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CO2 quantification in silicate glasses using μ-ATR FTIR spectroscopy

  • Maximilian Schanofski , Lennart Koch and Burkhard C. Schmidt
Published/Copyright: July 10, 2023
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American Mineralogist
From the journal American Mineralogist Volume 108 Issue 7

Abstract

A new method for measurements of high-CO2 concentrations in silicate glasses was established using micro–attenuated total reflectance (μ-ATR) Fourier transform infrared (FTIR) spectroscopy in the mid-IR (MIR) region. We studied two glass/melt compositions, namely leucitite and granite, to cover samples in which CO2 is dissolved as carbonate ions C O 3 2 − or as CO2 molecules C O 2 m o l . In the 3 leucitite glasses a carbonate absorption doublet with maxima at 1510 and 1430 cm–1 has shown to clearly separate from aluminosilicate lattice vibrations at lower wavenumbers. Due to the lower sensitivity of the μ-ATR method, we were able to measure high-CO2 contents c C O 2 > 0.5 w t % in experimental silicate glasses that would only be measurable with great dificulties using established transmission MIR measurements due to detector linearity limit efects even with very thin sample wafers. The peak heights of the 1430 cm–1 ATR band (A1430), normalized to the integral of the T-O lattice vibrations (T = Si, Al, Fe) at about 930 cm–1 (Int930) show a linear trend with CO2 contents in the range 0.2–4.3 wt%, yielding a linear correlation with cCO2 (wt%) = 0.4394 ± 0.006·A1430·10000/Int930. The normalization of the CO2 related band to a lattice vibration accounts for variations in the quality of contact between ATR crystal and sample, which has a direct effect on signal intensity.

In granitic glasses, where CO2 is dissolved as C O 2 m o l only, the asymmetric stretching vibration at 2350 cm–1 overlaps with the signal of atmospheric, gaseous CO2. As the ATR signal of dissolved CO2 is very weak, the atmospheric signal may dominate the spectrum. Since the absorbance spectrum is calculated by division of the single-channel sample spectrum by a single-channel reference spectrum measured in air, keeping the laboratory and spectrometer atmosphere as constant as possible during spectral acquisition can resolve the problem. Nonetheless, a procedure to subtract the signal of remaining atmospheric CO2 may still be required for the spectral evaluation. We studied a series of 5 granitic glasses with C O 2 m o l contents of 0.08 to 0.27 wt% and found an excellent linear relation between CO2 concentration and lattice vibration normalized ATR intensity of the 2350 cm–1 band: c C O 2 ( w t % ) = 0.2632 ± 0.0016·A2350·10000/Int990. Although the C O 2 m o l concentrations in our granitic glass series can still be analyzed without major difficulties by conventional transmission IR spectroscopy, our data demonstrate the potential of the ATR method for samples with higher CO2 contents or for samples where a high spatial resolution is required (melt inclusions, vesicular or partially crystallized glasses). The lower limits of the ATR method are approximately 0.2 wt% CO2 dissolved as carbonate groups or 0.1 wt% CO2 (or slightly less) dissolved in molecular form.

Keywords: ATR-micro spectroscopy; ATR FTIR; silicate glasses; carbon dioxide; CO2 quantification; CO2

Acknowledgments and Funding

The critical comments of Giada Iacono-Marziano and two other anonymous reviewers as well as from the associate editor Yann Morizet greatly improved the manuscript. We also thank Yann Morizet for the editorial handling. This research has been partly supported by the Deutsche Forschungsgemeinschaft research Grant FA 1477/1-1.

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Received: 2022-02-03
Accepted: 2022-08-24
Published Online: 2023-07-10
Published in Print: 2023-07-26

© 2023 by Mineralogical Society of America

Articles in the same Issue

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  11. Feiite: Synthesis, stability, and implications for its formation conditions in nature
  12. Thermal equation of state of Fe3O4 magnetite up to 16 GPa and 1100 K
  13. UHP eclogite from western Dabie records evidence of polycyclic burial during continental subduction
  14. CO2 quantification in silicate glasses using μ-ATR FTIR spectroscopy
  15. Local structure determination of Zn-smectite
  16. A new UHP unit in the Western Alps: First occurrence of coesite from the Monviso Massif (Italy)
  17. Mineral evolution and mineral niches of ammonium sulfates: The case of Pastora mine, Aliseda, Spain
  18. Discrete late Jurassic Sn mineralizing events in the Xianghualing Ore District, South China: Constraints from cassiterite and garnet U-Pb geochronology
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https://doi.org/10.2138/am-2022-8477
Keywords for this article
ATR-micro spectroscopy; ATR FTIR; silicate glasses; carbon dioxide; CO2 quantification; CO2

Articles in the same Issue

  1. On the origin of fluorine-poor apatite in chondrite parent bodies
  2. Fluorine behavior during experimental muscovite dehydration melting and natural partitioning between micas: Implications for the petrogenesis of peraluminous leucogranites and pegmatites
  3. Telescoped boiling and cooling mechanisms triggered hydrothermal stibnite precipitation: Insights from the world’s largest antimony deposit in Xikuangshan China
  4. MSA Distinguished Lecturer Series Correlations between cathodoluminescence intensity and aluminum concentration in low-temperature hydrothermal quartz
  5. Behavior of hydrogen defect and framework of Fe-bearing wadsleyite and ringwoodite at high temperature and high pressure
  6. What is mineral informatics?
  7. Metal source and hydrothermal evolution of the Jiaoxi quartz vein-type tungsten deposit (Tibet): Insights from textural and compositional variations of wolframite and scheelite
  8. Geochemical processes and mechanisms for cesium enrichment in a hot-spring system
  9. Identifying xenocrystic tourmaline in Himalayan leucogranites
  10. Contrasting alteration textures and geochemistry of allanite from uranium-fertile and barren granites: Insights into granite-related U and ion-adsorption REE mineralization
  11. Feiite: Synthesis, stability, and implications for its formation conditions in nature
  12. Thermal equation of state of Fe3O4 magnetite up to 16 GPa and 1100 K
  13. UHP eclogite from western Dabie records evidence of polycyclic burial during continental subduction
  14. CO2 quantification in silicate glasses using μ-ATR FTIR spectroscopy
  15. Local structure determination of Zn-smectite
  16. A new UHP unit in the Western Alps: First occurrence of coesite from the Monviso Massif (Italy)
  17. Mineral evolution and mineral niches of ammonium sulfates: The case of Pastora mine, Aliseda, Spain
  18. Discrete late Jurassic Sn mineralizing events in the Xianghualing Ore District, South China: Constraints from cassiterite and garnet U-Pb geochronology
  19. Ryabchikovite, CuMg(Si2O6), a new pyroxene group mineral, and some genetic features of natural anhydrous copper silicates
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