Simultaneous quantification of Bi(III) and U(VI) in environmental water samples with a complicated matrix containing organic compounds

Trace amounts of bismuth(III) and uranium(VI) can be simultaneously determined in a single scan by adsorptive cathodic stripping voltammetry in the presence of cupferron as a complexing agent. Optimal conditions were found to be: 0.1 mol?L^?1 acetate buffer (pH 5.3), 5?×?10^?5?mol?L^?1 cupferron, accumulation potential of ?0.25 V, and accumulation time of 30 s. The linear range of Bi(III) and U(VI) was observed over the concentration range from 2?×?10^?9 to 2?×?10^?7?mol?L^?1 and from 1?×?10^?8 to 5?×?10^?7?mol?L^?1, respectively. The influence of the main components of real water samples such as foreign ions and organic substances (surface active substances, humic substances) was precisely investigated. The method was applied to the simultaneous measurements of bismuth and uranium in natural water samples.     

Cloud point extraction–atomic absorption spectrometry for pre-concentration and determination of cadmium in cigarette samples

A new complexing agent, 2-((2-((1H-benzo[d]imidazole-2yl)methoxy)phenoxy)methyl)-1H-benzo[d]imidazole (BIMPI), was used in cloud point extraction and applied for selective pre-concentration of trace amounts of cadmium in cigarette samples. Cadmium was complexed with BIMPI in a buffer solution (pH?=?10) using Triton X-114 as surfactant and quantitatively extracted into a small volume of the surfactant-rich phase after centrifugation. Under optimized conditions (pH?=?10.0, 0.8?×?10^?4?mol?L^?1 BIMPI and 0.08 % (w/v) Triton X-114), calibration graph was linear in the range of 34.0–1,670.0 μg?L^?1. The proposed method was applied to the determination of Cd in various cigarette (tobacco) samples which gave satisfactory results.     

Environmental assessment of 2-mercaptobenzimidazole based on the surface plasmon resonance band of gold nanoparticles

A colorimetric assay method is described for the environmental detection of 2-mercaptobenzimidazole (MBI) using surface plasmon resonance of gold nanoparticles (AuNPs). Stable and dispersed AuNPs with intensified plasmon resonance were prepared in situ using a simple, rapid, and eco-friendly procedure by applying ascorbic acid as a reducer and cetyltrimethylammonium bromide as a stabilizer. The presence of MBI has a strong effect on the plasmon absorbance of AuNPs, which was employed for the detection of MBI. The calibration curve was linear in the range of 1.0?×?10^?6–5.5?×?10^?5 mol/L of MBI; the detection limit was 8.4?×?10^?7 mol/L. The relative standard deviations for eight replicate measurements of 3.0?×?10^?6 and 5?×?10^?5 mol/L MBI were 3.9 and 1.4 %, respectively. The method was successfully applied to the determination of MBI in tap, river, sea, and heat exchanger cooling water samples.     

Rapid spectrophotometric determination of trace amounts of palladium in water samples after dispersive liquid–liquid microextraction

A simple, rapid, and efficient dispersive liquid–liquid microextraction method, followed by UV–Vis spectrophotometry was developed for the preconcentration and determination of Pd ions in water samples. Pd ions react with α-furildioxime (chelating agent) to form a hydrophobic complex. Various parameters were altered to study and optimize their effects on the extraction efficiency, such as pH, ligand concentration, the type and volume of extraction and dispersive solvents, extraction time, and salt concentration. Under optimized conditions, the method exhibited an enrichment factor (C _org/C _aq) of 25 and recovery more than 98 % within a very short extraction time. The linearity of the method ranged from 10 to 200 μg?L^?1. The limit of detection was 1.1 μg?L^?1. The relative standard deviation for the concentration of 100 μg?L^?1 of Pd was 2.3 % (n?=?10). Finally, the developed method was successfully applied to the extraction and determination of Pd in tap, river, mineral, and sea water samples.     

A very sensitive flow-injection spectrophotometric determination method for iron (II) and total iron using 2′, 3, 4′, 5, 7-pentahydroxyflavone

In this study, an ultra-sensitive and highly selective, rapid flow-injection spectrophotometric method for the determination of iron (II) and total iron has been proposed. The method was based on the reaction between iron (II) and 2′, 3, 4′, 5, 7-pentahydroxyflavone in slightly acidic solution with a strong absorption at 415 nm. The carrier solution used was 1?×?10^?5 M 2′, 3, 4′, 5, 7-pentahydroxyflavone in 0.1 M HAc/Ac^? buffer solution at pH 4.5. Parameters that affect simultaneously the determination of iron (II) and interfering ions were tested. The relative standard deviation for the determination of 50 μg L^?1 iron (II) was 0.85 % (n?=?10), and the limit of detection (blank signal plus three times the standard deviation of the blank) was 3 μg L^?1, both based on injection volumes of 20 μL. The method has been successfully applied to the determination of iron (II) and total iron in water samples and ore samples. The method was verified by analysing a certified reference material Zn/Al/Cu 43XZ3F.     

Evaluation of optimal conditions for determination of low selenium content in shellfish samples collected at Todos os Santos Bay,Bahia, Brazil using HG-AFS

This work proposes a procedure for the determination of total selenium content in shellfish after digestion of samples in block using cold finger system and detection using atomic fluorescent spectrometry coupled hydride generation (HG AFS). The optimal conditions for HG such as effect and volume of prereduction KBr 10 % (m/v) (1.0 and 2.0 ml) and concentration of hydrochloric acid (3.0 and 6.0 mol L^?1) were evaluated. The best results were obtained using 3 mL of HCl (6 mol L^?1) and 1 mL of KBr 10 % (m/v), followed by 30 min of prereduction for the volume of 1 mL of the digested sample. The precision and accuracy were assessed by the analysis of the Certified Reference Material NIST 1566b. Under the optimized conditions, the detection and quantification limits were 6.06 and 21.21 μg kg^?1, respectively. The developed method was applied to samples of shellfish (oysters, clams, and mussels) collected at Todos os Santos Bay, Bahia, Brazil. Selenium concentrations ranged from 0.23?±?0.02 to 3.70?±?0.27 mg kg^?1 for Mytella guyanensis and Anomalocardia brasiliana, respectively. The developed method proved to be accurate, precise, cheap, fast, and could be used for monitoring Se in shellfish samples.     

New kinetic-spectrophotometric method for monitoring the concentration of iodine in river and city water samples

A new kinetic method has been developed for the determination of iodine in water samples. The method is based on the catalytic effect of I^? with the oxidation of Indigo Carmine (IC) by KBrO₃ in the sulfuric acid medium. The optimum conditions obtained are 0.16 M sulfuric acid, 1?×?10^?3 M of IC, 1?×?10^?2 M KBrO₃, reaction temperature of 35°C, and reaction time of 80 s at 612 nm. Under the optimized conditions, the method allowed the quantification of I^? in a range of 12–375 ng/mL with a detection limit of 0.46 ng/mL. The method was applied to the determination of iodine in river and city water samples with the satisfactorily results.     

The evaluation of the association constant between R-SN and Hg2+

The effective determination of heavy metals from environmental media is among the most important issues for many industrialized countries. The interaction between RS-N, as novel heavy metal probe, and metal ions was studied. RS-N shows selective color change from colorless to pink in the presence of Hg²⁺ in methanol/water solvent and the UV–Vis study shows peak at 560 nm. Fluorescence data revealed that the fluorescence enhance of RS-N by Hg²⁺ dramatically was the result of the formation of [Hg²⁺]RS-N complex. The effective association constants (K _a ) were 3.97?×?10⁵ and 0.204?×?10⁵ M^?1 for Hg²⁺ and Cu²⁺ to RS-N, respectively. The thermodynamic parameters, enthalpy change (ΔH ⁰) and entropy change (ΔS ⁰), were calculated to be ?6.431?±?0.226 kJ/mol and ?0.129?±?0.008 J/K/mol, respectively, according to van’t Hoff equation on the basis of Gibbs free energy (ΔG ⁰) ranged from ?33.8326 to ?28.5389 kJ/mol.     

Flow injection spectrophotometric determination of methamidophos using online hydrolysis

A new protocol for the online spectrophotometric determination of methamidophos has been developed. The method is based on online hydrolysis of methamidophos, and the resulting hydrolyzed product is reacted with sodium nitroproside to form a colored complex. The calibration curve is linear over the concentration range of 0.5–20 μgml^?–?1, with a molar absorptivity of 2.5×10⁴ L mol^?1 cm^?1. The method is fast and reproducible with a sample throughput of 90 samples/h. The method is successfully applied to formulations and real samples.     

Application of cold-induced aggregation microextraction as a fast,simple, and organic solvent-free method for the separation and preconcentration of Se(IV) in rice and various water samples

The developed method is based on cold-induced aggregation microextraction of Se(IV) using the 1-butyl-3-methylimidazolium hexafluorophosphate ionic liquid as an extractant followed by spectrophotometry determination. The extraction of Se(IV) was performed in the presence of dithizone as the complexing agent. In this method, a very small amount of 1-butyl-3-methylimidazolium hexafluorophosphate was added to the sample solution containing Se-dithizone complex. Then, the solution was kept in a thermostated bath at 50 °C for 4 min. Subsequently, the solution was cooled in an ice bath and a cloudy solution was formed. After centrifuging, the extractant phase was analyzed using a spectrophotometric detection method. Some important parameters that might affect the extraction efficiency were optimized (HCl, 0.6 mol L^?1; dithizone, 4.0?×?10^?6 mol L^?1; ionic liquid, 100 μL). Under the optimum conditions, good linear relationship, sensitivity, and reproducibility were obtained. The limit of detection (LOD) (3S_b/m) was 1.5 μg L^?1, and the relative standard deviation (RSD) was 1.2 % for 30 μg L^?1 of Se(IV). The linear range was obtained in the range of 5–60 μg L^?1. It was satisfactory to analyze rice and various water samples.     

Utility of cefixime as a complexing reagent for the determination of Ni(II) in synthetic mixture and water samples

A simple, sensitive, and accurate UV spectrophotometric method has been developed for the determination of nickel in synthetic mixture and water samples. The method is based on the complexation reaction of nickel ion with cefixime, thus leading to the formation of Ni–cefixime complex in ethanol-distilled water medium at room temperature. The complex showed the maximum absorption wavelength at 332 nm. Beer’s law is obeyed in the working concentration range of 0.447–4.019 μg?mL^?1 with apparent molar absorptivity of 7.314?×?10³?L?mol^?1?cm^?1 and Sandell’s sensitivity of 0.008 μg/cm²/0.001 absorbance unit. The limits of detection and quantitation for the proposed method are 0.016 and 0.054 μg?mL^?1, respectively. The factors such as cefixime concentration and solvent affecting the complexation reaction were carefully studied and optimized. The method is validated as per the International Conference on Harmonisation guideline. The method is successfully applied to the determination of Ni(II) in synthetic mixture and wadi water samples collected from Al Rustaq. The same water samples are also analyzed by atomic absorption spectrophotometry. Both methods determined the amount of Ni(II) in water sample and found to be approximately the same.     

Solid phase extraction and determination of Cr(III) by spectrophotometry using cefaclor as a complexing reagent and FAAS

The present study reports on the application of modified groundnut shell as a new, easily prepared, and stable sorbent for the extraction of trace amount of Cr(III) in aqueous solution. 2-Hydroxybenzaldiminoglycine was immobilized on groundnut shells in alkaline medium and then used as a solid phase for the column preconcentration of Cr(III). The elution was carried out with 3 mL of 2 mol?L^?1 HCl. The amount of eluted Cr(III) was determined by spectrophotometry using cefaclor as a complexing reagent and by flame atomic absorption spectrometry (FAAS). Different experimental variables such as pH, amount of solid sorbent, volume and concentration of eluent, sample and eluent flow rate, and interference of other metal ions on the retention of Cr(III) were studied. Under the optimized conditions, the calibration curves were found to be linear over the concentration range of 13–104 and 10–75 μg?L^?1 with a detection limit of 3.64 and 1.24 μg?L^?1 for spectrophotometric method and FAAS, respectively. An enrichment factor of 200 and RSD of ±1.19–1.49 % for five successive determinations of 25 μg?L^?1 were achieved. The column preconcentration was successfully applied to the analysis of tap water and underground water samples.     

Extraction of ultra traces of polychlorinated biphenyls in aqueous samples using suspended liquid-phase microextraction and gas chromatography-electron capture detection

This study reports the feasibility of applying directly suspended liquid-phase microextraction (DSLPME)-gas chromatography detection for the pre-concentration and determination of low levels of eight polychlorinated biphenyls (PCBs) in aqueous samples. The technique requires minimal sample preparation, analysis time and solvent consumption and represents significant advantages over conventional analytical methods. The experimental parameters such as salt content, sample temperature, stirring rate, extraction time, micro-drop volume and breakthrough volume were investigated and found to have significant influences on DSLPME. Under the optimal experimental conditions, the enrichment factor ranged from 578 to 729, and the recovery was above 93 %. Calibration curves possessed good linearity (R ²?>?0.99) over a wide concentration range of 0.1–10.0 μg L^?1 with limits of detection ranging from 0.01 to 0.07 μg L^?1. The relative standard deviations for 1.0 μg L^?1 of PCBs in water by using internal standard were in the range 2–14 % (n?=?3). The proposed simple, accurate and sensitive analytical method was applied successfully to the determination of trace amounts of PCBs in water samples.     

Assessment of cylindrospermopsin toxin in an arid Saudi lake containing dense cyanobacterial bloom

This study reports the presence of the cyanobacterial toxin cylindrospermopisn (CYN) and its producer Cylindrospermopsis raciborskii for the first time in Saudi freshwater sources. C. raciborskii was found in Gazan Dam Lake water with two morphotypes (coiled and straight). The appearance and cell density of this species was significantly positively related to high temperature and high ammonium concentrations, and negatively with nitrate and phosphate concentrations in the lake. Intracellular concentrations of CYN (4–173 μg L^?1) were associated with C. raciborskii rather than other cyanobacteria with a maximal value obtained in June 2011, coinciding with the highest bloom of this species (19?×?10⁷ trichome L^?1). CYN cell quotas (0.6–14.6 pg cell^?1) varied significantly along the study period and correlated with most environmental factors. The results of ELISA and liquid chromatography-mass spectrometry proved that the CYN production by strains of this species was isolated from this lake during the present study, with an amount reaching 568 μg g^?1. Extracellular CYN was also detected in cell-free lake water at concentrations 0.03–23.3 μg L^?1, exceeding the drinking water guideline value of 1 μg L^?1 during the Apr–Jul period. As this lake is an important source for drinking and irrigation waters, CYN monitoring should be included in the environmental and health risk assessment plans of these water bodies.     

Voltammetric determination of platinum at a lead film electrode in environmental water samples

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.     

Distributions, sources, and ecological risks of DDT-related contaminants in water, suspended particulate matter, and sediments from Haihe Plain, Northern China

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.     

Determination of hydrazine hydrate based on electrochemiluminescence of Ru(bpy) 3 2+

Considering of the basic properties and also the two nitrogen atoms in the structure, hydrazine hydrate was employed to be an amine additive candidate, to build a Ru(bpy) ₃ ²⁺ /hydrazine electrochemiluminescence (ECL) system, and ECL of Ru(bpy) ₃ ²⁺ has been employed for the determination of hydrazine hydrate in the paper. The result demonstrated that the logarithmic ECL increasing (ΔECL?=?ECL_{after addition of hydrazine}???ECL_{before addition of hydrazine}) versus the logarithmic concentration of hydrazine hydrate is linear over a concentration range of 1.0?×?10^?9 to 1.0?×?10^?5?mol/L, on both glassy carbon and Pt electrodes in a pH 9 phosphate buffer. The hydrazine hydrate detection limit was down to 1.0?×?10^?9?mol/L, comparatively lower than other detection methods. To check its applicability, the proposed method was applied to the determination of hydrazine hydrate added into a tap water sample with good reproducibility and stability. All these provide a possibility to develop a novel ECL detection method for hydrazine in water.     

Quantification of PAHs and chlorinated compounds by novel solid-phase microextraction based on the arrays of tin oxide nanorods

The results of an innovative study on a new and highly efficient stationary phase based on the SnO₂ nanorods coating on fused silica have been reported in this paper. SnO₂ nanorods have been grown on fused silica fibers using a hydrothermal process. The extraction properties of the fiber were investigated using headspace solid-phase microextraction (HS-SPME) mode coupled with gas chromatography–mass spectrometry detection for 1,4-dichloro-2-nitrobenzene, biphenyl, and acenaphthene. The effect of different variables on extraction efficiency was studied simultaneously using Box–Behnken method as experimental design. The variables of interest in the HS-SPME were salt effect, adsorption temperature, extraction, and desorption time. Under optimal conditions, the calibration curves were linear up to 10²–10⁵ ng?L^?1 (R ²?>?0.998) with detection limits of 10^?3, 10^?1, and 10 ng?L^?1 for acenaphthene, biphenyl, and 1,4-dichloro-2-nitrobenzene, respectively. The relative standard deviations for single fiber and fiber to fiber were less than 9.8 and 12.5 %, respectively. The high stability of the SnO₂ nanostructure coating is proved at relatively high temperatures (up to 300 °C) with a high extraction capacity and long lifespan (more than 100 times). By applying the proposed technique, promising recoveries (93–98 %) were obtained in the analysis of environmental water samples.     

The use of silica gel modified with allyl 6-methyl-4-phenyl-2-thioxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate for selective separation and preconcentration of lead in environmental samples

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.     

Assessment of physico-chemical qualities and heavy metal concentrations of Umgeni and Umdloti Rivers in Durban,South Africa

We assessed the effects of seasonal dynamics on the physico-chemical qualities and heavy metals concentrations of the Umgeni and Umdloti Rivers in Durban, South Africa. Water samples were taken from nine different sampling points and analysed for the following parameters; temperature, pH, turbidity, electrical conductivity (EC), biological oxygen demand (BOD₅), chemical oxygen demand (COD), phosphate (PO₄ ^2?), nitrate (NO₃ ^2?), ammonium (NH₄ ⁺), sulphate (SO₄ ^2?), lead (Pb²⁺), mercury (Hg²⁺), cadmium (Cd²⁺), aluminium (Al³⁺), and copper (Cu²⁺) using standard methods. The data showed variations it terms of the seasonal fluctuations and sampling regime as follows: temperature 12–26.5 °C; pH 5.96–8.45; turbidity 0.53–18.8 NTU; EC 15.8–5180 mS m^?1; BOD₅ 0.60–7.32 mg L^?1; COD 10.5–72.9 mg L^?1; PO₄ ^2??<?500–2,460 μg L^?1; NO₃ ^2? <0.05–4.21 mg L^?1; NH₄ ⁺?<?0.5–1.22 mg L^?1; SO₄ ^2? 3.90–2,762 mg L^?1; Pb²⁺ 0.023–0.135 mg L^?1; Hg²⁺ 0.0122–0.1231 mg L^?1 Cd²⁺ 0.068–0.416 mg L^?1; Al³⁺ 0.037–1.875 mg L^?1, and Cu²⁺0.006–0.144 mg L^?1. The concentrations of most of the investigated parameters exceeded the recommended limit of the South African Guidelines and World Health Organization tolerance limits for freshwater quality. We conclude that these water bodies are potentially hazardous to public health and this highlights the need for implementation of improved management strategies of these river catchments for continued sustainability.