【作者】 杨慧仙；

【导师】 李贵荣；

【作者基本信息】 南华大学 ， 卫生毒理学， 2006， 硕士

【摘要】 第一章，利用丹酰氯（DNS-Cl）与4-NP在碱性条件下反应，筛选出测定水样中痕量4-NP的共振光散射（RLS）体系：4-NP-Na₂CO₃-DNS-Cl，研究了该体系的RLS光谱特征，考察了溶液酸度、试剂用量、反应温度、反应时间和共存离子等因素对体系RLS强度的影响，优化了体系反应条件，确立了RLS强度改变值(ΔI_RLS=I-I₀)与4-NP浓度的线性关系，以此建立了测定4-NP的RLS新方法。 试验结果表明：在Na₂CO₃介质中，痕量的4-NP与DNS-Cl反应，产物在300nm～600nm之间有很强的RLS。在选定的测定波长λ_ex=λ_em=396.8nm处，RLS强度改变值(ΔI_RLS)与4-NP浓度在6.67×10^-4～6.00×10^-2μg／ml范围内呈良好的线性关系，相关系数0.9990，方法检出限0.200ng／ml。该方法在室温下进行，操作简便，具有灵敏度高、选择性好、成本低等特点。结合C₁₈柱固相萃取分离技术，应用于环境水样和合成水样中4-NP的测定，相对标准偏差小于3.80％，样品加标回收率为91.25％～94.50％。 第二章，利用I^-与Cd（Ⅱ）在酸性介质中形成的CdI₄^2-配阴离子，进一步与CV阳离子染料缔合，形成离子缔合物，离子缔合物因粒径增大，使体系RLS增强，以此建立RLS测定环境水样中Cd（Ⅱ）的新方法。实验研究了离子缔合物的共振光散射光谱特征，考察了溶液酸度、试剂用量、反应温度、反应时间和共存离子等因素对该体系RLS强度的影响，确立了体系的反应最适条件和RLS强度改变值(ΔI_RLS=I-I₀)与Cd（Ⅱ）浓度的线性关系。 结果表明：在稀H₂SO₄介质中，Cd（Ⅱ）与I^-形成的CdI₄^2-配阴离子，进一步更多还原

【Abstract】 In chapter 1, in order to establish a new method for the determination of trace 4-NP in environmental water samples, 4-NP was derivatized by dansyl chloride （DNS-C1） in base medium, and a resonance light scattering（RLS） system of 4-NP-Na₂CO₃-DNS-Cl was selected. The properties of the RLS spectra of the system were studied, and the significant parameters such as acidity in the system, reagent dosage, temperature, reaction time and foreign ions have been optimized using univariate method. The new method based on the linear relationship of the enhanced intensity （ΔIrls=I-I₀） of RLS in the system to the concentration of 4-nonylphenol was established.The results showed that the dansyl derivative resulted in significant enhancement of RLS from 300nm to 600nm in sodium carbonate medium. The RLS detection was performed at 396.8 nm. Under these conditions, 4-NP was showed good linearity in the range of 6.67×10^-46.00×10^-2μg/ml with correlation coefficient 0.9990, and the limit of detection was 0.200ng/ml. The proposed metheod combining with C₁₈ solid phase extraction can be operated conveniently at room temperature with high sensitivity and good selectivity and was applied to the determination of environmental and synthetic water samples, the recoveries were from 91.25% to 94.50% with a relative standard deviation of less than 3.80%.In chapter 2, utilizing crystal violet（CV） associating with CdI₄^2- formed by Cd（ II） with I^- in acid medium and the ionic associate resulting in enhancement of RLS owing to its size augmentation, the RLS new method for determining trace cadmium was proposed. The affecting factors on the strength of RLS in the system including更多还原