Precise Measurement of Carbon Concentration and Isotopic Ratios in Silicate Rocks by a High Sensitivity Elemental Analyzer Coupled with a Continuous Flow Isotope Mass Spectrometry

Xiang-ping ZHA; Bing GONG; Yong-fei ZHENG

doi:10.15898/j.cnki.11-2131/td.201611190174

Rock and Mineral Analysis > 2017 > 36(4): 327-339. > DOI: 10.15898/j.cnki.11-2131/td.201611190174

Xiang-ping ZHA, Bing GONG, Yong-fei ZHENG. Precise Measurement of Carbon Concentration and Isotopic Ratios in Silicate Rocks by a High Sensitivity Elemental Analyzer Coupled with a Continuous Flow Isotope Mass Spectrometry[J]. Rock and Mineral Analysis, 2017, 36(4): 327-339. DOI: 10.15898/j.cnki.11-2131/td.201611190174

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Precise Measurement of Carbon Concentration and Isotopic Ratios in Silicate Rocks by a High Sensitivity Elemental Analyzer Coupled with a Continuous Flow Isotope Mass Spectrometry

Key Laboratory of Crust-Mantle Materials and Environments, Chinese Academy of Sciences, School of Earth and Space Sciences, University of Science and Technology of China, Hefei 230026, China

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Received Date: November 18, 2016
Revised Date: March 09, 2017
Accepted Date: July 14, 2017
Published Date: March 31, 2017

Abstract

Highlights
· Micro-amounts of carbon isotopes are analyzed in silicate rocks by a high sensitivity elemental analyzer coupled with a continuous flow isotope mass spectrometrer.

· Potential silicate matrix effects on the carbon isotopic analyses have been investigated by measuring the mixtures of well-calibrated carbon reference materials and quartz powder.

· The calibration lines used to correct δ¹³C values of natural samples with low carbon content have been established by the measured raw values and the known values of reference materials mixing with quartz powder respectively, the carbon content of which compared with that of natural samples.

ABSTRACT

The precise and accurate analyses of minor carbon in silicate rocks can provide valuable insights into the origin of fluid and formation processes. The Elemental Analyzer-Isotope Ratio Mass Spectrometry (EA-IRMS) is a quick analytical method using small quantities of sample. In this study, EA-IRMS is applied to analyze carbon isotopic composition of trace carbon in silicate rock. Based on a series of tests, the key analytical parameters are confirmed. The normalization procedure and reference materials selection are as follows. ① Selection of standard materials with a wide carbon isotope composition range and reasonable carbon isotope distribution. Preparation of the mixtures of reference materials and super quality quartz power. ② A calibration curve was established using the measured values and certified values of the three reference materials similar to the samples. The measurement of natural samples is normalized to achieve an accurate determination of trace carbon content as low as 600 μg/g in silicate rocks and carbon isotopic composition. National standard material GBW04416 is used as an unknown sample to test the linear equations regressed with different contents. When the carbon content is no lower than 600 μg/g, the standard deviations are 0.02‰, 0.04‰, 0.05‰, -0.07‰, 0.11‰, respectively. For the mixture of MERCK and USGS24, the determined carbon isotopic composition and carbon content are comparable with the true value within analytic uncertainty. Therefore, the high precision and accuracy of carbon isotopic composition can be obtained for carbon content no less than 600 μg/g in 30 mg silicate rock. The carbon content of the sample was established based on the linear curve established by the peak area (peak intensity) of the standard mixture of different carbon contents and the corresponding content. Analytic uncertainty of carbon content of the sample is within 10%.
- elemental analyzer,
- carbon concentration,
- carbon isotope ratio,
- silicate rocks

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References (33)

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Precise Measurement of Carbon Concentration and Isotopic Ratios in Silicate Rocks by a High Sensitivity Elemental Analyzer Coupled with a Continuous Flow Isotope Mass Spectrometry

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