Application of Dispersive Liquid–Liquid Microextraction Based on Solidification of Floating Organic Droplet Multi‐residue Method for the Simultaneous Determination of Polychlorinated Biphenyls,Organochlorine, and Pyrethroid Pesticides in Aqueous Sample

Dispersive liquid–liquid microextraction based on solidification of floating organic droplet (DLLME‐SFO) technique was successfully applied for simultaneous assay of eight polychlorinated biphenyls, two organochlorine, and four pyrethroid pesticides multi‐residue in aqueous samples by using GC‐electron capture detection. The effects of various parameters such as kind of extractant and dispersant and volume of them, extraction time, effect of salt addition, and pH were optimized. As a result, 5.0 µL 1‐dodecanol was chosen as extraction solvent, 600 µL methanol were used as dispersive solvent without salt addition, pH was adjusted to 7. Under the optimized conditions, the limits of detection (LOD) were ranged from 1.4 to 8.3 ng L^?1. Satisfactory linear range was observed from 5.0 to 2000 ng L^?1 with correlation coefficient better than 0.9909. Good precisions were also acquired with RSD better than 13.6% for all target analytes. The enrichment factors of the method were ranged from 786 to 1427. The method can be successfully applied to simultaneous separation and determination of three class residues in real water samples and good recoveries were obtained ranging from 76 to 130, 73 to 129, and 78 to 130% for tap water, lake water, and industrial waste water, respectively.     

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.     

Determination of Trace Levels of Nickel and Manganese in Soil,Vegetable, and Water

A simple and reliable method for rapid and selective extraction and determination of trace levels of Ni²⁺ and Mn²⁺ was developed by ionic liquid (IL) based dispersive liquid–liquid microextraction coupled to flame atomic absorption spectrometry (FAAS) detection. The proposed method was successfully applied to the preconcentration and determination of nickel and manganese in soil, vegetable, and water samples. After preconcentration, the settled IL‐phase was dissolved in 100 µL of ethanol and aspirated into the FAAS using a home‐made microsample introduction system. Injection of 50 µL of each analyte into an air–acetylene flame provided very sensitive spike‐like and reproducible signals. Effective parameters such as pH, amount of IL, volume of the disperser solvent, concentration of the chelating agent, and effect of salt concentration were inspected by a (2^5‐1) fractional factorial design to identify the most important parameters and their interactions. Under optimum conditions, preconcentration of 10 mL sample solution permitted the detection of 0.93 µg L^?1 Ni²⁺ and 0.52 µg L^?1 Mn²⁺ with enrichment factors 77.2 and 82.6 for Ni²⁺ and Mn²⁺, respectively. The accuracy of the procedure was evaluated by analysis of a certified reference material (CRM TMDW‐500, drinking water).     

Ultrasound‐Assisted Emulsification–Microextraction Combined with Graphite Furnace Atomic Absorption Spectrometry for the Determination of Trace Lead in Water

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.     

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.     

The impact of the South–North Water Transfer Project (CTP)'s central route on groundwater table in the Hai River basin,North China

The central route of the South–North Water Transfer Project (CTP) is designed to divert approximately 9.5 billion m³ of water per year from the Han River, a major tributary of the Yangtze River, to the Hai River basin in the north China. The main purpose of this study is to assess the impact of CTP on groundwater table in the Hai River basin. Our study features a large‐scale distributed hydrological model that couples a physically based groundwater module, which is sub‐basin‐based, with a conceptual surface water module, which is grid‐based. There are several grids in each sub‐basin and water exchange among grid that are considered. Our model couples surface water module and groundwater module and calculates human water use at the same time. The simulation results indicate that even with the water supply by CTP, the groundwater table will continue to decline in the Hai River basin. However, the CTP water can evidently reduce the decline rate, helping alleviate groundwater overexploitation in Hai River region. Copyright © 2013 John Wiley & Sons, Ltd.