本文選題：磷酸鹽 + 熒光分析法��； 參考：《中國科學技術大學》2017年碩士論文

【摘要】：磷是自然界中一種極其重要的元素,但同時也是引起水體富營養(yǎng)化的主要元素之一。為了能夠有效地控制富營養(yǎng)化,我們必須清楚水體中磷酸鹽的含量。熒光分析法由于操作簡單、靈敏度高和選擇性好,近年來已成為環(huán)境檢測領域備受關注的分析方法。稀土配位聚合物具有獨特的熒光特性和結構可調整性,且鑭系元素銪離子與磷酸鹽具有較強的結合力,因此我們選擇形貌可控的鉑基配位聚合物(Eu-ICP)作為熒光探針來檢測水體中的磷酸鹽。另外,對于實際水樣中的磷酸鹽含量分析,定點定時的采樣方法難以及時、全面、客觀地反映水質安全狀況以及磷酸鹽的時空分布和化學狀態(tài),所以我們采用了薄膜梯度擴散(DGT)技術,并以碲化鎘量子點(CdTe QDs)與銪離子組成的熒光探針作為其結合相,探索了它們在實際水體中原位檢測磷酸鹽的可行性與準確性。本文的研究成果如下:1、采用簡單的溶劑熱法一步合成形貌均勻的Eu-ICP納米球,改變反應條件可調控其結構和形貌。該材料熒光性能優(yōu)異,在水環(huán)境介質中結構穩(wěn)定性好,其熒光強度在一定范圍內基本不受溶液pH和離子強度等因素的影響,可作為一種有效的熒光探針來選擇性地測定水體中的磷酸鹽含量,線性檢測范圍是2～100μM,檢測限為0.83μM。為了評估該熒光探針分析的準確性,Eu-ICP納米球被用來檢測實際水樣中的磷酸鹽含量,得到了令人滿意的加標回收率和較低的相對標準差。此外,我們分析了 Eu-ICP納米球檢測磷酸鹽的機理,并通過觀察Eu-ICP納米球與磷酸鹽相互作用前后結構和形貌的變化進行了驗證�？偟膩碚f,Eu-ICP納米球易于合成,水溶性和穩(wěn)定性良好,具有優(yōu)異的選擇性和靈敏度,可用于復雜水環(huán)境中的磷酸鹽含量分析。2、通過油浴回流法合成了巰基乙酸包覆的CdTe QDs,其與鑭系元素Eu~(3+)可組成熒光探針(CdTeQDs/Eu~(3+)),熒光強度在一定范圍內受溶液pH和離子強度等因素的影響較小,并對磷酸鹽具有優(yōu)異的選擇性響應,在10～200μM范圍內呈現(xiàn)良好的線性關系,檢測限為1.58μM。我們以該探針溶液作為DGT裝置的結合相,將其放入已知濃度的磷酸鹽溶液中,通過測定不同時間段的熒光強度計算得到了 CdTe QDs/Eu~(3+)-DGT的擴散系數(shù),并以此來檢測實際加標水樣中的磷酸鹽濃度,測試結果與標準鉬藍比色法的檢測結果相近,證明了該分析方法的可行性與準確性。
[Abstract]:Phosphorus is an extremely important element in nature, but it is also one of the main elements that cause eutrophication of water body. In order to effectively control eutrophication, we must know the amount of phosphate in water. Due to its simple operation, high sensitivity and good selectivity, fluorescence analysis has been paid more and more attention in the field of environmental detection in recent years. Rare earth coordination polymers have unique fluorescence properties and adjustable structure, and the lanthanide europium ions have strong binding force with phosphate. Therefore, we selected Pt-based coordination polymer Eu-ICP as fluorescence probe to detect phosphate in water. In addition, for the analysis of phosphate content in real water samples, the fixed point timing sampling method is difficult to reflect the safety of water quality and the temporal and spatial distribution and chemical state of phosphate in a timely, comprehensive and objective manner. So we have used the thin film gradient diffusion technique and the fluorescence probe composed of cadmium telluride quantum dot CdTe QDsand europium ion as its binding phase to explore the feasibility and accuracy of in situ detection of phosphate in real water. The results are as follows: 1. The uniform Eu-ICP nanospheres are synthesized by a simple solvothermal method. The structure and morphology of Eu-ICP nanospheres can be controlled by changing the reaction conditions. The material has excellent fluorescence properties and good structural stability in water environment. The fluorescence intensity of the material is not affected by pH and ionic strength of the solution in a certain range. It can be used as an effective fluorescence probe for the selective determination of phosphate content in water. The linear detection range is 200 渭 m and the detection limit is 0.83 渭 M. In order to evaluate the accuracy of the fluorescence probe analysis, Eu-ICP nanospheres were used for the determination of phosphate in real water samples. The satisfactory recoveries and lower relative standard deviations were obtained. In addition, we analyzed the mechanism of phosphate detection by Eu-ICP nanospheres, and verified by observing the structure and morphology of Eu-ICP nanospheres before and after the interaction between Eu-ICP nanospheres and phosphate. Generally speaking, Eu-ICP nanospheres are easy to synthesize, have good water solubility and stability, excellent selectivity and sensitivity. The CdTe QDscoated with thioglycolic acid and lanthanide Euclide 3) were synthesized by oil bath reflux method, which can be used to form a fluorescence probe, CdTeQDs- EEU ~ (3 +). The fluorescence intensity of CdTe QDs / EU ~ (3 +) is determined by solution pH and dissociation in a certain range. The influence of factors such as sub-strength is relatively small, And it has excellent selective response to phosphate, and the linear relationship is good in the range of 10 渭 m to 200 渭 M. the detection limit is 1.58 渭 M. The probe solution was used as the binding phase of the DGT unit, and was put into the phosphate solution with known concentration. The diffusion coefficient of CdTe QDsr / Euf3 / DGT was calculated by measuring the fluorescence intensity at different time periods. The results are close to those of standard molybdenum blue colorimetry, which proves the feasibility and accuracy of the method.
【學位授予單位】：中國科學技術大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：X832;O657.3

【參考文獻】

相關期刊論文 前5條

1 張瑩琪;馮文珊;陳林;;孔雀綠-磷鉬雜多酸分光光度法測定水樣中磷的含量[J];工業(yè)水處理;2011年12期

2 梁運江;謝修鴻;許廣波;趙長新;張立秋;;磷鉬藍比色法合適工作波長及線性范圍的探討[J];中國環(huán)境監(jiān)測;2007年01期

3 王慶霞;蘇苓;;孔雀綠體系流動注射光度法測定水中正磷酸鹽[J];環(huán)境監(jiān)測管理與技術;2006年06期

4 李山;劉丹;;磷鉬藍分光光度法測定水中磷的改進[J];化工環(huán)保;2006年01期

5 吳群娣,蔣治良;磷釩鉬雜多酸光化學分析法測定磷[J];分析科學學報;1999年06期

，

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