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The determination of size distribution of soot particles and agglomerates in oil samples using a Nanosight LM14 to perform Nanoparticle Tracking Analysis (NTA) is described. This is the first application of the technique to sizing soot-in-oil agglomerates and offers the advantages of relatively high rates of sample analysis and low cost compared to Transmission Electron Microscopy (TEM). Lubricating oil samples were drawn from the sump of automotive diesel engines run under a mix of light duty operating conditions. The oil samples were diluted with heptane before analysing. Results from NTA analysis were compared with the outputs of a more conventional analysis based on Dynamic Light Scattering (DLS). This work shows that soot-in-oil exists as agglomerates with average size of 115 nm. This is also in good agreement with TEM analysis carried out in a previous work. NTA can measure soot particles in polydisperse oil solutions and report the size distribution of soot-in-oil aggregates.

Morphology plays an important role in determining behaviour and impact of soot nanoparticles, including effect on human health, atmospheric optical properties, contribution to engine wear, and role in marine ecology. However, its nanoscopic size has limited the ability to directly measure useful morphological parameters such as surface area and effective volume. Recently, 3D morphology characterization of soot nanoparticles via electron tomography has been the subject of several introductory studies. So-called ‘3D-TEM’ has been posited as an improvement over traditional 2D-TEM characterization due to the elimination of the error-inducing information gap that exists between 3-dimensional soot structures and 2-dimensional TEM projections. Little follow-up work has been performed due to difficulties with developing methodologies into robust high-throughput techniques.

The size and morphology of soot particles and agglomerates extracted from lubricating oil drawn from the sump of a diesel engine have been investigated and compared using Transmission Electron Microscopy (TEM) and Nanoparticle Tracking Analysis (NTA). Samples were prepared for electron microscopy imaging by both centrifugation and solvent extraction to investigate the impact of these procedures on the morphological characteristics, such as skeleton length and width and circularity, of the obtained soot. It was shown that centrifugation increases the extent of agglomeration within the sample, with 15% of the agglomerates above 200 nm compared to only 11% in the solvent extracted soot. It was also observed that the width of centrifugation extracted soot was typically 10 nm to 20 nm larger than that of solvent extracted soot, suggesting that centrifugation forces the individual agglomerate chains together.