Effects of chemical pretreatments on δ18O measurements, chemical composition, and morphology of chironomid head capsules

Abstract

Stable oxygen isotope measurements on fossil chironomid head capsules from lake sediments show that these chitinous remains can be used to reconstruct past lake water δ18O and, indirectly, past climate change. We examined the impact of chemical pretreatment procedures on the chemical and stable oxygen isotope composition, and morphology of chironomid cuticles. Use of alkali, acids, and sodium chlorite alters the chemical composition and the morphological structure of chironomid cuticles by selective removal of chitin or proteins. Gas chromatograms of pyrolyzates show that NaClO2 causes deproteination, whereas the combined use of HCl and HF results in partial chitin removal. Head capsules pretreated with KOH contained both chitin- and protein-derived moieties, although the concentration of protein was reduced, especially after KOH treatment at high concentration (28%) and temperature (100°C). Scanning electron microscopy confirmed that a proteinaceous matrix is still present in modern and fossil head capsules after KOH treatment. This matrix, however, is largely absent in head capsules pretreated with NaClO2. A change in the proportion of chitin and proteins in our samples was associated with differences in chironomid δ18O values. Our results suggest that deproteination results in a relative increase of chironomid δ18O, whereas removal of chitin leads to decreased δ18O values. We therefore discourage the use of acids or prolonged (≥1 h) exposure to hot alkali (70°C) prior to chironomid δ18O analysis. Chitin purification by sodium chlorite causes significant weight loss, which may preclude down-core chironomid δ18O measurements. Caution and standardization are required when pretreating samples for chironomid δ18O analysis to ensure reliable, comparable, and reproducible results. © 2009 The Author(s).