【作者】 章表明；

【导师】 蒋治良；

【作者基本信息】 广西师范大学 ， 无机化学， 2005， 硕士

【摘要】 第一部分: 绪论综述了近年来,纳米微粒的制备方法、表征手段以及共振散射技术在纳米微粒研究和分析化学中的应用。综述了纳米硫化银、纳米硒的制备研究进展和氯氧化物的分析研究进展。 第二部分: 液相硫化银纳米微粒的共振散和荧光效应研究在阴离子表面活性剂十二烷基硫酸钠（SDS）和硫代乙酰胺（TAA）存在下,Ag⁺和S^2-反应生成较稳定的Ag2S 纳米微粒。光谱特性研究表明, Ag₂S 纳米微粒在470 nm 处产生1 个荧光峰,在470 nm 处产生1 个共振散射峰。TAA 和Ag⁺浓度对体系界面荧光的影响与此二种物质浓度对共振散射的影响一致。界面荧光与共振散射之间存在相关性。Ag⁺浓度在0～8.6 mg·L^-1 范围内与荧光和共振散射光强度都具有良好的线性关系。据此,可建立利用体系荧光或共振散射光测定Ag+的新方法。 第三部分:硒纳米微粒的共振散射光谱特性研究及其在维生素C 分析中的应用在盐酸介质中,维生素C 还原Se （Ⅵ）生成较稳定的硒纳米微粒。它在可见光范围内无明显特征吸收峰,在340、400、470 和520 nm 处产生四个共振散射峰和四个界面荧光峰。试剂浓度对共振散射强度ΔI340nm和界面荧光强度ΔF470nm的影响一致,共振散射和界面荧光之间存在相关性。维生素C 浓度在0.05～4.0 mg·^-1 和0.15～4.0 mg·L^-1 范围内分别与共振散射强度和荧光强度具有良好的线性关系。据此本文建立了一个检出限为0.01 mg·L^-1维生素C 的共振散射光谱新方法, 并用于合成样品和药品中VC 含量的分析,结果满意。更多还原

【Abstract】 PartⅠIntroduction Resonance scattering technology and the progress of its application in study nanoparticle systems and in analytical chemistry in resent years are introduced. The progress of preparation for Ag₂S and Se nanoparticles and the progress of ClO^-, ClO₂^-, ClO₂ and ClO₃-analysis are also introduced. PartⅡThe Interface Fluorescence and Resonance Scattering Spectral Properties of Ag2S nanoparticles in Liquid Phase In the presence of sodium dodecyl sulphate （SDS）, S^2- and Ag⁺ form Ag₂S nanoparticles. The resonance scattering and emission spectra of Ag₂S nanoparticles in liquid phase show that, Ag₂S anoparticles exhibit one strongest resonance scattering peak at 470 nm, and one strongest fluorescence peak at 470 nm when excited wavelength is at 200 nm. It is consistent that the effects on the concentration of TAA on the resonance scattering signals and fluorescence intensities and that of Ag⁺. There is the correlation between the fluorescence and resonance scattering. A new method for the determination of trace Ag⁺ with resonance scattering or fluorescence spectrum can be developed, owing to The Ag⁺ concentration is proportional to the intensity of resonance scattering or fluorescence at the range of 0-8.6 mg·L^-1. Part ⅢResonance Scattering Spectral Properties of Se nanoparticles and Its Application to determination of vitamin C In the medium of hydrochloric acid, Vitamin C（VC） reacts with Se（Ⅵ） to form Se nanoparticles. The particles do not exhibit any absorption peaks in the zone of visible light, but exhibit four resonance scattering peaks and four fluorescence peaks at 340, 400, 470 and 520 nm. The effects of reagents concentration on the intensity of resonance scattering signals at 340 nm （ΔI340nm） are consistent with that on the fluorescence intensity at 470nm （ΔF470nm）. There is the correlation between the interface fluorescence and resonance scattering. VC concentration is proportional to the ΔI340nm and ΔF470nm in the range of 0.05 to 4.0 mg·L-1 and 0.15 to 4.0 mg·L-1, respectively. Base on this fact, a new resonance scattering spectral （RSS） method has been proposed for the determination of VC. The detection limit is 0.01 mg·L-1. This method was used to determination of VC in pharmaceuticals and synthetic samples with satisfactory results. Part ⅣA Fluorescence Quenching Method for the Determination of Trace ClO-with ClO--I--Rhodamine 6G system In the medium of hydrochloric acid, ClO-reacts with excessive I-forming I3-. It combine respectively Rhodamine 6G （RhG）, Rhodamine S （RhS）, Rhodamine B （RhB） and butyl-Rhodamine B （b-RhB） to form association particles, which result fluorescence quenching of the RhG, RhS, RhB and b-RhB systems at 550, 550, 580 and 580 nm, respectively. The fluorescence quenching is proportional to the concentration of ClO-at the range of 0.015-0.43, 0.020-0.35, 0.020-0.51 and 0.020-0.35 mg·L-1 and the detect limits for each system are 0.010, 0.016, 0.028 and 0.029 mg·L-1, respectively. Based on these facts, fluorescence quench methods for determination of trace ClO-have been proposed. Owing to the system of RhG having high sensitivity and good stability, it has been applied to the determination of ClO-in bleaching powder and liquid, with satisfactory results. Part ⅤA new Sensitive and selective Fluorescence Method for Determination of Chlorine Dioxide in Water Using Rhodamine S Based on the capacity of chlorine dioxide to decolorize Rhodamine dyes in the presence of ammonia/ammonium chloride buffer, a sensitive, highly selective method for the determination of trace chlorine dioxide has been developed. The fluorescence quenching is proportional to the concentration of ClO2 at the range of 0.0060-0.450, 0.0373-0.996, 0.0830-3.06 and 0.139-2.50 mg·L-1 and the detect limits for each system are 0.003, 0.027, 0.064 and 0.123 mg·L-1, respectively. With high sensitivity and good selectivity, the Rhodamine S has been applied to the determination of ClO2 in synthetic samples and samples, with satisfactory results.更多还原