【摘要】：近年來(lái),貴金屬納米粒子因其獨(dú)特的光學(xué)和電學(xué)性質(zhì),在催化、藥物輸送、成像、醫(yī)學(xué)診斷和治療、生物傳感、環(huán)境分析等研究領(lǐng)域引起廣泛關(guān)注。本論文基于貴金屬納米粒子的表面催化活性,建立了一種以貴金屬納米粒子作為分析探針定量檢測(cè)水中硫離子濃度的新方法。該方法靈敏度高、選擇性好,且實(shí)現(xiàn)了硫離子的快速檢測(cè)。實(shí)驗(yàn)中,我們首先利用多元醇熱法制備了粒徑均一(15 nm)、在水溶液中穩(wěn)定分散的球形銀納米粒子。研究發(fā)現(xiàn),該銀納米對(duì)硼氫化鈉還原對(duì)硝基苯酚這一反應(yīng)具有較強(qiáng)的催化作用;當(dāng)在體系中加入不同濃度的硫氫化鈉溶液,使得銀納米粒子表面被部分或全部硫化(即催化劑中毒),從而抑制銀納米粒子對(duì)該反應(yīng)的催化活性,降低反應(yīng)速率。通過(guò)反應(yīng)速率常數(shù)與硫氫化鈉濃度之間的定量關(guān)系建立了水中硫離子的檢測(cè)新方法。該方法的檢測(cè)范圍為0.5 7.5μmol/L,且成功應(yīng)用于實(shí)際樣品的檢測(cè)。其次,基于貴金屬鈀超高的催化活性,我們合成了不同形貌(立方體、八面體)的鈀納米粒子作為分析探針,催化過(guò)氧化氫氧化3,3,5,5-四甲基聯(lián)苯胺(TMB)這個(gè)典型的催化氧化顯色反應(yīng),建立了一種檢測(cè)硫離子的高靈敏比色分析方法。實(shí)驗(yàn)中,我們首先使用邊長(zhǎng)為18 nm的鈀納米立方體作為探針,在室溫條件下催化該反應(yīng)。當(dāng)在體系中加入不同濃度的硫氫化鈉,使得鈀納米立方體表面被部分或全部硫化(即催化劑中毒),從而抑制鈀納米立方體對(duì)該反應(yīng)的催化活性,降低反應(yīng)速率。通過(guò)TMB在650 nm處的吸光度值與硫離子濃度之間的定量關(guān)系,建立了檢測(cè)硫離子的新方法。此外,我們還對(duì)比考察了具有不同表面晶面的八面體鈀納米粒子對(duì)該反應(yīng)的催化作用以及對(duì)分析方法靈敏度的影響。總之,本論文將貴金屬納米粒子的表面催化中毒效應(yīng)與分析化學(xué)有機(jī)結(jié)合起來(lái),并建立了檢測(cè)水環(huán)境中硫離子濃度的新方法。該方法具有操作簡(jiǎn)便、響應(yīng)快速、靈敏度高、選擇性高等優(yōu)點(diǎn)。
[Abstract]:In recent years, noble metal nanoparticles have attracted much attention in the fields of catalysis, drug delivery, imaging, medical diagnosis and treatment, biosensor and environmental analysis for their unique optical and electrical properties. Based on the surface catalytic activity of noble metal nanoparticles, a new method for quantitative determination of sulfur ion concentration in water using noble metal nanoparticles as analytical probe was developed. The method has the advantages of high sensitivity, good selectivity and rapid detection of sulfur ions. In the experiment, we first prepared spherical silver nanoparticles with uniform particle size (15 nm),) and stable dispersion in aqueous solution by polyol thermal method. It was found that the silver nanoparticles had a strong catalytic effect on the reduction of p-nitrophenol by sodium borohydride. The surface of silver nanoparticles was partially or completely sulfided (i.e. catalyst poisoning), which inhibited the catalytic activity of silver nanoparticles and reduced the reaction rate. A new method for the determination of sulfur ions in water was established by the quantitative relationship between the reaction rate constant and the concentration of sodium sulphide. The detection range of this method is 0. 5 渭 mol/L, and has been successfully applied to the detection of real samples. Secondly, based on the high catalytic activity of noble metal palladium, we synthesized palladium nanoparticles with different morphologies (cubes, octahedrons) as analytical probes. A highly sensitive colorimetric analysis method for the determination of sulfur ions was established by catalytic oxidation of hydrogen peroxide to 3 ~ (3) O _ (3) O _ (5) tetramethyl benzidine (TMB) as a typical catalytic oxidation reaction. In the experiment, the palladium nanocrystals with side length of 18 nm were first used as probes to catalyze the reaction at room temperature. When different concentrations of sodium sulphide were added to the system, the surface of the palladium nanocube was partially or completely sulfided (i.e. catalyst poisoning), which inhibited the catalytic activity of the nanocrystalline palladium cube and reduced the reaction rate. Based on the quantitative relationship between the absorbance of TMB at 650 nm and the concentration of sulfur ions, a new method for the determination of sulfur ions was established. In addition, the catalytic effect of octahedral palladium nanoparticles with different surface faces on the reaction and the sensitivity of the analytical method were investigated. In this paper, the surface catalytic poisoning effect of noble metal nanoparticles was combined with analytical chemistry, and a new method for the determination of sulfur ion concentration in water was established. This method has the advantages of simple operation, fast response, high sensitivity and high selectivity.
【學(xué)位授予單位】：重慶師范大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：O643.36;TB383.1

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本文編號(hào)：2281230