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1.
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   

2.
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   

3.
4-[N,N-(Diethyl)amino] benzaldehyde thiosemicarbazone (DEABT) is proposed as an analytical reagent for the spectrophotometric determination of platinum(IV). The DEABT forms 1:2 yellow complex with Pt(IV), which is sparingly soluble in water and completely soluble in water–ethanol–DMF medium. The Pt(IV)–DEABT complex shows maximum absorbance at 405 nm. Beer’s law is valid up to 7.80 μg cm???3, and optimum concentration range for the determination of platinum(IV) is 0.48–7.02 μg cm???3. The molar absorptivity and Sandell’s sensitivity of the method are found to be 1.755 × 104 dm3 mol???1 cm???1 and 0.0012 μg cm???2, respectively. The relative error and coefficient of variation (n?=?6) for the method does not exceed ±0.43% and 0.35%, respectively. Since the method tolerates a number of metal ions commonly associated with platinum, it can be employed for the determination of platinum in environmental samples, pharmaceutical samples, alloys, catalysts, and complexes. The method is rapid as the Pt(IV)–DEABT complex is soluble in water–ethanol–DMF medium and not requiring any time consuming extraction method for the complex.  相似文献   

4.
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   

5.
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   

6.
High selenium (Se) concentrations have been found in surface waters in the Kendrick Reclamation Project, Wyoming. Precipitation and irrigation water moving over seleniferous soils are contributing causes, and drought may exacerbate this. This study surveyed Se concentrations and discharges in local surface streams, irrigation drains, and the delivery canal. Sites were sampled monthly and analyzed for Se and total suspended solids (TSS). A completely randomized design with two factors (soil parent material and location, inside or outside irrigation district) was used. Mean Se concentrations were 64 μg L???1 inside the irrigation district on shale soils, 17 μg L???1 inside the district off shale soils, 5 μg L???1 outside the district on shale soils, and 3 μg L???1 outside the district off shale soils. Correlations between discharge and Se concentrations were generally negative, while correlations between discharge and Se load were generally positive. There was little correlation between load and concentration, and little correlation between TSS and Se. A comparison of Se concentrations in streams and drains showed Se concentrations were significantly higher (p?<?0.001) in streams during the irrigation season, but not in the off-season (p?=?0.515). We conclude that higher discharges decrease Se concentration, but increase load. Conversion from flood to sprinkle irrigation may increase Se concentrations by reducing discharge, but decrease Se loads going into the N. Platte River, and will likely alter the timing and magnitude of flows. Both load and concentration should be considered when implementing Se regulations and standards.  相似文献   

7.
A new kinetic method has been developed for the determination of nitrite in fruit juice samples. The method is based on the catalytic effect of nitrite with the oxidation of Nile Blue A (NBA) by KBrO3 in the sulfuric acid medium. The optimum conditions obtained are 1.2 mM sulfuric acid, 0.034 mM of NBA, 2.8?×?10?3 M KBrO3, reaction temperature of 20 °C, and reaction time of 100 s at 595.5 nm. Under the optimized conditions, the method allowed the quantification of nitrite in a range of 0.2–800 μg/mL with a detection limit of 0.02 μg/mL. The method was applied to the determination of nitrite in 15 brands of fruit juice samples.  相似文献   

8.
A field study was conducted on a small urban watershed (residential and golf course dominated) in southern Nevada to assess the concentration and speciation of selenium (Se) in a series of drain lines and monitoring wells and to quantify the mass discharge of Se from the drain system. Water samples were collected on a monthly basis and analyzed for total Se, selenate (SeO4 =) and selenite (SeO3 =). In addition, where possible, flow was assessed as was, temperature, redox potential, pH, dissolved oxygen (DO) along with all major cations and anions. The data were then modeled with PhreeqC to identify selenium speciation. Results revealed a SeO4 = dominated system with SeO4 = concentrations ranging from 13 to 62 ppb. In the monitoring wells, 66 % of the variation in the total Se concentration could be described based on depth to groundwater, temperature and sulfate concentrations (P?<?0.001). In particular, higher total Se concentrations were predicted for shallower depth to groundwater, suggesting the solubilization of Se evapo-concentrates near the surface could be reduced by lowering water tables. The highest of all correlations was found between SeO4 = concentrations (↑) and the sodium (↑) and DO (↑) concentrations in the monitoring wells (R 2?=?0.77, P?<?0.001). An excellent curvilinear relationship was found between total Se and the electrical conductivity in the water (R 2?=?0.73, P?<?0.001). Based on the Se data and time line identified in this study, high concentrations of Se could be expected to drain from this area for many years to come, with salinity acting as a good proxy for Se concentration. In the drain lines, Se concentrations were found to be invariant to flow (P?>?0.05). Flow discharge from the main drain system to the Las Vegas Wash was estimated at 559 acre feet during the 1 year study period. This flow was estimated to carry 4,203 Mg of salts 6.71 Mg of nitrate-N and 27.1 kg of total Se.  相似文献   

9.
A simple, rapid, and efficient dispersive liquid–liquid microextraction method, followed by UV–Vis spectrophotometry was developed for the preconcentration and determination of Pd ions in water samples. Pd ions react with α-furildioxime (chelating agent) to form a hydrophobic complex. Various parameters were altered to study and optimize their effects on the extraction efficiency, such as pH, ligand concentration, the type and volume of extraction and dispersive solvents, extraction time, and salt concentration. Under optimized conditions, the method exhibited an enrichment factor (C org/C aq) of 25 and recovery more than 98 % within a very short extraction time. The linearity of the method ranged from 10 to 200 μg?L?1. The limit of detection was 1.1 μg?L?1. The relative standard deviation for the concentration of 100 μg?L?1 of Pd was 2.3 % (n?=?10). Finally, the developed method was successfully applied to the extraction and determination of Pd in tap, river, mineral, and sea water samples.  相似文献   

10.
Quizalofop ethyl, a phenoxy propionate herbicide, is used for postemergence control of annual and perennial grass weeds in broad-leaved crops in India. The experiments were designed to study the dissipation kinetics of quizalofop ethyl on onion for two seasons. A simple, rapid, and sensitive method for estimation of quizalofop ethyl residues in onion and soil was developed and validated. The recoveries of quizalofop ethyl residues from onion and soil at different spiking level range from 84.81 to 92.68 %. The limit of quantification of this method was found to be 0.01 μg g?1. The risk assessment through consumption of the onion in comparison to its acceptable daily intake which is an important parameter for the safety of the consumer was also evaluated. Standardized methodology supported by recovery studies was adopted to estimate residues of quizalofop ethyl on onion and soil. The average initial deposits of quizalofop ethyl on onion were observed to be 0.25 and 0.33 mg kg?1, following single application of the herbicide at 50 g active ingredient (a.i.) ha?1 during 2009 and 2010, respectively. The half-life values (T 1/2) of quizalofop ethyl on onion crop were worked out to be 0.85 and 0.79 days, respectively, during 2009 and 2010. At harvest time, the residues of quizalofop ethyl on onion and soil were found to be below the determination limit of 0.01 mg kg?1 following single application of the herbicide at 50 and 100 g a.i. ha?1 for both the periods.  相似文献   

11.
The dissipation kinetics and method for estimation of residues of chlorpyrifos and lambda-cyhalothrin in cardamom were studied and developed. The limit of detection and limit of quantitation arrived for the compounds were 0.01 and 0.025 μg?g?1, respectively. Gas chromatographic response of chlorpyrifos and lambda-cyhalothrin residues was linear in the range of 0.01–0.50 μg?g?1 and the mean recovery obtained was 97.3 % for chlorpyrifos and 98.9 % for lambda-cyhalothrin with satisfactory relative standard deviation values. The mean initial residues of chlorpyrifos applied at a concentration of 0.05 % in cardamom was 2.5 μg?g?1 and the residue was 8.1 μg?g?1 after processing, with a processing factor of 3.24, while lambda-cyhalothrin when applied at 0.0025 % resulted in initial residues of 1.63 μg?g?1 that magnified to 4.86 μg?g?1 on curing, with a processing factor of 2.98. The half-life of chlorpyrifos was in the range of 5.1–5.24 days while that of lambda-cyhalothrin was in the range of 4.40–4.55 days. The processing factor arrived at in the above experiment lead to the conclusion that the residues of chlorpyrifos got magnified to 3.24–3.68 times and that of lambda-cyhalothrin got magnified to 2.98–3.46 times of initial residues, consequent to loss of weight due to dehydration during curing.  相似文献   

12.
The determination of mercury in crude oil and petroleum products is particularly difficult due to the volatile nature of both mercury and the matrix, which may lead to significant loss of the analyte. A simple extraction method for total mercury has been developed to determine total mercury in crude oil using cold vapor atomic fluorescence spectrometry. The homogenized crude oil sample was diluted to 5, 10, and 20 % (w/w) in toluene. The diluted crude oil samples were spiked with 10 and 40 μg/kg (w/w). The samples were extracted using an oxidant/acid solution, BrCl/HCl. The mercury was extracted into the aqueous phase; the ionic mercury was then reduced to volatile elemental mercury (Hg0) by stannous chloride (SnCl2). The mercury vapor was detected by Merlin cold vapor atomic fluorescence spectrometry at a 253.7-nm wavelength. The average recoveries for mercury in spiked diluted crude oil (10 and 40 μg/kg, w/w) were between 96 and 103 %, respectively, in 5 and 10 % spiked diluted crude oil. Whereas, low recoveries (<50 %) were recorded in 20 % diluted spiked crude oil. The method detection limit was calculated as t (0.01)(n ? 1)?×?SD where t is the student's value for 99 % confidence level and standard deviation estimate with n???1 degrees of freedom. The method detection limit was found to be 0.38 μg/kg based on 5 g of diluted crude oil sample. The method is sensitive enough to determine low levels of mercury in crude oil.  相似文献   

13.
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   

14.
In this study, a challenging preconcentration/separation method based on the sorption of manganese on ethylene glycol dimethacrylatemethacrylic acid copolymer (EGDMA-MA) treated with ammonium pyrrolidine dithiocarbamate (APDC) and its slurry analysis by electrothermal atomic absorption spectrometry was described. Optimum conditions for quantitative sorption, as well as for preparing a homogeneous and stable slurry were investigated. A 100-fold enrichment factor could be reached. The analyte element in certified sea-water and bovine-liver samples were determined in the range of 95% confidence level. The proposed technique is fast, simple, and the risk of contamination is low. The limit of detection of the method for manganese in the slurry of the blank subjected to the proposed procedure was 0.07 μg L?1 (3δ, N:10) corresponding to 0.56 μg kg?1 slurry.  相似文献   

15.
The dissipation and residues of bispyribac-sodium in rice cropping system were studied. Bispyribac-sodium residues were extracted by a simple analytical method based on QuEChERs and detected by LC-MS/MS. The limit of detection for bispyribac-sodium of this method was 0.375?×?10?3 ng. The limit of quantification (LOQ) was 5.0 μg/kg for rice plant samples, 2.0 μg/kg for rice hull, 0.2 μg/kg for water, and 0.1 μg/kg for soil and husked rice samples. The average recoveries of bispyribac-sodium ranged from 74.7 to 108 %, with relative standard deviations less than 13 %. The half-lives of bispyribac-sodium in rice plant, water, and soil were in the range of 1.4–5.6 days. More than 90 % of bispyribac-sodium residue dissipated within 5 days. The final residues of bispyribac-sodium in rice were all below LOQ at harvest time.  相似文献   

16.
This study focuses on mercury (Hg) bioaccumulation in Indian cat fish, Wallagoo attu and Mystus aor, from different rivers. Methyl mercury (MeHg) concentrations were determined in muscle tissue of two different parts, ventral and dorsal part, of each species and the levels of organic mercury were co-related with lipid content of each part. The MeHg concentrations increased in a linear fashion with both weight and age for these river species. The average concentration of MeHg was found to be 0.93?±?0.60 and 1.26?±?0.62 μg Hg g?1 (expressed in wet weight basis) for ventral and dorsal parts, respectively in W. attu and this was above the 0.25 μg Hg g?1 of wet weight, the limit set by the Prevention of Food Adulteration Act for the maximum level for consumption of fish exposed to mercury pollution. In M. Aor the concentration of MeHg was not above the standard limit but threatening, it was 0.22?±?0.07 and 0.23?±?0.08 μg Hg g?1 (expressed in wet weight basis) in dorsal and ventral parts, respectively.  相似文献   

17.
This work proposes the quantification of Cr (VI) ions in natural waters in trace level, using activated alumina (Al2O3) as preconcentration support, controlled in-line dissolution of the solidified chromophore diphenylcarbazide after heat treatment and spectrophotometric detection. The manifold ensures high sensitivity of analytical response, good repeatability, and stability. In this work, optimization of experimental conditions of a flow injection system was chosen as the parameters for greater sensitivity and better selectivity. The selected optimized conditions were 0.30 mol L?1 for H2SO4 concentration, system flow rate as 0.40 mL min?1, sample injection volume of 192.50 μL, 2 min for preconcentration time, and 0.10 mol L?1 for eluent concentration. The analytical curves obtained for real sample analysis show linear range from 0.192 to 0.961 μM, linear correlation coefficient R?=?0.9997 and LOD?=?0.024 μM. The preconcentration factor of about four times was obtained through the passage of 800 μL of a standard solution containing 0.961 μM of Cr (VI) through mini-column of preconcentration followed by elution at 192.5 μL of NH4OH 0.1 mol L?1 solution. The solid chromogenic reagent presented high durability (weeks in daily use with mass of 0.0993 g) and good reproducibility in analytical signal. The reactivation of the mini-column of alumina should be executed after ten injections of eluent, using 800 μL of HCl 0.02 mol L?1 solution in flow through the same. Each cycle of injection and elution of the sample takes about 5 min on the proposed terms. Despite the length of each cycle still be high, low concentrations can be detected using a technique of relatively low cost. This is due in part, the association dissolution of the chromogenic reagent directly in the line and the preconcentration step. Another important factor is the economy of reagent chromogenic, low generation of reject contributing to better quality of the environment, and the high potential for applications to work in field.  相似文献   

18.
A simple, sensitive, and accurate UV spectrophotometric method has been developed for the determination of nickel in synthetic mixture and water samples. The method is based on the complexation reaction of nickel ion with cefixime, thus leading to the formation of Ni–cefixime complex in ethanol-distilled water medium at room temperature. The complex showed the maximum absorption wavelength at 332 nm. Beer’s law is obeyed in the working concentration range of 0.447–4.019 μg?mL?1 with apparent molar absorptivity of 7.314?×?103?L?mol?1?cm?1 and Sandell’s sensitivity of 0.008 μg/cm2/0.001 absorbance unit. The limits of detection and quantitation for the proposed method are 0.016 and 0.054 μg?mL?1, respectively. The factors such as cefixime concentration and solvent affecting the complexation reaction were carefully studied and optimized. The method is validated as per the International Conference on Harmonisation guideline. The method is successfully applied to the determination of Ni(II) in synthetic mixture and wadi water samples collected from Al Rustaq. The same water samples are also analyzed by atomic absorption spectrophotometry. Both methods determined the amount of Ni(II) in water sample and found to be approximately the same.  相似文献   

19.
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   

20.
Supervised field trials were conducted at four different agro-climatic locations of India to evaluate the dissipation pattern and risk assessment of spiromesifen on tomato. Spiromesifen 240 SC was sprayed on tomato at 150 and 300 g a.i.?ha?1. Samples of tomato fruits were drawn at 0, 1, 3, 5, 7, 10 and 15 days after treatment and soil at 15 days after treatment. Quantification of residues was done on gas chromatograph–mass spectrophotometer in selective ion monitoring mode in the mass range of 271–274 (m/z). The limit of quantification of the method was found to be 0.05 mg kg?1, while the limit of determination was 0.015 mg kg?1. Residues were found below the LOQ of 0.05 mg kg?1 in 10 days at both the doses of application at all the locations. Spiromesifen dissipated with a half-life of 0.93–1.38 days at the recommended rate of application and 1.04–1.34 days at the double the rate of application. Residues of spiromesifen in soil were detectable level (<0.05 mg kg?1) after 15 days of treatment. A preharvest interval (PHI) of 1 day has been recommended on tomato on the basis of data generated under All India Network Project on Pesticide Residues. Spiromesifen 240 SC has been registered for its use on tomato by Central Insecticide Board and Registration Committee, Ministry of Agriculture, Government of India. The maximum residue limit (MRL) of spiromesifen on tomato has been fixed by Food Safety Standard Authority of India, Ministry of Health and Family Welfare, Government of India as 0.3 μg/g after its risk assessment.  相似文献   

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