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1.
A new, simple, sensitive, and selective spectrophotometric method for the determination of copper in water and soil samples has been demonstrated. The method is based on the reaction of Cu(I) with neocuproine (2,9-dimethyl-1, 10-phenanothroline) and extracted with N-phenyl benzimidoylthiourea in chloroform. The value of molar absorptivity of the complex in the term of Cu(I) is 1.45 × 105 L mol???1 cm???1 at λ max 460 nm in chloroform. The detection limit of copper in water and soil is 2 ng mL???1 and 4 ng g???1, respectively. The method is free from the interference of the ions commonly found to be associated with the copper determination in water and soil samples. The application of the proposed method has been successfully tested for the determination of copper in different types of water and soil samples.  相似文献   

2.
This study reports a very selective, easy, and precise method for rapid separation of trace amounts of copper in aqueous samples using octadecyl silica-bonded phase membrane disks modified by 2,2'-[ethane-1,2-diylbis(thio)]dianiline (EDTD) combined with flame atomic absorption spectrometric determination. In addition, the synthesis and spectral characterization of EDTD have been described in detail. All the affecting experimental variables such as pH, amount of modifier, eluent type, sample and eluent flow rate, interfering ions, and disk capacity were also investigated. The target analyte (trace copper) was quantitatively retained at pH?=?4 and eluted with 6.0 mL of 0.5 M HNO3 at flow rates of 40 and 10 mL min?1 for analyte passage and elution steps, respectively, through the disks modified with 17.0 mg of EDTD. The proposed method also allows an enrichment factor of about 500 and has a detection limit of 0.005 ng mL?1. The method has been successfully applied for isolation and determination of copper in different water samples, peppers, and standard alloys.  相似文献   

3.
In this study, a ternary Zr(IV) system with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) and fluoride was chosen on the basis of dispersive liquid–liquid microextraction method. Zirconium was extracted into the fine droplets of dichlorobenzene as extracting solvent. These drops dispersed as a cloud in the aqueous sample with the help of ultrasonic waves, and the procedure was done. Finally, atomic absorption spectrometry was applied for the determination of zirconium. The effects of different factors that influence complex formation and extraction, such as pH, amounts of complexing agents, type and volume of the extracting solvent, as well as sonication and centrifuging time, were optimized. Under optimum conditions, the calibration curve was linear in the range of 150.0–800.0 ng mL?1 with a limit of detection of 44.0 ng mL?1. Relative standard deviation was calculated to be 4.1 % (n?=?7, c?=?400.0 ng mL?1). The enrichment factor was 80. The proposed method was successfully used to determine the zirconium in several water, wastewater, and soil samples.  相似文献   

4.
Forty-eight air-filter samples (PM10) were analysed to identify the concentration level of partially leached metals (PLMs; As, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb and V) from Puebla City, México. Samples were collected during 2008 from four monitoring sites: (1) Tecnológico (TEC), (2) Ninfas (NIN), (3) Hermanos Serdán (HS) and (4) Agua Santa (AS). The results indicate that in TEC, As (avg. 424 ng m?3), V (avg. 19.2 ng m?3), Fe (avg. 1,202 ng m?3), Cu (avg. 86.6 ng m?3), Cr (41.9 ng m?3) and Ni (18.6 ng m?3) are on the higher side than other populated regions around the world. The enrichment of PLMs is due to the industrial complexes generating huge dust particles involving various operations. The results are supported by the correlation of metals (Mn, Cd and Co) with Fe indicating its anthropogenic origin and likewise, As with Cd, Co, Fe, Mn, Pb and V. The separate cluster of As, Fe and Mn clearly signifies that it is due to continuous eruption of fumaroles from the active volcano Popocatépetl in the region.  相似文献   

5.
In this research, a microfunnel-assisted headspace liquid-phase microextraction technique has been used in combination with hydride generation to determine arsenic (As) by UV–Vis spectrophotometry. The method is based on the reduction of As to arsine (AsH3) in acidic media by sodium tetrahydroborate (NaBH4) followed by its subsequent reaction with silver diethyldithiocarbamate (AgDDC) to give an absorbing complex at 510 nm. The complexing reagent (AgDDC) has been dissolved in a 1:1 (by the volume ratio) mixture of chloroform/chlorobenzene microdroplet and exposed to the generated gaseous arsine via a reversed microfunnel in the headspace of the sample solution. Several operating parameters affecting the performance of the method have been examined and optimized. Acetonitrile solvent has been added to the working samples as a sensitivity enhancement agent. Under the optimized operating conditions, the detection limit has been measured to be 0.2 ng mL?1 (based on 3sb/m criterion, n b?=?8), and the calibration curve was linear in the range of 0.5–12 ng mL?1. The relative standard deviation for eight replicate measurements was 1.9 %. Also, the effects of several potential interferences have been studied. The accuracy of the method was validated through the analysis of JR-1 geological standard reference material. The method has been successfully applied for the determination of arsenic in raw and spiked soft drink and water samples with the recoveries that ranged from 91 to 106 %.  相似文献   

6.
The paper presents the first report on the application of a lead film electrode for the determination of ultratrace concentrations of platinum. The procedure is based on preconcentration of the Pt(IV)-formaldehyde complexes at an in situ plated lead film electrode held at ?0.9 V (vs. Ag/AgCl), followed by a negatively sweeping differential pulse voltammetric scan. The composition of the supporting electrolyte, the influence of accumulation potential and time on the sensitivity of platinum responses are discussed. The detection limit of Pt(IV) with the accumulation time of 60 was equal to 9.2?×?10?12 mol L?1. The application of this method was tested by recovery of Pt(IV) from spiked environmental water samples.  相似文献   

7.
The presented results include decade of monitoring of the Vistula Lagoon waters and have been supplemented by the determination of chlorinated compounds, as well as on concentrations of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) in the sedimentation zone. Monitoring of river waters entering the Polish part of the lagoon and the lagoon waters confirmed the presence of plant protection chemical; the largest contributors has lindane (34%) and DDTtotal (21%); the same as for sediments were dominate lindane (19%) and DDTtotal (14%) within pp-DDT isomer dominate (13%). In the lagoon water, PCDD/Fs were determined within a range of 1.5–5.6 ng dm?3, leading to average toxicity of 0.18?±?0.13 ng TEQ·dm?3. In sediments, their concentrations fell within a range of 22.7–405.7 ng kg?1 dw and the average toxicity of the lagoon sediments was set at 5.00?±?1.98 ng TEQ·kg?1 dw. Both in water and sediments, the greatest share among PCDD/Fs has octa-chlorodibenzodioxin. Due to the hydromorphological conditions of the lagoon, the waters are mixed to the bottom causing the surface layer of sediment to become remobilized—this is suggested as the key factor when it comes to water recontamination and increased access of POPs to marine organisms.  相似文献   

8.
In this paper, a simple, fast, and inexpensive method is introduced for the simultaneous spectrophotometric determination of crystal violet (CV) and malachite green (MG) contents in aquatic samples using partial least squares regression (PLS) as a multivariate calibration technique after preconcentration by graphene oxide (GO). The method was based on the sorption and desorption of analytes onto GO and direct determination by ultraviolet–visible spectrophotometric techniques. GO was synthesized according to Hummers method. To characterize the shape and structure of GO, FT-IR, SEM, and XRD were used. The effective factors on the extraction efficiency such as pH, extraction time, and the amount of adsorbent were optimized using central composite design. The optimum values of these factors were 6, 15 min, and 12 mg, respectively. The maximum capacity of GO for the adsorption of CV and MG was 63.17 and 77.02 mg g?1, respectively. Preconcentration factors and extraction recoveries were obtained and were 19.6, 98% for CV and 20, 100% for MG, respectively. LOD and linear dynamic ranges for CV and MG were 0.009, 0.03–0.3, 0.015, and 0.05–0.5 (μg mL?1), respectively. The intra-day and inter-day relative standard deviations were 1.99 and 0.58 for CV and 1.69 and 3.13 for MG at the concentration level of 50 ng mL?1, respectively. Finally, the proposed DSPE/PLS method was successfully applied for the simultaneous determination of the trace amount of CV and MG in the real water samples.  相似文献   

9.
Polycyclic aromatic hydrocarbons (PAHs) are a major concern in environmental studies as many of them have been labeled as probable carcinogens by the International Agency for Research on Cancer (IARC 1983). Due to their lipophilic properties and resistance to degradation, PAHs can accumulate in organic tissue. As a consequence, alarming concentrations of these compounds have been found in many aquatic species. The European catfish (Silurus glanis) is a top food chain predator that is considered to be a reliable bio-indicator of environmental pollution. From 2009 to 2011, 54 specimens of S. glanis were captured from four different sites covering the area of the Po River basin (Northern Italy). Fish muscles were analyzed in the laboratory to determine the levels of nine PAHs, namely naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, pyrene, benz[a]anthracene, chrysene, and benz[a]pyrene (BaP), which were detected by high-performance liquid chromatography (HPLC). The total average concentration of PAHs was 26.90?±?49.50 ng g?1 (min 0.60, max 275.75 ng g?1). Analysis showed that 9.20 % of the fish muscles exceeded the maximum levels of 2 ng g?1 set for BaP by European regulations (Commission Regulation (EC), 2006). Values measured for benz[a]pyrene ranged from 0.05 to 8.20 ng g?1 (mean 1.07?±?1.58 ng g?1). Chrysene and benz[a]anthracene, both considered potential human carcinogens (PAH2), were found at levels of 4.40 and 0.05 ng g?1 (mean values), respectively. The highest mean concentration was recorded for anthracene (12.92 ng g?1), which has been recently included in the list of substances of very high concern (SVHC) as reported by the European Chemicals Agency (ECHA 1–9, 2009).  相似文献   

10.
New solid-phase extractor (MWCNTs-5-ASA) was synthesized via covalent immobilization of 5-aminsalicylic acid onto multi-walled carbon nanotubes (MWCNs). The success of the functionalization process was confirmed using Fourier transform infrared spectroscopy, scanning electron microscope, and surface coverage determination. Batch experiments were conducted as a function of pH to explore MWCNTs-5-ASA efficiency to extract several metal ions viz., Cr(III), Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Pb(II). It was found that Pb(II) exhibits the highest extraction percentage with maximum adsorption capacity 32.75 mg g?1. Its binding performance was well fitted with Langmuir sorption isotherm. On the other hand, the selective separation and preconcentration of trace Pb(II) under dynamic conditions prior to determination by inductively coupled plasma-optical emission spectrometry was investigated under different parameters. These included the rate of flow and volume of sample solution, in addition to the type of the eluate, its volume and concentration. The effect of a variety of foreign ions on the recovery percentage was also evaluated. Trace Pb(II) ions present in 500 mL aqueous solution adjusted to pH 4.0 were retained on 50 mg of MWCNTs-5-ASA and completely eluted using 4.0 mL of 2 M HNO3. The limit of detection and the precision of the method were 0.25 ng mL?1 and 2.8 %, respectively (N?=?5). This methodology has been applied for the determination of Pb(II) in water samples with good results.  相似文献   

11.
The aim of the present work is the assessment of a new sorbent, prepared using silica gel coated with a pyrimidine derivative (allyl 6-methyl-4-phenyl-2-thioxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate), for extraction and preconcentration trace amount of lead from different samples prior to determination by flame atomic absorption spectrometry. Common coexisting ions did not interfere with the separation and determination of lead at pH?6, so that lead ion completely adsorbed on the column. The limit of detection based on three times the standard deviation of the blank was found to be 0.53 ng?mL?1 in original solution. Obtained sorption capacity for 1 g sorbent was 5.0 mg Pb. The linearity was maintained in the concentration range of 0.1–30.0 ng?mL?1 for the concentrated solution. Eight replicate determinations of 2.0 μg?mL?1 of lead in the final solution gave relative standard deviation of ±2.6 %. The proposed method was successfully applied to the determination trace amounts of lead in the environmental samples such as carrot, rice, zardchoobe, and real water samples.  相似文献   

12.
The residual levels of dichlorodiphenyltrichloroethane (DDT) and its metabolites (DDXs, including p,p′-DDT, DDD, and DDE) in water, suspended particulate matter (SPM), and sediments from major rivers, lakes, and reservoirs in Haihe Plain were measured with a gas chromatograph equipped with a 63Ni microelectron capture detector. In the fall of 2004, the contents of the total DDXs in the water and SPM were 0.29?±?0.69 ng L?1 and 423.13?±?577.85 ng g?1 dry wt., respectively. In the spring of 2005, the total DDXs were 0.36?±?0.91 ng L?1 for water and 35.93?±?62.65 ng g?1 dry wt. for SPM. The average concentration of DDXs for sediments was 7.10?±?7.57 ng g?1 dry wt. during the two seasons. The Eastern-Hebei-Province Coastland River System was the most polluted, which was mainly attributable to the extensive use of DDT pesticide and dicofol in that system. Recent DDT inputs still occur in some regions, as indicated by DDT/(DDD + DDE) > 1 at 29–36 % of the sites for water and 55–61 % of the sites for SPM. The potential ecological risks of DDT in the water were assessed using a species sensitivity distribution model. Only shrimp and crabs were found to have potentially affected fraction values of 1.63?×?10?3 to 2.27?×?10?4, with probabilities beyond the hazardous concentration for 5 % of species (HC5) values of 1.90–2.56 %, suggesting only slight risks. DDXs in the sediments of some sites were also of potential risk to benthic organism based on consensus-based sediment quality guidelines.  相似文献   

13.
The levels of hexachlorocyclohexane (HCH) and dichloro-diphenyl-trichloroethane (DDT) in the water, suspended particulate matter (SPM), and sediments from Lake Small Baiyangdian were measured by gas chromatograph with a 63Ni microelectron capture detector. The residual levels of the total HCHs in the water, SPM, and sediments were 1.59?±?2.24 ng L?1, 25.42?±?1.72 ng g?1 dw (dry weight), and 0.86?±?1.44 ng g?1 dw, respectively. DDTs were not detected in the water samples. The concentrations of total DDTs were 158.79?±?1.67 ng g?1 dw in SPM and 0.46?±?1.97 ng g?1 dw in the sediments. Compared to other areas in China and abroad, the levels of residual HCH and DDT were relatively low in the water and sediments, but they were moderate to high in the SPM. Organic carbon partition coefficient values for HCH in this study were higher than previously published values and may reflect new input in this area. The residual HCHs in this area could be derived from a mixture of technical HCH and lindane because ongoing lindane use may be occurring. DDT in the majority of the study area was primarily attributed to historical discharge, but some regions may be receiving new input. The ecological risks of γ-HCH in the water were very low according to species sensitivity distribution models. The concentrations of HCH and DDT in the sediments from the study area did not exceed the sediment quality guidelines, which indicate little risk for benthic organisms.  相似文献   

14.
Pig manure (PM) is widely used as an organic fertilizer to increase yields of crops. Excessive application of compost containing relatively great concentrations of copper (Cu) and zinc (Zn) can change soil quality. To clarify the effects of different rates of application and to determine the optimal rate of fertilization, PM containing 1,115 mg Cu kg?1, dry mass (dm) and 1,497 mg Zn kg?1, dm was applied to alkaline soil at rates of 0, 11, 22, 44, 88, and 222 g PM kg?1, dm. Phospholipid fatty acids (PLFAs) were used to assess soil microbial community composition. Application of PM resulted in greater concentrations of total nitrogen (TN), NH4 +-N, NO3 ?-N, total carbon (TC), soil organic matter (SOM) but lesser pH values. Soils with application rates of 88–222 g PM kg?1, dm had concentrations of total and EDTA-extractable Cu and Zn significantly greater than those in soil without PM, and concentrations of T-Cu and T-Zn in these amended soils exceeded maximum limits set by standards in china. Except in the soil with a rate of 11 g PM kg?1, dm, total bacterial and fungal PLFAs were directly proportional to rate of application of PM. Biomasses of bacteria and fungi were significantly greater in soils with application rates of 44–222 g PM kg?1, dm than in the soil without PM. SOM, TC and EDTA-Zn had the most direct influence on soil microbial communities. To improve fertility of soils and maintain quality of soil, rate of application should be 22–44 g PM kg?1 dm, soil containing Cu and Zn.  相似文献   

15.
Mercury (Hg) is considered a global pollutant, and the scientific community has shown great concern about its toxicity as it may affect the biota of entire systems, through bioaccumulation and bioamplification processes of its organic form, methylmercury (MeHg), along food web. However, few research studies deal with bioaccumulation of Hg from marine primary producers and the first-order consumers. So, this study aims to determine Hg distribution and concentration levels in phytoplankton and zooplankton in the Cabo Frio Bay, Brazil, a site influenced by coastal upwelling. The results from Hg speciation analyses show that inorganic mercury Hg(II) was the predominant specie in plankton from this bay. The annual Hg species distribution in plankton shown mean concentration of 2.00?±?1.28 ng Hg(II)?g?1 and 0.15?±?0.08 ng MeHg g?1 wet weight (phytoplankton) and 2.5?±?2.03 ng Hg(II)?g?1 and 0.25?±?0.09 ng MeHg g?1 wet weight (zooplankton). Therefore, upwelling zones should be considered in the Hg biogeochemical cycle models as a process that enhances Hg(II) bioaccumulation in plankton, raising its bioavailability and shelf deposition.  相似文献   

16.
Street dusts collected from 20 locations in the Chang-Zhu-Tan (Changsha, Zhuzhou, and Xiangtan) region, Hunan, China, in May to July 2006, were investigated for sources of polycylic aromatic hydrocarbons (PAHs). The individual PAH concentrations were in the range of 10–4316 ng g?1, and ∑PAHs16 levels were in the range of 3,515–24,488 ng g?1, with a mean of 8,760 ng g?1. The high-molecular-weight PAHs (four to six rings), ranging from 47.51 to 82.11 %, with a mean of 74.79 %, were the dominant PAH compounds in almost all of the dusts. The isomer ratios suggested a rather uniform mixture of coal combustion and petroleum PAH sources. Factor analysis and multiple linear regression analysis indicate that the main sources of the 16 PAHs were coal combustion/vehicle exhaust, coking/petroleum, and plant combustion, with contribution rates of 50.9, 35.01, and 14.08, respectively. The spatial distributions of PAH concentrations were significantly related to the distribution of industries, traffic circulation, and farmland in this region.  相似文献   

17.
To assess the status of polycyclic aromatic hydrocarbon (PAH) contamination in sediments from the Bizerte Lagoon (northern Tunisia), 18 surface sediment samples were collected in March 2011 and analyzed for 14 US Environmental Protection Agency priority PAHs by high-performance liquid chromatography. The total concentrations of the 14 PAHs (ΣPAHs) ranged from 16.9 to 394.1 ng g?1 dry weight (dw) with a mean concentration of 85.5 ng g?1 dw. Compared with other lagoons, coasts, and bays in the world, the concentrations of PAHs in surface sediments of the Bizerte Lagoon are low to moderate. The PAHs’ composition pattern was dominated by the presence of four-ring PAHs (45.8 %) followed by five-ring (26.8 %) and three-ring PAHs (12.7 %). The PAH source analysis suggested that the main origin of PAHs in the sediments of the lagoon was mainly from pyrolytic sources. According to the numerical effect-based sediment quality guidelines of the USA, the levels of PAHs in the Bizerte Lagoon should not exert adverse biological effects. The total benzo[a]pyrene toxicity equivalent values calculated for the samples varied from 3.1 to 53.7 ng g?1 dw with an average of 10.6 ng g?1 dw.  相似文献   

18.
The Fusaro Lagoon is a shallow lagoon, located in SW Italy, largely influenced in the last decades by several anthropic impacts. The study examined the pollution status of the lagoon, during year 2011–2012 at nine sampling stations with the aim to find out proper measurements of water lagoon restoration. Concentrations of heavy metals (HMs) (aluminium [Al], barium [Ba], cadmium [Cd], copper [Cu], iron [Fe], manganese [Mn], vanadium [V] and zinc [Zn]) were examined in water, sediments and specimens of the ascidian Ciona intestinalis sp. A. Low levels of dissolved oxygen concentration were detected at many stations, with mean values of 5.2–6.4 mg L?1. The redox potential of surface waters was also low, ?2.7 to 50.7 mV. Sediments possessed high organic matter content, 17.7–29.4 %. In sediments, the mean Zn level, 251.4 mg kg?1, was about sixfold higher than that recorded in year 2000 (38.5 mg kg?1) and considerably higher than that recorded in 2007 (191 mg kg?1). The mean levels of Cd were outstandingly high, with a mean value of 70.5 mg kg?1, about 30- and 50-fold higher than those determined in 2000 and 2007, respectively. Cadmium (Cd), Cu and nickel (Ni) appeared in excess with respect to most current guidelines, reaching significant pollution levels. C. intestinalis sp. A was detected only at few stations, with metals accumulated preferentially in the body in respect to the tunic, from 1.2 times for Zn (178 mg kg?1) to 4.0 times for V (304 mg kg?1). Data suggests the necessity of an immediate action of eco-compatible interventions for environmental restoration.  相似文献   

19.
Silver is subject to significant interferences caused by high chloride concentrations in electrothermal atomic absorption spectrometry, thus its direct determination in aqua regia leaches from soils, sediments, and sludges is very difficult, especially when using instrumentation equipped with deuterium-lamp background correction (D2). In this study, the interference of the aqua regia medium was successfully eliminated using Pd–citric acid chemical modifier. This chemical modifier was found to be the most advantageous in comparison with Pd mixture with ascorbic acid, tartaric acid, or citric acid–Li based on its ability to suppress the interference originating from different chloride matrix. Palladium increases the analyte stability; citric acid serves as a reducing reagent, and furthermore, it helps to remove the interfering chlorides by forming HCl, in the drying step of the electrothermal program. In the presence of the modifier, the pyrolysis temperature can be adjusted up to 1,000 °C with no loss of the analyte. The obtained limit of detection and characteristic mass were 5 ng g?1 and 1.7 pg, respectively. The accuracy of the method was verified by means of six different reference samples and by comparing the results of the analysis of real samples with those obtained by inductively coupled plasma orthogonal acceleration time-of-flight mass spectrometer. The proposed method was applied to the Ag determination in soils, sediments, and sewage sludge samples from the Pardubice region in Czech Republic.  相似文献   

20.
Ambient air samples were collected at two different locations between 2011 and 2012 in Zhengzhou, China in order to assess the concentration level, health risks, as well as the sources of polycyclic aromatic hydrocarbons (PAHs) in particulate matter (PM2.5). The mean annual levels of PM2.5 observed at industry site and residential site were 172?±?121 and 160?±?72 μg m?3, respectively, which were about five times the annual value of proposed PM2.5 standard (35 μg m?3) in China. The PM2.5 in all daily samples (n?=?47) exceeds the proposed PM2.5 standard in China (75 μg m?3) at both industrial and residential sites. Seasonal variations of PM2.5 showed a clear trend of winter?>?autumn?>?spring?>?summer at both sites. The total concentrations of 16 PM2.5-associated PAHs ranged from 61?±?51 to 431?±?281 and 38?±?25 to 254?±?189 ng m?3, with mean value of 176?±?233 and 111?±?146 ng m?3 at industry and residential sites, respectively. The major species were fluoranthene, pyrene, chrysene, benzo[b]fluoranthene and benzo[k]fluoranthene, and the concentration levels of PAHs in PM2.5 were higher in winter than those of other seasons at both sites. The annual mean values of toxicity equivalency concentrations of ∑16PAHs in PM2.5 were 22.8 and 13.5 ng m?3 in industry and residential area, respectively. In this study, the risk level of adult citizens through inhalation exposure to PAHs was calculated. The average estimates of lifetime inhalation cancer risks were approximately 8.9?×?10?7 and 6.3?×?10?7 for industry and residential sites, respectively. The main sources of 16 PAHs from both diagnostic ratios and principle component analysis identified as vehicular emissions and coal combustion.  相似文献   

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