本文關(guān)鍵詞： 三維熒光光譜 農(nóng)藥廢水 在線監(jiān)測　出處：《合肥工業(yè)大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：工業(yè)排放廢水在線監(jiān)控對減少污染事故發(fā)生及保障環(huán)境水質(zhì)安全具有重要的現(xiàn)實意義。傳統(tǒng)檢測方法以色譜、質(zhì)譜及色譜-質(zhì)譜聯(lián)用等現(xiàn)場采樣-實驗室分析為主,光譜法具有無需樣品預(yù)處理、選擇性好、靈敏度高等特點,可實現(xiàn)水質(zhì)的在線、自動與實時檢測。因此,針對農(nóng)藥企業(yè)排放廢水在線監(jiān)測/監(jiān)控需求,以多菌靈、麥穗寧和西維因三種農(nóng)藥為研究對象,重點研究了三種農(nóng)藥的三維熒光光譜發(fā)射特性,以及三維熒光光譜技術(shù)用于廢水農(nóng)藥的快速定量分析能力。取得主要研究結(jié)果如下:(1)不同環(huán)境條件雜環(huán)農(nóng)藥三維熒光光譜發(fā)射特性研究。研究了三種農(nóng)藥在不同pH值和常見陰、陽離子條件下的三維熒光光譜發(fā)射特性,初步分析了Fe3+和Cu2+對三種農(nóng)藥的熒光猝滅機制。結(jié)果表明,多菌靈和麥穗寧均具有兩個熒光峰,西維因僅有一個熒光區(qū)域,三種農(nóng)藥的主要熒光峰分別位于λex/λem=280/300nm、310/340nm、280/335nm;多菌靈與麥穗寧隨pH值變化表現(xiàn)為相似的熒光發(fā)射特征,在酸性/堿性降低時,熒光強度增大;酸性條件下西維因的熒光發(fā)射強度無明顯變化,但在堿性條件下,隨pH值的減小熒光強度不斷增強;三種農(nóng)藥在pH值6.16-7.4范圍內(nèi)均可獲得較好的熒光發(fā)射特征。Fe3+和Cu2+的存在對三種農(nóng)藥的熒光發(fā)射強度均有較大影響,隨著離子濃度的增加熒光強度不斷降低,因此在實際測量中,需重點考慮Fe3+和Cu2+對測量結(jié)果的影響。(2)農(nóng)藥企業(yè)排放廢水在線監(jiān)測方法實驗研究。研究了基于三維熒光光譜技術(shù)的農(nóng)藥企業(yè)排放廢水在線監(jiān)測方法,實驗測量了三種農(nóng)藥的熒光發(fā)射強度隨濃度變化關(guān)系,計算分析了不同農(nóng)藥的檢測限,并對比研究了不同水體中高、低濃度農(nóng)藥的回收率與準(zhǔn)確性。結(jié)果表明:三種農(nóng)藥熒光發(fā)射強度隨濃度的增加均呈指數(shù)增長,濃度范圍覆蓋了現(xiàn)有已知農(nóng)藥工業(yè)排放限值;多菌靈、麥穗寧和西維因的檢測限分別為0.6μg.L-1、0.01μg.L-1和0.06μg.L-1,可滿足地表水與地下水痕量農(nóng)藥的檢測需求;不同濃度農(nóng)藥在礦泉水與水庫水體中的平均回收率均大于96%,平均相對誤差小于7%。研究結(jié)果為農(nóng)藥企業(yè)排放廢水的在線監(jiān)測/監(jiān)控以及周邊地表水/飲用水安全保障提供了方法。(3)高濃度下農(nóng)藥廢水三維熒光光譜特征及在線檢測分析方法研究。研究了高濃度條件下三種農(nóng)藥的熒光光譜特征以及不同積分寬度下的在線檢測定量分析方法。結(jié)果表明,多菌靈、麥穗寧的熒光特征區(qū)域隨濃度的增大發(fā)生紅移,致使定量分析誤差增大;基于不同發(fā)射波長范圍(10nm、5nm)和固定發(fā)射波長點做熒光特征做積分校正曲線,多菌靈和西維因熒光強度隨濃度呈指數(shù)增長,且相關(guān)系數(shù)分別為0.9999和0.9997,麥穗寧呈先增大后減小趨勢,相關(guān)系數(shù)分別為0.9995和0.9932。研究結(jié)果為高濃度下農(nóng)藥廢水的在線檢測定量分析提供了依據(jù),為進一步發(fā)展農(nóng)藥企業(yè)排放廢水快速在線監(jiān)測儀器奠定了基礎(chǔ)。
[Abstract]:On-line monitoring of industrial wastewater discharge has important practical significance in reducing pollution accidents and ensuring environmental water quality safety. The traditional detection method is chromatography. Mass spectrometry and chromatography-mass spectrometry are mainly used in the field sampling-laboratory analysis. The spectral method has the advantages of no sample pretreatment, good selectivity and high sensitivity, so it can realize on-line, automatic and real-time detection of water quality. In order to meet the demand of on-line monitoring and monitoring of wastewater discharged from pesticide enterprises, three pesticides, carbendazim, wheisuanning and carbaryl, were selected as the research objects, and the emission characteristics of three kinds of pesticides were mainly studied. And the rapid quantitative analysis of pesticide in wastewater by three dimensional fluorescence spectrometry. The main results are as follows: 1). Three dimensional fluorescence emission characteristics of heterocyclic pesticides under different environmental conditions were studied. The fluorescence quenching mechanism of three pesticides by Fe3 and Cu2 was preliminarily analyzed. The results showed that both carbendazim and maisuanning had two fluorescence peaks. Carbaryl has only one fluorescence region, and the main fluorescence peaks of the three pesticides are located at 位 ex / 位 emn 280 / 300 nm ~ (-1) 310 / 340 nm ~ (-1) ~ 280 / 335nm ~ (-1), respectively. Carbendazim and wheat panicle showed similar fluorescence emission characteristics with the change of pH value, and the fluorescence intensity increased with the decrease of acid / alkalinity. The fluorescence emission intensity of carbaryl did not change obviously under acidic condition, but the fluorescence intensity increased with the decrease of pH value in alkaline condition. The fluorescence emission characteristics of the three pesticides were obtained in the pH range of 6.16-7.4. The existence of Fe _ 3 and Cu2 had a great influence on the fluorescence emission intensity of the three pesticides. The fluorescence intensity decreases with the increase of ion concentration, so it is measured in practice. The influence of Fe3 and Cu2 on the measurement results should be considered. Experimental study on on-line monitoring method of wastewater discharge from pesticide enterprises. The method of on-line monitoring of wastewater discharge from pesticide enterprises based on three-dimensional fluorescence spectroscopy was studied. The relationship between fluorescence emission intensity and concentration of three pesticides was measured and the detection limits of different pesticides were calculated and analyzed. The recovery and accuracy of low concentration pesticides. The results showed that the fluorescence emission intensity of three pesticides increased exponentially with the increase of concentration, and the concentration range covered the known industrial emission limits of pesticides. The detection limits of carbendazim, wheisuanning and carbaryl were 0.6 渭 g 路L ~ (-1) and 0.06 渭 g 路L ~ (-1), respectively. The average recoveries of different concentrations of pesticides in mineral water and reservoir water were all greater than 96%. The average relative error is less than 7. The results provide a method for the on-line monitoring / monitoring of wastewater discharge from pesticide enterprises and the safety guarantee of peripheral surface water / drinking water. The characteristics of three dimensional fluorescence spectrum and on-line detection and analysis method of pesticide wastewater under high concentration were studied. The fluorescence spectrum characteristics of three pesticides under high concentration and the quantitative analysis method of on-line detection under different integral widths were studied. The fruit shows. The fluorescence characteristic region of carbendazim and wheat panning shifted red with the increase of concentration, which resulted in the increase of quantitative analysis error. The fluorescence intensity of carbendazim and carbaryl increased exponentially with the concentration of carbendazim and carbaryl. The correlation coefficients were 0.9999 and 0.9997, respectively. The correlation coefficients were 0.9995 and 0.9932, respectively. The results provided the basis for on-line detection and quantitative analysis of pesticide wastewater with high concentration. It lays a foundation for the further development of a fast on-line monitoring instrument for wastewater discharge from pesticide enterprises.
【學(xué)位授予單位】：合肥工業(yè)大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：X839.2

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