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1.
A simple and rapid ligand-less in situ surfactant-based solid phase extraction method for preconcentration of silver from water samples is developed. In this method, a cationic surfactant containing a proper alkyl group (n-dodecyltrimethylammonium bromide) is dissolved in the aqueous sample and then a proper ion-pairing agent (ClO4?) is added. Due to the interaction between surfactant and ion-pairing agent, solid particles are formed and used for adsorption of silver carbonate. After centrifugation, the sediment is dissolved in 2.0 mL 1 M HNO3 in ethanol and then aspirated directly into the flame atomic absorption spectrometer. Variables affecting the extraction efficiencies such as pH, concentrations of surfactant and CO32?, ion pair concentration, and extraction time, are optimized. Under such conditions, the calibration curve is linear from 3 to 700 μg L?1. Detection limit is 1.1 μg L?1 with an enrichment factor of 37. The relative standard deviation for eight replicate measurements of 100 μg L?1 is 2.1%. The method has been applied for the determination of silver in water samples.  相似文献   

2.
A cloud-point extraction (CPE) process using the nonionic surfactant, polyethylene glycol tert octylphenyl ether (Triton X-114) was employed for determination of Hg(II) ions in aqueous solutions. The method is based on the ion-pairing reaction of Hg(II) with Pyronin B (PyrB+) in the presence of excess iodide at pH 6.0 and extraction of the complex formed. The chemical variables affecting CPE efficiency were studied, and the analytical characteristics of the method were obtained. The calibration curves were linear in the range of 1–40 μg L?1 with the detection limits of 0.35 and 0.30 μg L?1 at 556 and 521 nm. Selectivity was also tested. The coefficients of variation of the method are 2.4% and 5.2% for five replicate measurements of mercury at levels of 10 and 25 μg L?1, respectively. The results obtained for two certified reference samples were in a good agreement with the certified values. The method was applied to the determination of total mercury in vegetable samples.  相似文献   

3.
A simple and efficient ionic liquid-based ligandless microextraction method has been developed for preconcentration of cadmium ions (Cd2+) as a step prior to its determination by flame atomic absorption spectrometry (FAAS) with a micro-sample introduction system. In this approach, the ionic liquid (IL) 1-butyl-3-methylimidazolium hexafluorophosphate [C4mim][PF6] and ethanol were used as extractant and dispersive solvents to preconcentrate the Cd2+ in different waters, acid digested scalp hair, and nail samples. Some analytical parameters influencing the extraction efficiency of Cd2+ and its subsequent determination, including pH, IL volume, dispersant solvent volume, sample volume, temperature, incubation time, and matrix effect, were optimized. Under optimal conditions, the limit of detection (LOD), limit of quantification (LOQ), and enhancement factor (EF) were 0.4 μg L?1, 1.3 μg L?1, and 50, respectively. The relative standard deviation (RSD) of 100 μgL?1 Cd2+ was 4.3% (n = 6). The validity of the proposed method was checked by determining Cd2+ in certified reference material (TM-25.3 fortified water) and standard addition; the results showed sufficient recovery (>98%) of Cd2+ within the certified value. The method was applied for preconcentration and determination of cadmium in waters and biological samples.  相似文献   

4.
The present work deals with the determination of uranium concentrations in drinking and ground water samples by laser fluorimetry and calculation of cumulative, age-dependent radiation doses to humans. The concentrations were found to be between 0.20 ± 0.03 and 64.0 ± 3.6 μg L?1, with an average of 11.1 ± 1.5 μg L?1, well within the drinking water limit of regulatory bodies. The concentrations of uranium increase with depth of water samples collection. The estimated annual ingestion dose due to the intake of uranium through drinking water for all age groups varied between 0.2 and 137 μSv a?1, with an average of 17.3 μSv a?1. The mean annual ingestion dose is 5% of the global average ingestion dose, for infants, marginally higher than for other age group. Most effective dose values were less than 20 μSv a?1.  相似文献   

5.
A Ethylene glycol dimethacrylate (EGDMA) methacrylic acid (MAA) resin was used for preconcentration of lead at trace levels in water samples. For this purpose, a flow-injection, solid phase extraction method was developed for the determination of lead by flame atomic absorption spectrometry. Lead ions were sorbed on a EGDMA–MAA column at pH 4, followed by an elution step using 288 µL of 4.0 M nitric acid solution and determination by flame atomic absorption spectrometry. Optimum conditions for quantitative sorption involving the pH, sample volume, loading and elution flow rates, eluent type, and volume were investigated. A 868-fold enrichment factor could be reached. The detection limit for the water samples, estimated from the noise on the signal obtained for 250 mL of 10 µg L?1 loaded at 4.9 mL min?1 was 1.04 µg L?1. The method was applied for lead determination in river water samples collected in Edirne, Turkey. Recoveries of spiked solutions (10 µg L?1) to river water samples were quantitative. Finally, the method was validated by the analysis of certified reference material SRM 2704 (Buffalo River Sediment).  相似文献   

6.
Abstract

A rapid and selective technique for extraction, preconcentration and determination of trace amounts of cobalt in water and pharmaceutical samples by air-assisted liquid–liquid microextraction combined with flame atomic absorption spectrometry is proposed. 1-Nitroso-2-naphthol is used as a complexing agent and 1-octanol as an extraction solvent. Parameters relevant for analytical effectivity, i.e. pH of sample solution, concentration of complexing agent, volume of extraction solvent, and number of extraction cycles are optimized using a Box–Behnken design. At optimum conditions, a dynamic linear range of 5–600?µg L?1 is obtained, with a limit of detection of 1.2?µg L?1. The method is used for determination of Co(II) in environmental water and pharmaceutical samples.  相似文献   

7.
The Sonbhadra district in the Singrauli area of Uttar Pradesh, India, has many coal mines and thermal power plants and is a critically polluted area. Many residents of this area reported adverse health conditions which may be linked to metal pollution, especially of mercury investigated here.

In May 2012, samples of water (23), soil (7), blood, hair, and nails from persons showing adverse health conditions selected at random were collected and analyzed for total mercury by atomic absorption spectrometry.

Twenty percent drinking water samples contained mercury from 3 to 26 μg L?1 (3–26 times the permissible limit). Soil samples had 0.5–10.1 mg kg?1 Hg.

The average concentrations of mercury in human blood, hair, and nails were found to be 34 μg L?1, 7.4 mg kg?1, and 0.8 mg kg?1, respectively. Mercury concentrations in the blood of these persons were 45 and 28 μg L?1 on average in the case of men and women. This is much higher than the safe level of 5.8 μg L?1 set by the United States Environmental Protection Agency (USEPA).

It was concluded that all residents of Sonbhadra sampled could be suffering from mercury toxicity as the area is polluted by Hg released from the coal-fired thermal power plants.  相似文献   

8.
A simple, fast, and low-cost analytical procedure was developed for trace-level determination of inorganic vanadium species by dispersive liquid–liquid microextraction in combination with spectrophotometry. Vanadium in pentavalent form, V(V), was quantitatively extracted into organic phase as 4-(2-pyridylazo)-recorcinol (PAR) complex in the presence of N-cetyl-N,N,N-trimethyl ammonium bromide (CTAB) as counter-ion. Vanadium (IV) was masked with 1,2-diaminocyclohexanetetraacetic acid to allow speciation analysis. Total vanadium was determined after oxidation of V(IV) to V(V). The main factors affecting preconcentration and spectrophotometric detection of vanadium species such as pH, concentration of PAR and CTAB, the type and volume of the extraction, and disperser solvents were optimized. The limit of detection and enhancement factor obtained under optimum conditions were found to be 0.06 μg L?1 and 98, respectively. Relative standard deviations for V(IV) and V(V) at 3.0 μg L?1 were less than 2.4%. The presented procedure was applied to environmental water samples for selective determination of vanadium species. Moreover, the method was applied to determination of vanadium in edible salt samples, due to its applicability in high-NaCl-containing solutions. The validity of proposed method was proven by spike recovery experiments and also independent analysis by inductively coupled plasma mass spectrometry.  相似文献   

9.
A simple, sensitive column solid-phase extraction procedure for separation and preconcentration of Cu(II), Ni(II), Co(II), and Cd(II) in spiked and natural water samples using 2,3-dihydroxynaphthalene-functionalized Amberlite XAD-4 (XAD-4-DHN) chelating resin prior to their determination by inductively coupled plasma atomic emission spectrometry was discussed. The optimum experimental parameters such as pH, volume of sample and eluent, flow-rates of uptake and stripping, and sorption capacity of the chelating resin, were evaluated. The effect of the electrolytes and the cations on the preconcentration of metal ions was also investigated. The chelating resin could be reused for more than 20 cycles of sorption–desorption without any significant change (<1.0%). Recoveries obtained from this method range from 96 to 102% with R.S.D of 2.50 (n = 4). The detection limits for Cu(II), Ni(II), Co(II), and Cd(II) were found to be 1.9, 0.9, 1.2 µg, and 1.4 µg L?1, respectively. The proposed method was applied for the determination of Cu(II), Ni(II), Co(II), and Cd(II) in spiked, tap water, and river water samples.  相似文献   

10.
A simple and sensitive solid phase extraction method was developed for simultaneous separation and preconcentration of gold and palladium ions with N-(4-methylphenyl)-2-{[(4-phenyl-5-pyridine-4-yl-4H-1,2,4-triazol-3-yl)thio]acetyl}hydrazine carbo thioamide complex on Amberlite XAD-1180 resin before their determination by flame atomic absorption spectrometry. Some analytical parameters such as HNO3 concentration of the sample solution, amount of complexing agent, sample volume, eluent type and volume, effects of foreign ions and adsorption capacity of the resin were investigated for quantitative recovery of gold and palladium ions. The effects of some anions and cations were also examined. Under optimum conditions, the detection limits for gold and palladium ions were found to be 0.29 and 0.19 μg L?1, respectively. The preconcentration factor for gold and palladium was 250. After being validated by standard addition and analysis of standard reference material, the procedure was successfully applied to the analysis of sea and stream water, anodic slime, gold ore, soil and electronic waste.  相似文献   

11.
A simple and totally organic-free (green) method, viz. headspace water-based liquid-phase microextraction combined with high-performance liquid chromatography-ultraviolet detection has been successfully developed for analysis of formic acid and acetic acid in environmental water samples. A microdrop of an aqueous solution of sodium hydroxide was suspended from the tip of a microsyringe needle over the headspace of the stirred sample solution containing the analytes at pH 1.0 for a given time. The microdrop was then retracted into the microsyringe, diluted with HPLC mobile phase, and injected to HPLC. Optimum efficiency has been achieved for: 3.0 µL NaOH microdrop (0.1 mol L?1) exposed for 15 min over the headspace of an aqueous sample of 6.5 mL at 55 °C, containing 15% w/v of Na2SO4, adjusted to pH = 1.0 and stirred at 750 rpm. Under these conditions, enrichment factors of 162 and 187, limits of detection of 0.3 and 0.1 µg L?1 (S/N = 3) with dynamic linear ranges of 1–500 and 0.5–500 µg L?1 were obtained for formic acid and acetic acid, respectively. A reasonable repeatability (5.8% ≤ RSD ≤ 8.8%, n = 6) and satisfactory linearity (r2 ≥ 0.997) illustrated the performance of the method.  相似文献   

12.
Controlled laboratory experiments were conducted to examine how photosynthesis and growth occur in Potamogeton wrightii Morong under different photoperiods and nutrient conditions. The experiment was based on a 3×2 factorial design with three photoperiods (16, 12 and 8 h) of 200 μE · m?2·s?1 irradiance and two nutrient conditions, high (90 μmol N · L?1·d?1 and 9 μmol P · L?1·d?1) and low (30 μmol N L?1·d?1 and 3 μmol P · L?1·d?1). After 14, 28, 56 and 70 days of growth, plants were harvested to determine net photosynthesis rate and various growth parameters. Above- and below-ground biomass were investigated on days 56 and 70 only. Plants under low nutrient conditions had greater leaf area, more chlorophyll a, a higher rate of net photosynthesis and accumulated more above- and below-ground biomass than plants in the high nutrient condition. Plants with an 8 h photoperiod in the low nutrient condition had a significantly higher rate of net photosynthesis, whereas 8 h photoperiod plants in the high nutrient condition had a lower rate of net photosynthesis and their photosynthetic capacity collapsed on day 70. We conclude that P. wrightii has the photosynthetic plasticity to overcome the effects of a shorter photoperiod under a tolerable nutrient state.  相似文献   

13.
Physicochemical analyses and cyanobacterial diversity of Ramgarh Lake water were performed at five sampling sites during winter, summer, and monsoon seasons. Higher load of solids, carbon, and nutrients were persistent throughout the analysis that indicates the conversion of lake from oligotrophic to eutrophic nature. High nutrients load enhanced cyanobacterial biomass, while low nutrients load produced relatively less biomass. The physicochemical parameters of water samples revealed minimum 2.9 mg L?1 dissolved oxygen (DO) at site-1 during summer, while maximum (5.6 mg L?1) at site-4 in monsoon season. Maximum biochemical oxygen demand (BOD) (40 mg L?1) and chemical oxygen demand (COD) (126 mg L?1) were recorded at site-1 during summer, whereas minimum BOD (18 mg L?1) and COD (52 mg L?1) were evident at site-3 in monsoon season. Minimum concentration of nitrate (0.72 mg L?1) was recorded at site-3 in summer, whereas maximum 2.7 mg L?1 was present at site-5 in winter season. The phosphate concentration was maximum (0.52 mg L?1) at site-5 in summer, and minimum (0.18 mg L?1) was observed at site-4 in monsoon season. Cyanobacterial diversity was higher during all the seasons, and dominated by the species of Microcystis at all the five sampling sites.  相似文献   

14.
Sea water and fish tissue samples were collected from nine sampling stations from the Great Bitter and El Temsah lakes in the Suez Canal and analysed for polycyclic aromatic hydrocarbon (PAH). The compositions of PAH determined in the dissolved fraction of sea water were measured in order to use them as chemical markers for identifying different sources of PAH pollution in this region. PAHs determined in fish tissues were measured for comparison with human health standards as consumption. The total mean PAHs concentrations in the sea water samples ranged from 0.28 to 39.57 μg l?1 with an overall mean of 10.78 and 12.38 μg l?1 for El Temsah and Bitter Lakes water, respectively. Total PAHs fractions recorded in muscle tissues of all different Osteicthyes fishes collected from Great Bitter lakes ranged from 5.8 to 218.5 μg g?1 with an overall mean of 57.98 μg g?1 during all seasons. However, they ranged from 68 to 623 μg g?1 with an overall mean of 87.69 μg g?1 recorded in El Temsah lake during four seasons (2003–2004). Benzo(a)pyrene was the most dominant PAHs found in the sea water samples from both lakes with an average concentration of 3.8 μ g l?1. Dibenzo(a,h)anthracene (DBA) was the most dominant PAHs recorded in fish samples. A maximum of 533 μg g?1 of DBA was recorded in Dahbana sp. collected from Bitter lakes during January 2004. However, a maximum of 68.7 μ g g?1 was recorded in Liza carinata species collected from El Temsah lake during July, 2004. The simultaneous occurrence of isomer ratios PHE/ANT<10 for all stations indicated that the major PAH input to water was from combustion of fossil fuel (pyrolytic source). The average ratios were 1.21 and 12.9 during winter (January 2004) and 4.3 and 8.63 during spring (April 2004) for all water samples of Great Bitter lakes and El Temsah lake, respectively. In addition, the present data demonstrate that PAHs from fossil fuel sources (MW<178) were the least significant source of PAHs in this region.  相似文献   

15.
Cleaning validation is a major challenge in multi-product pharmaceutical industries. UV spectrophotometric and HPLC methods have been developed and validated for determination of residual amount of Loratadine. Both methods were validated for linearity, range, accuracy, precision, and robustness. The limit of quantification was 1 mg L?1 by UV spectrophotometric method and 0.5 mg L?1 by HPLC method. A spike recovery study was done on a stainless steel (316 grade) plate and specific residual cleaning level (SRCL) was down to 6 μg 25.8 cm?2. Recovery was found to be more than 70%. Both methods were simple, highly sensitive, precise, and accurate, and have potential of being useful for routine quality control.  相似文献   

16.
Arsenic bioavailability in rock, soil and water resources is notoriously hazardous. Geogenic arsenic enters the body and adversely affects many biochemical processes in animals and humans, posing risk to public health. Chelpu is located in NE Iran, where realgar, orpiment and pyrite mineralization is the source of arsenic in the macroenvironment. Using cluster random sampling strategy eight rocks, 23 soils, 12 drinking water resources, 36 human urine and hair samples and 15 adult sheep urine and wool samples in several large-scale herds in the area were randomly taken for quantification of arsenic in rock/soil/water, wool/hair/urine. Arsenic levels in rock/soil/water and wool/hair/urine were measured using inductively coupled plasma spectroscopy and atomic absorption spectrophotometry, respectively. While arsenic levels in rocks, soils and water resources hazardously ranged 9.40–25,873.3 mg kg?1, 7.10–1448.80 mg kg?1 and 12–606 μg L?1, respectively, arsenic concentrations in humans’ hair and urine and sheep’s wool and urine varied from 0.37–1.37 μg g?1 and 9–271.4 μg L?1 and 0.3–3.11 μg g?1 and 29.1–1015 μg L?1, respectively. Local sheep and human were widely sick and slightly anemic. Hematological examination of the inhabitants revealed that geogenic arsenic could harm blood cells, potentially resulting in many other hematoimmunological disorders including cancer. The findings warn widespread exposure of animals and human in this agroecologically and geopolitically important region (i.e., its proximity with Afghanistan, Pakistan and Turkmenistan) and give a clue on how arsenic could induce infectious and non-infectious diseases in highly exposed human/animals.  相似文献   

17.
Dental and skeletal fluorosis is widespread in the Ethiopian Rift Valley region. Drinking water has been considered the main reason for the development of fluorosis, but dietary intake may also be a contributor in areas with high concentration of fluoride in water, soil, and biota. The purpose of this study is to assess the total daily dietary fluoride intake by adults in a rural part of the Ethiopian Rift Valley. The food, beverage, and water samples were collected from selected households of three neighboring villages with similar dietary pattern, but with different fluoride content in their water sources. Village A uses water with 1.0 mg L?1 fluoride, village B uses water with 3.0 mg L?1 fluoride, and village C uses water with 11.5 mg L?1 fluoride both for food preparation and for drinking. The level of fluoride was determined in all food ingredients, in the prepared food, beverages, and in the water used for food preparation and drinking. Recipe and food frequency questionnaires were used to gather household food preparation and consumption patterns. An alkali fusion method was used for digestion of food samples and for subsequent determination of fluoride with ion-selective electrode. The daily fluoride intake varied depending on its concentration in the water used for cooking and drinking. In households using water with 1 mg L?1, 3 mg L?1, and 11.5 mg L?1 fluoride, the total personal intake was found to be 10.5, 16.6, and 35.3 mg d?1, respectively. Contribution of the water to the daily fluoride intake was 33%, 58%, and 86%, respectively. Even in households using water containing fluoride at a concentration of 1 mg L?1, the daily intake was higher than the recommended safe intake of 1.5–4.0 mg d?1 for adults, which indicates that the fluoride intake through food may cause health risks. Minimizing the fluoride concentration in water to the lowest possible level will greatly reduce the daily intake. The form of fluorine (organic or inorganic) in the food items and the associated health risk factors need further investigation.  相似文献   

18.
The removal of arsenic from water with natural and modified clinoptilolite   总被引:1,自引:0,他引:1  
The presence of increased arsenic concentrations in Eastern Croatia is a consequence of the geological composition of the soil. Because of its known harmful effects, arsenic removal is of high importance and adsorption represents an attractive and economically efficient approach to arsenic removal. The use of zeolites obtained from the Donje Jesenje deposit, Croatia (CZ) and the Zlatokop deposit in Vranjska Banja, Serbia (SZ) in Na- and Fe–Na-modified forms was investigated in order to effectively remove arsenate and arsenite from aqueous solutions. The adsorption kinetics of arsenic was studied as a function of the initial arsenate and arsenite concentrations (30–300 μg · L?1), equilibration time (3–48 h), pH (5–10) and in the presence of sulfate and phosphate at initial concentrations of 0.2–0.5 mg · L?1. In order to estimate sorption constants designating the sorption capacity and affinity of the zeolites samples, the experimental results were fitted to the Langmuir and Freundlich sorption isotherms. Desorption tests conducted with 1–3 mol · L?1 HCl indicated that arsenate sorption was irreversible. The results obtained indicated that use of the Serbian zeolite in the Fe–Na-modified form (Fe–Na-SZ) was favourable for arsenate removal from water containing up to 30 μg As · L?1.  相似文献   

19.
The present study was conducted to establish the relationship between selected oxidative stress parameters and ultrastructural responses in liver tissue of Labeo rohita fingerlings exposed to cypermethrin. Fish were exposed to lethal (4.0 μg L?1) and sublethal (0.4 μg L?1) concentrations of cypermethrin for a period of 24, 48, 72 and 96 h for acute studies and 1, 5, 10 and 15 days for subacute studies, respectively. Results showed increased catalase (CAT) and protease activity, hydrogen peroxide (H2O2), malondialdehyde (MDA), protein carbonyls and free amino acid (FAA) levels at both concentrations. This suggests participation of free-radical-induced oxidative cell injury in mediating the hepatotoxicity of cypermethrin. In corroboration of this, ultrastructural lesions witnessed a reduction in the number of cell organelles, swollen, vacuolated and condensed mitochondria, dilated rough endoplasmic reticulum, and reduced numbers of smooth enodplasmic reticulum, peroxisomes and lysosomes at the lethal (4.0 μg L?1) concentration. At the sublethal (0.4 μg L?1) concentration, cytoplasmic vacuolation, condensed, vacuolated and swollen mitochondria, dilated rough endoplasmic reticulum and an absence of hepatocyte microvilli were prominent. Ultrastructural changes were exhibited as subcellular responses due to the imbalance in cellular oxidative status by means of oxidative damage.  相似文献   

20.
Forty-eight male Wistar albino rats were allocated to the four groups such that each comprised 12 animals. The first group was maintained as the control. In group 2, evening primrose oil was administered at a dose of 0.1 mL rat?1 day?1 (~500 mg kg?1 bw) into the stomach via gavage, whilst in group 3 sodium arsenide was administered at a concentration of 100 mg L?1 in ad-libitum drinking water for 30 days. The fourth group was given 0.1 mL rat?1 day?1 evening primrose oil into the stomach via gavage plus 100 mg L?1 of sodium arsenide in ad-libitum drinking water for 30 days. At the end of the 30th day, tissue (liver, lung, kidney, brain, heart, spleen, and testis) and blood samples were collected from each group. Malondialdehyde (MDA) and nitric oxide (NO) levels and superoxide dismutase, catalase and glutathione peroxidase activities were measured in the samples. Exposure to arsenic in rats causes oxidative stress by increasing lipid peroxidation (increase of MDA and NO levels) and altering the activity of antioxidant enzymes. Evening primrose oil did not have any adverse effects. Furthermore, it was ascertained that the administration of arsenic with evening primrose oil reduced the severity of oxidative stress.  相似文献   

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