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1.
An optical chemical sensor (optode) is proposed for the kinetic determination of nitrite ion. The optode was fabricated by the immobilization of methyl violet on a triacetylcellulose polymeric membrane. Methyl violet is covalently bonded to a transparent triacetylcellulose film. By immersion of the sensor into an acidic nitrite solution, the absorbance of the sensor at 596 nm decreases with time that is due to the reaction of nitrite with the immobilized methyl violet. A fixed time method of 15 min was used to monitor the reaction. The linear range for the determination of nitrite was 0.20–8.00 µg mL?1 and the limit of detection was 0.08 µg mL?1. The optodes were one‐shot, they had durability more than 2 months and were easily prepared. The optode was successfully applied to the determination of nitrite ion in spring water and sewage samples.  相似文献   

2.
The aim of this study is to investigate the concentrations of U, Th, V, Mo, and Zr in natural waters taken from Turkey. Among these water species, Lake Van is the largest soda lake and the fourth largest closed basin on Earth. The water samples were collected from 51 locations between 2008 and 2009. The inductively coupled plasma‐MS was used for determinations. The obtained U and Zr concentrations are in the range of 37–110 µg L?1 and 17–78 µg L?1 in Lake Van and 0.53–0.81 µg L?1 and 0.15–0.19 µg L?1 in Lake Hazar, respectively. The concentration of uranium in other studied waters varies from the lowest 0.09 µg L?1 in Tigris (Dicle) river to the highest 4.0 µg L?1 in Mediterranean Sea water. Mean Mo and V concentrations in the studied water samples were found to be in ranges of 0.1–17 and 2.7–113 µg L?1, respectively. The obtained highest U concentration in Lake Van correlates with the highest Mo and Zr levels compared to the Lake Hazar and river waters. These results imply that there is a young occurrence of uranium minerals around Lake Van. It is concluded that there is about 50.000 ton of uranium in Lake Van water.  相似文献   

3.
An on‐line solid phase extraction method for the preconcentration and determination of Cu(II) by flame atomic absorption spectrometry has been described. The procedure is based on the retention of Cu(II) ions at pH 6.0 on a minicolumn packed with Amberlite XAD‐1180 resin impregnated with chrome azurol S. After preconcentration, Cu(II) ions adsorbed on the impregnated resin were eluted by 1 mol L?1 HNO3 solution. Several parameters, such as pH, type of eluent, flow rates of sample and eluent solutions, amount of resin were evaluated. At optimized conditions, for 3.5 min of preconcentration time, the system achieved a detection limit of 1.0 µg L?1, and a relative standard deviation of 1.2% at 0.2 µg mL?1 copper. An enrichment factor of 56‐fold was obtained with respect to the copper determination. The proposed method was successfully validated by the analysis of standard reference material (TMDA 54.4 lake water) and recovery studies. The method was applied to the preconcentration of Cu(II) in natural water samples.  相似文献   

4.
In this study the occurrence of diclofenac and sub‐products in effluent emerging from the University Hospital at the Federal University of Santa Maria was investigated. One metabolite was identified and, in aqueous solution, three degradation products. The quantification was conducted by means of HPLC‐DAD, and the determination of metabolite and degradation products by LC–ESI–MS/MS–QTrap. For the HPLC‐DAD method, a 70:30 mixture of methanol/sodium phosphate was used in isocratic mode. For the LC–ESI–MS/MS–QTrap determinations, a mobile phase, where phase A was an ammonium acetate solution 5 × 10?3 mol L?1, and phase B was methanol (5 × 10?3 mol L?1)/ammonium acetate (9:1, v/v), on gradient mode. The LDs for the HPLC and LC–MS/MS methods, respectively, were 2.5 and 0.02 µg L?1, the LQs, 8.3 and 0.05 µg L?1, and the linear range from 10 up to 2000 µg L?1 and 0.05 up to 10 µg L?1. As expected, the LC–ESI–MS/MS–QTrap method was more sensitive and less laborious. The metabolite 4′‐hydroxy‐diclofenac was identified. Photolysis was used for the degradation studies and three products of diclofenac were identified (m/z of 214, 286 and 303) in aqueous solution. These results notwithstanding, no degradation products of diclofenac were found in the hospital effluent.  相似文献   

5.
Simple, rapid, and sensitive spectrophotometric methods have been proposed for the determination of cationic surfactants (CS) as cetyltrimethylammonium bromide (CTAB), dodecyltrimethylammonium (DTAB), and cetylpyridinium bromide (CPB). The methods are based on the effects of CSs on the complexes of Al3+ and Be2+ with Chrome Azurol S (CAS). The optimum reaction conditions such as CAS concentration, metal ion concentration, and pH have been studied and found to be 2.0 × 10?4 mol L?1 CAS, 0.5 mg L?1 Al3+ or 0.4 mg L?1 Be2+ and pH 5.4. The analytical characteristics of the methods such as limit of detections, limit of quantifications, and linear ranges have been obtained. CTAB, CPB, and DTAB could be determined by the Al–CAS complex in the ranges of 0.50–40.00, 0.20–10.00, and 0.40–10.00 µmol L?1, and for the Be–CAS complex in the ranges of 0.08–5.00, 0.08–3.00, and 0.20–6.00 µmol L?1, respectively. The limit of the detections of the method for the determination of CTAB, CPB, and DTAB for the Be–CAS complex has been found as 0.025, 0.024, and 0.061 µmol L?1, respectively. The interfering effect of some anions and cations was also tested. The method was applied to the determination of CS CTAB in conditioner shampoo and water samples.  相似文献   

6.
A simple and reliable method for rapid and selective extraction and determination of trace levels of Ni2+ and Mn2+ was developed by ionic liquid (IL) based dispersive liquid–liquid microextraction coupled to flame atomic absorption spectrometry (FAAS) detection. The proposed method was successfully applied to the preconcentration and determination of nickel and manganese in soil, vegetable, and water samples. After preconcentration, the settled IL‐phase was dissolved in 100 µL of ethanol and aspirated into the FAAS using a home‐made microsample introduction system. Injection of 50 µL of each analyte into an air–acetylene flame provided very sensitive spike‐like and reproducible signals. Effective parameters such as pH, amount of IL, volume of the disperser solvent, concentration of the chelating agent, and effect of salt concentration were inspected by a (25‐1) fractional factorial design to identify the most important parameters and their interactions. Under optimum conditions, preconcentration of 10 mL sample solution permitted the detection of 0.93 µg L?1 Ni2+ and 0.52 µg L?1 Mn2+ with enrichment factors 77.2 and 82.6 for Ni2+ and Mn2+, respectively. The accuracy of the procedure was evaluated by analysis of a certified reference material (CRM TMDW‐500, drinking water).  相似文献   

7.
The coprecipitation method is widely used for the preconcentration of trace metal ions prior to their determination by flame atomic absorption spectrometry (FAAS). A simple and sensitive method based on coprecipitation of Fe(III) and Ni(II) ions with Cu(II)‐4‐(2‐pyridylazo)‐resorcinol was developed. The analytical parameters including pH, amount of copper (II), amount of reagent, sample volume, etc., were examined. It was found that the metal ions studied were quantitatively coprecipitated in the pH range of 5.0–6.5. The detection limits (DL) (n = 10, 3s/b) were found to be 0.68 µg L?1 for Fe(III) and 0.43 µg L?1 for Ni(II) and the relative standard deviations (RSD) were ≤4.0%. The proposed method was validated by the analysis of three certified reference materials (TMDA 54.4 fortified lake water, SRM 1568a rice flour, and GBW07605 tea) and recovery tests. The method was successfully applied to sea water, lake water, and various food samples.  相似文献   

8.
A new method for determining lead (Pb) content was developed by dispersive liquid–liquid microextraction based on the solidification of floating organic droplets followed by flame atomic absorption spectrometry. Under optimum conditions, the calibration graph was linear within the Pb content range of 8.43–400 µg L?1 with a detection limit of 2.53 µg L?1. The relative standard deviation for 10 replicate measurements of 20 and 400 µg L?1 of Pb were 3.41 and 2.78%, respectively. The proposed method was assessed through the analysis of certified reference water and recovery experiments.  相似文献   

9.
As basis for the development of a sensitive analytical method for the determination of the insecticide alanycarb, a study of the differential pulse polarographic (DPP) reduction of alanycarb on a dropping mercury electrode (DME) was performed. The pesticide was found to give a single DP peak over the pH range 1.0 to 6.0 and the pH dependency of the peak potential showed a linear segment with a slope of 65.2 mV (at 20°C). For the analytical DPP method running at pH 6.0 (peak at –503.4 mV), the relationship between the peak current and alanycarb concentration was linear in the range of 1.10 to 9.76 μg mL–1 with a detection limit of 0.33 μg mL–1. The proposed method was applied for the determination of alanycarb in spiked dam water and orange juice samples. The recoveries calculated for both types of dam water and orange juice samples spiked with 12.0 μg mL–1 alanycarb were 96.3 and 99.0% with relative standard deviations of 5.2 and 1.3%, respectively. The sufficiently good recoveries and low relative standard deviations for the data reflect the high accuracy and precision of the proposed differential pulse polarographic method. The effects of diverse metal ions and other commonly used pesticides on the determination of alanycarb were also investigated.  相似文献   

10.
In this work, an analytical methodological study was carried out to determine the antimicrobials sulfamethoxazole and trimethoprim, as well as their metabolites, in hospital effluent. The determinations were conducted by liquid chromatography tandem mass spectrometry using a hybrid triple quadrupole‐linear ion trap mass spectrometer (LC‐QqLIT‐MS). The data acquisition was made in selected reaction monitoring (SRM) mode, in which two SRM transitions were monitored to ensure that the target compounds were accurately identified by the information dependent acquisition (IDA) function. The limits of detection (LOD) and quantification (LOQ) were 0.25 and 0.80 µg L?1 for sulfamethoxazole and 0.15 and 0.50 µg L?1 for trimethoprim. The linear range for the SMX was 0.8–100.0 µg L?1 and TMP was 0.5–100.0 µg L?1 on the basis of six‐point calibration curves generated by means of linear regression analysis. The coefficients of the correlation were higher than 0.999, which ensured the linearity of the method. The average concentration of sulfamethoxazole and trimethoprim found in hospital effluent was 27.8 and 6.65 µg L?1, respectively. The analytical methodology employed allowed two metabolites to be identified, N4‐acetyl‐sulfamethoxazole and α‐hydroxy‐trimethoprim. Fragmentation pathways were proposed.  相似文献   

11.
Water source and lake landscape position can strongly influence the physico‐chemical characteristics of flowing waters over space and time. We examined the physico‐chemical heterogeneity in surface waters of an alpine stream‐lake network (>2600 m a.s.l.) in Switzerland. The catchment comprises two basins interspersed with 26 cirque lakes. The larger lakes in each basin are interconnected by streams that converge in a lowermost lake with an outlet stream. The north basin is primarily fed by precipitation and groundwater, whereas the south basin is fed mostly by glacial melt from rock glaciers. Surface flow of the entire channel network contracted by ~60% in early autumn, when snowmelt runoff ceased and cold temperatures reduced glacial outputs, particularly in the south basin. Average water temperatures were ~4 °C cooler in the south basin, and temperatures increased by about 4–6 °C along the longitudinal gradient within each basin. Although overall water conductivity was low (<27 µS cm?1) because of bedrock geology (ortho‐gneiss), the south basin had two times higher conductivity values than the north basin. Phosphate‐phosphorus levels were below analytical detection limits, but particulate phosphorus was about four times higher in the north basin (seasonal average: 9 µg l?1) than in the south basin (seasonal average: 2 µg l?1). Dissolved nitrogen constituents were around two times higher in the south basin than in the north basin, with highest values averaging > 300 µg l?1 (nitrite + nitrate‐nitrogen), whereas particulate nitrogen was approximately nine times greater in the north basin (seasonal average: 97 µg l?1) than in the south basin (seasonal average: 12 µg l?1). Total inorganic carbon was low (usually <0·8 mg l?1), silica was sufficient for algal growth, and particulate organic carbon was 4·5 times higher in the north basin (average: 0·9 mg l?1) than in the south basin (average: 0·2 mg l?1). North‐basin streams showed strong seasonality in turbidity, particulate‐nitrogen and ‐phosphorus, and particulate organic carbon, whereas strong seasonality in south‐basin streams was observed in conductivity and dissolved nitrogen. Lake position influenced the seasonal dynamics in stream temperatures and nutrients, particularly in the groundwater/precipitation‐fed north‐basin network. Copyright © 2007 John Wiley & Sons, Ltd.  相似文献   

12.
Bezafibrate (BZF), a widely used lipid regulator, is a potential threat to ecosystems and human health in water, and the recent research showed that advanced oxidation processes (AOPs) are much more effective for BZF degradation. In this study, we investigated the photochemical decomposition of BZF in surface water and effluent from waste water treatment plants (WWTP) by UV/H2O2 process. The results showed that the UV/H2O2 process was a promising method to remove BZF at low concentration, generally at µg L?1 level. When initial concentrations reach 100 µg L?1 in the deionized water, >99.8% of BZF could be removed in 16 min under UV intensity of 61.4 µm cm?2, at the H2O2 concentration of 0.1 mg L?1, and neutral pH condition. Moreover, BZF degradation was inhibited in this process when humic acid (HA) and inorganic solution anions were added to the deionized water solutions, including chloride, nitrate, bicarbonate, and sulfate, significantly. In the surface water and effluent of WWTP, however, the removal efficiency of BZF was lower than that in the deionized water because of the interference of complex constituents in the surface water and effluent. Some main intermediates at the m/z range of 100–400 were observed by high performance LC‐MS (HPLC/MS) and a simple pathway of BZF degradation by UV/H2O2 was proposed.  相似文献   

13.
Soil denitrification in reservoir shoreline wetlands is an important process for removing excess inorganic nitrogen from upland runoff and controlling eutrophication in aquatic ecosystems. As yet, little is known about the influence of vegetation characteristics on the soil denitrification potential in reservoir shoreline wetlands, although vegetation can affect both denitrifying bacteria and soil properties. In this study, we measured the spatial variability of denitrification enzyme activity (DEA) using acetylene block method in shoreline wetlands of the Danjiangkou Reservoir, a water source of the South‐to‐North Water Transfer Project in China. Results indicated that DEA ranged from 0.001 to 2.449 µg N (N2O) g?1 h?1, with a mean of 0.384 µg N (N2O) g?1 h?1. DEA varied significantly among five representative plant communities and the highest DEA (0.248–2.449 µg N (N2O) g?1 h?1) was observed in the Polygonum hydropiper community. Plant biomass and vegetation cover were significantly and positively related to DEA and together explained 44.2% of the total variance. These results suggest that vegetation characteristics should also be considered in assessing soil denitrification capacity and restoring shoreline wetlands for nitrogen pollution removal in the Danjiangkou Reservoir after dam heightening.  相似文献   

14.
This study characterized sludge from an anoxic baffled reactor (ABR) used to treat textile dyeing wastewater. The process was run over 150 days. On day 152, five sludge samples were collected from compartments 1–5 of the ABR and a set of captive tests was conducted to investigate their particle size distributions (PSDs), dye biosorption and biodegradation properties, and dehydrogenase activity (DHA). The results indicated that the PSD of the five sludge samples from the ABR were similar. Methylene blue biosorption to the sludge samples followed the pseudo‐second‐order kinetic model and the actual biosorption process was controlled by external and intraparticle diffusion, simultaneously. After the sludge samples were cultivated for 24 h, the acid red GR dye removal efficiencies were 59.5, 68.3, 76.4, 61.5, and 65.4%, respectively. Eliminating dye biosorption, the dye biodegradation efficiencies were only 38.8, 46.3, 52.6, 48.3, and 46.0%, respectively. Furthermore, the DHA values were 28.2, 45.3, 56.5, 41.0, and 35.0 µg TF mL?1 h?1, respectively, and the DHA variation was in accordance with the dye biodegradation efficiency variation.  相似文献   

15.
Interest in preconcentration techniques for the determination of metals at ultratrace levels still continues increasingly because of some disadvantages of flameless atomic absorption spectrometry and the high costs of other sensitive methods in compared to flame atomic absorption spectrometry (FAAS). Among preconcentration techniques, solid‐phase extraction is the most popular because of a number of advantages. In this work, thiol‐containing sulfonamide resin was synthesized, characterized, and applied as a new sorption material for solid phase extraction and determination of lead in natural water samples. The optimization of experimental conditions was performed using the parameters including pH, contact time, and volumes of initial and elution solutions. After preconcentration procedure, FAAS was used for determinations. The synthesized resin exhibits the superiority in compared to the other adsorption reagents because of the fact that there is no necessity of any complexing reagent as well as high sorption capacity. Consequently, 280‐fold improvement in the sensitivity of analytical scheme was achieved by combining the slotted tube atom trap‐atomic absorption spectrometry (STAT‐FAAS) and the developed preconcentration method. The limit of detection was found to be 0.15 ng mL?1. The Pb2+ concentrations in the studied water samples were found to be in the range of 0.9–6.7 ng mL?1.  相似文献   

16.
The ultrasound‐assisted emulsification–microextraction (USAEME) method was combined with graphite furnace atomic absorption spectrometry (GFAAS) for the determination of trace Pb using dithizone (H2DZ) as chelating reagent. Some effective parameters influenced the detection and microextraction, such as ashing temperature and atomization temperature, pH, extraction solvent, sample volume, extraction time, and extraction temperature were selected and optimized. After extraction, the calibration curves for Pb was in the concentration range of 0.1–10 ng mL?1, and the linear equation was y = 0.097 x + 0.023 (R = 0.99). Under the optimized conditions, the detection limit of the method was 20 pg mL?1 with an enrichment factor of 70 and the relative standards deviation (RSD) for seven determinations of 1 ng mL?1 Pb was 11%. The proposed method was successfully applied to determine trace Pb in Yueya Lake water, pond water, and spiked samples. Furthermore, a certified reference material of Environment Water (GBW08607) was analyzed and the determined value was in good agreement with the certified value, which showed the accuracy, recovery, and applicability of the reported method.  相似文献   

17.
To investigate the levels of arsenic (As) in the water sources of Cankiri Province, the samples were collected from the stations of central Cankiri (n = 27) and Kursunlu town (n = 12) during 2009 and 2010. The concentrations of As were analyzed with an atomic absorption spectrophotometer, and then compared with permissible limit, 10 µg/L in drinking water, by Turkish legislation and World Health Organization (WHO). The As levels were higher than this limit (mean value 10–30 µg/L in 26 stations), whereas, they were found to be >30 µg/L in 12 sampling points. The water sources were categorized for health risk assessment such as reservoir, tap, well, and spring, and then chronic daily intake for oral and dermal exposure to As via drinking water, hazard quotient (HQ), and hazard index were calculated by using indices. The HQ values were found to be >1 in all samples of Cankiri Province. The effects of As on human health were then evaluated using carcinogenic risk (CR). CR values for As were also estimated to be >10?5 in drinking water samples of Cankiri Province and might exert potential CR for people. These assessments would point out required drinking water treatment strategy to ensure safety of consumers.  相似文献   

18.
Four field campaigns are carried out to quantify the methane (CH4) oxidation rate in Xiangxi Bay (XXB) of the Three Gorges Reservoir (TGR), China. The water depth of the sampling site varied from 13 to 30 m resulting from the water level fluctuation of the TGR. The CH4 oxidation rates are measured in situ as the decline of dissolved CH4 concentration versus time in incubated, and those rates. The CH4 oxidation rates range from 1.18 × 10?3 to 3.69 × 10?3 µmol L?1 h?1, with higher values and stronger variation during summer. A static floating chamber method is used to measure CH4 emitted to the atmosphere resulting in an annual mean flux of 4.79 µmol m?2 h?1. The CH4 emission rate is significantly negatively correlated with the water level. The results show that a large fraction of CH4 is consumed in the water column with a range of 28.97–55.90 µmol m?2 h?1, accounting for ≈69–98% of the total CH4 input into the water column, and more than 90% is consumed outside the summer, when the water level is lowest. Water depth, which is dominated by water level of the TGR, is a potentially important driver for CH4 oxidation and atmospheric emission in the tributary bay.  相似文献   

19.
Wetlands often form the transition zone between upland soils and watershed streams, however, stream–wetland interactions and hydrobiogeochemical processes are poorly understood. We measured changes in stream nitrogen (N) through one riparian wetland and one beaver meadow in the Archer Creek watershed in the Adirondack Mountains of New York State, USA from 1 March to 31 July 1996. In the riparian wetland we also measured changes in groundwater N. Groundwater N changed significantly from tension lysimeters at the edge of the peatland to piezometer nests within the peatland. Mean N concentrations at the peatland perimeter were 1·5, 0·5 and 18·6 µmol L?1 for NH4+, NO3? and DON (dissolved organic nitrogen), respectively, whereas peatland groundwater N concentration was 56·9, 1·5 and 31·6 µmol L?1 for NH4+, NO3? and DON, respectively. The mean concentrations of stream water N species at the inlet to the wetlands were 1·5, 10·1 and 16·9 µmol L?1 for NH4+, NO3? and DON, respectively and 1·6, 28·1 and 8·4 µmol L?1 at the wetland outlet. Although groundwater total dissolved N (TDN) concentrations changed more than stream water TDN through the wetlands, hydrological cross‐sections for the peatland showed that wetland groundwater contributed minimally to stream flow during the study period. Therefore, surface water N chemistry was affected more by in‐stream N transformations than by groundwater N transformations because the in‐stream changes, although small, affected a much greater volume of water. Stream water N input–output budgets indicated that the riparian peatland retained 0·16 mol N ha?1 day?1 of total dissolved N and the beaver meadow retained 0·26 mol N ha?1 day?1 during the study period. Nitrate dominated surface water TDN flux from the wetlands during the spring whereas DON dominated during the summer. This study demonstrates that although groundwater N changed significantly in the riparian peatland, those changes were not reflected in the stream. Consequently, although in‐stream changes of N concentrations were less marked than those in groundwater, they had a greater effect on stream water chemistry—because wetland groundwater contributed minimally to stream flow. Copyright © 2004 John Wiley & Sons, Ltd.  相似文献   

20.
Propane biosparging and bioaugmentation were applied to promote in situ biodegradation of 1,4‐dioxane at Site 24, Vandenberg Air Force Base (VAFB), CA. Laboratory microcosm and enrichment culture testing demonstrated that although native propanotrophs appeared abundant in the shallow water‐bearing unit of the aquifer (8 to 23 ft below ground surface [bgs]), they were difficult to be enriched from a deeper water‐bearing unit (82 to 90 feet bgs). Bioaugmentation with the propanotroph Rhodococcus ruber ENV425, however, supported 1,4‐dioxane biodegradation in microcosms constructed with samples from the deep aquifer. For field testing, a propane‐biosparging system consisting of a single sparging well and four performance monitoring wells was constructed in the deep aquifer. 1,4‐dioxane biodegradation began immediately after bioaugmentation with R. ruber ENV425 (36 L; 4 × 109 cells/mL), and apparent first‐order decay rates for 1,4‐dioxane ranged from 0.021 day?1 to 0.036 day?1. First‐order propane consumption rates increased from 0.01 to 0.05 min?1 during treatment. 1,4‐dioxane concentrations in the sparging well and two of the performance monitoring wells were reduced from as high as 1090 µg/L to <2 µg/L, while 1,4‐dioxane concentration was reduced from 135 µg/L to 7.3 µg/L in a more distal third monitoring well. No 1,4‐dioxane degradation was observed in the intermediate aquifer control well even though propane and oxygen were present. The demonstration showed that propane biosparging and bioaugmentation can be used for in situ treatment of 1,4‐dioxane to regulatory levels.  相似文献   

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