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1.
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   

2.
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   

3.
A stable extractor of metal ions was synthesized through azo linking of o‐hydroxybenzamide (HBAM) with Amberlite XAD‐4 (AXAD‐4) and was characterized by elemental analyses, IR spectral, and thermal studies. Its water regain value and hydrogen ion capacity were found to be 12.93 and 7.68 mmol g?1, respectively. The optimum pH range (with the half‐loading time [min], t1/2) for Cu(II), Cr(III), Ni(II), Co(II), Zn(II), and Pb(II) ions were 2.0–4.0 (5.5), 2.0–4.0 (7.0), 2.0–4.0 (8.0), 4.0–6.0 (9.0), 4.0–6.0 (12.0), and 2.0–4.0 (15.0), respectively. Comparison of breakthrough and overall capacities of the metals ascertains the high degree of column utilization (>70%). The overall sorption capacities for Cu(II), Cr(III), Ni(II), Co(II), Zn(II), and Pb(II) ions were found to be 0.29, 0.22, 0.20, 0.16, 0.13, and 0.11 mmol g?1 with the corresponding preconcentration factor of 400, 380, 380, 360, 320, and 320, respectively. The limit of preconcentration was in the range of 5.0–6.3 ng mL?1. The detection limit for Cu(II), Cr(III), Ni(II), Co(II), Zn(II), and Pb(II) were found to be 0.39, 0.49, 0.42, 0.59, 0.71, and 1.10 ng mL?1, respectively. The AXAD‐4‐HBAM has been successfully applied for the analysis of natural water, multivitamin formulation, infant milk substitute, hydrogenated oil, urine, and fish.  相似文献   

4.
A rapid and sensitive method for the determination of trace levels cadmium in water samples by flame atomic absorption spectrometry was developed. It is based on the online sorption of Cd(II) ions on a microcolumn packed with HCl treated bamboo charcoal. In a pH range of 5.0–7.5, Cd(II) ions were effectively retained on the microcolumn, which exhibited fast kinetics, permitting the use of high sample flow rates up to at least 12.8 mL/min without the loss of retention efficiency. The retained Cd(II) ions were quantitatively eluted with HCl (2.0 mol/L) for an online determination. With a preconcentration time of 80 s at a sample loading flow rate of 8.6 mL/min, a sensitivity enhancement factor of 63 was obtained compared with the slope of the linear portion of the calibration curves before and after preconcentration. The calibration graph using the preconcentration system for cadmium was linear with a correlation coefficient of 0.9997, at levels from 1–40 ng/mL. The precision (RSD) for 11 replicate measurements were 3.2% for the determination of 5 ng/mL Cd(II) and 1.8% for 20 ng/mL Cd(II), respectively, and the detection limit (3s) was 0.36 ng/mL. The accuracy was assessed through the determination of a certified reference material, and also through recovery experiments.  相似文献   

5.
The concentration levels of Cd (25 ng l?1), Cu (0.45 μg l?1), Ni (0.48 μg l?1), Fe (0.2–7.0 μg l?1), Pb (40 ng l?1) and Zn (0.80 μg l?1) have been determined in the Danish Sounds and in the Kattegat. Different sampling techniques have been used and analyses have been carried out separately by two different investigators, both using freon-extraction followed by determination by atomic absorption spectrometry (a.a.s.). Except for iron, found mainly in the particulate phase, the metals are found predominantly in a dissolved and labile (extractable) form. The results are compared with trace metal levels found in the two main water masses entering the Kattegat—the North Sea and the Baltic Sea.  相似文献   

6.
Effect of Mixtures of Heavy Metals on the Biological Treatment of Sewages Containing Naphthalenesulfonic Acid Biological wastewater treatment processes can be destabilized considerably by heavy metals. In this investigation, the effect of loadings of heavy metals on the degradation of naphthalene-2-sulfonic acid (2NS) by immobilized bacteria in continuously operated airlift-loop reactors was studied. Shock loadings with mixtures of cadmium and nickel, or cadmium and zinc, respectively, resulted in increases in inhibition compared to those observed with the single metals. In contrast, the 2NS-degradation was less inhibited by shock loadings with mixtures of nickel and zinc than by the single metal ions. Repeated shock loadings up to 100 mg L?1 nickel and 1000 mg L?1 zinc effected an adaptation of the microorganisms. Continuous loadings with up to 10 mg L?1 cadmium and nickel each, or with 50 mg L?1 nickel and 210 mg L?1 zinc, respectively, did not inhibit the degradation of 2NS. The permanent loadings led to an adaptation of the bacteria with an increased biosynthesis of proteins from 0.2 to 0.5 g g?1 cell dry weight. However, if the immobilized cells were incubated with mixtures of cadmium and nickel, the specific polysaccharide content decreased to less than 0.2 g g?1 cell dry weight, resulting in a detachment of the biofilms.  相似文献   

7.
Tissue cadmium and zinc levels in Steller sea lions have been analysed to elucidate the body distribution of these metals and their age-related accumulation. A significant correlation between age (0.7–8.8 year old) and renal and hepatic cadmium concentration was noted. Of the tissues examined, the kidney manifested the highest cadmium content (mean: 20.9 μg g?1 dry wt). A similar zinc distribution pattern was observed; its concentration was more uniform among tissues than that of cadmium. The tissue cadmium concentration in the Steller sea lion was lower than in other pinnipeds from various areas, possibly due to their feeding habits which may represent a major pathway of metal accumulation.  相似文献   

8.
The loss of cadmium and zinc from solutions contained in glass and polystyrene vessels has been determined at different metal concentrations (0.2–3 μg ml?1). A substantial amount (37%) of cadmium was lost after 15 days, while 4% zinc was lost after 50 h. In view of this metal loss, it is stressed that interpretation of graphs, calculations and deductions cannot be made on the basis of spiking amounts alone. It is also suggested that in accumulation experiments use should be made of precontaminated apparatus and the fate of metals for each experiment must be monitored separately. These precautions were omitted in 62% of all papers dealing with metal pollution published by one serious biological journal in 1979. This greatly reduces the value of the reported results and conclusions. Similarly, many earlier papers and reviews reporting acute toxicity concentrations should be viewed with extreme caution.  相似文献   

9.
Lime softening produces an estimated 10,000 metric tons of dry drinking water treatment wastes (DWTW) per year, costing an estimated one billion dollars annually for disposal worldwide. Lime softening wastes have been investigated for reuse as internal curing agents or supplementary cementitious materials in concrete as well as a high-capacity sorbent for heavy metal removal. Lead, cadmium, and zinc are common heavy metals in groundwater contaminated by mine tailings. Cement-based filter media (CBFM) are a novel material-class for heavy metal remediation in groundwater. This study investigated the incorporation of DWTW as a recycled, low-cost additive to CBFM for the removal of lead, cadmium, and zinc. Jar testing at three different metal concentrations and breakthrough column testing using synthetic groundwater were performed to measure removal capacity and reaction kinetics. Jar testing results show as DWTW content increases at low concentrations, removal approaches 100% but at high metal concentrations removal decreases due to saturation or exhaustion of the removal mechanisms. Removal occurs through the formation of metal carbonate precipitates, surface sorption, and ion exchange with calcium according to the preferential series Pb+2 > Zn+2 > Cd2+. Removal kinetics were also measured through column testing and exceeded estimated calculations derived from batch jar testing isotherms due to the large formation of oolitic metal carbonates. Lead, cadmium, and zinc was concentrated in the column precipitates from 0.29, 0.23, and 20.0 μg/g in the influent solution to approximately 200, 130, 14,000 μg/g in the reacted DWTW-CBFM. The control and DWTW-CBFM columns had statically similar removal for zinc and lead. In the DWTW-CBFM, cadmium had decreased removal of approximately 25% due to proportionately decreased hydroxide content from cement replacement with 25% DWTW. This study shows the potential for DWTW as an enhancement to CBFM, thereby valorizing an otherwise waste material. Furthermore, the concentrative abilities of CBFM through precipitate and oolitic mineral formation could provide a minable waste product and close the waste-product cycle for DWTW.  相似文献   

10.
Based on the study of Beijing PM10 bioreactivity with the newly developed plasmid DNA assay method, and analysis for trace elements of PM10, the cause of plasmid DNA damage by PM10 was investigated. The study showed that plasmid DNA oxidative damages by PM10 are of difference in different seasons at various areas. The concentrations of TM50 of PM10 in whole samples respectively collected at urban and comparison sites during winter were 900 μg mL−1 and 74 μg mL−1, while those in their corresponding soluble fractions were 540 μg mL−1 and 86 μg mL−1. In contrast, TM50 contents of PM10 from summer whole samples at urban areas and comparison sites were 116 μg mL−1 and 210 μg mL−1, whereas those in their soluble fractions were 180 μg mL−1 and 306 μg mL−1. The difference of bioreactivity of Beijing PM10 resulted from the variation of trace elements. The oxidative damage of plasmid DNA caused by Pb, Zn, As in PM10 (whole sample) was relatively strong. TM50 and Mn, V, Zn display stronger correlation in the soluble fraction. It implies that Zn could be the major trace element in Beijing PM10 which contributes to oxidative damage to plasmid DNA.  相似文献   

11.
Trace metal clean sampling and analysis techniques were used to examine the temporal patterns of Hg, Cu, and Zn concentrations in shallow ground water, and the relationships between metal concentrations in ground water and in a hydrologically connected river. Hg, Cu, and Zn concentrations in ground water ranged from 0.07 to 4.6 ng L−1, 0.07 to 3.10 μg L−1, and 0.17 to 2.18 μg L−1, respectively. There was no apparent seasonal pattern in any of the metal concentrations. Filtrable Hg, Cu, and Zn concentrations in the North Branch of the Milwaukee River ranged from below the detection limit to 2.65 ng Hg L−1,0.51 to 4.30 μg Cu L−1, and 0.34 to 2.33 μg Zn L−1. Thus, metal concentrations in ground water were sufficiently high to account for a substantial fraction of the filtrable trace metal concentration in the river. Metal concentrations in the soil ranged from 8 to 86 ng Hg g−1, 10 to 39 μg Cu g−1, and 15 to 84 μg Zn g−1. Distribution coefficients, KD, in the aquifer were 7900,22,000, and 23,000 L kg−1 for Hg, Cu, and Zn, respectively. These values were three to 40 times smaller than KD values observed in the Milwaukee River for suspended particulate matter.  相似文献   

12.
This work describes the modification of silica gel with dimethylglyoxime, in order to prepare an effective sorbent for the preconcentration and determination of copper. The sorption capacity of dimethylglyoxime‐modified silica‐gel (DMGMS) was 71.37 mg g–1 and the optimum pH for the quantitative recovery of copper was found to be 5.0. The optimum flow rate, sorbent amount, and sample volume were 1 mL min–1, 300 mg, and 50 mL, respectively. 10 mL of 0.1 mol L–1 HCl was the most suitable eluent. The detection limit of copper was 6.0 ng mL–1. The recommended method, for the determination of copper, is simple and reliable, without any notable matrix effect and can be successfully applied to environmental water samples. Copper recovery in the range from 99–100% was obtained from seawater and thermal spring water using this method. The method was applied to standard reference materials, NIST‐1515 (apple leaves) and NIST‐1643e (simulated fresh water), for the determination of copper and the results were in good agreement with certified values.  相似文献   

13.
Cyanuric acid is a suspected gastrointestinal or liver toxicant in humans. Therefore, determination of trace cyanuric acid is very important, in this work a novel, sensitive, and reliable method was developed using differential pulse polarography. Optimum conditions for analytical determination were found to be at a pH of 9.5, Britton–Robinson at a reduction potential of ?105 mV. Experimental results indicate an excellent linear correlation between the peak current and the concentration in the range of cyanuric acid from 0.5 to 27.0 µM (0.06–3.5 µg mL?1) with a correlation coefficient of 0.997. The limit of detection and limit of quantification were obtained as 0.15 and 0.5 µM (0.02–0.06 µg mL?1), respectively. The proposed method was successfully applied to the determination of cyanuric acid in pool water and in spiked milk. Cyanuric acid level in swimming pool water was found as 2.54 ± 0.47 µg mL?1 (19.7 ± 2.29 µM) in swimming pool water for N = 4 and 95% confidence interval. The recoveries were found to be sufficient. Also, the standard deviation of the data was low which shows high accuracy and precision of proposed differential pulse polarographic method. The influences of some other commonly found inorganic salts on the determination of cyanuric acid were also examined. Some interfering species were eliminated using complexing agents, e.g., EDTA.  相似文献   

14.
C. K. Jain  I. Ali 《水文研究》2000,14(2):261-270
The effects of solution pH, sediment dose, contact time, and particle size on the adsorption of cadmium ions on bed sediments have been studied for a highly polluted river in western Uttar Pradesh, India. The role of the coarser sediment and the clay and silt fractions has been examined. The optimum contact time needed to reach equilibrium is of the order of 30 and 60 min for 0–75 μm and 210–250 μm sediment size, respectively. The extent of cadmium adsorption increases with increasing pH and adsorbent doses and decreases with adsorbent particle size. The important geochemical phases, iron and manganese oxide, provide the active support material for the adsorption of cadmium. The competitive experiments conducted in the presence of lead and zinc ions indicate that both the ions suppress the ability of cadmium to adsorb on to sediments. The Langmuir and Freundlich adsorption models were used to determine the mechanistic parameters associated with the adsorption process. Copyright © 2000 John Wiley & Sons, Ltd.  相似文献   

15.
Cadmium,zinc, copper,and barium in foraminifera tests   总被引：1，自引：0，他引：1  
The concentrations of cadmium, zinc, copper and barium have been determined on 2-mg samples of single-species foraminifera populations. Cleaning techniques were tested using North Atlantic core tops, and followed by a detailed downcore study for the last 30,000 years in South Atlantic core V22-174. Raw foram tests cleaned by crushing followed by ultrasonic removal of fine-grained material, and dissolved in a pH 5.5 acetate buffer, contain appreciable amounts of trace elements associated with ferromanganese and alumino-silicate contaminants. A reductive/complexing cleaning treatment reduces ferromanganese contamination by 1–2 orders of magnitude. Acetate buffers at pH 5.5 complex iron and raise the solubility of ferromanganese oxides; these buffers are unsuitable for separating carbonate lattice-bound trace elements from the fraction associated with ferromanganese phases. Improved mechanical and ultrasonic reductive cleaning combined with a mild dissolution in distilled water under 1 atm.PCO2 reduces contaminant levels another order of magnitude. The Cd and Zn concentrations (order 10?8 mole Cd/mole Ca and 10?5 mole Zn/mole Ca) of species with low surface area show an increase with decreasing isotopic temperatures. This increase is consistent with the increasing concentrations of these metals from low values in surface waters to higher values at depth. The variance of Cd and Zn over the last 30,000 years in the central South Atlantic is consistent with the probable variability of the dissolved trace elements at the calcification levels of the species analyzed. Cu and Ba are irreproducible and probably sensitive to residual contaminant phases. The trace element content of the tests differs from levels observed in a recent coprecipitation study. Foraminifera may be a significant vector in zinc cycling in the ocean.  相似文献   

16.
A bloom of Chlamydomonas botryopara was observed in an extremely acid coal mining pond (pH 2.5) with high concentrations of iron and aluminium (1160...3760 mg L–1 Fe, 133...387 mg L–1 Al). Cell density of algae was counted as 6.45 · 106 mL–1 corresponding to 700 mg L–1 fresh weight and 2660 μg L–1 chlorophyll‐a. The nutrient concentrations were 3.5 mg L–1 soluble reactive phosphorus and 0.15 mg L–1 dissolved inorganic nitrogen. This observation supports the hypothesis that a low nutrient availability rather than extreme conditions (e.g. high acidity and low pH) limit the development of phytoplankton in many acidified lakes.  相似文献   

17.
In this study, remediation results of trace metals in natural water and treated water using three functionalized nanofiber mats of cellulose and chitosan are reported. The nanofiber materials, packed in mini-columns, were employed for the remediation of five toxic trace metals (Cd, Pb, Cu, Cr and Ni) from natural water samples. Trace metals in real water samples were undetectable as the concentrations were lower than the instrument’s detection limits of 0.27 × 10−3 (Cd) and 4.2 × 10−2 (Pb) μg mL−1, respectively. However, after percolation through the functionalised biosorbents in cartridges, detectability of the metal ions was enhanced. The starting volume of the natural water sample was 100 mL, which was passed through a column containing the nanofibers sorbent and the retained metals eluted with 5 mL of 2.0 M nitric acid. The eluate was analyzed for metals concentrations. An enrichment factor of 20 for the metals was realized as a result of the pre-concentration procedure applied to handle the determination of the metals at trace levels. The order of remediation of the studied metals using the nanofibers was as follows: chitosan/PAM-g-furan-2,5-dione < cellulose-g-furan-2,5-dione < cellulose-g-oxolane-2,5-dione. The modified biopolymer nanofibers were able to adsorb trace metals from the river water and treated water, thereby confirming their capability of water purification. These materials are proposed as useful tools and innovative approach for improving the quality of drinking for those consumers in small scale households.  相似文献   

18.
Increasing research has suggested that biosolids generated from municipal wastewater treatment can be a major sink for many pharmaceuticals and personal care products (PPCPs) and their land application potentially introduces these contaminants into the terrestrial and aquatic environments. In this study, methods were developed for the analysis of 14 PPCPs in biosolids and soils using pressurized liquid extraction, solid phase extraction and liquid chromatography‐tandem mass spectrometry. Recoveries were over 50% for all analytes except diphenhydramine (?30%) in soils. Soil properties or type of biosolids showed minor effects on method recoveries. Estimated method limits of quantification (LOQ) range from 0.1–15 ng g–1 for soil and 0.3–27 ng g–1 for biosolids. A field study utilizing the methods revealed that other than carbamazepine‐10,11‐epoxide, all targeted compounds were detected in biosolids. Diphenhydramine, fluoxetine, triclosan and triclocarban were detected up to the μg g–1 range with the highest concentration of 23 μg g–1 for triclocarban. Seven of the PCCPs found in biosolids were also detected in agricultural soils amended with these biosolids and several (carbamazepine, diphenhydramine, and triclocarban) appeared to be persistent in soils. Triclocarban was also found most abundant in soils with the highest average concentration of 0.2 μg g–1 while the rest of compounds were in the lower ng g–1 range. Generally, the concentrations found on the fields were 2–3 degrees of magnitude lower than in the biosolids, which is likely to be due to dilution, degradation and leaching processes.  相似文献   

19.
A cloud point extraction procedure is presented for the preconcentration and simultaneous determination of Ag+ and Pd2+ in various samples. After complexation with 2‐((2‐((1H‐benzo[d]imidazole‐2‐yl)methoxy)phenoxy)methyl)‐1H‐benzo[d]imidazol (BIMPI), which was used as a new chelating agent, analyte ions were quantitatively extracted to a phase rich in Triton X‐114 following centrifugation, and determination was carried out by flame atomic absorption spectrometry (FAAS). Under the optimum experimental conditions (i. e., pH = 7.0, 15.0·10–5 mol/L BIMPI and 0.036% (w/v) Triton X‐114), calibration graphs were linear in the range of 28.0–430.0 μg/L and 57.0–720.0 μg/L with detection limits of 10.0 and 25.0 μg/L for Ag+ and Pd2+, respectively. The enrichment factors were 35.0 and 28.0 for Ag+ and Pd2+, respectively. The method has been successfully applied to evaluate these metals in some real samples, including waste water, soil and hydrogenation catalyst samples.  相似文献   

20.
Removal of copper, nickel, and zinc ions from synthetic electroplating rinse water was investigated using cationic exchange resin (Ceralite IR 120). Batch ion exchange studies were carried out to optimize the various experimental parameters (such as contact time, pH, and dosage). Influence of co‐existing cations, chelating agent EDTA on the removal of metal ion of interest was also studied. Sorption isotherm data obtained at different experimental conditions were fitted with Langmuir, Freundlich, Redlich–Peterson, and Toth models. A maximum adsorption capacity of 164 mg g?1 for Cu(II), 109 mg g?1 for Ni(II), and 105 mg g?1 for Zn(II) was observed at optimum experimental conditions according to Langmuir model. The kinetic data for metal ions adsorption process follows pseudo second‐order. Presence of EDTA and co‐ions markedly alters the metal ion removal. Continuous column ion exchange experiments were also conducted. The breakeven point of the column was obtained after recovering effectively several liters of rinse water. The treated rinse water could be recycled in rinsing operations. The Thomas and Adams–Bohart models were applied to column studies and the constants were evaluated. Desorption of the adsorbed metal ions from the resin column was studied by conducting a model experiments with Cu(II) ions loaded ion exchange resin column using sulfuric acid as eluant. A novel lead oxide coated Ti substrate dimensionally stable (DSA) anode was prepared for recovery of copper ions as metal foil from regenerated liquor by electro winning at different current densities (50–300 A cm?2).  相似文献   

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