A synthetic standard for the analysis of carbon isotopes of carbon in silicates, and the observation of a significant water-associated matrix effect

Christopher H. House

Due to the biogeochemical fractionation of isotopes, organic material can be heterogeneous at the microscale. Because this heterogentiy preserves in the rock record, the microscale measurement of carbon isotopes is an important frontier of geobiology. Such analyses via secondary ion mass spectrometry (SIMS) have been, however, held back by the lack of an appropriate homogeneous synthetic standard that can be shared between laboratories. Such a standard would need to yield a carbon signal intensity within the same instrument dynamic range as that found for typical rocks, exhibit minimal matrix effects under typical SIMS conditions, and be widely available. In this work, five possible standards were tested with repeated δ(13)C ion microprobe measurements against the PPRG #215-1 Precambrian chert that has been used as a working standard for these types of analyses by several laboratories. Results showed that silica powder, pressed, and bonded with Ceramacast 905 produced a useful synthetic standard. The material produced has a secondary ion carbon yield of only about 15× that of the PPRG #215-1 organic-rich chert. Finally, the material, once dried sufficiently, did not demonstrate an observable matrix effect when the carbon isotopes were measured. Another similar material (silica nanopowder, pressed, and bonded with Aremco-Bond 526N) appears to have retained its hydration after a substantial effect to dry it. The isotopes measurements of this more hydrated material showed a significant matrix effect that was diminished by intense pre-sputtering. The results indicate water can affect SIMS carbon isotopic measurements, and an intense beam reduces the effect. A hydrated standard might be useful to monitor the effect. A suitable artificial standard for SIMS isotopic measurements of organic material in rocks has been found, and it will allow an acute growth in both the quantity and quality of studies of ancient carbon at the microscale. Also, this work has revealed a novel water-associated matrix effect for carbon isotopes. This newly revealed matrix effect is important because it might have misled previous research. The effect could lead to increased observed heterogeneity of partially hydrated samples and/or produced systematic differences between natural targets and the standards used.