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Study On The Sample Pre-treatment And High-performance Liquid Chromatography Analysis Of PAHs

Posted on:2017-04-22Degree:MasterType:Thesis
Country:ChinaCandidate:Y Y ZongFull Text:PDF
GTID:2271330503974276Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
Polycyclic aromatic hydrocarbons(PAHs) are organic compounds with two or more benzene rings. They exists widely in the environment and can induce skin cancer, scrotum cancer, lung cancer and other diseases. The presence of PAHs can cause great harm to human health. There are many reports about the PAHs, and the analytical method included high performance liquid chromatography with fluorescence detector, high performance liquid chromatography with mass spectrometry detector, gas chromatography with mass spectrometry detector and so on.When analyzing of PAHs in environment samples, the most common problem is the low level of PAHs in samples. It is essential to establish a pretreatment method to pre-concentrate the PAHs before analysis. Pretreatment technology in literature is numerous, including solid phase extraction, microwave assisted extraction, ultrasonic assisted extraction, cloud point extraction. But there are many disadvantages in traditional pretreatment methods, such as complicated steps and large consumption of organic solvents. Several new pretreatment methods are established in our study, which all are rapid, simple and effective.Chapter Ⅰ, established quntum dots(QDs) extraction-high performance liquid chromatography method for detectiong the PAHs in water samples. The QDs were synthesised in our own labtarory. Optimize the species of QDs, extraction time, elution solvents and elution time. Under the optimal conditions, twelve PAHs completed separated in 30 min. The LODs were in the range of 1.00-100.00 ng/L, and the RSD of peak area were in the range of 1.45%-3.40%, the recoveries were in the range of 72.64%-95.93%.Chapter Ⅱ, Au protected by MMTA coupled Fe3O4@Si O2 nanoparticals were sysnthesised by chemical coupling method. And the material was characterized by transmission electron microscope(TEM), fourier transform infrared spectroscopy(FT-IR), X-ray diffraction(XRD) and X-ray photoelectron spectroscopy(XPS). And it was used as a novel solid–phase extraction adsorbent to extract 14 PAHs in water samples in environment. The extracted water samples were detected by HPLC-FLD. Under the optimal conditions, 14 PAHs were completed separated in 15 min, the LODs were in the range of 0.25-37.50 ng/L, and the RSD of peak area were in the range of 1.56%-3.47%, the recoveries were in the range of 80.00%-120.00%. But the regeneration of adsorbent sysnthesised by ourselves was poor.Chapter Ⅲ, to improve the poor regeneration of the adsorbent, Au nanoparticals protected by citric acid bonding of Fe3O4@Si O2 were sysnthesised by physical mixture. And the material was characterized by transmission electron microscope(TEM), fourier transform infrared spectroscopy(FT-IR), X-ray diffraction(XRD) and X-ray photoelectron spectroscopy(XPS). And it was used as a novel solid-phase extraction adsorbent to extract 14 PAHs in water samples in environment. The extracted water samples were detected by HPLC-FLD. Under the optimal conditions, 14 PAHs completed separated in 15 min, the LODs were in the range of 0.50-75.00 ng/L, and the RSD of peak area were in the range of 1.09%-2.54%, the recoveries were in the range of 70.00%-113.33%.
Keywords/Search Tags:Polycyclic aromatic hydrocarbons, Quntum Dots extraction, Magnetic solid-phase extraction, High performance liquid chromatography
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