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1.
A method for the determination of nickel in water was developed. The procedure involves preconcentration of nickel by using dispersive liquid–liquid microextraction. The Ni(II) ions were extracted in chloroform in the form of complex with the reagent 2‐(2′‐benzothiazolylazo)‐p‐cresol. Ethanol was used as the disperser solvent. After injection of the extracting mixture in a solution of nickel, a cloudy mixture was observed. A quick centrifugation induces phase separation and thus the settling of rich phase. The nickel content in the rich phase is measured by flame atomic absorption spectrometry. Under optimal conditions, the limit of detection and quantification obtained were 1.4 and 4.7 µg L?1, respectively. Some parameters used to characterize preconcentration systems, such as enrichment factor and consumption index were calculated and resulted in 29 and 0.34 mL, respectively. After optimization of variables and determination of analytical characteristics, the method was used for the analysis of certified reference materials (BCR‐713: wastewater, effluent and BCR‐414: plankton) and real water samples.  相似文献   

2.
Waste water from ammunition production sites and aqueous samples (ground and surface water) on or near former military sites on which explosives were produced or filled, e.g. into shells, may be contaminated by the original explosives—mainly nitrotoluenes (such as dinitrotoluenes, trinitrotoluene (TNT)) and nitramines (such as hexogen (RDX), octogen (HMX), and tetryl) or hexyl, but also by byproducts and compounds formed by biodegradation of the explosives such as aminonitrotoluenes, chlorinated nitrobenzenes and nitrophenols. These compounds can be extracted from aqueous samples by liquid/liquid extraction (using dichloromethane or toluene) or by solid phase extraction using C-18 adsorbents with high recoveries (usually ≥85%) provided they contain only one amino group. Nitrotoluenes, chlorinated nitrobenzenes and aminonitrotoluenes (nitrotoluidines) may be determined by gas chromatography (GC) using selective detectors such as an electron capture detector (ECD), a nitrogen-phosphorus detector (NPD) or a chemiluminescence detector (thermal energy analyzer, TEA). The use of combined gas chromatography/mass spectrometry (GC/MS) under electron impact conditions is even more specific. Detection limits comparable to an ECD or NPD, however, are only achieved if the mass spectrometer is operated under selected ion monitoring (SIM). Nitrophenols are derivatized after extraction by heptafluorobutyric anhydride or by acetic anhydride where the latter method can be directly applied to the aqueous sample. The nitramine explosives, such as RDX, HMX, and tetryl, hexyl, the nitrate esters, such as nitropenta (PETN) and nitroguanidine as well as picric acid cannot, or only with difficulty, be analyzed by gas chromatography. They may be determined by high performance liquid chromatography (HPLC) with UV-detection. The HPLC analysis can be extended to include also nitrotoluenes and nitroaminotoluenes.  相似文献   

3.
In this study, a new solid‐phase extraction procedure has been developed for preconcentration and determination of Co ions in different water samples by flame atomic absorption spectrometry (FAAS). Cobalt was preconcentrated as N,N′‐bis(pyridine‐2‐yl‐methyl)benzene‐1,4‐diamine (Co‐BPMBDA) from sample solutions using a column containing Amberlite XAD‐7 and was determined. In order to achieve the best performance for the method, effects of several parameters such as pH, concentrations of ligand, sample flow rate, eluent, and matrix ions on the method efficiency were investigated. Under optimum conditions, the preconcentration factor was found to be 200 for 1000 mL waters samples. Detection limit based on the 3Sb criterion was calculated as 0.24 µg/L for 100 mL of sample solution and relative standard deviation was found to be 1.8%. The method was applied to determine the trace amounts of cobalt in water samples.  相似文献   

4.
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   

5.
Fulvic acids of different origin, spray deposited on polished silicon after dissolution in high‐purity water without any additives, were analysed by time‐of‐flight secondary ion mass spectrometry (TOF‐SIMS) in combination with oblique 24...36 keV SF5+ ion bombardment. The observed, highly reproducible mass spectra cover more than five orders of magnitude in dynamic range, without background subtraction. Apart from lines due to atomic ions and low‐mass ion fragments, the mass spectra exhibit broad maxima between m/z 200...350, mainly due to a beat‐like superposition of lines at every single mass number, up to at least m/z 400. In the negative ion spectra the beats have a spacing of m/z 14, corresponding to a CH2‐unit. The high‐mass tails of the spectra extend well beyond m/z 5000, with similar slopes in the positive and the negative ion mass spectra. The negative spectra appear to be less affected by fragmentation products than the positive spectra. Fulvic acids (FAs) of different origin show distinctly different spectra, with mean masses ranging between m/z ≈ 450 and 580 (for a low‐mass cut‐off m/z 150). To further verify the ability of TOF‐SIMS to detect molecules and clusters with masses significantly above the maxima of the FA spectra, samples of glycyrrhizic acid (GA, as GA ammonium salt with molecular weight 840) were also analysed. Parent ions as well as multimers (GA)n were observed as positive and negative ions, up to n = 4 (m/z 3320). The results are compared with spectra recently obtained by other mass spectrometric techniques.  相似文献   

6.
A new separation and preconcentration technique based on coprecipitation of Cu(II) and Ni(II) ions by the aid of Mo(VI)/di‐tert‐butyl{methylenebis[5‐(chlorobenzyl)‐4H‐1,2,4‐triazol‐3,4‐diyl]}biscarbamate (BUMECTAC) precipitate has been established. The Mo(VI)/BUMECTAC precipitate was dissolved by concentrated HNO3 and the solution was completed to 5.0 mL with distilled/deionized water. The levels of the analyte ions were determined by flame atomic absorption spectrometer. The effects of experimental conditions like HNO3 concentration, amount of BUMECTAC and Mo(VI), sample volume, etc. and also the influences of some foreign ions were investigated in detail on the quantitative recoveries of analyte ions. The preconcentration factors were found to be 40 for Cu(II) and 100 for Ni(II) ions. The detection limits for Cu(II) and Ni(II) ions based on 3σ (N:10) were 0.43 and 0.70 µg L?1, respectively. The relative standard deviations were found to be lower than 4.0% for both analyte ions. The accuracy of the method was checked by spiked/recovery tests and the analysis of two certified reference materials (Environment Canada TM‐25.3 and CRM‐SA‐C Sandy Soil C). The procedure was successfully applied to sea water and stream water as liquid samples and baby food as solid sample in order to determine the levels of Cu(II) and Ni(II) ions.  相似文献   

7.
High resolution gas chromatography (HRGC) with ECD, NFID and MSD is a very efficient determination method for pesticides in water. Because of their relatively low concentrations in aquatic systems enrichment and preconcentration procedures are essential. Some examples for pesticide determination by GC methods are given. Potentials and limitations of HRGC for pesticide analysis are also discussed. An extensive pesticide analysis in water has to include different methods like HRGC, HPLC and GC/MS.  相似文献   

8.
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   

9.
Grassland degradation resulting from global climate change, overgrazing, and rodent damage is expected to influence the magnitude of canopy hydrological fluxes because of reduced vegetation biomass and changed species composition. The objectives of this study were to estimate herbaceous canopy rainfall storage capacity (S) along three different stages of sub‐alpine grassland degradation (non‐degraded, lightly degraded and moderately degraded) in the Qinghai–Tibetan Plateau, China, and relate changes in S to canopy properties. An artificial wetting method and the water budget balance method, using rain simulations, were used for estimating S. Grassland degradation significantly reduced S. In non‐degraded, lightly degraded and moderately degraded grasslands, S estimated using the artificial wetting method were 0.612 ± 0.08 mm, 0.289 ± 0.04 mm, and 0.217 ± 0.01 mm, respectively; S estimated using the water budget balance method were 0.979 ± 0.32 mm, 0.493 ± 0.13 mm, and 0.419 ± 0.09 mm, respectively. These changes could be explained by accompanying changes in above‐ground biomass and leaf area index, as well as changes in species composition. Species‐specific rainfall storage capacity varied by a factor of 2.7 among the investigated species, with graminoids having the lowest values. Leaf area index was more correlated to S than was canopy coverage. Converting fresh weight of non‐leaf tissues into effective leaf area of the corresponding species and then introducing a coefficient of leaf area according to the specific storage capacity of leaves improved the linear relationship between S and leaf area index. Copyright © 2011 John Wiley & Sons, Ltd.  相似文献   

10.
An optimized analysis method based on headspace liquid phase microextraction (HS‐LPME) and gas chromatography coupled with mass spectrometry was proposed for the determination of trihalomethanes (THMs) in drinking water. The response surface method (RSM) was used to optimize the extraction of THMs for analysis by HS‐LPME. The temperature, extraction time and NaCl concentration were found to be important extraction parameters. The coefficient of determination (R2) for the model was 94.97%. A high probability value (P < 0.0001) for the regression indicated that the model had a high level of significance. The optimum conditions were seen to be: temperature 42.0°C, NaCl concentration 0.30 g/mL, and extraction time 28 min. The response variable was the summation of the THMs chromatography peak areas and the reproducibility of this was investigated in five replicate experiments under the optimized conditions. The relative standard deviations (RSD%) of the THMs ranged from 8.0–11.6%. The limits of detection (LODs), based on a signal‐to‐noise ratio (S/N) of three ranged from 0.42–0.78 μg/L, and were lower than the maximum limits for THMs in drinking water established by the WHO.  相似文献   

11.
Micropollutants cover a variety of compounds that mainly originate from the pharmaceutical and agricultural sectors. Even at trace concentrations, the discharge of micropollutants into water bodies pose a serious threat to the environment and human health. Their removal from wastewaters at treatment plants before their discharge into the environment has become one of the leading topics of research. Physical, chemical, and biological treatment methods have been listed in the literature for efficient removal of a variety of pollutants. In this study, seven micropollutants, namely 4‐tert‐octylphenol, atrazine, 2,4,6‐trichlorophenol, fluoxetine, estrone, penconazole, and di‐n‐octyl phthalate, are spiked into municipal simulated synthetic wastewater and treated by a laboratory‐scale electrooxidation (EO) system using oxidized titanium and graphite electrode as anode and cathode, respectively. Sensitive determination of the selected micropollutants by gas chromatography–mass spectrometry (GC‐MS) before and after treatment is performed after their pre‐concentration using an eco‐friendly switchable solvent liquid‐phase microextraction method (SSLPME). The pH value, applied current, and reaction period are optimized to enhance the removal efficiency of micropollutants. Results show that the highest removal efficiency of all micropollutants is obtained at pH 3, 20 min reaction period, and 3 A applied current. The operational costs are also investigated in this study.  相似文献   

12.
Rainfall was simulated on unconfined plots on regolith in debris flow source areas using a portable simulator. In total, 351 simulations were carried out on steep slopes (27–54°) with rainfall intensities of 28–291 mm/h. From these rainfall simulations the infiltration parameters sorptivity (S) and steady-state infiltration capacity (K) of the regolith, and a threshold for the occurrence of micro-scale mass movements, were obtained. Two evaluation methods were used to obtain the infiltration parameters K and S. The ‘infiltration envelope’ method uses rainfall intensity and time to ponding from multiple tests and fits an infiltration envelope through the data from which K and S can be obtained. The ‘constant runoff’ method uses rainfall intensity and overland flow intensity to calculate K, after which S can be calculated in several ways by using time to ponding. The constant runoff method produced K values of 16.6–128 mm/h, which usually show a log-normal distribution. K values depend on the regolith parent material and rainfall intensity. Using this method, S values are 0.088–0.381 cm/min1/2. The infiltration envelope method produced K values of 9.8–131 mm/h and S values of 0.14–0.32 cm/min1/2. It can be argued that both methods overestimate K as well as S, but quantitative relations between measured/calculated and actual values of K and S have not yet been obtained. At high rainfall intensities, typically 100 mm/h or more, micro-scale mass movements sometimes occur. A lower threshold curve for the occurrence of these micro-scale mass movements has been constructed. It is a function of both slope angle and rainfall intensity. The micro-scale mass movements could play an important part in the initiation of debris flows in the study area, possibly by delivering sediment to overland flow. On the very steep slopes, the sediment-rich overland flow can easily mobilize coarse material.  相似文献   

13.
Dissolved high molecular weight organic substances, like humic substances, can be characterized with regard to their molecular weight distribution using gel filtration chromatography (GFC). In addition, the adsorption properties, for example on activated carbon, can be described, if the substances are separated by hydrophobic interaction chromatography (HIC) in different fractions using a chromatographic column with a hydrophobic matrix. The retention time (Rt) of single chemical substances in this column can be used to characterize the hydrophobicity or hydrophility of each compound as well as of the high molecular weight organic matter. The hydrophobic interaction between the matrix of the column and the dissolved chemical compounds also depends on the hydrophobicity of the gel and the composition of the eluent. Relations between retention times, log P-coefficients (octanol/water partition) and K-values of isotherms on activated carbon (Freundlich equation) were found.  相似文献   

14.
This paper presents the results from analyses of water samples from 15 Bulgarian reservoirs and lakes for detection of microcystins presence by high‐performance liquid chromatography (HPLC) coupled to a ultraviolet (UV) and photo diode array (PDA) detector. In 3 of the studied drinking water reservoirs cyanobacterial blooms were not detected. Cyanobacterial blooms were observed in 6 of 12 investigated water bodies used for fishing and water sports. Microcystis was the dominant cyanobacterial genus. The concentration of total microcystins in the biomasses ranged from 8 to 1070 μg g–1 (d.w.). Microcystin‐LR and microcystin‐RR were the predominant microcystins, followed by microcystin‐YR. Presence of dissolved microcystins was obtained in one water sample with concentration of total microcystins 1.64 μg L–1. Presence of microcystin‐LF and ‐LW or unknown peaks possessing characteristic microcystin‐like UV‐spectra were not detected. Those first results for occurrence of microcystins in some Bulgarian reservoirs and lakes are a contribution to the knowledge on their distribution.  相似文献   

15.
A simple, rapid, and accurate method was developed for separation and preconcentration of trace levels of iron(III) and zinc(II) ions in environmental samples. Methyl‐2‐(4‐methoxy‐benzoyl)‐3‐(4‐methoxyphenyl)‐3‐oxopropanoylcarbamate (MMPC) has been proposed as a new complexing agent for Fe(III) and Zn(II) ions using solvent extraction prior to their determination by flame atomic absorption spectrometry (FAAS). Fe(III) and Zn(II) ions can be selectively separated from Fe(II), Pb(II), Co(II), Cu(II), Mn(II), Cr(III), Ni(II), Cd(II), Ag(I), Au(III), Pd(II), Cr(VI), and Al(III) ions in the solution by using the MMPC reagent. The analytical parameters such as pH, sample volume, shaking time, amount of MMPC reagent, volume of methyl isobutyl ketone (MIBK), effect of ionic strength, and type of back extractant were investigated. The recovery values for Fe(III) and Zn(II) ions were greater than 95% and the detection limits for Fe(III) and Zn(II) ions were 0.26 and 0.32 µg L?1, respectively. The precision of the method as the relative standard deviation changed between 1.8 and 2.1%. Calibration curves have a determination coefficient (r2) of at least 0.997 or higher. The preconcentration factor was found to be 100. Accuracy of the method was checked by analyzing of a certified reference material and spiked samples. The developed method was applied to several matrices such as water, hair, and food samples.  相似文献   

16.
Limited urban water supplies in southwestern USA cause water managers and planners to re‐assess water losses and needs from consumptive water use by riparian vegetation. Here, we report on field measurements of evapotranspiration (ET) for inland saltgrass [Distichlis spicata var. stricta (L.) Greene]; a once common riparian plant native to the desert southwest. The objective was to develop a saltgrass crop coefficient, Kc, similar to agricultural crop coefficients commonly used in irrigation water management. The developed Kc, in conjunction with the local climate, can then be used to assess the water savings that may be achieved in riparian zones for saltgrass versus invasive species and for use in irrigation management and scheduling of saltgrass in urban setting. The ET of saltgrass was measured in its native riparian setting located in the flood plain of the Rio Grande, north of Caballo Lake, New Mexico, in 2011 using an eddy covariance technique in the energy budget method. Total ET of 692 mm was measured during the growing season (n = 241 days) and 837 mm during the year. The American Society of Civil Engineers standardized ET for short crop (ETso) was calculated using climate data measured at the study site as 1560 mm during the growing season and 1870 mm during the year. Crop coefficients (ET/ETso) were fitted with a polynomial equation as a function of day of the year to develop saltgrass Kc function. A graphical and simplified method of computing Kc as a function of day of the year and crop season was also developed as an alternative method. Copyright © 2013 John Wiley & Sons, Ltd.  相似文献   

17.
This work presents a solid phase extraction (SPE) method for simultaneous preconcentration of trace elements in water samples prior to their ICP-OES determination. Dowex 50W-x8 and Chelex-100 resins were used as SPE sorbent materials for preconcentration of trace Cd, Co, Cr, Cu, Fe, Ni, Pb and Zn. The optimum sample pH, eluent concentration and sample flow rates were found to 6, 3.0 mol L−1 and 3.0 mL min−1, respectively. In terms of multi-element preconcentration capabilities, Dowex 50W-x8 appeared to be a better sorbent. The recoveries for all the tested analytes were >95%. However, Chelex-100 showed a better performance in terms of recovery (>95%) towards Cu, Fe and Zn. Under optimized conditions using Dowex 50W-x8, the relative standard deviations for different metals were <3%. The limits of detection and limits of quantification ranged from 0.01–0.39 μg L−1 and 0.05–0.1.3 μg L−1, respectively. The accuracy of the preconcentration method was confirmed by spike recovery test and the analysis of certified reference materials. The SPE method was applied for preconcentration of the analyte ions in tap water, bottled water and wastewater samples.  相似文献   

18.
The deposition of fog to a wind‐exposed 3 m tall Puerto Rican cloud forest at 1010 m elevation was studied using the water budget and eddy covariance methods. Fog deposition was calculated from the water budget as throughfall plus stemflow plus interception loss minus rainfall corrected for wind‐induced loss and effect of slope. The eddy covariance method was used to calculate the turbulent liquid cloud water flux from instantaneous turbulent deviations of the surface‐normal wind component and cloud liquid water content as measured at 4 m above the forest canopy. Fog deposition rates according to the water budget under rain‐free conditions (0·11 ± 0·05 mm h?1) and rainy conditions (0·24 ± 0·13 mm h?1) were about three to six times the eddy‐covariance‐based estimate (0·04 ± 0·002 mm h?1). Under rain‐free conditions, water‐budget‐based fog deposition rates were positively correlated with horizontal fluxes of liquid cloud water (as calculated from wind speed and liquid water content data). Under rainy conditions, the correlation became very poor, presumably because of errors in the corrected rainfall amounts and very high spatial variability in throughfall. It was demonstrated that the turbulent liquid cloud water fluxes as measured at 4 m above the forest could be only ~40% of the fluxes at the canopy level itself due to condensation of moisture in air moving upslope. Other factors, which may have contributed to the discrepancy in results obtained with the two methods, were related to effects of footprint mismatch and methodological problems with rainfall measurements under the prevailing windy conditions. Best estimates of annual fog deposition amounted to ~770 mm year?1 for the summit cloud forest just below the ridge top (according to the water budget method) and ~785 mm year?1 for the cloud forest on the lower windward slope (using the eddy‐covariance‐based deposition rate corrected for estimated vertical flux divergence). Copyright © 2006 John Wiley & Sons, Ltd.  相似文献   

19.
Gaschromatographic Determination of Diethylenetriaminepentaacetic Acid in Surface Water. A method for the determination of diethylenetriaminepentaacetic acid (DTPA) is reported. The determination is based on the preconcentration on a strong base anion exchange resin, esterification with n-propanol and following gaschromatographic separation using a N-selective detector. The sensitivity of the method, including enrichment, is 1 μg/L in river water. The identity of DTPA in river water was proved by mass spectrography. The method can be used also for the quantitative determination of nitrilotriacetic acid (NTA), ethylenediaminetetraacetic acid (EDTA), cyclohexanediaminetetraacetic acid (CDTA) and ethyleneglycolbis-(2-aminoethylether)-N,N,N′,N′-tetraacetic acid (EGTA). The method was used to examine river water. An investigation along the river Rhine, taking grab samples from January and february 1992 showed that DTPA was present in some sampling places in similiar concentrations as NTA and EDTA.  相似文献   

20.
湖泊蒸发量的准确估算对于水文学、气象学和湖泊学等研究有重要的意义.基于2013-2015年太湖水量收支资料、气象观测数据和稳定同位素观测资料,采用稳定同位素质量守恒模型、水量平衡法和Priestley-Taylor模型估算太湖蒸发量,分析太湖蒸发量的季节变化和年际变化特征,并以Priestley-Taylor模型结果为参考值,评价水量平衡法和同位素质量守恒方程的计算精度.结果表明:5-9月太湖蒸发量较高,冬季最低.2013-2015年太湖年总蒸发量分别为1069、894和935 mm,蒸发量的年际变化受到天气条件的影响.2013年12月2014年11月期间,用Priestley-Taylor模型计算的湖泊蒸发量为885 mm;同位素质量守恒模型的估算结果较一致,为893 mm;而水量平衡方程的估算结果明显偏高,为1247 mm.  相似文献   

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