Extraction of calcareous dacryoconarid microfossils from limestones and mudrocks by surfactants paired with freeze-thaw processing

Abstract

Microfossils offer a wealth of paleoenvironmental information, but their extraction from consolidated material, especially ancient rocks, is time-consuming and often lacks systematic methodological development. This study examined the efficacy of repeated freeze-thaw processing paired with different surfactants (anionic, cationic, and detergent) on the extraction of fossils from the order Dacryoconarida, conically shaped calcareous microfossils that occur in diverse marine facies of the Devonian Period. A stepwise technique was developed involving saturation of rocks in either 18 Ω water or 25% NaCl, followed by freezing and then boiling in surfactant (Pinequat, Decon 90, or Calgon in Na₂CO₃ solution). In comparison with saturation in NaCl solution, saturation in water generally had higher yields of disaggregated material and more intact fossils. All surfactants performed better at extraction compared to boiling in pure water. Across all lithologies examined, Na₂CO₃-buffered Calgon (sodium hexametaphosphate) disaggregated rock most efficiently, but Na₂CO₃ solution alone generally had the highest yield of total and intact fossil specimens. Pinequat, a cationic surfactant, yielded more disaggregate for siliclastic samples compared to calcareous samples, but had lower fossil yield. Decon 90, an anionic surfactant, performed better at disaggregating limestones and had higher fossil extraction efficiency than Pinequat across all lithologies. Freeze-thaw processing pairing water saturation and 5% Na₂CO₃ simmering is an effective treatment for the disaggregation of rocks to extract analytically viable amounts of dacryoconarids from fossiliferous samples. This pairing had greater fossil extraction potential than surfactants at the concentrations tested in this study and is recommended if the elemental composition of the target rocks is unconstrained.