Pb2+ ion in some real samples with high recoveries (>93%) and reasonable relative standard deviation (RSD < 2%).  相似文献   

7.
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   

8.
A novel potentiometric sensor, based on carbon paste electrode (CPE), modified with ion-imprinted polymer (IIP) and multi-walled carbon nanotubes (MWCNTs), is introduced for detection of chromium (III). The IIP nanomaterial was synthesised and characterised by using scanning electron microscopy and Fourier Transform Infrared. The modification of the CPE with the IIP (as a ionophore) resulted in an all-solid-state Cr(III)-selective sensor. However, the presence of appropriate amount of MWCNTs in the electrode composition was found to be necessary to observe Nernstian response. The optimised electrode composition was 76.7% graphite, 14.3% binder, 5% IIP, and 4% CNT. The proposed sensor exhibited Nernstian slope of 20.2 ± 0.2 mV decade?1 in the working concentration range of 1.0 × 10?6?1.0 × 10?1 mol L?1 (52 µg L?1–5.2 g L?1), with a detection limit of 5.9 × 10?7 mol L?1 (30.68 µg L?1) and a fast response time of less than 40 s. It displayed a stable potential response in the pH range of 2–5. It exhibited also high selectivity over some interfering ions. The proposed sensor was successfully applied for the determination of Cr(III) in real samples (sea, river water and soil).  相似文献   

9.
In this work, a glassy carbon electrode (GCE) modified with poly (diphenylamine)/multi-walled carbon nanotubes-β-cyclodextrin (PDPA/MWCNT-β-CD) film was constructed and used for the determination of 4-nitrophenol (4-NP). Diphenylamine was successfully electropolymerised onto MWCNT-β-CD-modified GCE by cyclic voltammetry in monomer solution and 5 mol L?1 H2SO4. The surface morphology of PDPA/MWCNT-β-CD film was characterised using scanning electron microscopy and electrochemical impedance spectroscopy. After adsorption of 4-NP on PDPA/MWCNT-β-CD at 0.2 V for 150 s, it showed a well-defined reduction peak in phosphate buffer solution at pH = 7. The PDPA/MWCNT-β-CD film enhanced the reduction peak current due to the complex formation between β-CD and 4-NP, presence of conductive polymer film as electron transfer mediator and also ability of MWCNTs for strong adsorptive and catalytic effect. Peak current increased linearly with 4-NP concentration in the range of 0.1 to 13.9 µg L?1. The detection limit was obtained as 0.02 µg L?1, which is better than other reported detection limits for the determination of 4-NP. The results showed that modified electrode has good sensitivity and selectivity. This sensor was used for the determination of 4-NP in water samples.  相似文献   

10.
《Analytical letters》2012,45(1-3):12-24
A simple and sensitive flow-injection method is reported for the determination of retinol and α-tocopherol in human blood serum and pharmaceuticals. The method is based on the reduction of vanadium(V) by retinol and α-tocopherol and subsequent reaction of reduced vanadium with luminol to generate chemiluminescence signal. The optimized conditions allow a linear calibration range of 30–2850 µg L?1 and 5–4300 µg L?1 for retinol and α-tocopherol, with relative standard deviations of 1.2–4.6% and 1.5–5.6%, respectively. The detection limits for retinol and α-tocopherol, defined as three times the standard deviation of measured blanks were 23 µg L?1 and 2.15 µg L?1, respectively. The proposed method allowed up to 20 determinations h?1. The tolerance amount of foreign ions/compounds on the determination of retinol and α-tocopherol was also examined. The method was applied to the determination of retinol and α-tocopherol in human blood serum and pharmaceutical samples using hexane extraction with recoveries in the range of 92 ± 2 to 96 ± 1%, and the results obtained were compared with HPLC reference method.  相似文献   

11.
A vortex-assisted dispersive liquid–liquid microextraction method in combination with UV–Vis spectrophotometry was developed for the simultaneous extraction and determination of iron species. In this method, Fe2+ and Fe3+ were complexed with pyridine-2-amidoxime, neutralized through ion pair formation with sodium dodecyl sulfate, and extracted into the fine droplets of chloroform. After centrifugation, the absorbance of the extracted complexes was recorded in the wavelength range of 360–700 nm. The parameters affecting the extraction efficiency such as the pH, the type and volume of the extraction solvent, ligand concentration, and sample volume were optimized. The individual iron species was then determined by means of the orthogonal signal correction–generalized partial least squares method. Under the optimized conditions, the calibration curves were linear over the range of 2.0–100 and 3.0–200 µg L?1 with detection limits of 0.4 µg L?1 for Fe2+ and 0.8 µg L?1 for Fe3+, respectively. The relative standard deviations for intra- and inter-day assays (n = 5) were 2.3 and 4.0 for Fe2+ at 50 µg L?1 and 2.7 and 4.3 for Fe3+ at 30 µg L?1, respectively. The enhancement factors of 77 and 69 were achieved for Fe2+ and Fe3+, respectively. The proposed method was successfully applied to the determination of iron species in water samples.  相似文献   

12.
A modified hollow-fiber-supported dispersive liquid-liquid microextraction (HF-DLLME) method was developed for the determination of aflatoxins and ochratoxin A in food samples. The various parameters affecting the efficiency of extraction, such as pH, salt addition, extraction time, stirring rate, desorption time, type and volume of extractant and disperser solvents were carefully studied and optimized using two step strategies. The linearity of the evaluated results was 0.1 to 30?μg L?1 for aflatoxins and 0.1 to 20?μg L?1 for ochratoxin A, with regression coefficients (R2) exceeding 0.9990. The precision was satisfactory with relative standard deviation values less than 11%. The method accuracy was within the recommended range from 70% to 120% and analyte accuracy between 83% and 101%. The limits of detection and quantification were in the range from 0.04 to 0.06?μg L?1 and 0.08 to 0.13?μg L?1, respectively, for multi-aflatoxins, and 0.02 to 0.04?µg L?1 and 0.08 to 0.10?µg L?1, respectively, for ochratoxin A. The developed method was successfully applied for the determination of mycotoxins in food samples.  相似文献   

13.
《Analytical letters》2012,45(13):1971-1985
Abstract

Arsenic(V) [As(V)] was reduced to As(0) at pH 0.0 and As(III) at pH 4.5 on a carbon-paste electrode modified with hematite, which allowed their selective determination. Arsenic(V) suffered interference from copper (Cu) and bismuth (Bi). Arsenic(III) was almost free of them. Humic acid did not affect the signal of As(V) but increased the signal of As(III). Arsenic was preconcentrated at ?0.8 V for 100 s. The response was linear up to 70 µg L?1 for As(V) and 50 µg L?1 for As(III). The limits of detection were 2 µg L?1 and 5 µg L?1 respectively. This method was applied to drinking water and compost lixiviate.  相似文献   

14.
The present study describes chelation of Pb(II) with ascorbic acid and formation of a charge-transfer sensitive ion-pair in the presence of Rhodamine 6G at pH 5.5, and then its extraction to the micellar phase of non-ionic surfactant, PONPE 7.5 by an ultrasound-assisted cloud point extraction method before analysis by FAAS. The various variables affecting ion-pair formation and extraction efficiency were studied and optimised. Under the optimised conditions, the good linear relationships in the ranges of 0.4–150 μg L?1 and 0.8–120 μg L?1 for solvent-based calibration and matrix-matched calibration curves, respectively, were achieved with a pre-concentration factor of 71.4 from pre-concentration of 50-mL sample. Moreover, the limits of detection with good sensitivity enhancements of 124 and 114.5 were 0.13 and 0.24 μg L?1, respectively, while the intra-day and inter-day precision (as RSD%, for five replicate measurements of 5 and 100 μg L?1 in the same day and three succeed days) were in range of 2.8–5.4% and 3.7–6.3%, respectively. The matrix effect on triplicate determination of 50 µg L?1 Pb(II) was also investigated. The accuracy of the method was statistically verified by the analysis of two certified reference materials (CRMs) after digestion with acid mixtures (HNO3-H2O2-HF and HNO3-H2O2) and dilution at suitable ratios. It has been observed that there is statistically not a significant difference between the certified- and found-values. The accuracy was also controlled using the pre-treated sample solutions spiked at different concentration levels, and the good spiked recoveries were obtained in range of 90–102.8%. The method was successfully applied to the determination of trace amounts of lead in water and food matrices with satisfactory results.  相似文献   

15.
In this work, magnetic solid-phase extraction based on sodium dodecyl sulfate-coated Fe3O4 nanoparticles has been successfully applied for extraction and preconcentration of trace amounts of nystatin from water and vaccine samples prior to high-performance liquid chromatography–ultraviolet detection. Various experimental parameters affecting extraction and recovery of the analyte, such as the amount of sodium dodecyl sulfate, pH of the sample solution, salt concentration, extraction time, sample volume and desorption conditions, were systematically studied and optimized. Under optimized conditions, nystatin was quantitatively extracted. Proper linear range with good coefficient of determination, (R 2 > 0.99) and limit of detection and quantification (based on signal-to-noise ratios of 3 and 10) of 2.0 and 5.0 µg L?1, over the investigated concentration range (5–700 µg L?1), were obtained, respectively. The intra-day and inter-day relative standard deviations at 50 µg L?1 level of NYS were 1.4 and 4.5% based on six replicate determinations. The accuracy of the method was evaluated by recovery measurements on spiked samples. Suitable recoveries of 96–102 and 26–44% were achieved (at spiked levels of 50, 300 and 500 µg L?1) for water and vaccine samples, respectively.  相似文献   

16.
《Analytical letters》2012,45(11):1426-1439
In this study, optimized ultrasound-assisted emulsification–microextraction (USAEME) combined with inductively coupled plasma-optical emission spectrometry (ICP-OES) was applied to simultaneous determination of trace levels of lanthanum (La) and cerium (Ce) in water and biological samples. 5,6,14,15-dibenzo-1,4-dioxa-8,12-diazacyclopentadecane (a dioxa-diazamacrocycle) was used as chelating agent. Tetrachloroethylene was selected as extraction solvent. The effective parameters of USAEME including pH, salt effect, ultrasonic time, temperature, volume of extraction solvent, and concentration of the chelating agent were studied by a fractional factorial design to identify the significant parameters and their interactions. The results showed that pH and concentration of chelating agent were significant. In the next step, to optimize important parameters, a central composite design was performed. Under the optimal conditions (5.5 for pH and 180 mg L?1 for concentration of chelating agent) the calibration graphs were linear in the range of 0.1–1000 for La and 1–1000 µ g L?1 for Ce. The determination coefficients (R2) were 0.999 and 0.998 for La and Ce, respectively. The limits of detection were 0.012 for La and 0.61 µ g L?1 for Ce. The relative standard deviations (RSD %, n = 7) at 200 µ g L?1 were 3.5% for La and 3.1% for Ce. The method was successfully applied to the analysis of La and Ce in real water samples with the recoveries in the range of 93–99%  相似文献   

17.
This study presents an easy and cost-effective flow-based cloud point extraction (CPE) method for determining partial amounts of two organophosphorus pesticides (phosalone and ethion) in seawater by HPLC–UV–Vis. In continues CPE methodology, the effect of the different column packing type such as carbon nanotube, polyacrylonitrile nanofiber and fiberglass on pesticide extraction was investigated. The Triton X-100 was utilized as nonionic surfactant, and moreover, effect of different parameters such as pH, temperature, extraction time, surfactant concentration, type and volume of the eluent solution on the extraction efficiency was optimized. Under optimum conditions, the figures of merit of the method for phosalone and ethion were obtained as: the enrichment factor (172 and 166), line range (0.8–300 and 0.5–300 µg L?1, R 2 = 0.9973 and 0.9982), relative standard deviation in concentration of 200 µg L?1 (%RSD = %5.4 and %7.99, N = 5) and limit of detection (LOD = 0.24 and 0.14 µg L?1). The suggested method was successfully used for determination of phosalone and ethion in Chabahar Bay seawaters with satisfactory results.  相似文献   

18.
《Analytical letters》2012,45(12):1846-1856
A preconcentration methodology utilizing the cloud point phenomenon is described for the determination of copper by flame atomic absorption spectrometry. The reagent Sulfathiazolylazo resorsin was used as a complexing agent. The preconcentration factor of 25-fold was obtained. The calibration curve is linear in the range of 4–400 µ g L?1 with a limit of detection of 0.64 µ g L?1. The relative standard deviation (n = 5, 12 µ g L?1) was 3.5%. The cloud point is formed in the presence of phenol at room temperature. The method was successfully applied to the determination of copper in water samples and a standard reference material.  相似文献   

19.
《Analytical letters》2012,45(5):761-777
This article reviews the use of square wave anodic stripping voltammetry for the simultaneous determination of ecotoxic metals (Pb, Cd, Cu, and Zn) on a bismuth-film (BiFE) electrode. The BiFE was prepared in situ on a glassy-carbon electrode (GCE) from the 0.1 mol L?1 acetate buffer solution (pH 4.5) containing 200 µg L?1 of bismuth (III). The addition of hydrogen peroxide to the electroanalytical cell proved beneficial for the interference-free determination of Cu (II) together with zinc, lead, and cadmium, using the BiFE. The experimental variables were investigated and optimized with the view to apply this type of voltammetric sensor to real samples containing traces of these metals. The performance characteristics, such as reproducibility, decision limit (CCa), detection capability (CCβ), sensitivity, and accuracy indicated that the method holds promise for trace Cu2+, Pb2+, Cd2+, and Zn2+ levels by employment of Hg-free GCE with SWASV. CCa, and CCβ were calculated according to the Commission Decision of 12 August 2002 (2002/657/EC). Linearity was observed in the range 20–280 µg L?1 for zinc, 10–100 µg L?1 for lead, 10–80 µg L?1 for copper, and 5–50 µg L?1 for cadmium. Using the optimized conditions, the stripping performance of the BiFE was characterized by low limits of detection (LOD). Finally, the method was successfully applied in real as well as in certified reference water samples.  相似文献   

20.
In the present study, an environment-friendly sample preparation method termed ionic liquid-based dispersive liquid–liquid microextraction combined with flame atomic absorption spectrometry has been developed for the determination of Pb(II) ion in water samples prior to flame atomic absorption spectrometry determination. In this method, ionic liquid was used as an extraction solvent instead of the organic solvent used in the conventional dispersive liquid–liquid microextraction (DLLME) assay, and there is no need for a chelating agent. Several variables that may affect extraction efficiencies, including pH, the volume of ionic liquid, the type and volume of disperser solvent, salt addition, and the time for centrifugation and extraction were studied and optimised. Under the optimised conditions, the calibration curve exhibited linearity over the range of 20.0–1000.0 μg L?1. The enrichment factor and the limit of detection based on 3Sb/m were 35.0 and 5.9 μg L?1, respectively. Seven replicate determination of a solution containing of 100.0 μg L?1 Pb(II) ions gave a relative standard deviation of ±2.1%. Finally, the feasibility of the proposed method for Pb(II) determination was assessed by the analysis of certi?ed reference material and various water samples and the satisfactory results were obtained.  相似文献   

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