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1.
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   

2.
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   

3.
A new spectrophotometric method is reported for the determination of nanomolar level of malachite green in surface water samples. The method is based on the catalytic effect of silver nanoparticles on the oxidation of malachite green by hexacyanoferrate (III) in acetate–acetic acid medium. The absorbance is measured at 610 nm with the fixed-time method. Under the optimum conditions, the linear range was 8.0?×?10?9–2.0?×?10?7?mol?L?1 malachite green with a correlation coefficient of 0.996. The limit of detection (S/N?=?3) was 2.0?×?10?9?mol?L?1. Relative standard deviation for ten replicate determinations of 1.0?×?10?8?mol?L?1 malachite green was 1.86 %. The method is featured with good accuracy and reproducibility for malachite green determination in surface water samples without any pre-concentration and separation step.  相似文献   

4.
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   

5.
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   

6.
A modified LC-MS method for the analysis of mepiquat residue in wheat, potato, and soil was developed and validated. A hydrophilic interaction liquid chromatographic column has been successfully used to retain and separate the mepiquat. Mepiquat residue dynamics and final residues in supervised field trials at Good Agricultural Practice (GAP) conditions in wheat, potato, and soil were studied. The limits of quantification for mepiquat in all samples were all 0.007 mg kg?1, which were lower than their maximum residue limits. At fortification levels of 0.04, 0.2, and 2 mg kg?1 in all samples, recoveries ranged from 77.5 to 116.4 % with relative standard deviations of 0.4–7.9 % (n?=?5). The dissipation half-lives (T 1/2) of mepiquat in soil (wheat), wheat plants, soil (potato), and potato plants were 4.5–6.3, 3.0–5.6, 2.2–4.6, and 2.4–3.2 days, respectively. The final residues of mepiquat were below 0.153 mg kg?1 in soil (wheat), 0.052–1.900 mg kg?1 in wheat, below 0.072 mg kg?1 in soil (potato), and below 1.173 mg kg?1 in potato at harvest time. Moreover, pesticide risk assessment for all the detected residues was conducted. A maximum 0.0012 % of acceptable daily intake (150 mg kg?1) for national estimated daily intake indicated low dietary risk of these products.  相似文献   

7.
This paper highlights the levels of anions (nitrate, nitrite, sulfate, bromide, chloride, and fluoride) and cations (potassium, sodium, magnesium, and calcium) in selected springs and groundwater sources in the urban-west region of Zanzibar Island. The levels of total dissolved solids (TDS) and sodium adsorption ratio (SAR) were also studied. Thirty water samples were collected in December 2012 from various types of water sources, which included closed hand-dug wells (CHDW), open hand-dug wells (OHDW), springwater (SW), public bore wells (PBW), and bore wells owned by private individuals (BWP), and analyzed after filtration and sometimes dilution. The cations were analyzed using inductively coupled plasma-optical emission spectrometry (ICP-OES). The anions were analyzed by chemically suppressed ion chromatography (IC). The ranges of the levels of the investigated parameters were as follows: Na 13.68–3,656 mg L?1, K 2.66–583 mg L?1, Mg 0.63–131.10 mg L?1, Ca 16.79–189.9 mg L?1, Cl? 8.61–4,340.97 mg L?1, F? 0–1.02 mg L?1, Br? 0–10.88 mg L?1, NO3 ? 0.18–342.4 mg L?1, NO2 ? 0–1.39, SO4 2? 4.43–534.02 mg L?1, TDS 7–6,380 mg L?1, and SAR 0.63–50. Except fluoride, most of the studied parameters in the water samples had concentrations beyond the permissible limits of the World Health Organization (WHO). The elevated concentrations are a result of seepage of contaminated water from on-site septic tanks, pit latrines, landfill leachates, fertilizer applications, and domestic effluents. These results should alert domestic water stakeholders in Zanzibar to the urgent task of initiating a quick mitigation response to control these alarming water risks.  相似文献   

8.
A new method has been developed to determine heptachlor and its metabolites heptachlor-exo-epoxide and heptachlor-endo-epoxide in pork. The pork samples were extracted with acetone–n-hexane (2:8, V:V) and cleaned up by gel permeation chromatography and florisil solid-phase extraction cartridge. The extract was then determined by gas chromatography equipped with electron capture detector (GC-ECD), followed by validation using gas chromatography–mass spectrometry (GC–MS) with negative chemical ionization. Linearity of calibration curves ranged from 0.01 to 0.5 mg L?1, with correlation coefficients of more than 0.9980 for GC-ECD and GC–MS, respectively. At spiked concentrations of 0.01, 0.05, and 0.1 mg kg?1, the average recovery and relative standard deviation values were 87.1–102.2 and 4.0–11.3 %, respectively. The limit of quantification for each analyte was 0.01 mg kg?1, which satisfied the current maximum residue limit permitted in pork. Our results showed that the method developed was successfully used to determine heptachlor and heptachlor epoxide residues in real pork samples.  相似文献   

9.
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   

10.
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   

11.
A novel and robust method for the simultaneous determination of lead, cadmium, arsenic, and nickel in atmospheric particulate matter by multi-element electrothermal atomic absorption spectrometry was developed, using zirconium–iridium coating as permanent modifier (140 μg Zr and 4 μg Ir). After 300 atomization cycles, it was necessary to add 2 μg of Ir. Due to the varying concentrations of Pb in atmospheric particulate matter, lead was monitored at two wavelengths, at the less sensitive line of 261.4 nm for high concentration samples (>20 μg?L?1) or at 283.3 nm for the low concentration samples. Matrix-matched calibration had to be performed for quantitative recoveries (96–102 %). Following this approach, the four elements were determined in atmospheric particulate matter samples from an industrial area near the city of Athens in two different time periods (cold–warm) with limits of detection of 5.5 ng?m?3 for Pb at 261.4 nm and 0.29 ng?m?3 at 283.3 nm, 0.019 ng?m?3 for Cd, 0.14 ng?m?3 for As, and 0.22 ng?m?3 for Ni. Lead, Cd, and As levels were very low, whereas Ni content was at comparable levels with other areas worldwide.  相似文献   

12.
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   

13.
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   

14.
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   

15.
The aim of this study was to evaluate the incidence of total aflatoxin (AF), ochratoxin A, T-2 toxin, deoxynivalenol (DON), zearalenone (ZEA), and fumonisin (FB) in dairy cattle, beef cattle, and lamb–calf feeds. A total of 180 dairy cattle, beef cattle, and lamb–calf feeds (60 samples each) were randomly collected from farms, feed mills, and villages in Burdur province, between September 2006 and August 2007. All samples were analyzed by the competitive Enzyme Linked Immuno Sorbent Assay (ELISA). The most frequent mycotoxin detected was total AF, which was found in 108 samples (60 %) in concentrations ranging from 3.82 to 116.83 μg?kg?1, followed by DON that was detected in 87 samples (48.3 %), in concentrations ranging from 18.50 to 500 μg?kg?1. Ochratoxin A (OTA), T-2 toxin, ZEA, and FB were found in 84 (46.7 %), 85 (47.2 %), 57 (31.7 %), and 19 (10.6 %) samples, respectively, in concentrations of 1.01 to 15.85 μg?kg?1 for OTA, 3.85 to 52.36 μg?kg?1 for T-2 toxin, 2.10 to 29.30 μg?kg?1 for ZEA, and 2.69 to 4.96 mg?kg?1 for FB. It was concluded that feed samples in Burdur province were contaminated by mycotoxins, and the levels of total aflatoxin in the samples were considered a risk to animal health.  相似文献   

16.
We assessed the effects of seasonal dynamics on the physico-chemical qualities and heavy metals concentrations of the Umgeni and Umdloti Rivers in Durban, South Africa. Water samples were taken from nine different sampling points and analysed for the following parameters; temperature, pH, turbidity, electrical conductivity (EC), biological oxygen demand (BOD5), chemical oxygen demand (COD), phosphate (PO4 2?), nitrate (NO3 2?), ammonium (NH4 +), sulphate (SO4 2?), lead (Pb2+), mercury (Hg2+), cadmium (Cd2+), aluminium (Al3+), and copper (Cu2+) using standard methods. The data showed variations it terms of the seasonal fluctuations and sampling regime as follows: temperature 12–26.5 °C; pH 5.96–8.45; turbidity 0.53–18.8 NTU; EC 15.8–5180 mS m?1; BOD5 0.60–7.32 mg L?1; COD 10.5–72.9 mg L?1; PO4 2??<?500–2,460 μg L?1; NO3 2? <0.05–4.21 mg L?1; NH4 +?<?0.5–1.22 mg L?1; SO4 2? 3.90–2,762 mg L?1; Pb2+ 0.023–0.135 mg L?1; Hg2+ 0.0122–0.1231 mg L?1 Cd2+ 0.068–0.416 mg L?1; Al3+ 0.037–1.875 mg L?1, and Cu2+0.006–0.144 mg L?1. The concentrations of most of the investigated parameters exceeded the recommended limit of the South African Guidelines and World Health Organization tolerance limits for freshwater quality. We conclude that these water bodies are potentially hazardous to public health and this highlights the need for implementation of improved management strategies of these river catchments for continued sustainability.  相似文献   

17.
The aim of the present work is the assessment of a new sorbent, prepared using silica gel coated with a pyrimidine derivative (allyl 6-methyl-4-phenyl-2-thioxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate), for extraction and preconcentration trace amount of lead from different samples prior to determination by flame atomic absorption spectrometry. Common coexisting ions did not interfere with the separation and determination of lead at pH?6, so that lead ion completely adsorbed on the column. The limit of detection based on three times the standard deviation of the blank was found to be 0.53 ng?mL?1 in original solution. Obtained sorption capacity for 1 g sorbent was 5.0 mg Pb. The linearity was maintained in the concentration range of 0.1–30.0 ng?mL?1 for the concentrated solution. Eight replicate determinations of 2.0 μg?mL?1 of lead in the final solution gave relative standard deviation of ±2.6 %. The proposed method was successfully applied to the determination trace amounts of lead in the environmental samples such as carrot, rice, zardchoobe, and real water samples.  相似文献   

18.
The results of an innovative study on a new and highly efficient stationary phase based on the SnO2 nanorods coating on fused silica have been reported in this paper. SnO2 nanorods have been grown on fused silica fibers using a hydrothermal process. The extraction properties of the fiber were investigated using headspace solid-phase microextraction (HS-SPME) mode coupled with gas chromatography–mass spectrometry detection for 1,4-dichloro-2-nitrobenzene, biphenyl, and acenaphthene. The effect of different variables on extraction efficiency was studied simultaneously using Box–Behnken method as experimental design. The variables of interest in the HS-SPME were salt effect, adsorption temperature, extraction, and desorption time. Under optimal conditions, the calibration curves were linear up to 102–105 ng?L?1 (R 2?>?0.998) with detection limits of 10?3, 10?1, and 10 ng?L?1 for acenaphthene, biphenyl, and 1,4-dichloro-2-nitrobenzene, respectively. The relative standard deviations for single fiber and fiber to fiber were less than 9.8 and 12.5 %, respectively. The high stability of the SnO2 nanostructure coating is proved at relatively high temperatures (up to 300 °C) with a high extraction capacity and long lifespan (more than 100 times). By applying the proposed technique, promising recoveries (93–98 %) were obtained in the analysis of environmental water samples.  相似文献   

19.
A new electrochemical adsorptive stripping voltammetry method was developed for the determination of trace amounts of copper in food and water samples. The study of electrochemical behavior of Cu ion indicated that Cu(II) and Schiff base formed a complex in H3BO4–NaOH buffer solution (pH?=?7.25). An accumulation potential of ?100 mV (vs Ag/AgCl) was applied while the solution was stirred for 60 s. The response curve was recorded by scanning the potential, and the peak current of ?0.31 V (vs Ag/AgCl) was recorded. The peak current and concentration of copper accorded with linear relationship in the range of 0.04–120 ng mL?1. The relative standard deviation (for 12 ng mL?1 of copper) was 1.73 %, and the detection limit was 0.007 ng mL?1. The possible interference of some common ions was studied. The proposed method was applied to the determination of copper in water, rice, wheat, tea, milk, and tomato with satisfactory results.  相似文献   

20.
This study analyzes the concentrations and health risks of fluoride in 249 drinking water samples collected from different regions of Anhui Province in China. Results indicated that fluoride content in drinking water ranged from 0.12 to 1.94 mg L?1 (mean?=?0.57 mg L?1) in the following order: Huaibei plain region > Jianghuai hill region ≈ Dabieshan mountainous region > plain along the Yangtze River region > southern Anhui mountainous region. The fluoride contents were less than 0.50 mg L?1 in 66.66 % of the drinking water samples, 0.51–1.0 mg L?1 in 23.29 %, and higher than 1.0 mg L?1 in 12.04 %. The fluoride levels in some samples were lower than the recommended values for controlling dental caries (0.50–1.0 mg L?1). The total fluoride intake from drinking water was between 0.14 and 2.33 mg per day in different regions of the province, supposing an individual consumes 1.2 L of water per day. Therefore, measures should be taken to increase fluoride intake in the Jianghuai hill region, Dabieshan mountainous region, plain along the Yangtze River, and southern Anhui mountainous region to control dental caries. On the other hand, the fluoride levels must be reduced in the Huaibei plain region to decrease endemic fluorosis. The results serve as crucial guidelines for managing fluoride safety in drinking water and controlling endemic fluorosis in different regions of Anhui Province.  相似文献   

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