关于DAM异构体采用高效液相色谱分析的可行性研究论文.docVIP

关于DAM异构体采用高效液相色谱分析的可行性研究 DAM是生产MDI系列产品的重要原料，而DAM中二环各异构体的含量是工艺调节参数的重要依据。多年以来DAM异构体含量的分析方法无国标和企标，一直采用万华企业标准——气相色谱法从2003用至未曾更新，直到2011年才在气相分析方法中加入反吹装置以保护色谱柱，但效果不是很明显。基于日常工作中出现的各种异常情况，本次实验主要根据样品的性质，探究采用高效液相色谱法分析DAM异构体，用外标法定量，辅之以合适的分析条件来准确的分析出DAM异构体含量，减小误差来源。同时通过样品稳定性测试、气相与液相分析方法对比、人员比对等措施将DAM液相分析方法逐渐完善并形成标准方法。 本法对DAM异构体的检测限暂未测定，线性系数为0.9999，平均回收率为99.89。该方法适合DAM异构体的分析。 关键词：DAM异构体 外标法 高效液相色谱 梯度洗脱 ABSTRACT DAM is one of the important raw materials MDI production series products, the content of each isomer and DAM on the technology transfer is the important basis of refs. For years DAM isomer content analysis method, no national standard and enterprise standard, has been using wanhua enterprise standard - gas chromatography. Since 2003 applications for many years have not update, it was not until 2011 in the gas phase analysis method to add reverse blowing device to protect the chromatographic column, but the effect is not obvious. Based on in the daily work of all kinds of anomalies, this experiment mainly according to the nature of the sample probe DAM isomers by high performance liquid chromatography analysis, the quantitative by external standard method, supplemented by the appropriate conditions to accurate analysis the DAM isomer content, reduce the error source. Through stability test sample at the same time, gas phase, liquid phase analysis method than measures such as contrast, personnel, will gradually perfect DAM liquid phase analysis method and standard method is formed. Detection limit of this law applicable to DAM isomers, temporarily not determine the linear coefficients is 0.9999, the average recovery was 99.89. This method is suitable for the analysis of DAM isomers. Keywords: DAM isomer 、external standard method、 HPLC、 gradient elution 目录 第一章 绪论 6 1.1 DAM简介 6 1.1.1 DAM组成及结构特点 6 1.1.2用途及注意事项 6 1.1.3 DAM中二环含量 7 1.1.4 影响DAM中二环含量因素 7 1.2高效液相色谱法简介 7 1.2.1系统组成 8 1.2.2工作原理 8 1.2.3色谱特点 8 1.2.4应用 9 1.2.5注意事项 9 1.3本课题研究的目的、意义及主要内容 10 第二章 气相色谱分析DAM异构体