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On Soot Sampling: Considerations when Sampling for TEM Imaging and Differential Mobility Spectrometer

机译:关于烟灰采样:针对TEM成像和差分移动光谱仪采样时的考虑因素

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Particulate matter (PM) has been sampled from a compression ignition engine using a differential mobility spectrometer (Cambustion DMS 500) and for imaging in a transmission electron microscope (TEM) with the aim of coupling these two measuring techniques. A known issue when coupling these two methods is that a devise like the DMS samples all PM, and the TEM only soot. To help resolve this issue, a thermal denuder was designed and built to remove all volatile organic compounds (VOC) from the sample prior to entering the DMS. For TEM imaging, soot was either collected directly onto a TEM grid using the thermophoretic effect or collected onto quartz filters with the soot then transferred onto the TEM grids. The direct to grid technique did not work after the denuder due to the gas temperature being too low for the thermophoretic effect; hence the reason to collect some soot using the quartz filters. Soot was removed from the filters using an ethanol wash/sonication technique. Morphology; diameter of gyration, projected area, primary particle size and fractal dimension have been compared between the two TEM sampling techniques, with or without the denuder. Denuder effectiveness has been assessed using TGA analysis of sampled soot. Issues concerning the sampling process itself are outlined. A comparison between the TEM and the DMS results is conducted with the discrepancies between them discussed. Direct and filter sampling gave similar results as long as the sonication process and grid prep is done properly, otherwise the filter wash technique results in a number of clusters of agglomerates which distorts the post processing and morphological data.
机译:使用差分迁移率光谱仪(Cambusion DMS 500)从压缩点火发动机采集颗粒物质(PM)并用于在透射电子显微镜(TEM)中成像,其目的是耦合这两个测量技术。耦合这两种方法时的已知问题是像DMS样本一样设计,并且TEM仅烟灰。为了帮助解决这个问题,设计了热脱位器,并在进入DMS之前从样品中除去所有挥发性有机化合物(VOC)。对于TEM成像,使用致硫化效果直接收集到TEM网格上,或者将烟灰收集到石英过滤器上,然后转移到TEM网格上。由于气温对于硫化机效果而言,直接栅格技术在裸露的情况下不起作用;因此,使用石英滤波器收集一些烟灰的原因。使用乙醇洗涤/超声技术从过滤器中除去烟灰。形态学;在两个TEM采样技术之间,有或没有剥落器,比较了旋转直径,投影区域,初级粒度和分形尺寸。使用取样烟灰的TGA分析评估了剥裸者的有效性。概述了有关采样过程本身的问题。 TEM与DMS结果之间的比较是以他们讨论的差异进行的。直接和滤波器采样具有类似的结果,只要正确完成超声处理和网格预制,否则滤清器洗涤技术会导致许多聚集簇扭曲后处理和形态数据。

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