Flame Atomic Absorption Spectrometry Determination of Trace Amounts of Cadmium and Zinc in Water Samples after Preconcentration onto Modified Amberlite XAD‐4 Resin

In the present article, a procedure for the simultaneous separation and preconcentration of trace amounts of cadmium and zinc is proposed. It is based on the adsorption of cadmium and zinc ions onto a column of Amberlite XAD‐4 resin loaded with aluminon reagent. Cadmium and zinc ions are quantitatively retained on the column in the pH range from 6.5–7.5, at a flow rate of 2 mL min^–1. The cadmium and zinc ions are eluted with 5.0 mL of 5 mol L^–1 HNO₃ solution. Cadmium and zinc are measured by flame atomic absorption spectrometry (FAAS). In the present case, 0.1 μg of cadmium and 0.5 μg of zinc can be concentrated in the column from 1000 mL of aqueous sample, where their concentrations are as low as 0.1 and 0.5 ng mL^–1, respectively. The relative standard deviations, for seven replicated determinations of 1.0 μg mL^–1 of cadmium and zinc, are 1.2 and 1.1%, respectively. The detection limits for cadmium and zinc in the original solution are 0.02 and 0.11 ng mL^–1, respectively. The interference of a large number of anions and cations has been studied and the optimized conditions are utilized for the determination of trace amounts of cadmium and zinc in different environmental and standard samples.     

Dispersive Liquid–Liquid Microextraction for Preconcentration and Determination of Nickel in Water

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.     

Development of Dispersive Liquid–Liquid Microextraction Based on Solidification of Floating Organic Drop for the Determination of Trace Lead in Water

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

Assessment of Trace Metal Contamination of Drinking Water in the Pearl Valley,Azad Jammu and Kashmir

The aim of this study was to assess trace metal contamination of drinking water in the Pearl Valley, Azad Jammu and Kashmir (Pakistan). The objectives were to determine physical properties and the dissolved concentration of five trace metals, i. e., lead, copper, nickel, zinc, and manganese, in drinking water samples collected from various sites of municipal water supply, natural water springs and wells in the valley. Concentrations of the metals in the water samples were determined by flame atomic absorption spectrometry. Results showed physical parameters, i. e., appearance, taste and odor within acceptable limits and pH was between 5.5 and 7.0. The observed concentrations of the metals varied between sources of water samples and between sampling sites. Maximum dissolved concentration observed was 4.7 mg/L for Pb and Mn, 4.6 mg/L for Zn, 2.9 mg/L for Ni and 2.8 mg/L for Cu. The observed concentrations of the metals were compared with the World Health Organization's guideline values for drinking water. Overall, the quality of water samples taken from the water springs at Mutyal Mara and Bonjosa was good; however, the water quality was unsuitable for drinking in Kiraki, Kharick, and Pothi Bala localities particularly. Finally, the authors discuss possible causes for increased concentrations of the trace metals in drinking water in the study area.     

Speciation and Determination of Inorganic Mercury and Methylmercury by Headspace Single Drop Microextraction and Electrothermal Atomic Absorption Spectrometry in Water and Fish

In this study, headspace single drop microextraction (HS‐SDME) method in combination with electrothermal atomic absorption spectrometry (ETAAS) method was developed and validated for the speciation and determination of inorganic mercury (iHg) and methylmercury (MeHg). MeHg and iHg species were reduced to volatile methylmercury hydride (CH₃HgH) and elemental mercury, respectively, in the presence of NaBH₄ and trapped onto a drop of acceptor phase in the tip of a microsyringe. Thiourea and ammonium pyrrolydinedithiocarbamate (APDC) were tested as the acceptor phase. The experimental parameters of the method such as microextraction time, temperature, NaBH₄ concentration, acceptor phase concentration, and pH of the medium were investigated to obtain distinctive conditions for mercury species. Possible interference effects have also been investigated. In order to validation of the method, analytical figures of merits such as accuracy, precision, limit of detection (LOD), limit of quantitation (LOQ), and linear working range have been evaluated. Accuracy of the method has been verified by analyzing certified reference materials (BCR 453 Tuna fish) and spiked samples. The proposed method was applied for the speciation and determination of mercury species in water and fish samples. Mercury species (MeHg and iHg) have been determined in the real samples with a relative error less than 10%.     

Effect of Sample Digestion,Air Filter Contamination,and Post‐adsorption on the Analysis of Trace Elements in Air Particulate Matter

Inductively coupled plasma atomic emission spectrometry and inductively coupled plasma MS are the major analytical tools for trace elements in environmental matrices, however, the underestimate of certain trace elements in analysis of air particulate matter by these two techniques has long been observed. This has been attributed to incomplete sample digestion. Here, we demonstrate that the combined effects of sample digestion, air filter impurities, and post‐adsorption of the analytes contribute to the interference of the analysis. Particular attention should be paid to post‐adsorption of analytes onto air filters after acid digestion.     

Development of an Analytical Method for the Determination of Trace Lead in Lake Water Samples by Flame Atomic Absorption Spectrophotometry after Vortex Assisted-Stearic Acid Coated Magnetic Nanoparticle Based Extraction

In the present study, a method is proposed for the determination of lead at trace levels by slotted quartz tube-flame atomic absorption spectrophotometry (SQT-FAAS) after preconcentration with stearic acid coated magnetic nanoparticle-based dispersive solid phase extraction (SA-MNP-DSPE). The slotted quartz tube (SQT) is used to enhance the analyte atom residence time in the light path. Stearic acid coated magnetic iron oxide (Fe₃O₄) nanoparticles, which can be easily collected with an external magnet, are used as adsorbent in the extraction process. The limit of detection (LOD) and the limit of quantitation (LOQ) values of the proposed method are obtained as 0.90 and 2.9 µg L⁻¹, respectively. The method allows high repeatability in a wide linear range between 5.0 and 250 µg L⁻¹, and the relative standard deviation for six replicates is 5.8%. The detection power is enhanced by about 77-fold compared to the regular flame atomic absorption spectrophotometry (FAAS) system. The method is validated by recovery experiments to four different lake water samples. After the spiking tests, good recovery results are calculated between 97% and 106%. These results show that lead can be detected at low levels in lake water samples with high sensitivity, accuracy, and precision.     

On‐line Solid Phase Extraction of Copper in Water Samples with Flow Injection Flame Atomic Absorption Spectrometry

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

Cloud Point Extraction for the Preconcentration of Silver and Palladium in Real Samples and Determination by Atomic Absorption Spectrometry

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.     

Evaluation of Two Low‐Cost–High‐Performance Adsorbent Materials in the Waste‐to‐Product Approach for the Removal of Pesticides from Drinking Water

This study evaluates the performance of two low cost and high performance adsorption materials, i.e., activated carbon produced from two natural waste products: Bamboo and coconut shell, in the removal of three pesticides from drinking water sources. Due to the fact that bamboo and coconut shell are abundant and inexpensive materials in many parts of the world, they respond to the “low‐cost” aspect. The adsorption capacities of two local adsorbents have been compared with commercial activated carbon to explore their potential to respond to the “high quality” aspect. Two pesticides were selected, namely dieldrin and chlorpyrifos, because they are commonly used in agriculture activities, and may remain in high concentrations in surface water used as drinking water sources. The results indicate that the adsorption of pesticides on activated carbons is influenced by physico‐chemical properties of the activated carbon and the pesticides such as the presence of an aromatic ring, and their molar mass. The activated carbon produced from bamboo can be employed as low‐cost and high performance adsorbent, alternative to commercial activated carbon for the removal of pesticides during drinking water production. The performance of activated carbon from bamboo was better due to its relatively large macroporosity and planar surface. The effect of adsorbent and pesticide characteristics on the performance was derived from batch experiments in which the adsorption behavior was studied on the basis of Freundlich isotherms.     

Spatio‐temporal variability of water and energy fluxes – a case study for a mesoscale catchment in pre‐alpine environment

Water and energy fluxes at and between the land surface, the subsurface and the atmosphere are inextricably linked over all spatio‐temporal scales. Our research focuses on the joint analysis of both water and energy fluxes in a pre‐alpine catchment (55 km²) in southern Germany, which is part of the Terrestrial Environmental Observatories (TERENO). We use a novel three‐dimensional, physically based and distributed modelling approach to reproduce both observed streamflow as an integral measure for water fluxes and heat flux and soil temperature measurements at an observation location over a period of 2 years. While heat fluxes are often used for comparison of the simulations of one‐dimensional land surface models, they are rarely used for additional validation of physically based and distributed hydrological modelling approaches. The spatio‐temporal variability of the water and energy balance components and their partitioning for dominant land use types of the study region are investigated. The model shows good performance for simulating daily streamflow (Nash–Sutcliffe efficiency > 0.75). Albeit only streamflow measurements are used for calibration, the simulations of hourly heat fluxes and soil temperatures at the observation site also show a good performance, particularly during summer. A limitation of the model is the simulation of temperature‐driven heat fluxes during winter, when the soil is covered by snow. An analysis of the simulated spatial fields reveals heat flux patterns that reflect the distribution of the land use and soil types of the catchment. The water and energy partitioning is characterized by a strong seasonal cycle and shows clear differences between the selected land use types. Copyright © 2016 The Authors Hydrological Processes Published by John Wiley & Sons Ltd.     

Sensitive Ion‐Flotation Separation of Ag(I) Traces Using 2‐(2‐Methoxyphenyl)benzimidazole before Flame Atomic Absorption Spectrometric Determination in Water

A sensitive, reliable, and environmentally friendly method for simple separation and preconcentration of Ag(I) traces in aqueous samples is presented prior to their flame atomic absorption spectrometric determinations. At pH 7.0, Ag(I) was separated with 2‐(2‐methoxyphenyl)benzimidazole (MPBI) as a new complexing agent and floated after adding sodium dodecyl sulfate (SDS) as a foaming reagent. The floated layer was then dissolved in proper amount of concentrated nitric acid in methanol and introduced to the flame atomic absorption spectrometer (FAAS). The effects of pH, concentration of MPBI, type and amount of surfactant as the floating agent, type and amount of eluting agent, and influence of foreign ions on the recovery of the analyte ion were investigated. Also, using a nonlinear curve fitting method, the formation constant of 1.62 × 10⁶ was obtained for Ag(I)–MPBI complex. The analytical curve was linear in the range of 1.8 × 10^?7–1.7 × 10^?6 mol/L for determination of Ag(I). The relative standard deviation (RSD; N = 10) corresponding to 0.7 × 10^?6 mol/L of Ag(I), the limit of detection (10 blanks), and the enrichment factor were obtained as 1.7%, 2.9 × 10^?8 mol/L, and 43.0, respectively. The proposed procedure was then applied successfully for determination of silver ions in different water samples.     

The Use of Polyphenolic Compounds from Black Tea for the Solid Phase Extraction and Determination of Trace Iron in Drinking Water

A simple and selective solid phase extraction procedure for the trace analysis of iron(III) in water samples has been developed. Sodium dodecyl sulfate coated alumina, modified with polyphenolic compounds (extracted from black tea) was used for the extraction and preconcentration of iron(III) from water samples before determination by flame atomic absorption spectrometry. Due to the complexation reaction between iron(III) and polyphenol compounds, iron(III) was quantitatively extracted on the proposed sorbent and then eluted by 2.0 mL of HCl (1.0 mol/L). The effects of extraction parameters, such as pH and volume of sample solution, amount of polyphenolic compounds, type of eluting agent and the effect of interfering ions on the extraction of iron(III), were investigated. It was found that the proposed method had a good linear range (15.0–100.0 μg/L) and a low detection limit (10.0 μg/L). The procedure was successfully applied for iron determination in drinking water samples.