本文關(guān)鍵詞： 貴金屬納米光學(xué)探針 Cu2+ Mn2+ Cr3+ Cr2O72- 快速比色 區(qū)分檢測　出處：《安慶師范學(xué)院》2015年碩士論文　論文類型：學(xué)位論文

【摘要】：現(xiàn)代工業(yè)的快速發(fā)展和人類對資源的掠奪性開采導(dǎo)致重金屬引起的水體環(huán)境污染嚴重。因此,實現(xiàn)對污染水體中重金屬離子的快速靈敏檢測,具有重要意義。目前,國內(nèi)外檢測污染水體中重金屬離子的方法主要借助于精密分析儀器,然而這些方法存在檢測費用昂貴、樣品前處理復(fù)雜、檢測時間較長等缺陷。貴金屬納米顆粒膠體的濃度、粒徑大小及形貌變化都會引起其表面等離子體共振吸收發(fā)生變化,從而導(dǎo)致溶膠顏色發(fā)生改變。因此,通過裸眼比色或紫外可見吸收光譜分析可實現(xiàn)對水體中重金屬離子的檢測。已報道的基于貴金屬納米顆粒的光學(xué)探針通常只能實現(xiàn)對單一重金屬離子的檢測或?qū)Χ喾N重金屬離子同時檢測但無法逐一區(qū)分;而實際環(huán)境水體中可能同時被兩種或兩種以上的重金屬離子污染。為進一步拓展貴金屬納米光學(xué)探針的應(yīng)用,本論文設(shè)計并研發(fā)了重金屬雙離子響應(yīng)型貴金屬納米光學(xué)探針,通過對反應(yīng)條件的調(diào)控,可實現(xiàn)對兩種重金屬離子的區(qū)分檢測。具體研究內(nèi)容如下:1)Cu2+/Mn2+響應(yīng)型銀納米光學(xué)探針的研究:室溫下以硼氫化鈉還原制備出采用焦磷酸鈉(Na4P2O7)和羥丙基甲基纖維素(HPMC)功能化的銀納米顆粒(Ag NPs),其粒徑約為15 nm,在水溶液中的分散性良好。在酸性環(huán)境中,Ag NPs被Cu2+氧化刻蝕,導(dǎo)致溶膠顏色由亮黃色變?yōu)闊o色;在堿性環(huán)境中,P2O74-與Mn2+發(fā)生配位反應(yīng)誘導(dǎo)Ag NPs發(fā)生團聚,導(dǎo)致溶膠顏色由亮黃色變?yōu)楹稚Ｓ纱丝蓪崿F(xiàn)對Cu2+和Mn2+的裸眼比色檢測,檢測限(LOD)分別為0.05μmol/L和0.5μmol/L,由于銀納米顆粒表面等離子體共振吸收也相應(yīng)發(fā)生了變化,通過紫外可見分光光度計(UV-vis)可實現(xiàn)低濃度的定量檢測,最低檢測限分別為2.0 nmol/L和20nmol/L。此外,該銀納米光學(xué)探針對Cu2+和Mn2+具有優(yōu)異的選擇性,且已成功實現(xiàn)對實際環(huán)境水樣的區(qū)分檢測。2)Cr3+/Cr2O72-響應(yīng)型金納米光學(xué)探針的研究:以沒食子酸還原并包裹制得功能化的金納米顆粒(GA-Au NPs),其粒徑約為30 nm,在水溶液中的分散性良好。在掩蔽劑硫代硫酸鈉和檸檬酸鈉存在下,該GA-Au NPs可實現(xiàn)對Cr3+的快速檢測,無其他離子干擾;在掩蔽劑乙二胺四乙酸二鈉(EDTA)的存在下,該GA-Au NPs可實現(xiàn)對Cr2O72-的快速檢測,無其他離子干擾。通過對實驗條件的優(yōu)化,該金納米光學(xué)探針對Cr3+和Cr2O72-具有優(yōu)異的選擇性和靈敏度。研究發(fā)現(xiàn),鉻離子(Cr3+和Cr2O72-)與沒食子酸通過絡(luò)合作用誘導(dǎo)Au NPs團聚,導(dǎo)致Au NPs溶膠顏色及表面等離子體共振吸收發(fā)生變化,根據(jù)該反應(yīng)機理可實現(xiàn)對總鉻離子的裸眼比色檢測,檢測限為1.5μmol/L,通過紫外可見分光光度計可實現(xiàn)對總鉻離子低濃度的定量檢測,檢測限為0.05μmol/L。在掩蔽劑存在的條件下(硫代硫酸鈉和檸檬酸鈉掩蔽Cr2O72-實現(xiàn)對Cr3+的檢測;EDTA掩蔽Cr3+實現(xiàn)對Cr2O72-的檢測)可實現(xiàn)對Cr3+或Cr2O72-的檢測,裸眼比色檢測Cr3+和Cr2O72-的檢測限分別為1.5μmol/L和2μmol/L,UV-vis檢測限分別為0.1μmol/L和0.1μmol/L。此外,利用該金納米光學(xué)探針實現(xiàn)了對實際環(huán)境水樣中Cr3+和Cr2O72-的區(qū)分檢測。
[Abstract]:The rapid development of modern industry and human resources of the predatory exploitation caused serious environmental pollution caused by heavy metals in water. Therefore, to achieve rapid and sensitive detection of heavy metal ions in polluted water, which is of great significance. At present, at home and abroad to detect the pollution of heavy metals in water from the method mainly depends on the precision analysis instruments, however these methods exist detection of expensive, complex sample preparation, detection time and other defects. The concentration of noble metal nanoparticles, particle size and morphology change will cause the surface plasmon resonance absorption changes, resulting in sol color change. Therefore, the naked eye color or UV Vis absorption spectrum analysis can be realized detection of heavy metal ions in water. The realization of optical probe of noble metal nanoparticles usually only on a single heavy metal ion based on the reported Detection of heavy metal ions or multiple simultaneous detection but cannot distinguish one by one; but the actual environment in water may also be two or more than two kinds of heavy metals pollution. In order to further expand the application of noble metal nano optical probe, this thesis presents the design and development of the heavy metal ion response double noble metal nano optical probe, through the regulation of the reaction conditions, can distinguish between detection of two kinds of heavy metal ions. The specific contents are as follows: 1) of silver nano optical probe response Cu2+/Mn2+ at room temperature by reduction of sodium borohydride was prepared using sodium pyrophosphate (Na4P2O7) and hydroxypropyl methyl cellulose (HPMC) silver nanoparticles functionalized (Ag NPs), and its diameter is about 15 nm, in aqueous solution with good dispersion. In the acidic environment, Ag NPs by Cu2+ oxidation etching, resulting in color changed from light yellow to colorless; in alkaline environment, P2O74- The coordination reaction induced by Ag NPs and Mn2+ together, resulting in the color changed from light yellow to brown. It can be realized on the Cu2+ and Mn2+ of the naked eye colorimetric detection, detection limit (LOD) were 0.05 mol/L and 0.5 mol/L, the silver nanoparticles surface plasmon resonance absorption have been changed and through the ultraviolet visible spectrophotometer (UV-vis) can realize the quantitative detection of low concentration, the minimum detection limit of 2 nmol/L and 20nmol/L. respectively. In addition, the silver nano optical probe has excellent selectivity to Cu2+ and Mn2+, and has been successfully achieved to detect.2 on the actual environmental samples) of gold nano optical probe the response of Cr3+/Cr2O72- to gold nanoparticles prepared and gallic acid reduction package functionalized (GA-Au NPs), the particle size is about 30 nm, in aqueous solution with good dispersion. In the presence of masking agent of sodium thiosulfate and Sodium Citrate under The GA-Au, NPs can achieve rapid detection of Cr3+, no other ion interference; masking agent in two sodium ethylenediaminetetraacetic acid (EDTA) in the presence of the GA-Au NPs can achieve the rapid detection of Cr2O72-, no other ion interference. By optimizing the experimental conditions, the gold nano optical probe has excellent selectivity and the sensitivity of Cr3+ and Cr2O72-. The study found that chromium ions (Cr3+ and Cr2O72-) and gallic acid by complexation induced by Au NPs in Au NPs sol agglomeration, color and surface plasmon resonance absorption changes, according to the reaction mechanism of total chromium ion uncorrected colorimetric detection, the detection limit is 1.5 mol/L, the UV VIS spectrophotometer can realize quantitative detection of total chromium ions of low concentration, the detection limit is 0.05 mol/L. in the presence of masking agent (sodium thiosulfate and sodium citrate to mask Cr2O72- Cr3+ to achieve the examination Test; EDTA masking Cr3+ achieve the detection of the Cr2O72-) can realize the detection of Cr3+ or Cr2O72-, the naked eye were 1.5 mol/L and 2 mol/L than the detection limit of color detection of Cr3+ and Cr2O72-, the detection limit of UV-vis were 0.1 mol/L and 0.1 mol/L. in addition, the gold nano optical probe is realized the detection of Cr3+ and Cr2O72- between the actual environmental samples.

【學(xué)位授予單位】：安慶師范學(xué)院
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：O657.3;TB383.1

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