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|標題:||Green Analytical Methodologies for the Rapid Analysis of Organochlorine Compounds in Aqueous Samples using Microwave Assisted Graphene and Polymeric Hollow Fiber based Micro-Extraction Techniques Coupled with Gas Chromatography|
Ponnusamy, Vinoth Kumar
Green analytical methodology
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|摘要:||In recent years, the scientific community has grabbed much interest in the development of environmentally friendly activities. Green analytical chemistry (GAC) mainly pursues the objectives of replacing toxic reagents, and miniaturizing and rapid analytical methodologies, so as to minimize environmental and human hazards by replacing polluting methods with clean ones.
This dissertation strikes at the heart of one of the major challenges associated with green sample preparation, developments on miniaturized or environmental-friendly micro-extraction techniques based analytical methodologies. The work described involves the development of novel sorbent coating material for solid-phase microextraction, and exploration of hollow fiber based liquid-phase microextraction system coupled with clean energy for the rapid analysis of interesting analytes of environmental concern.
In Chapter 2, a simple, rapid and sensitive analytical method for determining dichlorodiphenyltrichloroethane (DDT) and its main metabolites in aqueous samples has been developed using one-step microwave-assisted controlled-temperature headspace liquid-phase micro-extraction (MA-CT-HS-LPME) technique coupled with gas chromatography-electron capture detection (GC-ECD). Parameters influencing the extraction efficiency were thoroughly optimized and the best extraction was achieved using 10 mL aqueous sample at pH 6 and 4 µL of 1-octanol as the LPME solvent, sampling at 34℃ for 6.5 min under 249 W of microwave irradiation. Under optimum conditions, detection limits were between 20 and 30 ngL¯¹ for four interested analytes (DDT and its main metabolites), and precision was in the range of 3.2-11.3% RSD. The proposed method was validated with real water samples, and the results indicated that the spiked recovery was between 95.5 and 101.3% for agricultural field water, and between 93.5% and 98% for river water.
In Chapter 3, few-layer, less thickness graphene nanosheets (GNSs) were synthesized using a rapid and novel microwave assisted synthetic method for the application as a novel coating material for SPME fiber. Microwave synthesized GNSs were verified by powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission-scanning electron microscopy (FE-SEM) and high-resolution transmission electron microscope (HR-TEM).
In Chapter 4, GNSs coated solid phase microextraction (SPME) fiber was prepared by immobilizing microwave synthesized GNSs on a stainless steel wire. GNS-SPME fiber was characterized using FE-SEM and the results showed that the GNSs coating was homogeneous, porous, and possessed large specific area. The performance and feasibility of the GNSs coated SPME fiber was evaluated under one-step microwave assisted (MA) controlled-temperature (CT) headspace (HS) SPME followed by gas chromatography (GC) with electron capture detection (ECD) for five organochlorine pesticides (OCPs) as model compounds in aqueous samples. Under the optimized conditions, detection limits for the OCPs varied between 0.16 and 0.92 ngL¯¹ and linear ranges varied between 1 and 1500 ngL¯¹, with correlation coefficients ranging from 0.9985 to 0.9998, and RSDs in the range of 3.6 – 15.8% (n = 5). The method was successfully applied to the analyses of real water samples with recoveries from 80.5 to 105.1% for river water and from 85.7 to 106.5% for lake water. In comparison with the commercial polydimethylsiloxane fiber, the GNS coated fiber showed better extraction efficiency, higher mechanical and thermal stability, and lower production cost.
Above results demonstrated that the proposed methods were simple, rapid, efficient pretreatment and environmentally-friendly procedures and thus the developed methods were proved to serve as novel and green analytical methodological approaches for the rapid determination of OCCs in aqueous sample.|
近年來由於環保意識高漲，因此開發具環保概念之綠色方法廣受到科學家之重視。綠色分析化學(GAC) 主要的目的為減少或取代有毒溶劑與試劑之使用，並開發微小化與快術的分析方法，以減少對人體與環境之危害。基於上述之理由，本研究之主要目的於發展符合綠色前處理觀念之微小化且環保微萃取技術應用於分析方法中，其中包含以新興吸附化合物塗覆之固相微萃取法與液相微萃取技術結合綠色能源於環境中微量物質萃取之應用。 首先開發一簡單、快速且靈敏之微波輔助控溫頂空液相微萃取結合氣相層析法-電子捕捉偵測器之分析方法，於環境水樣中滴滴梯(DDT)與其代謝物之偵測。研究結果顯示取pH調整為6.0水樣品10毫升，以4 μL正辛醇為萃取溶劑，於微波功率249瓦、34°C下萃取6.5分鐘，為最佳萃取條件。所開發方法在最佳條件下分析水樣中滴滴梯類化合物之偵測極限介於20 ~ 30 ngL-1之間，精密度介於3.2 ~ 11.3%之間。分析農田中水樣品與河水樣品可得到回收率分別介於95.5 ~ 101.3% 與 93.5 ~ 98% 之間。 另一研究主要是利用快速且新穎之微波輔助合成技術，應用於合成具有多層且厚度為奈米級的石墨烯(GNSs)材質，並利用X光粉末繞射儀(XRD)、X射線光電子能譜(XPS)、場發射電子顯微鏡(FE-SEM)與高解析度穿透式電子顯微鏡(HR-TEM)等儀器，檢測所合成材質之性質。以合成之石墨烯材料做為吸附材質，塗覆於固相微萃取法之不銹鋼金屬絲上，成為一石墨烯塗覆之固相微萃取纖維。經場發射電子顯微鏡檢測後證明所自製之固相微萃取塗覆纖維，為均勻塗覆且具有多孔性與高吸附面積之特性。本研究並將自製石墨烯塗覆之固相微萃取纖維，以微波輔助控溫頂空固相微萃取法結合氣相層析法電子捕捉偵測器之方法，分析水樣中五種有機氯農藥，並針對所開發方法進行方法確效之探討。在最佳條件下，分析水中有機氯農藥之偵測極限介於0.16 ~ 0.92 ngL-1之間，分析線性範圍為1 ~ 1500 ngL-1，線性相關係數介於0.9985 ~ 0.9998之間，方法精密度則介於 3.6 ~ 15.8% 之間 (n=5)。所開發方法於萃取河水與湖水中有機氯農藥之回收率則介於80.5 ~ 105.1% 與85.7 ~ 106.5%之間。實驗證明以塗覆石墨烯之固相微萃取技術，與市售塗覆聚二甲基矽氧烷(PDMS)之固相微萃取技術進行比較，結果可得知，以石墨烯為塗覆材質之固相微萃取法具有較佳之萃取效率、耐用性、熱穩定性與低成本等優點。 由上述研究結果可得知，所開發之微波輔助控溫頂空液相微萃取法與石墨烯塗覆固相微萃取技術，為簡單、快速、具高萃取效率與環保之樣品前處理技術。本研究並證明所開發之新興綠色分析方法，可提快速分析水樣中微量有機氯化合物之參考。
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