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Useful references for calcium carbonate samples
IAEA Isotope Hydrology Laboratory Publications
δ18O based paleotemperature equation from carbonates.
Dual-Inlet Source Mixing Characterization.
Meijer et al., Cross contamination in dual inlet isotope ratio mass spectrometers, International Journal of Mass Spectrometery, 198, 45-61, 2000.
McCrea, J. M., On the Isotopic Chemistry of Carbonates and a Paleotemperature Scale, J. Chem. Phys. 18, 849 (1950); doi:10.1063/1.1747785
Tyler B. Coplen, Carol Kendall & Jessica Hopple, Comparison of stable isotope reference samples, Nature 302, 236 - 238 (17 March 1983); doi:10.1038/302236a0
Kaiser, J., Reformulated 17O correction of mass spectrometric stable isotope measurements in carbon dioxide and a critical apraisal of histroic 'absolute' carbon and oxygen isotope ratios, Geochimica et Cosmochimica Acta, 72, 1312-1334 (2008)
Brand, W., Assonov, S. & Tyler B. Coplen, Correction for the 17O interference in δ(13C) measurements when analyzing CO2 with stable isotope mass spectrometry (IUPAC Technical Report), Pure and Applied Chemistry, 82, 8, 1719-1733 (2010)
For those of you running aragonite for d18O using phosphoric acid digestion: raise your hand if you take into account the different acid fractionation of aragonite relative to calcite as in Kim et al. 2007.
Kim S-T, Mucci A, Taylor BE. 2007. Phosphoric acid fractionation factors for calcite and aragonite between 25 and 75 *C: revisited. Chemical Geology 246: 135-146.
If you run the kiel at 70*C, your aragonites would be 0.3772 permil heavier. Thank you.
The selective acid extraction method of Al-Aam et al. (1990). has been commonly used to distinguish the C and O isotopic composition of different carbonate components that are composed of the mixture of calcite and dolomite. The mixture powder (~50 mg) was reacted in three steps: (1) with >100% H3PO4 at 25°C for 2 h in vacuum to extract CO2 from the calcite fraction, (2) continuously with >100% H3PO4 at 25°C for 24 h in vacuum to extract CO2 from the calcite-dolomite mixture, (3) the remaining material was reacted at 50°C for more than 100 h to obtain CO2 from the dolomite. A further discussion on this method was presented by Yui and Gong (2003).
Al-Aasm, I.S., Taylor, B.E., South, B., 1990. Stable isotope analysis of multiple carbonate samples using selective acid extraction. Chem. Geol. 80, 119-125.
Yui, T.-F. and Gong, S.-Y., 2003. Stoichiometry effect on stable isotope analysis of dolomite. Chem. Geol. 201, 359-368.
There has been a discuss on this among apatite dissolvers recently. It is very important to heat, under vacuum for at least an hour, to remove water and then to load the samples immediately for the run.
Ross Secord at Nebraska heats to as high as 200°C (). Most everyone else heats to 65-80°C.
DO NOT heat at very high T (>200°C). You will begin to lose carbonate. I think 200°C is a little risky, but Ross has a specific scientific question that justifies higher temperatures.
Kiel Carbonate Device and MAT 253 Manuals and Brochures.