本文選題：磷酸鹽 + 熒光分析法　； 參考：《中國(guó)科學(xué)技術(shù)大學(xué)》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(shí)也是引起水體富營(yíng)養(yǎng)化的主要元素之一。為了能夠有效地控制富營(yíng)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(jiǎn)單、靈敏度高和選擇性好,近年來(lái)已成為環(huán)境檢測(cè)領(lǐng)域備受關(guān)注的分析方法。稀土配位聚合物具有獨(dú)特的熒光特性和結(jié)構(gòu)可調(diào)整性,且鑭系元素銪離子與磷酸鹽具有較強(qiáng)的結(jié)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(lái)檢測(cè)水體中的磷酸鹽。另外,對(duì)于實(shí)際水樣中的磷酸鹽含量分析,定點(diǎn)定時(shí)的采樣方法難以及時(shí)、全面、客觀地反映水質(zhì)安全狀況以及磷酸鹽的時(shí)空分布和化學(xué)狀態(tài),所以我們采用了薄膜梯度擴(kuò)散(DGT)技術(shù),并以碲化鎘量子點(diǎn)(CdTe QDs)與銪離子組成的熒光探針作為其結(jié)合相,探索了它們?cè)趯?shí)際水體中原位檢測(cè)磷酸鹽的可行性與準(zhǔn)確性。本文的研究成果如下:1、采用簡(jiǎn)單的溶劑熱法一步合成形貌均勻的Eu-ICP納米球,改變反應(yīng)條件可調(diào)控其結(jié)構(gòu)和形貌。該材料熒光性能優(yōu)異,在水環(huán)境介質(zhì)中結(jié)構(gòu)穩(wěn)定性好,其熒光強(qiáng)度在一定范圍內(nèi)基本不受溶液pH和離子強(qiáng)度等因素的影響,可作為一種有效的熒光探針來(lái)選擇性地測(cè)定水體中的磷酸鹽含量,線性檢測(cè)范圍是2～100μM,檢測(cè)限為0.83μM。為了評(píng)估該熒光探針?lè)治龅臏?zhǔn)確性,Eu-ICP納米球被用來(lái)檢測(cè)實(shí)際水樣中的磷酸鹽含量,得到了令人滿意的加標(biāo)回收率和較低的相對(duì)標(biāo)準(zhǔn)差。此外,我們分析了 Eu-ICP納米球檢測(cè)磷酸鹽的機(jī)理,并通過(guò)觀察Eu-ICP納米球與磷酸鹽相互作用前后結(jié)構(gòu)和形貌的變化進(jìn)行了驗(yàn)證�？偟膩�(lái)說(shuō),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(fù)雜水環(huán)境中的磷酸鹽含量分析。2、通過(guò)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(qiáng)度在一定范圍內(nèi)受溶液pH和離子強(qiáng)度等因素的影響較小,并對(duì)磷酸鹽具有優(yōu)異的選擇性響應(yīng),在10～200μM范圍內(nèi)呈現(xiàn)良好的線性關(guān)系,檢測(cè)限為1.58μM。我們以該探針溶液作為DGT裝置的結(jié)合相,將其放入已知濃度的磷酸鹽溶液中,通過(guò)測(cè)定不同時(shí)間段的熒光強(qiáng)度計(jì)算得到了 CdTe QDs/Eu~(3+)-DGT的擴(kuò)散系數(shù),并以此來(lái)檢測(cè)實(shí)際加標(biāo)水樣中的磷酸鹽濃度,測(cè)試結(jié)果與標(biāo)準(zhǔn)鉬藍(lán)比色法的檢測(cè)結(jié)果相近,證明了該分析方法的可行性與準(zhǔn)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(xué)位授予單位】：中國(guó)科學(xué)技術(shù)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：X832;O657.3

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