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1.
Spectrophotometry in combination with ionic liquid-based dispersive liquid–liquid microextraction (DLLME) was applied for the extraction and determination of formaldehyde in real samples. The method is based on the reaction of formaldehyde with methyl acetoacetate in the presence of ammonia. The variation in the absorbance of the reaction product was measured at 375?nm. An appropriate mixture of ethanol (disperser solvent) and ionic liquid, 1-hexyl-3-methylimidazoliumhexafluoro-phosphate [C6MIM][PF6] (extraction solvent) was rapidly injected into a water sample containing formaldehyde. After extraction, sedimented phase was analyzed by spectrophotometry. Under the optimum conditions, the calibration graph was linear in the range of 0.1–20?ng?mL?1 with the detection limit of 0.02?ng?mL?1 and limit of quantification of 0.08?ng?mL?1 for formaldehyde. The relative standard deviation (RSD%, n?=?5) for the extraction and determination of 0.8?ng?mL?1 of formaldehyde in the aqueous samples was 2.5%. The results showed that DLLME is a very simple, rapid, sensitive, and efficient analytical method for the determination of trace amounts of formaldehyde in wastewaters and detergents, and suitable results were obtained.  相似文献   

2.
A simple and sensitive solid phase extraction (SPE) method on multiwalled carbon nanotubes (MWCNTs) is presented for the determination of cadmium, lead, nickel, copper, and zinc at trace levels combined with flame atomic absorption spectrometry. The effects of parameters like pH, sample volume, sample and eluent flow rates, eluent concentration, and volume and type of eluent on the recovery of trace elements was examined. The metals retained on the nanotube at pH 6.5 as α-benzoin oxime complexes were eluted by 10 mL 2 M HNO3 in acetone. The influence of matrix ions on the developed method was also evaluated. The preconcentration factor of the method was found to be 50. The detection limits for Cd(II), Pb(II), Ni(II), Cu(II), and Zn(II) were found as 1.7, 5.5, 6.0, 2.3, and 2.4 μg L?1, respectively. To test the accuracy of the method, the method was applied to TMDA-70 fortified lake water and Spinach 1570A standard reference materials. Addition recovery studies were applied to tap water and cracked wheat samples, and determination of the analyte elements was carried out in some food samples with good results.  相似文献   

3.
Studies concerning the lability and bioavailability of trace metals have played a prominent role in the search for contamination of water resources. This work describes the first application yet of the diffusive gradients in thin films technique (DGT) to the determination of the fraction of free plus labile metals in waters from the Amazon Basin. Due to the complexity of the use of DGT for samples with low ionic strength and high organic matter content (characteristic of Amazonian rivers), a new analytical procedure was developed. The method is based on the determinations of apparent diffusion coefficients (Dap) in the laboratory, by performing deployments in samples collected in the corresponding sites of study. The Dap thereby determined is then used for in situ measurements. The suitability of the proposed approach for determination of labile Al, Cd, Co, Cu, Mn, Ni, and Zn in the Amazon River and Rio Negro (English: Black River) was evaluated. Except for Co, Mn (in a deployment at Rio Negro), Ni and Zn (in a deployment at Amazon River), labile in situ measurements were lower or similar to dissolved concentrations, indicating suitability of the proposed approach.  相似文献   

4.
In this study, an ultra-sensitive and highly selective, rapid flow-injection spectrophotometric method for the determination of iron (II) and total iron has been proposed. The method was based on the reaction between iron (II) and 2′, 3, 4′, 5, 7-pentahydroxyflavone in slightly acidic solution with a strong absorption at 415 nm. The carrier solution used was 1?×?10?5 M 2′, 3, 4′, 5, 7-pentahydroxyflavone in 0.1 M HAc/Ac? buffer solution at pH 4.5. Parameters that affect simultaneously the determination of iron (II) and interfering ions were tested. The relative standard deviation for the determination of 50 μg L?1 iron (II) was 0.85 % (n?=?10), and the limit of detection (blank signal plus three times the standard deviation of the blank) was 3 μg L?1, both based on injection volumes of 20 μL. The method has been successfully applied to the determination of iron (II) and total iron in water samples and ore samples. The method was verified by analysing a certified reference material Zn/Al/Cu 43XZ3F.  相似文献   

5.
The developed method is based on cold-induced aggregation microextraction of Se(IV) using the 1-butyl-3-methylimidazolium hexafluorophosphate ionic liquid as an extractant followed by spectrophotometry determination. The extraction of Se(IV) was performed in the presence of dithizone as the complexing agent. In this method, a very small amount of 1-butyl-3-methylimidazolium hexafluorophosphate was added to the sample solution containing Se-dithizone complex. Then, the solution was kept in a thermostated bath at 50 °C for 4 min. Subsequently, the solution was cooled in an ice bath and a cloudy solution was formed. After centrifuging, the extractant phase was analyzed using a spectrophotometric detection method. Some important parameters that might affect the extraction efficiency were optimized (HCl, 0.6 mol L?1; dithizone, 4.0?×?10?6 mol L?1; ionic liquid, 100 μL). Under the optimum conditions, good linear relationship, sensitivity, and reproducibility were obtained. The limit of detection (LOD) (3Sb/m) was 1.5 μg L?1, and the relative standard deviation (RSD) was 1.2 % for 30 μg L?1 of Se(IV). The linear range was obtained in the range of 5–60 μg L?1. It was satisfactory to analyze rice and various water samples.  相似文献   

6.
A procedure is detailed for the selective analysis of trace aluminum by flame atomic absorption spectrophotometer coupled with off-line column separation and preconcentration. Chelating resin was synthesized by covalent functionalization of Amberlite XAD-16 by 2-(2-hydroxyphenyl) benzoxazole. The modified resin was characterized using FT-IR spectroscopy, energy dispersive x-ray analysis, elemental analysis, thermogravimetric analysis/differential thermal analysis, and minimum energy run. The optimum sorption was at pH 9?±?0.1 with corresponding t 1/2 of only 7 min. Many competitive anions and cations studied did not interfere at all in the selective determination of Al(III), at the optimized conditions. The resin shows maximum sorption capacity of 21.58 mg g?1 and can be regenerated up to 75 cycles without any discernible capacity loss. The Langmuir isotherm model provides the better correlation of the experimental data (r 2?=?0.999) in comparison to Freundlich isotherm model, while the Scatchard analysis revealed homogeneous binding sites in the chelating resin. Analytical figures of merit were evaluated by accuracy (standard reference materials and recovery experiment), precision (RSD <5 %), and detection limit (2.8 μg L?1). The applicability was demonstrated by analysis of trace aluminum in biological, environmental, and food samples.  相似文献   

7.
A solid phase extraction method for the determination of gold(III) at trace levels by flame atomic absorption spectrometer (FAAS) was developed. The method was based on retention of gold as chloro complexes through the Amberlite XAD-2000. The effect of some analytical parameters including hydrochloric acid concentration, sample volume, sample and eluent flow rates, eluent volume, eluent concentration and interfering ions on the recovery of gold(III) was investigated. The retention of gold(III) from 1.5 mol l−1 HCl solution and the recovery of gold with 0.07 mol l−1 NH3 solution were quantitative (≥95%). The relative standard deviation (RSD) was calculated as 3.2% (n = 10). The detection limit for gold was 2 μg l−1. The accuracy was checked with the determination of gold spiked an artificial seawater and a pure copper samples.  相似文献   

8.
Highly rapid and selective vortex-assisted liquid–liquid microextraction based on solidification of organic drop has been used for determination of cobalt ion. 2-Nitroso-1-naphthol (2N1N) was used as a selective complexing agent to form stable cobalt–2N1N complex which can be extracted with 1-undecanol at a short time by the assistance of vortex agitator system followed by its determination using flame atomic absorption spectrometry. In vortex assisted, vigorous vortex stream as well as the vibrant effect of vortex system cause very fine droplets of extraction solvent to be produced and extraction occurred at a short time. Some parameters influencing the extraction process such as pH of samples, concentration of 2-nitroso-1-naphthol, extraction solvent volume, extraction time, ionic strength and surfactant addition, as well as interferences were evaluated in detail and optimum conditions were selected. At the optimum conditions, the calibration curve was linear in the range of 15 to 400 μg L?1 of cobalt ions. The relative standard deviation based on ten replicate analysis of sample solution containing 50 μg L?1 of cobalt was 3.4 %. The detection limit (calculated as the concentration equivalent to three times of the standard deviation of the blank divided by the slope of the calibration curve after preconcentration) was 5.4 μg L?1. The accuracy of the proposed method was successfully evaluated by the analysis of certified reference materials. This selective and highly rapid method was used for determination of cobalt ions in different water samples.  相似文献   

9.
This article analyses elemental composition of suspended particulate matter (SPM) samples collected monthly from 1999 to 2005 at two locations in Yokohama, Japan. Microwave digestion and inductively coupled plasma mass spectroscopy was employed to measure Mg, Al, Ca, V, Cr, Mn, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Ag, Cd, Cs, Ba, Pb, and Bi. Water-soluble ions (Na?+?, NH4 ?+?, K?+?, Ca2?+?, Cl???, NO3 ???, and SO4 2???) and carbonaceous mass (elemental and organic carbon) were detected using ion chromatograph and CHN analyzer, respectively. The results indicate that the composition of SPM on one of the sites is determined by automobile emissions and on the other by industrial combustions. The impact of the emission regulations for automobiles in large Japanese cities, which were enacted during 2002 and 2003, on the SPM composition of the samples is also studied.  相似文献   

10.
A novel nanomaterial has been developed for speciation of Cr(III) and Cr(VI) in water and soil samples. In this study, a new type of alumina-coated magnetite nanoparticles (Fe3O4/Al2O3 NPs) modified by the surfactant Triton X-114 has been successfully synthesized and used in magnetic mixed hemimicelles solid-phase extraction procedure. The procedure was based on the reaction of chromium(III) with 1-(2-pyridilazo)-2-naphtol as a ligand, yielding a complex, which was entrapped “in situ” in the surfactant hemimicelles. The concentration of chromium(III) was determined using flame atomic absorption spectrometry. After reduction of Cr(VI) to Cr(III) by ascorbic acid, the system was applied to the total chromium. Cr(VI) was then calculated as the difference between the total Cr and the Cr(III) content. This method can also be used for complicated matrices such as soil samples without any special pretreatment. Under the optimum conditions of parameters, the recoveries of Cr(III) by analyzing the spiked water and soil samples were between 98.6 and 100.8 % and between 96.5 and 100.7 %, respectively. Detection limits of Cr(III) were between 1.4 and 3.6 ng?mL?1 for water samples and 5.6 ng?mg?1 for soil samples.  相似文献   

11.
In this work are presented results of the complex study of two significant solid environmental samples: gravitation dust sediments (industrial pollutants, potential source of risk elements input to soils) and soils (component of the environment, potential source of risk elements input to food web). The first phase of this study was focused on the study of the significant chemical properties (phase composition, content of organic and inorganic carbon) of the dust and soil samples. In the second phase, the fractionation analysis was used on the evaluation of the mobility of chosen risk elements (Cu, Ni, Pb, Zn) in the studied samples. The single-step extractions were applied in the order of the isolation of the element forms (fractions), with different mobilities during defined ecological conditions by utilization of the following reagents: 1 mol dm − 3 NH4NO3 for isolation of the “mobile” fraction, 0.05 mol dm − 3 ethylenediaminetetraacetic acid and 0.43 mol dm − 3 CH3COOH for isolation of the “mobilizable” fraction, and 2 mol dm − 3 HNO3 for isolation of all releasable forms. On the basis of the results obtained in this study, it is possible to state that different origins and positions of solid environmental samples in the environment reflect in different chemical properties of their matrix. The different properties of the sample matrix result in different mobilities of risk elements in these kinds of samples. The fractionation analysis with single-step extraction for isolation element fractions is the method most suitable for easy checking of environmental pollution and for evaluation of risk elements cycle in the environment.  相似文献   

12.
In this study, a ternary Zr(IV) system with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) and fluoride was chosen on the basis of dispersive liquid–liquid microextraction method. Zirconium was extracted into the fine droplets of dichlorobenzene as extracting solvent. These drops dispersed as a cloud in the aqueous sample with the help of ultrasonic waves, and the procedure was done. Finally, atomic absorption spectrometry was applied for the determination of zirconium. The effects of different factors that influence complex formation and extraction, such as pH, amounts of complexing agents, type and volume of the extracting solvent, as well as sonication and centrifuging time, were optimized. Under optimum conditions, the calibration curve was linear in the range of 150.0–800.0 ng mL?1 with a limit of detection of 44.0 ng mL?1. Relative standard deviation was calculated to be 4.1 % (n?=?7, c?=?400.0 ng mL?1). The enrichment factor was 80. The proposed method was successfully used to determine the zirconium in several water, wastewater, and soil samples.  相似文献   

13.
A new kinetic method has been developed for the determination of iodine in water samples. The method is based on the catalytic effect of I? with the oxidation of Indigo Carmine (IC) by KBrO3 in the sulfuric acid medium. The optimum conditions obtained are 0.16 M sulfuric acid, 1?×?10?3 M of IC, 1?×?10?2 M KBrO3, reaction temperature of 35°C, and reaction time of 80 s at 612 nm. Under the optimized conditions, the method allowed the quantification of I? in a range of 12–375 ng/mL with a detection limit of 0.46 ng/mL. The method was applied to the determination of iodine in river and city water samples with the satisfactorily results.  相似文献   

14.
New solid-phase extractor (MWCNTs-5-ASA) was synthesized via covalent immobilization of 5-aminsalicylic acid onto multi-walled carbon nanotubes (MWCNs). The success of the functionalization process was confirmed using Fourier transform infrared spectroscopy, scanning electron microscope, and surface coverage determination. Batch experiments were conducted as a function of pH to explore MWCNTs-5-ASA efficiency to extract several metal ions viz., Cr(III), Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Pb(II). It was found that Pb(II) exhibits the highest extraction percentage with maximum adsorption capacity 32.75 mg g?1. Its binding performance was well fitted with Langmuir sorption isotherm. On the other hand, the selective separation and preconcentration of trace Pb(II) under dynamic conditions prior to determination by inductively coupled plasma-optical emission spectrometry was investigated under different parameters. These included the rate of flow and volume of sample solution, in addition to the type of the eluate, its volume and concentration. The effect of a variety of foreign ions on the recovery percentage was also evaluated. Trace Pb(II) ions present in 500 mL aqueous solution adjusted to pH 4.0 were retained on 50 mg of MWCNTs-5-ASA and completely eluted using 4.0 mL of 2 M HNO3. The limit of detection and the precision of the method were 0.25 ng mL?1 and 2.8 %, respectively (N?=?5). This methodology has been applied for the determination of Pb(II) in water samples with good results.  相似文献   

15.
Quercetin (3,3,4,5,7-pentahydroxyflavone) chemically bonded through pyran rearrangement on modified controlled pore silica glass (QCPSG) with a capacity 0.213 mmol/g was used for solid phase extraction of some toxic metal and metalloid ions. The newly designed QCPSG quantitatively sorbs As(V), Cd(II), Hg(II), and Pb(II) at the pH range 7.5–8.5 after 10 min of stirring. HCl (1 mol L???1) instantaneously elutes all the metal ions. The sorption capacity of the ion collector is 0.42, 0.46, 0.53, and 0.49 mmol g???1 for As(V), Cd(II), Hg(II), and Pb(II), respectively, whereas the preconcentration factor is 200. The effect of NaCl, Na2SO4, NaF, NaBr, Na3PO4, and other interfering salts on the sorption of metal ions (50 μg L???1) was reported. Analytical detection limits of As(V), Cd(II), Hg(II), and Pb(II) were 4.18, 2.44, 15.86, and 25.00 pg mL???1, respectively. QCPSG was used in the separation of the investigated metal ions from some natural water samples collected from diverse origins followed by determination by inductively coupled plasma–mass spectrometry. The data were compared with those obtained by the standard methods of determination using atomic absorption (hydride generation, HGAAS and after solvent extraction with ammonium pyrolidine dithiocarbamate/methyl isobutyl ketone). The suggested solid phase extraction method was found accurate with no random error.  相似文献   

16.
A total of 16 people died and over 500 people were hospitalized due to diarrhoeal illness in the Bholakpur area of Hyderabad, India on 6th May 2009. A study was conducted with immediate effect to evaluate the quality of municipal tap water of the Bholakpur locality. The study consists of the determination of physico-chemical properties, trace metals, heavy metals, rare earth elements and microbiological quality of drinking water. The data showed the variation of the investigated parameters in samples as follows: pH 7.14 to 8.72, EC 455 to 769 μS/cm, TDS 303.51 to 515.23 ppm and DO 1.01 to 6.83 mg/L which are within WHO guidelines for drinking water quality. The water samples were analyzed for 27 elements (Li, Be, B, Na, Mg, Al, Si, K, Ca, V, Cr, Mn, Fe, Ni, Co, Cu, Zn, As, Se, Rb, Sr, Mo, Ag, Cd, Sb, Ba and Pb) using inductively coupled plasma-mass spectrometry (ICP-MS). The concentrations of Fe (0.12 to 1.13 mg/L), Pb (0.01 to 0.07 mg/L), Cu (0.01 to 0.19 mg/L), Ni (0.01 to 0.15 mg/L), Al (0.16 to 0.49 mg/L), and Na (38.36 to 68.69 mg/L) were obtained, which exceed the permissible limits of the World Health Organization (WHO) for drinking water quality guidelines. The remaining elements were within the permissible limits. The microbiological quality of water was tested using standard plate count, membrane filtration technique, thermotolerant coliform (TTC), and most probable number (MPN) methods. The total heterotrophic bacteria ranged from 1.0 × 105 to 18 × 10cfu/ml. Total viable bacteria in all the water samples were found to be too numerable to count and total number of coliform bacteria in all water samples were found to be of order of 1,100 to >2,400 MPN index/100 ml. TTC tested positive for coliform bacteria at 44.2°C. All the water samples of the study area exceeded the permissible counts of WHO and that (zero and minimal counts) of the control site (National Geophysical Research Institute) water samples. Excessively high colony numbers indicate that the water is highly contaminated with microorganisms and is hazardous for drinking purposes. Bacteriological pollution of drinking water supplies caused diarrhoeal illness in Bholakpur, which is due to the infiltration of contaminated water (sewage) through cross connection, leakage points, and back siphoning.  相似文献   

17.
Seventeen fog events were sampled in Baton Rouge, Louisiana during 2002–2004 as part of characterizing wet deposition by fogwater in the heavily industrialized corridor along the Louisiana Gulf Coast in the United States. These samples were analyzed for chemical characteristics such as pH, conductivity, total organic and inorganic carbon, total metals and the principal ion concentrations. The dominant ionic species in all samples were NH4+, NO3, Cl and SO42−. The pH of the fogwater sampled had a mean value of 6.7 with two cases of acidic pH of 4.7. Rainwater and fogwater pH were similar in this region. The acidity of fogwater was a result of NO3 but partly offset by high NH4+. The measured gaseous SO2 accounted for a small percentage of the observed sulfate concentration, indicating additional gas-to-particle conversion of SO2 to sulfate in fogwater. The gaseous NOx accounted for most of the dissolved nitrate and nitrite concentration in fogwater. The high chloride concentration was attributable to the degradation of chlorinated organics in the atmosphere. The metal composition was traced directly to soil-derived aerosol precursors in the air. The major metals observed in fogwater were Na, K, Ca, Fe, Al, Mg and Zn. Of these Na, K, Ca and Mg were predominant with mean concentrations > 100 μM. Al, Fe and Zn were present in the samples, at mean concentrations < 100 μM. Small concentrations of Mn (7.8 μM), Cu (2 μM), Pb (0.07 μM) and As (0.32 μM) were also observed in the fogwaters, and these were shown to result from particulates (PM2.5) in the atmosphere. The contribution to both ions and metals from the marine sources in the Louisiana Gulf Coast was minimal. The concentrations of all principal ionic species and metals in fogwater were 1–2 orders of magnitude larger than in rainwater. Several linear alkane organic compounds were observed in the fogwater, representing the contributions from petroleum products at concentrations far exceeding their aqueous solubility. A pesticide (atrazine) was also observed in fogwater, representing the contribution from the agricultural activities nearby.  相似文献   

18.
A new complexing agent, 2-((2-((1H-benzo[d]imidazole-2yl)methoxy)phenoxy)methyl)-1H-benzo[d]imidazole (BIMPI), was used in cloud point extraction and applied for selective pre-concentration of trace amounts of cadmium in cigarette samples. Cadmium was complexed with BIMPI in a buffer solution (pH?=?10) using Triton X-114 as surfactant and quantitatively extracted into a small volume of the surfactant-rich phase after centrifugation. Under optimized conditions (pH?=?10.0, 0.8?×?10?4?mol?L?1 BIMPI and 0.08 % (w/v) Triton X-114), calibration graph was linear in the range of 34.0–1,670.0 μg?L?1. The proposed method was applied to the determination of Cd in various cigarette (tobacco) samples which gave satisfactory results.  相似文献   

19.
A novel improved preconcentration method known as rapidly synergistic cloud point extraction (RS-CPE) was established for nickel preconcentration and determination prior to its determination by flame atomic absorption spectrometry. In this work, the traditional CPE pattern was changed and greatly simplified in order to be applicable in metal extraction and detection. This method was accomplished in room temperature in 1 min. Non-ionic surfactant Triton X-114 was used as extractant. Octanol worked as cloud point revulsant and synergic reagent. The various parameters affecting the extraction and preconcentration of nickel such as sample pH, 2,2′-Furildioxime concentration, amounts of octanol, amounts of Triton X-114, type of diluting solvent, extraction time, and ionic strength were investigated and optimized. Under optimal conditions, the calibration curve showed an excellent linearity in the concentration range of 2–200 μg L?1, and the limit of detection was 0.6 μg L?1 for nickel. The developed method was successfully applied for the determination of nickel in food and water samples. The results showed that, the proposed method can be used as a cheap, rapid, and efficient method for the extraction and preconcentration of nickel from real samples.  相似文献   

20.
This study reports a very selective, easy, and precise method for rapid separation of trace amounts of copper in aqueous samples using octadecyl silica-bonded phase membrane disks modified by 2,2'-[ethane-1,2-diylbis(thio)]dianiline (EDTD) combined with flame atomic absorption spectrometric determination. In addition, the synthesis and spectral characterization of EDTD have been described in detail. All the affecting experimental variables such as pH, amount of modifier, eluent type, sample and eluent flow rate, interfering ions, and disk capacity were also investigated. The target analyte (trace copper) was quantitatively retained at pH?=?4 and eluted with 6.0 mL of 0.5 M HNO3 at flow rates of 40 and 10 mL min?1 for analyte passage and elution steps, respectively, through the disks modified with 17.0 mg of EDTD. The proposed method also allows an enrichment factor of about 500 and has a detection limit of 0.005 ng mL?1. The method has been successfully applied for isolation and determination of copper in different water samples, peppers, and standard alloys.  相似文献   

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