Analytical validation on carbon and oxygen isotopic measurement of small carbonate samples by using IsoPrime100 mass spectrometer
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This paper focused on analytical validation such as the amount needed, time drift, repeatability, memory effect, analytical precision and accuracy on carbon/oxygen isotopic measurement of small carbonate samples (10–80 µg) using an IsoPrime100 mass spectrometer. 10 µg of carbonate samples yielded mass 44-intensity of 2 nA. The minimum amount needed was 10 μg and the repeatability was around 0.1 ‰ (1 s.d.). Through 24-h measurement there was no temporal variation of δ13C, but that of δ18O showed variation with decreasing the amount of CO2 reference gas, suggesting that δ18O values need to conduct time drift correction. Inter-sample memory effect was not observed, indicating that IsoPrime100 mass spectrometer with CO2 purification system is adequately evacuated after each analysis by means of pumping system. Moreover, IAEA-CO-1 and JAMSTEC-WS values calibrated by international reference NBS19 agree within error with the reference values, demonstrating the accuracy of our analytical procedure on carbon/oxygen isotopic measurement of carbonate samples. This paper offers insights into analytical validation procedure when setting up a mass spectrometer on isotopic analyses of small carbonate samples.
KeywordsCarbonate Carbon isotopes Oxygen isotopes Validation Mass spectrometry
We are grateful to Dr. S. Sakai (JAMSTEC) for useful comments related to experimental techniques. We appreciate Geological and Nuclear Science Ltd for the measurement of JAMSTEC-WS isotopic data. This study was supported by Program for Next Generation World-Leading Researchers of the Japan Society for the Promotion of Science (NEXT Program; GR063).
Compliance with ethical standards
This study was supported by Program for Next Generation World-Leading Researchers of the Japan Society for the Promotion of Science (NEXT Program; GR063).
Conflict of interest
The authors declare that they have no conflict of interest.
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