The aim of this work was to develop a method to comprehensively characterize extracts from polyamide 11 powder samples used in the laser sintering process. Firstly, high resolution mass spectrometry was applied to identify low molecular compounds in the material. Secondly, by means of an inverse gradient high-performance liquid chromatography (HPLC) in combination with a triple detection system consisting of a diode array detector (DAD), a mass spectrometer (MS), and a charged aerosol detector (CAD), a method was established to determine the amount of monomer and oligomers up to the linear tetramer and cyclic pentamer. Furthermore, the oxidation stabilizer identified as Irganox 1098 was determined. The DAD was utilized for the quantification of the UV-active oxidation stabilizer. Thus, to be able to extract the low molecular weight compounds, various protocols were studied and finally accelerated solvent extraction was used. As there is a lack of commercial standards of polyamide 11 related oligomers, these compounds were detected with the CAD, taking advantage of its uniform response behavior in conjunction with an inverse gradient HPLC protocol. In addition, the MS was utilized as a qualitative detector for peak identification. The information regarding low molecular weight compounds are required as the powder is subject to the thermal loading of the sintering process, which influences the composition of the low molecular weight compounds. Thus, the method was applied to new and oven-aged polyamide 11 samples. Finally, it was possible to monitor the change of low molecular weight compounds in stressed polyamide 11 powder samples.

这项工作的目的是开发一种方法，以全面表征激光烧结工艺中使用的聚酰胺11粉末样品的提取物。首先，采用高分辨率质谱法鉴定材料中的低分子化合物。其次，借助反相梯度高效液相色谱（HPLC）结合由二极管阵列检测器（DAD），质谱仪（MS）和带电气溶胶检测器（CAD）组成的三重检测系统，建立了测定直链四聚体和环状五聚体的单体和低聚物数量的方法。此外，确定了鉴定为Irganox 1098的氧化稳定剂。DAD用于定量UV活性氧化稳定剂。因此，为了能够提取低分子量化合物，研究了各种方案，最后使用了加速溶剂萃取。由于缺乏与聚酰胺11相关的低聚物的商业标准，因此利用CAD来检测这些化合物，充分利用了其均一的响应特性以及反相梯度HPLC方案。此外，MS用作峰鉴定的定性检测器。由于粉末受到烧结过程的热负荷的影响，因此需要有关低分子量化合物的信息，这会影响低分子量化合物的组成。因此，该方法被应用于新的和老化的聚酰胺11样品。最后，可以监测应力聚酰胺11粉末样品中低分子量化合物的变化。