Development of an efficient and sensitive analytical method for the determination of copper at trace levels by slotted quartz tube atomic absorption spectrometry after vortex-assisted dispersive liquid-liquid microextraction in biota and water samples using a novel ligand

This study describes the determination of trace levels of copper by slotted quartz tube atomic absorption spectrometry after dispersive liquid-liquid microextraction. A ligand synthesized from the reaction of salicylaldehyde and 1-naphthylamine was used to form coordinate copper complex prior to extraction. All parameters that influence the output of complex formation, extraction, and instrumental measurement were optimized to enhance the absorbance signal of copper. Under the optimum conditions, about 104-fold enhancement in sensitivity was recorded over the conventional flame atomic absorption spectrometer, corresponding to a 0.51 ng/mL detection limit. The percent relative standard deviation calculated for the lowest concentration (4.8%) indicated high precision for the experimental procedure. Accuracy and applicability of the optimum method were determined by performing spiked recovery tests on urine, lake water, and mineral water samples. Satisfactory recovery results were obtained between 82.2 and 106.3% at four different concentrations. Matrix matching method was also performed to increase the accuracy of quantification, and the percent recovery calculated for 175 ng/mL was 105.14%.     

Variations of measured and simulated soil-loss amounts in a semiarid area in Turkey

The main goal of this research was soil-loss determination and comparison of the plot measurement results with simulation model (universal soil loss equation (USLE)) results in different land use and slope classes. The research took place in three different land-use types (Scotch pine forest, pasture land, and agricultural land) and in two different slope classes (15–20%, 35–40%). Within six measurement stations (for each land-use type and slope class-one station), totally 18 measurement plots have been constituted, and soil-loss amount measurements have been investigated during the research period (3 years along). USLE simulation model is used in these measurement plots for calculation the soil-loss amounts. The results pointed out that measured (in plots) and simulated (with USLE) soil-loss amounts differ significantly in each land-use type and slope class.     

Determination of heavy metal concentrations in street dusts in Istanbul E-5 highway

Components and quantity of street dust are environmental pollution indicators especially in big cities. Street dust is generally composed of car exhaust gas originated particles and wind-transported particles. Heavy metals, which are found in street dust, such as Pb, Cu, Mn, Zn, Cd and Ni are significant for environmental pollution. According to the kind of vehicle in traffic, quantity and type of heavy metals vary in street dust. The use of leaded gasoline gives a boost to the importance of lead level especially in street dust even at the start of 21st century. These metals possess bioaccumulation property, and the possibility of the amount of these metals reaching a critical value and threatening human health increases the importance of this issue. In this study, street dusts have been collected from E-5 Highway from Topkapi to Avcilar regions that spans about 18 km in Istanbul, Turkey, and Pb, Cu, Mn, Zn, Cd and Ni concentrations have been detected in street dust. Twenty-two street dust samples were taken from a total of 22 different points at previously decided 14 main areas. Analyses were conducted using Leeds Public Analyst method. According to the results of this study, Pb, Cu and Zn concentrations in E-5 Highway between Topkapi and Avcilar region in Istanbul were higher than maximum concentration levels of these heavy metals in normal soil. This situation indicates that there is heavy metal pollution in the inspected area in E-5 Highway in Istanbul.     

Simultaneous determination of iprodione,procymidone, and chlorflurenol in lake water and wastewater matrices by GC-MS after multivariate optimization of binary dispersive liquid-liquid microextraction

This study reports the optimization of a binary dispersive liquid-liquid microextraction method for the determination of iprodione, procymidone, and chlorflurenol by gas chromatography mass spectrometry. The study was aimed at using two extraction solvents to increase the extraction efficiency of all analytes. The binary solvents recorded results higher than the mono-solvents. After examining the effects of main experimental parameters and their interactions by analysis of variance, 200 μL of binary mixture (dichloromethane and 1,2-dichloroethane), 2.5 mL of ethanol, and 15 s vortex were obtained as optimum parameters. The detection and quantification limits calculated for the analytes were found to be between 0.30–1.6 and 1.0–5.3 ng/mL, respectively. Enhancement in detection power calculated as a ratio of the binary extraction detection limit to the detection limit of direct GC-MS analysis was 105-, 214-, and 233-fold for chlorflurenol, iprodione, and procymidone, respectively. In order to check the accuracy of the developed method, recovery study was performed. Water sampled from a lake and two wastewater samples from treatment facilities were spiked at two concentrations, and the percent recovery calculated for the samples ranged between 87 and 116%. These results confirmed the suitability of the method to real samples for accurate determination of the analytes at trace levels.     

A novel liquid-liquid extraction for the determination of naphthalene by GC-MS with deuterated anthracene as internal standard

Polycyclic aromatic hydrocarbons are known for their carcinogenic and mutagenic effects on human health. This therefore calls for the regulation of their concentrations in air, water, and soil. Naphthalene as the simplest in structure of the polycyclic aromatic hydrocarbons is mainly used as a starter material for other chemicals but also has impacts on human health. A method is therefore proposed for the determination of naphthalene in water samples by gas chromatography mass spectrometry after liquid-liquid extraction. The extraction method was optimized to improve the extraction output, thereby lowering the limit of detection. The limits of detection and quantification obtained for naphthalene were 4.4 and 14.6 ng mL^?1, respectively. Deuterated anthracene was used as internal standard to enhance the precision of the method, for which a relative standard deviation of 4.3% was obtained. The percent recovery of naphthalene obtained from tap water was ranged between 93.8 and 102.2.     

Simultaneous determination of estrone and selected pesticides in water medium by GC-MS after multivariate optimization of microextraction strategy

A sensitive and accurate analytical method based on dispersive liquid-liquid microextraction was developed for the simultaneous determination of selected pesticides, hormones, and endocrine disruptors by GC-MS. The optimum conditions of the extraction procedure were determined using an experimental design of factors significantly affecting the extraction output. Analysis of variance (ANOVA) was used to evaluate the main effects of experimental factors and their interactions. The limit of detection values determined for the analytes under optimum experimental conditions were found to be between 0.30–2.0 ng/mL. The linear calibration plot of analytes span across a wide concentration range and low %RSD values from replicate measurements indicated good precision of the developed method. Spiked recovery tests were also performed on municipal wastewater, well water, lake water, sea water, and tap water matrices to determine the method’s accuracy and applicability to water samples. The recovery results obtained were satisfactory for all water samples.     

Determination of lead, cadmium and copper in roadside soil and plants in Elazig, Turkey

The concentrations of lead, cadmium and copper in roadside soil and plants in Elazig, Turkey were investigated. Soil samples were collected at distances of 0, 25 and 50 m from the roadside. The concentrations of lead, cadmium and copper were measured by Flame Atomic Absorption Spectrophotometry (FAAS). A slotted tube atom trap (STAT) was used to increase the sensitivity of lead and cadmium in FAAS. Lead concentrations in soil samples varied from 1.3 to 45 mg kg⁻¹ while mean lead levels in plants ranged from120 ng g⁻¹ for grape in point-4 to 866 ng g⁻¹ for apple leaves in point-2. Lead analyses showed that there was a considerable contamination in both soil and plants affected from traffic intensity. Overall level of Cd in soil samples lies between 78 and 527 ng/g while cadmium concentration in different vegetations varied in the range of 0.8–98.0 ng g⁻¹. Concentrations of copper in soil and plant samples were found in the range of 11.1–27.9 mg kg⁻¹ for soil and 0.8–5.6 mg kg⁻¹ for plants. Standard reference material (SRM) was used to find the accuracy of the results of soil analyses.     

Simultaneous determination of selected endocrine disrupter compounds in wastewater samples in ultra trace levels using HPLC-ES-MS/MS

An analytical procedure for the simultaneous determination of six selected endocrine disrupter compounds (EDCs: diltiazem, progesterone, benzyl butyl phthalate (BBP), estrone, carbamazepine (Cbz), acetaminophen) was developed by liquid chromatography electrospray ionization tandem mass spectrometry (HPLC-ES-MS/MS). All of the parameters for HPLC and ES-MS/MS systems including mobile phase composition, flow rate, and sample injection volume were optimized to obtain not only the best separation of species interested but also low detection limits. Reverse phase chromatography coupled to ES-MS/MS was used for the separation and detection of EDCs. Formic acid (0.10% ) and 5.0 mM ammonium formate were selected as mobile phase composition in gradient elution. Detection limits for diltiazem, progesterone, BBP, estrone, Cbz, and acetaminophen were found to be 0.13, 0.12, 0.04, 0.13, 0.12, and 0.05 ng/mL, respectively. Influent and effluents from three different wastewater treatment plants located in Ankara, i.e., rotating flat-sheet membrane unit, pilot type flat-sheet membrane unit located at METU Campus and samples from Ankara central wastewater treatment plant were analyzed for their EDCs contents under the optimum conditions.     

Sensitive determination of cadmium using solidified floating organic drop microextraction-slotted quartz tube-flame atomic absorption spectroscopy

In this study, solidified floating organic drop microextraction (SFODME) by 1-undecanol was combined with slotted quartz tube flame atomic absorption spectrometry (SQT-FAAS) for the determination of cadmium at trace levels. Formation of a complex with 4,4′-dimethyl-2,2′-bipyridine facilitated the extraction of cadmium from aqueous solutions. Several chemical variables were optimized in order to obtain high extraction outputs. Parameters such as concentration of the ligand, pH, and amount of buffer solution were optimized to enhance the formation of cadmium complex. The SFODME method was assisted by dispersion of extractor solvent into aqueous solutions using 2-propanol. Under the optimum extraction and instrumental conditions, the limit of detection and limit of quantitation values obtained for cadmium using the combined methods (SFODME-SQT-FAAS) were found to be 0.4 and 1.3 μg L^?1, respectively. Matrix effects on the method were also examined for tap water and wastewater, and spiked recovery results were found to be very satisfactory.

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Graphical Abstract SFODME-SQT-FAAS system for sensitive determination of cadmium