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A protocol for preparing subfossil chironomid head capsules (Diptera: Chironomidae) for stable isotope analysis in paleoclimate reconstruction and considerations of contamination sources
Authors:Y Wang  D R Francis  D M O’Brien  M J Wooller
Institution:Y. Wang, D. R. Francis, D. M. O’Brien and M. J. Wooller
Abstract:Several techniques are available to examine the isotopic composition of historic lake waters, providing data that can subsequently be used to examine environmental changes. A recently-developed technique is the stable oxygen isotope analysis of subfossil chironomid (Diptera: Chironomidae) head capsules (mostly chitin) preserved in lake sediments. This technique involves a high Temperature Conversion Elemental Analyzer (TC/EA), which has been a relatively recent addition to the suite of online peripherals for analyzing the stable isotopic composition of organic samples. The highly precise and accurate 18O/16O and D/H measurements obtainable using the TC/EA with samples in the microgram range make this instrumentation suitable for studying geochemical and biological processes. Preparation of organic samples for isotopic analysis typically requires first weighing each sample into silver/tin capsules. These capsules can introduce oxygen and hydrogen contamination (a “blank effect”), which is especially problematic for analysis of small organic samples (e.g. less than 100 μg). Here we tested tin and silver capsules from two manufacturers and a range of sizes to assess contamination to small organic samples on the TC/EA. We also assessed how a method for cleaning silver capsules affected our analysis of commercial chitin. In general, capsules made of silver have less detectible oxygen than those made of tin, and capsules from the two manufacturers varied in their detectible oxygen. There was no detectable H contamination from silver capsules. In addition to our empirical findings, we present a model demonstrating the influence that contaminant oxygen can have on the δ18O of small organic samples. Sample mass becomes an important issue for such analyses. In light of our findings, we recommend a minimum sample mass ≥50 μg (approximately 120 whole chironomid head capsules) on a TC/EA-IRMS (Deltaplus XP system). Finally, we present a detailed protocol for preparing and transferring chironomid head capsules into silver capsules that minimizes the influence of contaminant oxygen. This protocol provides the paleo-community with another potential method for reconstructing paleoenvironments.
Keywords:TC/EA-IRMS  Blank silver capsule  Tin capsule  Chitin  Stable oxygen and hydrogen isotopic compositions  Chironomidae
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