【作者】 游水英；

【导师】 周光明；

【作者基本信息】 西南大学 ， 分析化学， 2006， 硕士

【摘要】 色谱分离技术与化学发光检测技术的联合应用,是现代痕量分析中一项非常活跃的、具有广阔应用前景的研究。目前,这种方法已经广泛应用于环境分析、药物分析、临床检验、工业分析等领域。 本文主要由两部分组成,第一部分是综述,简单地介绍了低压离子色谱及其应用进展,并对近年来化学发光检测技术在环境分析中的应用加以评述。 第二部分为研究报告,主要利用低压离子色谱分离技术与化学发光检测技术联用,检测一些阴阳离子。具体内容如下: 1、低压离子色谱分离化学发光检测水中痕量硫离子 在碱性条件下,硫离子对鲁米诺和高碘酸钾化学发光反应有很强的增敏作用。基于此,本文结合流动注射技术,将低压离子色谱与化学发光联用检测痕量硫离子。在最佳实验条件下,硫离子浓度在4.0×10^-2～1.0mg/L范围内与发光强度呈良好的线性关系;检测限（3σ）为5.0×10^-3mg/L;相对标准偏差为0.5%(n=11,0.10mg/LS^2-)。该方法用于环境水样中S^2-的测定,结果令人满意。 2、低压离子色谱分离化学发光在线检测环境水样中痕量亚硝酸根离子和硫离子 研究了低压离子色谱分离—柱后鲁米诺化学发光检测方法,并分离测定了NO₂^-和S^2-,以碳酸钠作为洗脱液,Luminol-H₂O₂-NO₂^-(或S^2-)作为化学发光检测体系,对NO₂^-和S^2-两种阴离子进行在线检测。测定的线性范围分别为NO₂^-:5×10^-8～10^-6g/mL;S^2-:1×10^-8～6×10^-7g/mL。检测限NO₂^-为:3×10^-9g/mL,S^2-为:1.4×10^-9g/mL。该方法用于水样中NO₂^-和S^2-含量的测定,结果满意。更多还原

【Abstract】 The studies of applications of low-pressure ion chromatography with chemiluminescence detector were carried out in this work. It has been widely used applied in environmental analysis and pharmic analysis and medicinal analysis industrial analysis. There are two parts in the dissertation.A review of the application of low-pressure ion chromatography and chemiluminescence in the environmental analysis is described in the first one, and then some research reports were given in the other part. Some kind of ions were separated and determined by low-pressure ion chromatography with chemilunescence detection, and therefore good results were obtained.1. On-line Determination of Trace Sulfide in Water by Low-pressure Ion Chromatography with Chemiluminescence DetectionThe separation and determination of trace sulfide in water, combined with flow injection analysis is carried out by low ion chromatography with chemiluminescence detection. It is based on the enhancement of CL reaction of KIO₄ with luminol. The relationship between the CL intensity and the concentration of sulfide is linear in the range of 4.0 × 10^-2l .0 mg/L. The relative standard deviation is 0.5% （n=11, c=0.10mg/L）.The detection limit is 5.0×10^-3mg/L. The method has been applied to the determination of sulfide in water with satisfactory results.2. On-line Determination of NO₂^- and S^2- by Low-pressure Ion Chromatography with Chemiluminescence DetectionThe separations and determinations of NO2" and S2’ by low-pressure ion chromatography with chemiluminescence detection were investigated first time. The separation was carried out on anion separation column by the mobile phases of Na2CC>3 solution, Luminol-H2C>2- NO2XS2") system was used as the flow injection chemiluminescence analysis system. Under the optimum conditions, the linear range for NO2’is SxlO’^lO"6 g/mL, S2’lxl0"8⁶xl0’7 g/mL;the detection limit for NO2’ is 3><l0"9 g/mL,S2’ 1.4xlO’9 g/mL. The method has been applied to the determination of nitrite and sulfide in water with satisfactory result.3. Determination of trace lead （ II ） in industrial waste water by flow injection/coupled chemiluminescence reaction with enhancementA novel flow injection chemiluminescence enhancement method for the determination of Pb（ II） based on the replacement of Fe（ II） by Pb（ II） from Fe（ II ）-EDTA complex, and the subsequent chemiluminescence reaction of Fe（ II ）-luminol-RhB. The method is simple, rapid, and sensitive to determine Pb（II） in the range of 1.0xl0’3¹.0xl0"’ mg.L"1 with a detection limit of 3X10"4 mg.L"1. The relative standard deviation is 3.2% for the determination of l.OxlO’2 mg.L’’ Pb（II） （n=ll）. The method has been applied to determine Pb（II） in industrial waste water with satisfactory results.更多还原