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1.
A simple and reliable method for rapid and selective extraction and determination of trace levels of Ni2+ and Mn2+ was developed by ionic liquid (IL) based dispersive liquid–liquid microextraction coupled to flame atomic absorption spectrometry (FAAS) detection. The proposed method was successfully applied to the preconcentration and determination of nickel and manganese in soil, vegetable, and water samples. After preconcentration, the settled IL‐phase was dissolved in 100 µL of ethanol and aspirated into the FAAS using a home‐made microsample introduction system. Injection of 50 µL of each analyte into an air–acetylene flame provided very sensitive spike‐like and reproducible signals. Effective parameters such as pH, amount of IL, volume of the disperser solvent, concentration of the chelating agent, and effect of salt concentration were inspected by a (25‐1) fractional factorial design to identify the most important parameters and their interactions. Under optimum conditions, preconcentration of 10 mL sample solution permitted the detection of 0.93 µg L?1 Ni2+ and 0.52 µg L?1 Mn2+ with enrichment factors 77.2 and 82.6 for Ni2+ and Mn2+, respectively. The accuracy of the procedure was evaluated by analysis of a certified reference material (CRM TMDW‐500, drinking water).  相似文献   

2.
A cloud point extraction procedure is presented for the preconcentration and simultaneous determination of Ag+ and Pd2+ in various samples. After complexation with 2‐((2‐((1H‐benzo[d]imidazole‐2‐yl)methoxy)phenoxy)methyl)‐1H‐benzo[d]imidazol (BIMPI), which was used as a new chelating agent, analyte ions were quantitatively extracted to a phase rich in Triton X‐114 following centrifugation, and determination was carried out by flame atomic absorption spectrometry (FAAS). Under the optimum experimental conditions (i. e., pH = 7.0, 15.0·10–5 mol/L BIMPI and 0.036% (w/v) Triton X‐114), calibration graphs were linear in the range of 28.0–430.0 μg/L and 57.0–720.0 μg/L with detection limits of 10.0 and 25.0 μg/L for Ag+ and Pd2+, respectively. The enrichment factors were 35.0 and 28.0 for Ag+ and Pd2+, respectively. The method has been successfully applied to evaluate these metals in some real samples, including waste water, soil and hydrogenation catalyst samples.  相似文献   

3.
Interest in preconcentration techniques for the determination of metals at ultratrace levels still continues increasingly because of some disadvantages of flameless atomic absorption spectrometry and the high costs of other sensitive methods in compared to flame atomic absorption spectrometry (FAAS). Among preconcentration techniques, solid‐phase extraction is the most popular because of a number of advantages. In this work, thiol‐containing sulfonamide resin was synthesized, characterized, and applied as a new sorption material for solid phase extraction and determination of lead in natural water samples. The optimization of experimental conditions was performed using the parameters including pH, contact time, and volumes of initial and elution solutions. After preconcentration procedure, FAAS was used for determinations. The synthesized resin exhibits the superiority in compared to the other adsorption reagents because of the fact that there is no necessity of any complexing reagent as well as high sorption capacity. Consequently, 280‐fold improvement in the sensitivity of analytical scheme was achieved by combining the slotted tube atom trap‐atomic absorption spectrometry (STAT‐FAAS) and the developed preconcentration method. The limit of detection was found to be 0.15 ng mL?1. The Pb2+ concentrations in the studied water samples were found to be in the range of 0.9–6.7 ng mL?1.  相似文献   

4.
An on‐line solid phase extraction method for the preconcentration and determination of Cu(II) by flame atomic absorption spectrometry has been described. The procedure is based on the retention of Cu(II) ions at pH 6.0 on a minicolumn packed with Amberlite XAD‐1180 resin impregnated with chrome azurol S. After preconcentration, Cu(II) ions adsorbed on the impregnated resin were eluted by 1 mol L?1 HNO3 solution. Several parameters, such as pH, type of eluent, flow rates of sample and eluent solutions, amount of resin were evaluated. At optimized conditions, for 3.5 min of preconcentration time, the system achieved a detection limit of 1.0 µg L?1, and a relative standard deviation of 1.2% at 0.2 µg mL?1 copper. An enrichment factor of 56‐fold was obtained with respect to the copper determination. The proposed method was successfully validated by the analysis of standard reference material (TMDA 54.4 lake water) and recovery studies. The method was applied to the preconcentration of Cu(II) in natural water samples.  相似文献   

5.
Organic phosphonates are widely used, and in general, they are not easily biodegradable. Therefore, our interest was focussed on the development of an analytical method for the trace-level determination of organic phosphonates in water. Our method combines preconcentration of the analytes by evaporating the water sample with the methylation of the phosphonates using diazomethane. Analysis of the totally methylated phosphonates is done by liquid chromatography coupled with mass Spectrometry by the particle-beam interface. The derivatives could be clearly identified by their electron impact mass spectra as well as their chemical ionisation mass spectra. The totally methylated phosphonates can be separated by liquid chromatography using a 125 mm × 4 mm LiChrospher 100 Diol column and a gradient mobile phase containing n-hexane and isopropyl alcohol. After optimizing preconcentration and derivatization procedures as well as all particle-beam and mass spectra conditions, detection limits in the low ppb range were attained.  相似文献   

6.
In this study, a new sorbent is synthesized using surface imprinting technique. Cu(II)‐imprinted multiwalled carbon nanotube sorbent (Cu(II)‐IMWCNT) is used as the solid phase in the solid‐phase extraction method. After the preconcentration procedure, Cu(II) ions are determined by high‐resolution continuum source atomic absorption spectrometry. A total of 0.1 mol L?1 ethylenediaminetetraacetic acid (EDTA) is used to remove Cu(II) ions from the sorbent surface. The optimum experimental conditions for effective preconcentration of Cu(II), parameters such as pH, eluent type and concentration, flow rate, sample volume, sorbent capacity, and selectivity are investigated. The synthesized solid phase is characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. The maximum adsorption capacities of Cu(II)‐IMWCNT and non‐imprinted solid phases are 270.3 and 14.3 mg g?1 at pH 5, respectively. Under optimum experimental conditions for Cu(II) ions, the limit of detection is 0.07 μg L?1 and preconcentration factor is 40. In addition, it is determined to be reusable without significant decrease in recovery values up to 100 adsorption–desorption cycles. Cu(II)‐IMWCNT have a high stability. To check the accuracy of the developed method, certified reference materials, and water samples are analyzed with satisfactory analytical results.  相似文献   

7.
In this study, a new solid‐phase extraction procedure has been developed for preconcentration and determination of Co ions in different water samples by flame atomic absorption spectrometry (FAAS). Cobalt was preconcentrated as N,N′‐bis(pyridine‐2‐yl‐methyl)benzene‐1,4‐diamine (Co‐BPMBDA) from sample solutions using a column containing Amberlite XAD‐7 and was determined. In order to achieve the best performance for the method, effects of several parameters such as pH, concentrations of ligand, sample flow rate, eluent, and matrix ions on the method efficiency were investigated. Under optimum conditions, the preconcentration factor was found to be 200 for 1000 mL waters samples. Detection limit based on the 3Sb criterion was calculated as 0.24 µg/L for 100 mL of sample solution and relative standard deviation was found to be 1.8%. The method was applied to determine the trace amounts of cobalt in water samples.  相似文献   

8.
A new separation and preconcentration technique based on coprecipitation of Cu(II) and Ni(II) ions by the aid of Mo(VI)/di‐tert‐butyl{methylenebis[5‐(chlorobenzyl)‐4H‐1,2,4‐triazol‐3,4‐diyl]}biscarbamate (BUMECTAC) precipitate has been established. The Mo(VI)/BUMECTAC precipitate was dissolved by concentrated HNO3 and the solution was completed to 5.0 mL with distilled/deionized water. The levels of the analyte ions were determined by flame atomic absorption spectrometer. The effects of experimental conditions like HNO3 concentration, amount of BUMECTAC and Mo(VI), sample volume, etc. and also the influences of some foreign ions were investigated in detail on the quantitative recoveries of analyte ions. The preconcentration factors were found to be 40 for Cu(II) and 100 for Ni(II) ions. The detection limits for Cu(II) and Ni(II) ions based on 3σ (N:10) were 0.43 and 0.70 µg L?1, respectively. The relative standard deviations were found to be lower than 4.0% for both analyte ions. The accuracy of the method was checked by spiked/recovery tests and the analysis of two certified reference materials (Environment Canada TM‐25.3 and CRM‐SA‐C Sandy Soil C). The procedure was successfully applied to sea water and stream water as liquid samples and baby food as solid sample in order to determine the levels of Cu(II) and Ni(II) ions.  相似文献   

9.
The coprecipitation method is widely used for the preconcentration of trace metal ions prior to their determination by flame atomic absorption spectrometry (FAAS). A simple and sensitive method based on coprecipitation of Fe(III) and Ni(II) ions with Cu(II)‐4‐(2‐pyridylazo)‐resorcinol was developed. The analytical parameters including pH, amount of copper (II), amount of reagent, sample volume, etc., were examined. It was found that the metal ions studied were quantitatively coprecipitated in the pH range of 5.0–6.5. The detection limits (DL) (n = 10, 3s/b) were found to be 0.68 µg L?1 for Fe(III) and 0.43 µg L?1 for Ni(II) and the relative standard deviations (RSD) were ≤4.0%. The proposed method was validated by the analysis of three certified reference materials (TMDA 54.4 fortified lake water, SRM 1568a rice flour, and GBW07605 tea) and recovery tests. The method was successfully applied to sea water, lake water, and various food samples.  相似文献   

10.
A simple, rapid, and accurate method was developed for separation and preconcentration of trace levels of iron(III) and zinc(II) ions in environmental samples. Methyl‐2‐(4‐methoxy‐benzoyl)‐3‐(4‐methoxyphenyl)‐3‐oxopropanoylcarbamate (MMPC) has been proposed as a new complexing agent for Fe(III) and Zn(II) ions using solvent extraction prior to their determination by flame atomic absorption spectrometry (FAAS). Fe(III) and Zn(II) ions can be selectively separated from Fe(II), Pb(II), Co(II), Cu(II), Mn(II), Cr(III), Ni(II), Cd(II), Ag(I), Au(III), Pd(II), Cr(VI), and Al(III) ions in the solution by using the MMPC reagent. The analytical parameters such as pH, sample volume, shaking time, amount of MMPC reagent, volume of methyl isobutyl ketone (MIBK), effect of ionic strength, and type of back extractant were investigated. The recovery values for Fe(III) and Zn(II) ions were greater than 95% and the detection limits for Fe(III) and Zn(II) ions were 0.26 and 0.32 µg L?1, respectively. The precision of the method as the relative standard deviation changed between 1.8 and 2.1%. Calibration curves have a determination coefficient (r2) of at least 0.997 or higher. The preconcentration factor was found to be 100. Accuracy of the method was checked by analyzing of a certified reference material and spiked samples. The developed method was applied to several matrices such as water, hair, and food samples.  相似文献   

11.
This work describes the modification of silica gel with dimethylglyoxime, in order to prepare an effective sorbent for the preconcentration and determination of copper. The sorption capacity of dimethylglyoxime‐modified silica‐gel (DMGMS) was 71.37 mg g–1 and the optimum pH for the quantitative recovery of copper was found to be 5.0. The optimum flow rate, sorbent amount, and sample volume were 1 mL min–1, 300 mg, and 50 mL, respectively. 10 mL of 0.1 mol L–1 HCl was the most suitable eluent. The detection limit of copper was 6.0 ng mL–1. The recommended method, for the determination of copper, is simple and reliable, without any notable matrix effect and can be successfully applied to environmental water samples. Copper recovery in the range from 99–100% was obtained from seawater and thermal spring water using this method. The method was applied to standard reference materials, NIST‐1515 (apple leaves) and NIST‐1643e (simulated fresh water), for the determination of copper and the results were in good agreement with certified values.  相似文献   

12.
Sequential extraction procedures are widely used to characterize the different operational fractions with different potential toxicity of metals in environmental solid samples. The present work describes the application of different analytical approaches for sequential extraction of aluminum to evaluate its mobility, availability, and persistent chemical forms in sediment samples of different fresh water ecosystems (lake, canal, and river). The conventional BCR three‐stage sequential extraction procedure (C‐BCR) was modified at each stage, by applying ultrasonic device (U‐BCR), in order to shorten the required shaking time of 16 h for each three steps (excluding the hydrogen peroxide digestion in step 3, which was not performed with ultrasonic bath), could be completed in 40, 50, and 45 min, respectively. The aluminum in all extracts were determination by atomic absorption spectrometry using nitrous oxide – acetylene flame. The accuracy of results obtained from C‐BCR and proposed U‐BCR was verified with literature reported values of certified sediment sample (BCR 701). The overall recoveries of aluminum obtained by proposed U‐BCR were found in the range of 96.7–113% of those values obtained with C‐BCR for all fractions. Use of ultrasonic device, provided a large saving in extraction time relative to conventional shaking. It was observed that major part of Al in real sediment samples (80–83% of total Al) were bound to residual fraction. The acid soluble fraction of aluminum extracted by 0.11 mol/L CH3COOH has good correlation with aluminum content in corresponding water samples of each ecosystem.  相似文献   

13.
An optimized analysis method based on headspace liquid phase microextraction (HS‐LPME) and gas chromatography coupled with mass spectrometry was proposed for the determination of trihalomethanes (THMs) in drinking water. The response surface method (RSM) was used to optimize the extraction of THMs for analysis by HS‐LPME. The temperature, extraction time and NaCl concentration were found to be important extraction parameters. The coefficient of determination (R2) for the model was 94.97%. A high probability value (P < 0.0001) for the regression indicated that the model had a high level of significance. The optimum conditions were seen to be: temperature 42.0°C, NaCl concentration 0.30 g/mL, and extraction time 28 min. The response variable was the summation of the THMs chromatography peak areas and the reproducibility of this was investigated in five replicate experiments under the optimized conditions. The relative standard deviations (RSD%) of the THMs ranged from 8.0–11.6%. The limits of detection (LODs), based on a signal‐to‐noise ratio (S/N) of three ranged from 0.42–0.78 μg/L, and were lower than the maximum limits for THMs in drinking water established by the WHO.  相似文献   

14.
Conflicting sorption coefficients for ortho‐phenylphenol (OPP) have been reported in the literatures, which resulted in the conflicting assessments on OPP mobility in soil. To ascertain the sorption coefficient of OPP, batch experiments were performed based on OECD guideline 106, using three types of soils. Headspace solid‐phase microextraction (HS‐SPME) and GC‐MS were applied to the determination of OPP concentration in the liquid phase. The sorption isotherms obtained for all three soils under equilibrium conditions were described well, assuming linear sorption. The organic carbon normalized distribution coefficients (Koc) ranged from 894 to 1703 L kg?1, which suggested that OPP is moderately mobile in soil. The results also showed that the Koc value of OPP can be predicted precisely from Kow, whereas it was underestimated by one order of magnitude when water solubility is used.  相似文献   

15.
This work presents a solid phase extraction (SPE) method for simultaneous preconcentration of trace elements in water samples prior to their ICP-OES determination. Dowex 50W-x8 and Chelex-100 resins were used as SPE sorbent materials for preconcentration of trace Cd, Co, Cr, Cu, Fe, Ni, Pb and Zn. The optimum sample pH, eluent concentration and sample flow rates were found to 6, 3.0 mol L−1 and 3.0 mL min−1, respectively. In terms of multi-element preconcentration capabilities, Dowex 50W-x8 appeared to be a better sorbent. The recoveries for all the tested analytes were >95%. However, Chelex-100 showed a better performance in terms of recovery (>95%) towards Cu, Fe and Zn. Under optimized conditions using Dowex 50W-x8, the relative standard deviations for different metals were <3%. The limits of detection and limits of quantification ranged from 0.01–0.39 μg L−1 and 0.05–0.1.3 μg L−1, respectively. The accuracy of the preconcentration method was confirmed by spike recovery test and the analysis of certified reference materials. The SPE method was applied for preconcentration of the analyte ions in tap water, bottled water and wastewater samples.  相似文献   

16.
A stable extractor of metal ions was synthesized through azo linking of o‐hydroxybenzamide (HBAM) with Amberlite XAD‐4 (AXAD‐4) and was characterized by elemental analyses, IR spectral, and thermal studies. Its water regain value and hydrogen ion capacity were found to be 12.93 and 7.68 mmol g?1, respectively. The optimum pH range (with the half‐loading time [min], t1/2) for Cu(II), Cr(III), Ni(II), Co(II), Zn(II), and Pb(II) ions were 2.0–4.0 (5.5), 2.0–4.0 (7.0), 2.0–4.0 (8.0), 4.0–6.0 (9.0), 4.0–6.0 (12.0), and 2.0–4.0 (15.0), respectively. Comparison of breakthrough and overall capacities of the metals ascertains the high degree of column utilization (>70%). The overall sorption capacities for Cu(II), Cr(III), Ni(II), Co(II), Zn(II), and Pb(II) ions were found to be 0.29, 0.22, 0.20, 0.16, 0.13, and 0.11 mmol g?1 with the corresponding preconcentration factor of 400, 380, 380, 360, 320, and 320, respectively. The limit of preconcentration was in the range of 5.0–6.3 ng mL?1. The detection limit for Cu(II), Cr(III), Ni(II), Co(II), Zn(II), and Pb(II) were found to be 0.39, 0.49, 0.42, 0.59, 0.71, and 1.10 ng mL?1, respectively. The AXAD‐4‐HBAM has been successfully applied for the analysis of natural water, multivitamin formulation, infant milk substitute, hydrogenated oil, urine, and fish.  相似文献   

17.
In this study the occurrence of diclofenac and sub‐products in effluent emerging from the University Hospital at the Federal University of Santa Maria was investigated. One metabolite was identified and, in aqueous solution, three degradation products. The quantification was conducted by means of HPLC‐DAD, and the determination of metabolite and degradation products by LC–ESI–MS/MS–QTrap. For the HPLC‐DAD method, a 70:30 mixture of methanol/sodium phosphate was used in isocratic mode. For the LC–ESI–MS/MS–QTrap determinations, a mobile phase, where phase A was an ammonium acetate solution 5 × 10?3 mol L?1, and phase B was methanol (5 × 10?3 mol L?1)/ammonium acetate (9:1, v/v), on gradient mode. The LDs for the HPLC and LC–MS/MS methods, respectively, were 2.5 and 0.02 µg L?1, the LQs, 8.3 and 0.05 µg L?1, and the linear range from 10 up to 2000 µg L?1 and 0.05 up to 10 µg L?1. As expected, the LC–ESI–MS/MS–QTrap method was more sensitive and less laborious. The metabolite 4′‐hydroxy‐diclofenac was identified. Photolysis was used for the degradation studies and three products of diclofenac were identified (m/z of 214, 286 and 303) in aqueous solution. These results notwithstanding, no degradation products of diclofenac were found in the hospital effluent.  相似文献   

18.
The present paper proposes the application of multiwalled carbon nanotubes (MWCNTs) as a solid adsorbent for selective separation/preconcentration of silver(I) in water samples prior to flame atomic absorption spectrometry. The procedure is based on the solid phase extraction of Ag(I)–2‐mercaptobenzothiazole chelate on MWCNTs. The elution step is carried out with 5 mL of 2 mol L?1 HNO3 in acetone solution at a flow rate of 1.0 mL min?1. The influences of the various analytical parameters including pH of the solution, eluent type, sample volume, flow rates of eluent, matrix ions were investigated for optimization of the presented procedure. Tests of addition/recovery for analyte ion in real samples were performed with satisfactory results. Preconcentration factor and limit of detection for Ag(I) were 160 and 0.21 µg L?1, respectively. The synthesized MWCNT exhibited excellent stability in eluent solution and its adsorption capacity was 5.4 mg of silver per gram of sorbent. The proposed method was successfully applied to trace silver determination in a variety of environmental water samples.  相似文献   

19.
The present work investigated the biosorption of nickel from synthetic and electroplating industrial effluents using a green marine algae Ulva reticulata. Preliminary batch results imply that pH 4.5 was optimum for nickel uptake and the isotherm experiments conducted at this pH condition indicated that U. reticulata can biosorb 62.3 mg g–1 nickel ions from synthetic solutions, according to the Langmuir model. Desorption was effective and practical using 0.1 M CaCl2 (pH 2.5, HCl) and the biomass was regenerated and reused for three cycles. Continuous biosorption experiments were performed in an upflow packed column (2 cm I.D and 35 cm height). Among the two electroplating effluents used, effluent‐1 is characterized by excess co‐ions and high nickel ion content. This influenced the column nickel uptake with U. reticulata exhibiting 52.1 mg g–1 in the case of effluent‐1 compared to 56.5 mg g–1 in the case of synthetic solution. On the other hand U. reticulata performed well in effluent‐2 with uptakes of 53.3 and 54.3 mg g–1 for effluent‐2 and synthetic solution, respectively. Mathematical modeling of column experimental data was performed using nonlinear forms of the Thomas‐ and modified dose‐response models, with the latter able to simulate breakthrough curves with high correlation coefficients.  相似文献   

20.
A sensitive, reliable, and environmentally friendly method for simple separation and preconcentration of Ag(I) traces in aqueous samples is presented prior to their flame atomic absorption spectrometric determinations. At pH 7.0, Ag(I) was separated with 2‐(2‐methoxyphenyl)benzimidazole (MPBI) as a new complexing agent and floated after adding sodium dodecyl sulfate (SDS) as a foaming reagent. The floated layer was then dissolved in proper amount of concentrated nitric acid in methanol and introduced to the flame atomic absorption spectrometer (FAAS). The effects of pH, concentration of MPBI, type and amount of surfactant as the floating agent, type and amount of eluting agent, and influence of foreign ions on the recovery of the analyte ion were investigated. Also, using a nonlinear curve fitting method, the formation constant of 1.62 × 106 was obtained for Ag(I)–MPBI complex. The analytical curve was linear in the range of 1.8 × 10?7–1.7 × 10?6 mol/L for determination of Ag(I). The relative standard deviation (RSD; N = 10) corresponding to 0.7 × 10?6 mol/L of Ag(I), the limit of detection (10 blanks), and the enrichment factor were obtained as 1.7%, 2.9 × 10?8 mol/L, and 43.0, respectively. The proposed procedure was then applied successfully for determination of silver ions in different water samples.  相似文献   

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