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1.
A solid‐phase extraction (SPE)‐gas chromatography (GC)‐mass spectrometry (MS) analytical method was developed for the simultaneous analysis of natural free estrogens and their conjugates in wastewater samples. Natural free estrogens and their conjugates in wastewater were successfully separated by the oasis hydrophilic‐lipophilic balance solid phase extraction (Oasis HLB SPE) method, and the conjugates were initially enzyme hydrolyzed by β‐glucuronidase or arylsulfatase from Helix pomatia prior to derivatization. N‐methyl‐N‐(tert‐butyldimethylsilyl)trifluoroacetamide (MTBSTFA) plus 1% tert‐butyldimetheylchlorosilane (TBDMCS) was chosen as the derivatization reagent, and the most appropriate conditions of derivatization were determined to be at 95°C for 90 min. The recovery ratios of nine target chemicals were determined by spiking them in 1 L of ultra‐purified water or the influent of a wastewater treatment plant (WWTP). The recovery ratios of six out of nine for the analytes ranged from 73.3–114.9% with relative standard deviations (RSD) from 1.6–19.9%. The established method was successfully applied to environmental wastewater samples which were collected from one municipal wastewater treatment plant (WWTP) in Osaka, Japan, for the determination of natural free estrogens and their conjugates. In the influent sample, E1, E2, E1‐3S, E3‐3S, and E1‐3G were detected at concentrations of 16.6, 9.6, 8.2, 21.9, and 3.2 ng L–1, respectively. However, only E1 was detected at a high concentration of 44 ng L–1 in the effluent sample, suggesting that it is the dominant natural free estrogen in the effluent.  相似文献   

2.
Conflicting sorption coefficients for ortho‐phenylphenol (OPP) have been reported in the literatures, which resulted in the conflicting assessments on OPP mobility in soil. To ascertain the sorption coefficient of OPP, batch experiments were performed based on OECD guideline 106, using three types of soils. Headspace solid‐phase microextraction (HS‐SPME) and GC‐MS were applied to the determination of OPP concentration in the liquid phase. The sorption isotherms obtained for all three soils under equilibrium conditions were described well, assuming linear sorption. The organic carbon normalized distribution coefficients (Koc) ranged from 894 to 1703 L kg?1, which suggested that OPP is moderately mobile in soil. The results also showed that the Koc value of OPP can be predicted precisely from Kow, whereas it was underestimated by one order of magnitude when water solubility is used.  相似文献   

3.
Natural estrogens from humans increasingly attract attention because of their strong endocrine disrupting potency. The discharge of sewage water is considered as the most important source of these endocrine disrupting chemicals (EDCs) in the environment. Therefore, a GC‐MS method was developed for the simultaneous analysis of six natural free estrogens and their sulfate conjugates in municipal wastewater, in which natural free estrogens and sulfate conjugates were successfully separated from an Oasis HLB solid phase extraction (SPE) cartridge with two different eluents, and the sulfate conjugates were then transformed to their corresponding free estrogens by acid solvolysis. Before the analysis with GC‐MS, samples were derivatized by N,O‐bis (trimethylsilyl) trifluoroacetamide (BSTFA) plus 1% trimethylchlorosilane (TMCS) at 80°C for 40 min. Satisfactory recoveries ranging from 64 to 112.3% were obtained by spiking ultra‐purified water, raw, and treated municipal wastewater with the six estrogens at 50, 100, and 50 ng/L, respectively. The method was successfully applied to wastewater samples from one WWTP, which suggested that E1 was the dominant natural estrogens in effluent and E3‐3S was one of the conjugates possibly occurring in the effluent.  相似文献   

4.
In the present study an analytical method was tested for the determination of selected pesticides and metabolites using solid‐phase extraction (SPE) and gas chromatography ion‐trap mass spectrometry (GC‐MS). The extraction efficiency of C18, Isolut ENV+, and Lichrolut EN for SPE was compared for trifluralin, fenitrothion, endosulfan, propargite, 2,4‐D, 3‐methyl‐4‐nitrophenol, 2‐(4‐tert‐butylphenoxy)cyclohexanol, endosulfan sulfate, and 2,4‐dichlorophenol. Isolut ENV+ and C18 showed good results as sorbents and acetone as an elution solvent for SPE for the selected pesticides. Recoveries varied between 36% and 176% with a relative standard deviation of 2...18%. Because of coextracts from the SPE materials, recovery values higher than 100% were obtained for fenitrothion, endosulfan sulfate, and 2,4‐D with C18 as well as for endosulfan sulfate and 3‐methyl‐4‐nitrophenol with Isolut ENV+. A standard addition method was used to verify the occurrence of coextracts in the sample after SPE.  相似文献   

5.
Freeze‐coring and bulk sampling are routine methods used to sample subsurface spawning gravel under shallow water. Both methods have limitations. Freeze‐coring is not believed to representatively sample coarse grain sizes and the sample volumes are relatively small. Conversely, when bulk sampling, even within an enclosure, some fine sediment is suspended and washed away from the sample. This paper assesses the biases in sampling performance between the two methods and determines whether the loss of fines that occurs when bulk sampling could be predicted and thus corrected for. At six riffles the spawning substrate was sampled under approximately 50 cm of water with a bulk sample and three adjacent freeze‐cores. For each riffle, data from the two samples were combined using the method of Fripp and Diplas (1993) and the resultant composite sample was compared with the original freeze‐core and bulk samples to assess the relative precision and biases of the two techniques. On average, the D50 of the bulk samples was 4 mm larger and a one‐third loss of the <2 mm fraction occurred compared with the composite samples. In contrast, freeze‐core samples contain on average 32% more sediment >16 mm compared with composite samples. Based on six samples, taken from six riffles, the amount of sediment finer than 0·5 mm lost using our bulk sampling technique with an enclosure appears to be predictable and correctable. Copyright © 2005 John Wiley & Sons, Ltd.  相似文献   

6.
In wind‐driven rains, wind velocity and direction are expected to affect not only energy input of rains but also shallow ?ow hydraulics by changing roughness induced by raindrop impacts with an angle on ?ow and the unidirectional splashes in the wind direction. A wind‐tunnel study under wind‐driven rains was conducted to determine the effects of horizontal wind velocity and direction on sediment transport by the raindrop‐impacted shallow ?ow. Windless rains and the rains driven by horizontal wind velocities of 6 m s?1, 10 m s?1, and 14 m s?1 were applied to three agricultural soils packed into a 20 by 55 cm soil pan placed on both windward and leeward slopes of 7 per cent, 15 per cent, and 20 per cent. During each rainfall application, sediment and runoff samples were collected at 5‐min intervals at the bottom edge of the soil pan with wide‐mouth bottles and were determined gravimetrically. Based on the interrill erosion mechanics, kinetic energy ?ux (Ern) as a rainfall parameter and product of unit discharge and slope in the form of qbSco as a ?ow parameter were used to explain the interactions between impact and ?ow parameters and sediment transport (qs). The differential sediment transport rates occurred depending on the variation in raindrop trajectory and rain intensity with the wind velocity and direction. Flux of rain energy computed by combining the effects of wind on the velocity, frequency, and angle of raindrop impact reasonably explained the characteristics of wind‐driven rains and acceptably accounted for the differences in sediment delivery rates to the shallow ?ow transport (R2 ≥ 0·78). Further analysis of the Pearson correlation coef?cients between Ern and qSo and qs also showed that wind velocity and direction signi?cantly affected the hydraulics of the shallow ?ow. Ern had a smaller correlation coef?cient with the qs in windward slopes where not only reverse splashes but also reverse lateral raindrop stress with respect to the shallow ?ow direction occurred. However, Ern was as much effective as qSo in the sediment transport in the leeward slopes where advance splashes and advance lateral raindrop stress on the ?ow occurred. Copyright © 2004 John Wiley & Sons, Ltd.  相似文献   

7.
We investigate the use of the short‐lived fallout radionuclide beryllium‐7 (7Be; t1/2 = 53·4 days) as a tracer of medium and coarse sand (0·25–2 mm), which transitions between transport in suspension and as bed load, and evaluate the effects of impoundment on seasonal and spatial variations in bed sedimentation. We measure 7Be activities in approximately monthly samples from point bar and streambed sediments in one unregulated and one regulated stream. In the regulated stream our sampling spanned an array of flow and management conditions during the annual transition from flood control in the winter and early spring to run‐of‐the‐river operation from late spring to autumn. Sediment stored behind the dam during the winter quickly became depleted in 7Be activity. This resulted in a pulse of ‘dead’ sediment released when the dam gates were opened in the spring which could be tracked as it moved downstream. Measured average sediment transport velocities (30–80 metres per day (m d?1)) exceed those typically reported for bulk bed load transport and are remarkably constant across varied flow regimes, possibly due to corresponding changes in bed sand fraction. Results also show that the length scale of the downstream impact of dam management on sediment transport is short (c. 1 km); beyond this distance the sediment trapped by the dam is replaced by new sediment from tributaries and other downstream sources. Copyright © 2006 John Wiley & Sons, Ltd.  相似文献   

8.
The study of bedload transport processes is constrained by an inability to monitor the mass, volume and grain size distribution of sediment in transport at high temporal frequencies. Building upon a previously published design, we have integrated a high‐resolution (1392 × 1024 pixels) video camera with a light table to continuously capture images of 2–181 mm material exiting a flume. The images are continuously recorded at a rate of 15 to 20 frames per second and are post‐processed using LabView(?) software, yielding continuous grain‐size‐specific transport information on a per second basis. The video capture rate is sufficient to record multiple images of each grain leaving the flume so that particle velocities can be measured automatically. No manual image processing is required. After calibration the method is accurate and precise for sediment in the 2 mm through to 45 mm grain size classes compared with other means of measuring bedload. Based on a set of validation samples, no statistically significant difference existed between the D10, D16, D25, D50, D75, D84, D90 and D95 determined by sieving captured samples and the Di values determined with the system. On average the system overpredicted transport by 4 per cent (n = 206, SD = 42%). This error can be corrected easily by simply weighing the mass of sediment that leaves the flume. The technology is relatively inexpensive and provides high‐resolution data on coarse sediment transport out of a flume. Copyright © 2008 John Wiley & Sons, Ltd.  相似文献   

9.
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   

10.
Stream–subsurface exchange plays a significant role in the fate and transport of contaminants in streams. It has been modelled explicitly by considering fundamental processes such as hydraulic exchange, colloid filtration, and contaminant interactions with streambed sediments and colloids. The models have been successfully applied to simulate the transport of inorganic metals and nutrients. In this study, laboratory experiments were conducted in a recirculating flume to investigate the exchange of a hydrophobic organic contaminant, p,p′‐dichloro‐diphenyl‐dichloroethane (DDE), between a stream and a quartz sand bed. A previously developed process‐based multiphase exchange model was modified by accounting for the p,p′‐DDE kinetic adsorption to and desorption from the bed sediments/colloids and was applied to interpret the experimental results. Model input parameters were obtained by conducting independent small‐scale batch experiments. Results indicate that the immobilization of p,p′‐DDE in the quartz sand bed can occur under representative natural stream conditions. The observed p,p′‐DDE exchange was successfully simulated by the process‐based model. The model sensitivity analysis results show that the exchange of p,p′‐DDE can be sensitive to either the sediment sorption/desorption parameters or colloidal parameters depending on the experimental conditions tested. For the experimental conditions employed here, the effect of colloids on contaminant transport is expected to be minimal, and the stream–subsurface exchange of p,p′‐DDE is dominated by the interaction of p,p′‐DDE with bed sediment. The work presented here contributes to a better mechanistic understanding of the complex transport process that hydrophobic organic contaminants undergo in natural streams and to the development of reliable, predictive models for the assessment of impacted streams. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

11.
The artificial reservoir Lagoa da Pampulha in central Brazil has been increasingly affected by sediment deposition and pollution from urban and industrial sources. This study investigates water chemistry and heavy metal concentrations and their fractionation in the lake sediment using ICP-OES, ICP-MS, and XRD analyses. Fractionation analysis was done by sequential extraction under inert gas as well as after oxidation. The lake exhibits a permanent stratification with an oxygen-free hypolimnion below 2 m depth. Nutrient concentrations are enriched for phosphorous components (SRP, PO4). In the sediment it was not possible to detect oxygen. Carbon, sulfur, and most of the analyzed heavy metals are enriched in the top sediment layer with a pronounced downward decrease, indicating the presence of an anthropogenic influence. Statistical analysis, including correlations and a Principal Component Analysis (PCA) of depth-related total concentration data, helps to distinguish presumably anthropogenic heavy metals from geogenic components. Some samples with high element concentrations in the sediment also show elevated concentrations in their pore water. Analyses of element distribution between sediment and pore water suggest a strong bonding of heavy metals to the anoxic sediment. The trend towards elevated solubility in the pore water of oxidized samples is clear for most of the analyzed elements. Fractionation analysis reveals characteristic associations of selected elements to specific mineral bonding forms. In addition, it indicates that the behavior of heavy metals in the sediment is strongly influenced by organic substances. These substances provide buffering against oxidation, acidification, and metal release. The high nutrient loading causes reducing conditions in the lake sediment. These conditions trigger the accumulation of sediments rich in S2−, which stabilizes the fixation of heavy elements. In the future, care must be taken to reduce the supply of contaminants and to prevent the release of heavy metals from sediments dredged for remediation purposes.  相似文献   

12.
A three year monitoring programme of gully‐head retreat was established to assess the significance of sediment production in a drainage network that expanded rapidly by gully‐head erosion on the low‐angled alluvio‐lacustrine Njemps Flats in semi‐arid Baringo District, Kenya. This paper discusses the factors controlling the large observed spatial and temporal variation in gully‐head retreat rates, ranging from 0 to 15 m a?1. The selected gullies differed in planform and in runoff‐contributing catchment area but soil material and land use were similar. The data were analysed at event and annual timescales. The results show that at annual timescale rainfall amount appears to be a good indicator of gully‐head retreat, while at storm‐event timescale rainfall distribution has to be taken into account. A model is proposed, including only rainfall (P) and the number of dry days (DD) between storms: which explains 56 per cent of the variation in retreat rate of the single‐headed gully of Lam1. A detailed sediment budget has been established for Lam1 and its runoff‐contributing area (RCA). By measuring sediment input from the RCA, the sediment output by channelized flow and linear retreat of the gully head for nine storms, it can be seen that erosion shifts between different components of the budget depending on the duration of the dry period (DD) between storms. Sediment input from the RCA was usually the largest component for the smaller storms. The erosion of the gully head occurred as a direct effect of runoff falling over the edge (GHwaterfall) and of the indirect destabilization of the adjacent walls by the waterfall erosion and by saturation (GHmass/storage). The latter component (GHmass/storage) was usually much larger that the former (GHwaterfall). The sediment output from the gully was strongly related to the runoff volume while the linear retreat, because of its complex behaviour, was not. Overall, the results show that the annual retreat is the optimal timescale to predict retreat patterns. More detailed knowledge about relevant processes and interactions is necessary if gully‐head erosion is to be included in event‐based soil erosion models. Copyright © 2001 John Wiley & Sons, Ltd.  相似文献   

13.
Streambed horizontal hydraulic conductivity (Kh) has a substantial role in controlling exchanges between stream water and groundwater. We propose a new approach for determining Kh of the shallow streambed sediments. Undisturbed sediment samples were collected using tubes that were horizontally driven into streambeds. The sediment columns were analysed using a permeameter test (PT) on site. This new test approach minimizes uncertainties due to vertical flow in the vicinity of test tube and stream stage fluctuations in the computation of the Kh values. Ninety‐eight PTs using the new approach were conducted at eight sites in four tributaries of the Platte River, east‐central Nebraska, USA. The Kh values were compared with the nondirectional hydraulic conductivity values (Kg) determined from 12 empirical grain‐size analysis methods. The grain‐size analysis methods used the same sediment samples as Kh tests. Only two methods, the Terzaghi and Shepherd methods, yielded Kg values close to the Kh values. Although the Sauerbrei method produced a value relatively closer to Kh than other nine grain‐size analysis methods, the values from this method were not as reliable as the methods of Terzaghi and Shepherd due to the inconsistent fluctuation of the average estimates at each of the test sites. The Zunker, Zamarin, Hazen, Beyer, and Kozeny methods overestimated Kh, while the Slichter, US Bureau of Reclamation (USBR), Harleman, and Alyamani and Sen methods underestimated Kh. Any of these specific grain‐size methods might yield good estimates of streambed Kh at some sites, but give poor estimates at other sites, indicating that the relationship between Kg and Kh is significantly site dependent in our study. Copyright © 2011 John Wiley & Sons, Ltd.  相似文献   

14.
It has generally been assumed that diffusive sediment transport on soil‐mantled hillslopes is linearly dependent on hillslope gradient. Fieldwork was done near Santa Barbara, California, to develop a sediment transport equation for bioturbation by the pocket gopher (Thomomys bottae) and to determine whether it supports linear diffusion. The route taken by the sediment is divided into two parts, a subsurface path followed by a surface path. The first is the transport of soil through the burrow to the burrow opening. The second is the discharge of sediment from the burrow opening onto the hillslope surface. The total volumetric sediment flux, as a function of hillslope gradient, is found to be: qs (cm3 cm−1 a−1) = 176(dz/dx)3 − 189(dz/dx)2 + 68(dz/dx) + 34(dz/dx)0·4. This result does not support the use of linear diffusion for hillslopes where gopher bioturbation is the dominant mode of sediment transport. A one‐dimensional hillslope evolution program was used to evolve hillslope profiles according to non‐linear and linear diffusion and to compare them to a typical hillslope. The non‐linear case more closely resembles the actual profile with a convex cap at the divide leading into a straight midslope section. Copyright © 2000 John Wiley & Sons, Ltd.  相似文献   

15.
Xunhong Chen 《水文研究》2011,25(2):278-287
Characterization of streambed hydraulic conductivity from the channel surface to a great depth below the channel surface can provide needed information for the determination of stream‐aquifer hydrologic connectedness, and it is also important to river restoration. However, knowledge on the streambed hydraulic conductivity for sediments 1 m below the channel surface is scarce. This study describes a method that was used to determine the distribution patterns of streambed hydraulic conductivity for sediments from channel surface to a depth of 15 m below. The method includes Geoprobe's direct‐push techniques and Permeameter tests. Direct‐push techniques were used to generate the electrical conductivity (EC) logs and to collect sequences of continuous sediment cores from river channels, as well as from the alluvial aquifer connected to the river. Permeameter tests on these sediment cores give the profiles of vertical hydraulic conductivity (Kv) of the channel sediments and the aquifer materials. This method was applied to produce Kv profiles for a streambed and an alluvial aquifer in the Platte River Valley of Nebraska, USA. Comparison and statistical analysis of the Kv profiles from the river channel and from the proximate alluvial aquifer indicates a special pattern of Kv in the channel sediments. This depth‐dependent pattern of Kv distribution for the channel sediments is considered to be produced by hyporheic processes. This Kv‐distribution pattern implied that the effect of hyporheic processes on streambed hydraulic conductivity can reach the sediments about 9 m below the channel surface. Copyright © 2010 John Wiley & Sons, Ltd.  相似文献   

16.
The organic composition and organic‐inorganic interaction in paper mill sludge (PS) solvent extracts (hexane, ethyl acetate, acetone and ethanol) and humic fractions, humic acid (HA) and humin (HU) were studied by electron paramagnetic resonance spectroscopy (EPR), proton and carbon‐13 nuclear magnetic resonance spectroscopy (1H NMR; 13C NMR), Fourier‐transformed infrared spectroscopy (FTIR), and ultraviolet‐visible spectroscopy (UV‐vis). The strategy of fractionating the PS, sequentially, with organic solvents of increasing polarity is a reliable analytical procedure for humic substance sample separation because it results in more purified fractions. FTIR, 1H NMR and 13C NMR results showed that hexane extract consisted mainly of aliphatic hydrocarbon structures. Their contents in the extracts decreased as the polarity of the extracting solvent increased and the content of oxygen functional groups increased. Carboxylic and carboxylate functional groups were found in the acetone extract, and ester and ether functions were predominantly found in the ethanol extract. EPR spectra revealed some Fe3+ complexes with rhombic structure (g1 = 4.3; g2 = 9.0) in the humic fractions and in all solvent extracts, except hexane. Quasi‐octahedral Fe3+ complexes (g = 2.3; ΔHpp ≤ 400 G) were found in the HU fraction and in the acetone extract. The organic free radical content in the HA fraction was higher than the non‐fractionated PS sample and HU fraction.  相似文献   

17.
It is well known that sediment properties, including sediment‐associated chemical constituents and sediment physical properties, can exhibit significant variations within and between storm runoff events. However, the number of samples included in suspended sediment studies is often limited by time‐consuming and expensive laboratory procedures after stream water sampling. This restricts high frequency sampling campaigns to a limited number of events and reduces accuracy when aiming to estimate fluxes and loads of sediment‐associated chemical constituents. In this study, we address the potential of a portable ultraviolet–visible spectrophotometer (220–730 nm) to estimate suspended sediment properties in a resource efficient way. Several field deployable spectrophotometers are currently available for in‐stream measurements of environmental variables at high temporal resolution. These instruments have primarily been developed and used to quantify solute concentrations (e.g. dissolved organic carbon and NO3‐N), total concentrations of dissolved and particulate forms (e.g. total organic carbon) and turbidity. Here we argue that light absorbance values can be calibrated to estimate sediment properties. We present light absorbance data collected at 15‐min intervals in the Weierbach catchment (NW Luxembourg, 0.45 km2) from December 2013 to January 2015. In this proof‐of‐concept study, we performed a local calibration using suspended sediment loss‐on‐ignition (LOI) measurements as an example of suspended sediment property. We assessed the performance of several regression models that relate light absorbance measurements with the percentage weight LOI. The MM‐robust regression method presented the lowest standard error of prediction (0.48%) and was selected for calibration (adjusted r2 = 0.76 between observed and predicted values). The model was then used to predict LOI during a storm runoff event in December 2014. This study demonstrates that spectrophotometers can be used to estimate suspended sediment properties at high temporal resolution and for long‐time spans in a simple, non‐destructive and affordable manner. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

18.
Robin T. Clarke 《水文研究》2015,29(12):2694-2703
When ‘fingerprinting’ is used to identify what proportions Ps (s = 1, …, g) of suspended sediment come from g different source areas, measures of the uncertainties in estimates of the Ps are also required. These uncertainties are influenced by two kinds of correlation whose effects are rarely recognized in the literature. These are (i) correlation between the estimated Ps because they must add to 1 and (ii) correlation between the geochemical tracers measured in sediment samples. This paper uses bootstrap procedures to identify joint confidence regions for the estimated proportions [responding to correlation of type (i)] and to explore alternatives to the ‘standard’ least‐squares criterion used to estimate the proportions when tracer measurements are correlated [correlation of type (ii)]. Using a limited dataset with three sediment source areas for illustration (g = 3), results were obtained from 5000 bootstrap samples, using two criteria (standard and generalized least squares, GLS) with two inequality constraints: (a) 0 ≤ Ps ≤ 1, where Ps is the fraction of suspended sediment contributed by the s‐th source area (s = 1, 2, 3) and (b) 0 < Ps < 1, which, the paper argues, better represents reality. Approximate 95% confidence regions for the Ps, given by the two criteria and two inequality constraints, were compared. Using inequality constraint (a), the confidence region given by the GLS criterion was slightly smaller than that given by the standard; using constraint (b), the two confidence regions' boundaries were almost identical, suggesting that the effects of correlations between tracers were not large for the dataset used. For both criteria, the scatter amongst estimated proportions Ps obtained by bootstrapping was large, raising issues concerning the efficiency of sampling and the allocation of sampling effort, both in source areas and in transported suspended sediment. The results suggest that apparently small differences in the constraints applied to the proportions Ps can give quite different numerical results. Copyright © 2014 John Wiley & Sons, Ltd.  相似文献   

19.
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   

20.
Accumulation rates of marine and terrigenous organic carbon in the continental margin sediments off southwestern Taiwan were estimated from the measured concentrations and isotopic compositions of total organic carbon (TOC) and previously reported sedimentation rates. Surficial sediments were collected from the study area spanning from the narrow shelf near the Kaoping River mouth to the deep slope with depths reaching almost 3000 m. The average sediment loading of Kaoping River is 17 Mt/yr, which yields high sediment accumulation rates ranging from 0.08 to 1.44 g cm−2 yr−1 in the continental margin. About half of the discharged sediments were deposited on the margin within 120 km of the river mouth. Carbon isotopic compositions of terrestrial and marine end-members of organic matter were determined, respectively, based on suspended particulate matter (SPM) collected from three major rivers in the southwestern Taiwan and from an offshore station. All samples were analyzed for the TOC content and its isotopic composition (δ13Corg). The SPM samples were also analyzed for the total nitrogen (TN) content. TOC content in marine sediments ranges from 0.45% to 1.35% with the highest values on the upper slope near the Kaoping River mouth. The TOC/TN ratio of the SPM samples from the offshore station is 6.8±0.6, almost identical to the Redfield ratio, indicating their predominantly marine origin; their δ13Corg values are also typically marine with a mean of −21.5±0.3‰. The riverine SPM samples exhibit typical terrestrial δ13Corg values around −25‰. The δ13Corg values of surficial sediments range from −24.8‰ to −21.2‰, showing a distribution pattern influenced by inputs from the Kaoping River. The relative contributions from marine and terrestrial sources to sedimentary organic carbon were determined by the isotope mixing model with end-member compositions derived from the riverine and marine SPM. High fluvial sediment inputs lead to efficient trapping of organic carbon over a wide range of water depth in this continental margin. The marine organic accumulation rate ranges from 1.6 to 70 g C m−2 yr−1 with an area weighted mean of 4.2 g C m−2 yr−1, which is on a par with the mean terrestrial contribution and accounts for 2.3% of mean primary production. The depth-dependent accumulation rate of marine organic carbon can be simulated with a function involving primary productivity and mineral accumulation rate, which may be applicable to other continental margins with high sedimentation rates. Away from the nearshore area, the content of terrigenous organic carbon in surficial sediments decreases with distance from the river mouth, indicating its degradation in marine environments.  相似文献   

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