【作者】 赵景红；

【导师】 关亚风；

【作者基本信息】 中国科学院研究生院（大连化学物理研究所） ， 分析化学， 2006， 博士

【摘要】 针对某些特殊类样品,本论文发展出相应的进样方法、技术并研制出相应的装置,与色谱和色谱/质谱联用分析,解决了这些特殊样品的分析难题。论文第二章发展出用石英纤维部分填充的单收口内衬管-热脱附-气相色谱/质谱联用,对所收集的大气可吸入颗粒物样品,定性定量测定了细粒子中的半挥发有机物。分别采用FID、MS、PFPD、NPD检测器,测定了北京、重庆、宁波三个城市、七级不同粒径颗粒物上的多环芳烃、正构烷烃、含硫及含氮化合物。第三章设计了基于静态顶空原理的变压器油中溶解气体在线采集装置,结合小体积动态预浓缩技术与微型气相色谱仪联用,实现了对变压器油中C2烃类溶解气体的在线分析。系统测量了C2烃类溶解气体分配系数与温度的关系,得到了经验公式并用于实际油样中C2烃的定量分析。第四章采用液相十通阀、毛细管阻尼器和石英毛细管样品管,设计了高压液-气混合样品的进样装置,实现了直接进样气相色谱分析,一次进样得到液-气所有组分的面积归一化结果。考察了阻尼管尺寸、进样时间、进样体积、辅助载气流量等参数,研究了溶剂洗脱和无歧视柱上进样校正两种定量方法。在线测定了乙烯齐聚合成己烯-1中试装置中高压气-液反应物及高压地下石油样品组成。第五章设计了在线负压气体采集进样装置,用于负压气体样品的在线采集直接质谱分析。双流路设计的采样和标气校准装置,可以在线配制标准气体,实现在线校正。解决了化学激光负压冷阱尾气组成的在线分析问题。更多还原

【Abstract】 This dissertation describes a number of new technologies and methods for sample introduction of special samples in gas chromatographic analysis, or gas chromatography/mass spectroscopic analysis.Chapter 2 introduces a partially packed liner for holding the sample of collected air particulate matters (PM10), followed by a thermal desorption- GC/MS for trace analysis of semi-volatile organic compounds on the particulates. The simple design eliminates contamination of the analytical system from fine particulates, and avoids any adsorption of target compounds in a liner to be analyzed. The trace PAHs, alkanes, organic sulfur and organic nitrogen compounds on PM10 were determined by GC coupled with FID, MS, PFPD and NPD detectors, respectively. The kinds and contents of semi-volatile organic compounds on seven different size particulates collected in Beijing, Chongqing and Ningbo were determined and compared.Chapter 3 reports an on-line headspace-sampling device for dissolved gases in transformer oil, and coupled it to a small volume dynamic pre-concentration device and a micro-GC, for the determination of C2 hydrocarbons. The effect of temperature on partition coefficients of C2 hydrocarbon gases was measured systematically and formulas between partition coefficient and temperature were更多还原