Affiliation:
1. US Geological Survey, Central Energy Resources Science Center Denver Colorado USA
2. Department of Geoscience University of Wisconsin‐Madison Madison Wisconsin USA
3. Lamont‐Doherty Earth Observatory of Columbia University Palisades New York USA
4. Department of Earth & Planetary Sciences University of California Davis Davis California USA
Abstract
AbstractRationaleThe use of secondary ion mass spectrometry (SIMS) to perform micrometer‐scale in situ carbon isotope (δ13C) analyses of shells of marine microfossils called planktic foraminifers holds promise to explore calcification and ecological processes. The potential of this technique, however, cannot be realized without comparison to traditional whole‐shell δ13C values measured by gas source mass spectrometry (GSMS).MethodsPaired SIMS and GSMS δ13C values measured from final chamber fragments of the same shell of the planktic foraminifer Orbulina universa are compared. The SIMS–GSMS δ13C differences (Δ13CSIMS‐GSMS) were determined via paired analysis of hydrogen peroxide‐cleaned fragments of modern cultured specimens and of fossil specimens from deep‐sea sediments that were either untreated, sonicated, and cleaned with hydrogen peroxide or vacuum roasted. After treatment, fragments were analyzed by a CAMECA IMS 1280 SIMS instrument and either a ThermoScientific MAT‐253 or a Fisons Optima isotope ratio mass spectrometer (GSMS).ResultsPaired analyses of cleaned fragments of cultured specimens (n = 7) yield no SIMS–GSMS δ13C difference. However, paired analyses of untreated (n = 18) and cleaned (n = 12) fragments of fossil shells yield average Δ13CSIMS‐GSMS values of 0.8‰ and 0.6‰ (±0.2‰, 2 SE), respectively, while vacuum roasting of fossil shell fragments (n = 11) removes the SIMS–GSMS δ13C difference.ConclusionsThe noted Δ13CSIMS‐GSMS values are most likely due to matrix effects causing sample–standard mismatch for SIMS analyses but may also be a combination of other factors such as SIMS measurement of chemically bound water. The volume of material analyzed via SIMS is ~105 times smaller than that analyzed by GSMS; hence, the extent to which these Δ13CSIMS‐GSMS values represent differences in analyte or instrument factors remains unclear.
Funder
National Science Foundation
U.S. Department of Energy
Subject
Organic Chemistry,Spectroscopy,Analytical Chemistry