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1.
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   

2.
The present study reports on the application of modified groundnut shell as a new, easily prepared, and stable sorbent for the extraction of trace amount of Cr(III) in aqueous solution. 2-Hydroxybenzaldiminoglycine was immobilized on groundnut shells in alkaline medium and then used as a solid phase for the column preconcentration of Cr(III). The elution was carried out with 3 mL of 2 mol?L?1 HCl. The amount of eluted Cr(III) was determined by spectrophotometry using cefaclor as a complexing reagent and by flame atomic absorption spectrometry (FAAS). Different experimental variables such as pH, amount of solid sorbent, volume and concentration of eluent, sample and eluent flow rate, and interference of other metal ions on the retention of Cr(III) were studied. Under the optimized conditions, the calibration curves were found to be linear over the concentration range of 13–104 and 10–75 μg?L?1 with a detection limit of 3.64 and 1.24 μg?L?1 for spectrophotometric method and FAAS, respectively. An enrichment factor of 200 and RSD of ±1.19–1.49 % for five successive determinations of 25 μg?L?1 were achieved. The column preconcentration was successfully applied to the analysis of tap water and underground water samples.  相似文献   

3.
An analytical method for the determination of diflufenican, mepanipyrim, pretilachlor, and fipronil in water samples was developed using single drop microextraction in the direct immersion mode and gas chromatography–mass spectrometry. A factorial fractionated design of type 26–1 at two levels was performed, to study the influence of experimental variables such as ionic strength, pH, agitation speed, extraction time, drop volume, and sample volume. To establish the optimal conditions for the variables that were significant, a Doehlert design was performed. The optimum conditions of extraction were 1 μL of heptane immersed in 4.0 mL of sample with continuous agitation at 500 rpm for 30 min at room temperature. The developed method proved to have good linearity for the range studied. The detection limits were 0.07 μg L?1 for diflufenican, 0.03 μg L?1 for mepanipyrim, 0.08 μg L?1 for pretilachlor, and 1.39 μg L?1 for fipronil. The method was validated on river water samples, showing the absence of matrix effect and recoveries ranged from 90.1 to 107.8 %. The results show that the method developed is accurate, sensitive, rapid, simple, and low cost, so it is recommended for application in the analysis of these different classes of pesticides in water samples.  相似文献   

4.
In this work, spectrophotometer was used as a detector for the determination of uranium from water, biological, and ore samples with a flow injection system coupled with solid phase extraction. In order to promote the online preconcentration of uranium, a minicolumn packed with XAD-4 resin impregnated with nalidixic acid was utilized. The system operation was based on U(VI) ion retention at pH 6 in the minicolumn at flow rate of 15.2 mL min?1. The uranium complex was removed from the resin by 0.1 mol dm?3 HCl at flow rate of 3.2 mL min?1 and was mixed with arsenazo III solution (0.05 % solution in 0.1 mol dm?3 HCl, 3.2 mL min?1) and driven to flow through cell of spectrophotometer where its absorbance was measured at 651 nm. The influence of chemical (pH and HCl (as eluent and reagent medium) concentration) and flow (sample and eluent flow rate and preconcentration time) parameters that could affect the performance of the system as well as the possible interferents was investigated. At the optimum conditions for 60 s preconcentration time (15.2 mL of sample volume), the method presented a detection limit of 1.1 μg L?1, a relative standard deviation (RSD) of 0.8 % at 100 μg L?1, enrichment factor of 30, and a sample throughput of 42 h?1, whereas for 300 s of the preconcentration time (76 mL of sample volume), a detection limit of 0.22 μg L?1, a RSD of 1.32 % at 10 μg L?1, enrichment factor of 150, and a sampling frequency of 11 h?1 were reported.  相似文献   

5.
This study reports the feasibility of applying directly suspended liquid-phase microextraction (DSLPME)-gas chromatography detection for the pre-concentration and determination of low levels of eight polychlorinated biphenyls (PCBs) in aqueous samples. The technique requires minimal sample preparation, analysis time and solvent consumption and represents significant advantages over conventional analytical methods. The experimental parameters such as salt content, sample temperature, stirring rate, extraction time, micro-drop volume and breakthrough volume were investigated and found to have significant influences on DSLPME. Under the optimal experimental conditions, the enrichment factor ranged from 578 to 729, and the recovery was above 93 %. Calibration curves possessed good linearity (R 2?>?0.99) over a wide concentration range of 0.1–10.0 μg L?1 with limits of detection ranging from 0.01 to 0.07 μg L?1. The relative standard deviations for 1.0 μg L?1 of PCBs in water by using internal standard were in the range 2–14 % (n?=?3). The proposed simple, accurate and sensitive analytical method was applied successfully to the determination of trace amounts of PCBs in water samples.  相似文献   

6.
Exposure to arsenic in arsenic endemic areas is most remarkable environmental health challenges. Although effects of arsenic contamination are well established, reports are unavailable on probable seasonal variation due to changes of food habit depending on winter and summer seasons, especially for endemic regions of Nadia district, West Bengal. Complete 24-h diets, drinking–cooking water, first morning voided urine samples, and diet history were analyzed on 25 volunteers in arsenic endemic Chakdah block of Nadia district, once in summer followed by once in winter from the same participants. Results depicted no seasonal variation of body weight and body mass index. Arsenic concentration of source drinking and cooking water decreased (p?=?0.04) from 26 μg L?1 in summer to 6 μg L?1 in winter season. We recorded a seasonal decrease of water intake in male (3.8 and 2.5 L day ?1) and female (2.6 and 1.2 L day?1) participants from summer to winter. Arsenic intake through drinking water decreased (p?=?0.04) in winter (29 μg day?1) than in summer (100 μg day?1), and urinary arsenic concentration decreased (p?=?0.018) in winter (41 μg L?1) than in summer (69 μg L?1). Dietary arsenic intake remained unchanged (p?=?0.24) over the seasons. Hence, we can infer that human health risk assessment from arsenic needs an insight over temporal scale.  相似文献   

7.
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   

8.
Concentrations of mercury and arsenic in fish from the Persian Gulf were determined by graphite furnace atomic absorption spectrometry. Concentrations of the metals in muscle samples were 0.049–0.402 μg g?1 for mercury and 0.168–0.479 μg g?1 for arsenic, with means of 0.133 and 0.312 μg g?1, respectively. The maximum daily consumption rate (grams per day) and meal consumption limit (meals per month) was calculated to estimate health risks associated with fish consumption. According to the results, the maximum allowable consumption rate varies between 8–56 and 15–96 g/day base on mercury and arsenic content, respectively. The results of this study indicate that the concentration of mercury and arsenic is well below the maximum permissible levels for mercury (0.5 μg g?1) and arsenic (6 μg g?1) according to international standards.  相似文献   

9.
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   

10.
A simple, rapid, and efficient sample pretreatment technique, based on solvent-based de-emulsification dispersive liquid–liquid microextraction (SD-DLLME), followed by high performance liquid chromatography (HPLC) has been developed for simultaneous preconcentration and trace detection of 2,4-dichlorophenoxyacetic acid (2,4-D) and 2-methyl-4-chlorophenoxyacetic acid (MCPA) in water and urine samples. Some parameters such as acidity of solution, the amount of salt, type, and volume of extraction solvents, type of disperser/de-emulsifier solvent, and its volume were investigated and optimized. Under optimum extraction conditions, the limits of detections (LODs) of this method for MCPA and 2,4-D were 0.2 and 0.6 μg L?1 (based on 3Sb/m) in water and 0.4 and 1.6 μg L?1 in urine, respectively. Furthermore, dynamic linear range of this method for MCPA and 2,4-D was 1–300 and 2–400 μg L?1, repectively. Finally, the applicability of the proposed method was evaluated by extraction and determination of the herbicides in urine and different water samples.  相似文献   

11.
The Mondego River estuary demonstrates signs of pollution, but the levels of endocrine disrupting compounds (EDCs), such as the natural (17β-estradiol and estrone) and pharmaceutical (17α-ethynylestradiol) estrogens, xenoestrogenic industrial pollutants (4-octylphenol, 4-nonylphenol, and their mono- and diethoxylates and bisphenol A), phytoestrogens (formononetin, biochanin A, daidzein, and genistein), and sitosterol were either poorly or never measured in this area. Thus, to conclude about the influx of EDCs in this estuary, water samples were taken every 2 months, during 1 year (2010) in low tide, at eight sites distributed along the estuary. Water samples (1 L) were preconcentrated in the Oasis HLB cartridges and cleaned in silica cartridges before their analysis by GC-MS. In summer, potentially hazardous amounts of estrogens (≈26 ng L?1), alkylphenols (≈11.5 μg L?1), alkylphenolethoxylates (≈13 μg L?1), and phytoestrogens (≈5.6 μg L?1) were measured. These data suggest that changes in the hydrodynamics of the estuary coupled with the increase of water temperatures interfere with the amount of EDCs in the water. Complementary physicochemical parameters also point to high levels of anthropogenic pollution in this area. Globally, the estrogenic load, expressed in ethynylestradiol equivalents, attained 71.8 ng L?1 demonstrating that, all together, the measured EDCs pose important health risks for both biota and humans.  相似文献   

12.
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   

13.
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   

14.
In Cambodia, groundwater has been contaminated with arsenic, and purification of the water is an urgent issue. From 2010 to 2012, an international collaborative project between Japan and Cambodia for developing arsenic-removing technology from well water was conducted and supported by the foundation of New Energy and Industrial Technology Development Organization, Japan. Quality of well water was surveyed in Kandal, Prey Veng, and Kampong Cham Provinces, and a monitoring trial of the arsenic removal equipment using our patented amorphous iron (hydr)oxide adsorbent was performed. Of the 37 wells surveyed, arsenic concentration of 24 exceeded the Cambodian guideline value (50 μg L?1), and those of 27 exceeded the WHO guideline for drinking water (10 μg L?1). Levels of arsenic were extremely high in some wells (>1,000–6,000 μg L?1), suggesting that arsenic pollution of groundwater is serious in these areas. Based on the survey results, 16 arsenic removal equipments were installed in six schools, three temples, two health centers, four private houses, and one commune office. Over 10 months of monitoring, the average arsenic concentrations of the treated water were between 0 and 10 μg L?1 at four locations, 10–50 μg L?1 at eight locations, and >50 μg L?1 at four locations. The arsenic removal rate ranged in 83.1–99.7 %, with an average of 93.8 %, indicating that the arsenic removal equipment greatly lower the risk of arsenic exposure to the residents. Results of the field trial showed that As concentration of the treated water could be reduced to <10 µg L?1 by managing the As removal equipment properly, suggesting that the amorphous iron (hydr)oxide adsorbent has high adsorbing capacity for As not only in the laboratory environment but also in the field condition. This is one of the succeeding As removal techniques that could reduce As concentration of water below the WHO guideline value for As in situ.  相似文献   

15.
Monitoring of heavy metals was conducted in the Yamuna River considering bioaccumulation factor, exposure concentration, and human health implications which showed contamination levels of copper (Cu), lead (Pb), nickel (Ni), and chromium (Cr) and their dispersion patterns along the river. Largest concentration of Pb in river water was 392 μg L?1; Cu was 392 μg L?1 at the extreme downstream, Allahabad and Ni was 146 μg L?1 at midstream, Agra. Largest concentration of Cu was 617 μg kg?1, Ni 1,621 μg kg?1 at midstream while Pb was 1,214 μg kg?1 at Allahabad in surface sediment. The bioconcentration of Cu, Pb, Ni, and Cr was observed where the largest accumulation of Pb was 2.29 μg kg?1 in Oreochromis niloticus and 1.55 μg kg?1 in Cyprinus carpio invaded at Allahabad while largest concentration of Ni was 174 μg kg?1 in O. niloticus and 124 μg kg?1 in C. carpio in the midstream of the river. The calculated values of hazard index (HI) for Pb was found more than one which indicated human health concern. Carcinogenic risk value for Ni was again high i.e., 17.02?×?10?4 which was larger than all other metals studied. The results of this study indicated bioconcentration in fish due to their exposures to heavy metals from different routes which had human health risk implications. Thus, regular environmental monitoring of heavy metal contamination in fish is advocated for assessing food safety since health risk may be associated with the consumption of fish contaminated through exposure to a degraded environment.  相似文献   

16.
Nascent Amberlite XAD-4 has been used as the polymeric support for the synthesis of a stable extractor of metal ions, by incorporating phthalic acid through azo bridging. Elemental analyses and infra-red spectral and thermal studies were carried out for its characterization. The water regain value and hydrogen ion capacity were found to be 12.50 and 5.75 mmol g?1, respectively. The optimum pH range for the maximum sorption of Ni(II), Mn(II), Cu(II), Zn(II), Cd(II), Cr(III), and Co(II) was observed at pH 5.5–8.0 with the corresponding half-loading time (t 1/2) of 9, 5, 9, 9, 3, 9, and 5 min, respectively. The preconcentration factor for Ni(II), Mn(II), Cu(II), Zn(II), Cd(II), Cr(III), and Co(II) are 190, 190, 190, 180, 180, 160, and 160, with the corresponding limit of preconcentration in the range of 5.25–6.25 μg L?1. The detection limits, for flame atomic absorption spectrophotometry, were found to be 0.62, 0.60, 0.65, 0.75, 0.72, 0.84, and 0.85 μg L?1, respectively. Method has been successfully applied to the analysis of water samples, multivitamin formulations, infant food substitutes, hydrogenated oil, and fishes.  相似文献   

17.
Ethyl(2-ethylamino)thiophenol-2,6-pyridinedicarboxylate (ETPD) was synthesized from the reaction of disodium pyridine-2,6-dicarboxylate with 1,2-dibromoethane in methanol, followed by treatment with 2-aminothiophenol. The spectral characterization of ETPD is described in detail. This electron-donating agent was successfully utilized for simultaneous enrichment of ultra trace levels of copper and lead in a wide variety of samples. By passing the aqueous solutions through octadecylsilyl bonded phase membrane disks impregnated with 12 mg of ETPD at flow rates of 45 mL min?1, Cu and Pb were selectively trapped on the disk surface over the pH range 3.0 to 7.0, whereas most other ions were negligibly retained. Numerous chemical parameters affecting sorption and subsequent elution were also investigated. The target ions were stripped from the disk surfaces by reverse flow, at rates of 12 mL min?1, and were immediately introduced to the nebulizer of an atomic absorption spectrometer. This inexpensive and off-line method offers enrichment factors of 400 and 300 and detection limits of 2.5 and 0.2 μg L?1 for copper and lead, respectively. The potential applicability of the method was confirmed by its reliable use in quantification of these elements in some real water samples, industrial effluents, three tea samples and peppers, as well as by comparison with graphite furnace atomic absorption spectrometric determinations.  相似文献   

18.
This study reports the presence of the cyanobacterial toxin cylindrospermopisn (CYN) and its producer Cylindrospermopsis raciborskii for the first time in Saudi freshwater sources. C. raciborskii was found in Gazan Dam Lake water with two morphotypes (coiled and straight). The appearance and cell density of this species was significantly positively related to high temperature and high ammonium concentrations, and negatively with nitrate and phosphate concentrations in the lake. Intracellular concentrations of CYN (4–173 μg L?1) were associated with C. raciborskii rather than other cyanobacteria with a maximal value obtained in June 2011, coinciding with the highest bloom of this species (19?×?107 trichome L?1). CYN cell quotas (0.6–14.6 pg cell?1) varied significantly along the study period and correlated with most environmental factors. The results of ELISA and liquid chromatography-mass spectrometry proved that the CYN production by strains of this species was isolated from this lake during the present study, with an amount reaching 568 μg g?1. Extracellular CYN was also detected in cell-free lake water at concentrations 0.03–23.3 μg L?1, exceeding the drinking water guideline value of 1 μg L?1 during the Apr–Jul period. As this lake is an important source for drinking and irrigation waters, CYN monitoring should be included in the environmental and health risk assessment plans of these water bodies.  相似文献   

19.
This work proposes a procedure for the determination of total selenium content in shellfish after digestion of samples in block using cold finger system and detection using atomic fluorescent spectrometry coupled hydride generation (HG AFS). The optimal conditions for HG such as effect and volume of prereduction KBr 10 % (m/v) (1.0 and 2.0 ml) and concentration of hydrochloric acid (3.0 and 6.0 mol L?1) were evaluated. The best results were obtained using 3 mL of HCl (6 mol L?1) and 1 mL of KBr 10 % (m/v), followed by 30 min of prereduction for the volume of 1 mL of the digested sample. The precision and accuracy were assessed by the analysis of the Certified Reference Material NIST 1566b. Under the optimized conditions, the detection and quantification limits were 6.06 and 21.21 μg kg?1, respectively. The developed method was applied to samples of shellfish (oysters, clams, and mussels) collected at Todos os Santos Bay, Bahia, Brazil. Selenium concentrations ranged from 0.23?±?0.02 to 3.70?±?0.27 mg kg?1 for Mytella guyanensis and Anomalocardia brasiliana, respectively. The developed method proved to be accurate, precise, cheap, fast, and could be used for monitoring Se in shellfish samples.  相似文献   

20.
The prevalence of fluorosis is mainly due to the consumption of more fluoride (F?1) through drinking water, vegetables, and crops. The objective of the study was mapping of F?1 endemic area of Newai Tehsil, Tonk district, Rajasthan, India. For the present study, water, soil (0–45 cm), and vegetation samples were collected from 17 villages. Fluoride concentration in water samples ranged from 0.3 to 9.8 mg/l. Out of 17 villages studied, the amounts of F?1 content of eight villages were found to exceed the permissible limits. Labile F?1 content and total F?1 content in soil samples ranges 11.00–70.05 mg/l and 50.3–179.63 μg g?1, respectively. F?1 content in tree species was found in this order Azadirachta indica 47.3255.76 μg g?1 > Prosopis juliflora 40.16–49.63 μg g?1 > Acacia tortilis 34.39–43.60 μg g?1. While in case of leafy vegetables, F?1 content order was Chenopodium album 54.23–98.42 μg g?1 > Spinacea oleracea 30.41–64.09 μg g?1 > Mentha arvensis 35.4851.97 μg g?1. The order of F?1 content in crops was found as 41.04 μg g?1 Pennisetum glaucum > 13.61 μg g?1 Brassica juncea > 7.98 μg g?1 Triticum sativum in Krishi Vigyan Kendra (KVK) farms. Among vegetation, the leafy vegetables have more F?1 content. From the results, it is suggested that the people of KVK farms should avoid the use of highly F?1 containing water for irrigation and drinking purpose. It has been recommended to the government authority to take serious steps to supply drinking water with low F?1 concentration for the fluorosis affected villages. Further, grow more F?1 hyperaccumulator plants in F?1 endemic areas to lower the F?1 content of the soils.  相似文献   

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