A preparation sequence for multi-analysis of µm-sized extraterrestrial and geological samples

1Alice Aléon-Toppani,1Rosario Brunetto,2Jérôme Aléon,1,3,4Zelia Dionnet,1Stefano Rubino,1,2Dan Levy,5David Troadec,6François Brisset,7Ferenc Borondics,7Andrew King
Meteoritics & Planetary Science (in Press) Link to Article [https://doi.org/10.1111/maps.13696]
1Institut d’Astrophysique Spatiale, UMR 8617, CNRS, Univ. Paris-Saclay, Bât 120-121, 91405 Orsay Cedex, France
2Institut de Minéralogie, de Physique des Matériaux et de Cosmochimie, UMR 7590, Sorbonne Université, Museum
National d’Histoire Naturelle, CN RS, IRD, 61 rue Buffon, 75005 Paris, France
3INAF-IAPS, Rome, Italy
4DIST-Università Parthenope, Naples, Italy
5Institut d’électronique de microélectronique et de nanotechnologie, UMR 8520, Laboratoire central, Cité scientifique, Avenue Henri Poincaré, CS, 60069, 59652 Villeneuve d’Ascq Cedex, France
6Institut de Chimie Moléculaire et des Matériaux d’Orsay, CNRS, UMR 8182, Univ. Paris-Saclay, Orsay, France
7SOLEIL Synchrotron, Gif-sur-Yvette, France
Published by arrangement with John Wiley & Sons

With the recent and ongoing sample return missions and/or the developments of nano- to microscale 3-D and 2-D analytical techniques, it is necessary to develop sample preparation and analysis protocols that allow combination of different nanometer- to micrometer-scale resolution techniques and both maximize scientific outcome and minimize sample loss and contamination. Here, we present novel sample preparation and analytical procedures to extract a maximum of submicrometer structural, mineralogical, chemical, molecular, and isotopic information from micrometric heterogeneous samples. The sample protocol goes from a nondestructive infrared (IR) tomography of ~10 to ~70 µm-sized single grains, which provides the distribution and qualitative abundances of both mineral and organic phases, followed by its cutting in several slices at selected sites of interest for 2-D mineralogical analysis (e.g., transmission electron microscopy), molecular organic and mineral analysis (e.g., Raman and/or IR microspectroscopy), and isotopic/chemical analysis (e.g., NanoSIMS). We also discuss here the importance of the focused ion beam microscopy in the protocol, the problems of sample loss and contamination, and at last the possibility of combining successive different analyses in various orders on the same micrometric sample. Special care was notably taken to establish a protocol allowing correlated NanoSIMS/TEM/IR analyses with NanoSIMS performed first. Finally, we emphasize the interest of 3-D and 2-D IR analyses in studying the organics–minerals relationship in combination with more classical isotopic and mineralogical grain characterizations.

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