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Abstract: NanoSIMS is a relatively new technology that is being applied to ancient carbonaceous structures to gain insight into their biogenicity and syngeneity. NanoSIMS studies of well preserved organic microfossils from the Neoproterozoic (∼0.8Ga) Bitter Springs Formation have established elemental distributions in undisputedly biogenic structures. Results demonstrate that sub-micron scale maps of metabolically important elements (carbon [C], nitrogen [measured as CN ion], and sulfur [S]) can be correlated with kerogenous structures identified by optical microscopy. Spatial distributions of C, CN, and S in individual microfossils are nearly identical, and variations in concentrations of these elements parallel one another. In elemental maps, C, CN, and S appear as globules, aligned to form remnant walls or sheaths of fossiliferous structures. The aligned character and parallel variation of C and CN are the strongest indicators of biogenicity. Nitrogen/carbon atomic ratios (N/C) of spheroids, filaments, and remnants of a microbial mat suggest that N/C may reflect original biochemical differences, within samples of the same age and degree of alteration. Silicon (Si) and oxygen (O) maps illustrate that silica is intimately interspersed with organic carbon of the microfossils. This relationship is likely to reflect the process of silica permineralization of biological remains and thus may be an indicator of syngeneity of the fossilized material with the mineral matrix. The NanoSIMS characterization of Bitter Springs microfossils can be used as a baseline for interpreting less well preserved carbonaceous structures that might occur in older or even extraterrestrial materials. An example of such an application is provided by comparison of Bitter Springs results with NanoSIMS of Archaean carbonaceous structures from Western Australia, including a spheroid in the ∼3Ga Farrel Quartzite and material in a secondary vein in the 3.43Ga Strelley Pool Chert. Results reinforce a biogenic, syngenetic interpretation for the Archaean spheroid. NanoSIMS has several advantages in the study of ancient organic materials: the technique allows characterization of extremely small structures that are present in low concentrations; organic matter does not have to be isolated by acid treatment but can be analyzed in polished thin section; preparation is simple; samples are minimally altered during analysis; results provide sub-micron scale spatial distribution coupled with concentration information for at least five elements; the biologically important elements of carbon and nitrogen can be assessed; and the ability to study organic remains in situ permits petrographic assessment of spatial relationships between organic matter and mineral constituents. These advantages could be of significant benefit for interpretation of poorly preserved and fragmentary carbonaceous remains that might occur in some of Earth''s oldest samples as well as in meteorites or extraterrestrial material brought to Earth in future planetary missions. [Copyright &y& Elsevier]