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Application Of Magnetic Microspheres Modified With Imidazole Ionic Liquid In Environmental Water Samples Analysis

Posted on:2021-01-22Degree:MasterType:Thesis
Country:ChinaCandidate:J H XuFull Text:PDF
GTID:2381330614469701Subject:Analytical Chemistry
Abstract/Summary:
Nowadays,in the process of society development,the water pollution is one of the important problems that need to be solved urgently.The establishment of efficient and environmentally friendly sewage treatment and pollutant detection methods is a significant guarantee for human sustainable survival and development.In this work,Fe3O4 modified with a chlorinated polystyrene layer were synthesized by mini-emulsion polymerization.Then,six imidazole ionic liquids grafted onto the surface of the magnetic core by imidazole and chlorine atom chemical bonding method and anion exchange method.Then these magnetic microspheres modified with imidazole ionic liquid were applied to the separation and analysis of various pollutants in environmental water samples.Firstly,six imidazole ionic liquid-modified magnetic polystyrene microspheres were used as solid emulsifiers and(+)-Limonene as the organic phase to construct a magnetic Pickering emulsion with water.Through the optical microscope observation,these magnetic Pickering emulsion were divided into oil in water type(O/W)constructed by hydrophilic Fe3O4@PS[im-C1]Cl,Fe3O4@PS[im-C1]PF6,Fe3O4@PS[im-C4]Cl and water in oil type(W/O)constructed by hydrophobic Fe3O4@PS[im-C4]PF6,Fe3O4@PS[im-C8]Cl and Fe3O4@PS[im-C8]PF6.In addition,single factor method was used to investigate the stability of Pickering emulsion.The result showed that the amount of solid emulsifiers had the greatest influence on the stability of emulsion.As for aqueous p H=5~13,it was conducive to emulsion construction.When p H=1,the height of the emulsion layer was reduced significantly.The volume ratio of oil and water would affect the height of the emulsion layer but the effect was not obvious and the ionic strength of water had no effect on the stability.Furthermore,three O/W type Pickering emulsions mentioned above were selected for purification treatment of simulated wastewater which containing three polycyclic aromatic hydrocarbons or four phenols pollutants.The influence factors on extraction like type and dosage of solid emulsifiers and type of organic phase were investigated.Finally,5 m L Fe3O4@PS[im-C1]PF6(1.5wt%)was selected as solid emulsifiers,the extraction efficiency of the magnetic Pickering emulsion constructed by(+)-Limonene for three PAHs and four phenols was 96.7%~98.8%and50.0%~85.3%.Another magnetic Pickering emulsion constructed by butyl acetate,which extraction efficiency for three PAHs was 93.9%~95.8%and four phenolic compounds was 90.3%~91.7%.Relatively,the magnetic Pickering emulsion constructed by(+)-limonene was selective in extraction of different pollutants.Compared with other two purification methods,the Pickering emulsion liquid membrane method was not only simple and efficient,but also easy to control and separate.The emulsion was resistant to acids,alkalis and salt.The solid emulsifier could be reused.Secondly,a magnetic solid-phase extraction with the ionic liquid-modified magnetic nanomaterials as adsorbents and hydrophobic natural eutectic solvent(NADES)as elution solvents has been developed for the determination of six phenolic compounds in environmental water sample combined with gas chromatography coupled to tandem mass spectrometry.Compared to conventional solvent,the NADES were not only more environmentally friendly but also had the effect of enhancing the signal and improving the trailing peak of six phenolic target compounds in GC-MS.Through comparative experiments,it was found that the enhancement effect of NADES on chlorophenols was more significant than on alkyl phenols.While the composition of NADES was different,its enhancement effect on target phenols was also different.The greater polarity of hydrogen bond donors in NADES,the stronger the enhancement effect.The adsorbent type,the dosage of adsorbent,the time of ultrasonic-assisted extraction,the p H of the water sample,the ionic strength of the water sample,and the maximum loading volume conditions were optimized by a single factor method.The optimal conditions were follows:25 mg Fe3O4@PS[im-C1]Cl as the adsorbent dispersed into 25 m L water(p H=8,without adjusting ionic strength)with ultrasonic extraction for 180 s.Under the optimal conditions,three actual water samples in Hangzhou area were analyzed by the proposed method.Good linearity were obtained in the concentration rang of 1~500μg/L,with the correlation coefficients ranged from 0.9993~0.9999.The LODs(S/N=3)and LOQs(S/N=10)for six phenolic compounds were 0.02~1.5μg/L and 0.05~5μg/L,respectively.The recoveries of three spiked levels were 72.8%~108.3%.The proposed method was proved to be fast,simple,environmentally friendly and the absorbents could be recycled three times.
Keywords/Search Tags:Imidazole ionic liquid, Magnetic material, Pickering emulsion, Hydrophobic natural eutectic solvent, Magnetic solid-phase extraction
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