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Coupled thermogravimetry, mass spectrometry, and infrared spectroscopy for quantification of surface functionality on single-walled carbon nanotubes

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Abstract

We have successfully applied coupled thermogravimetry, mass spectrometry, and infrared spectroscopy to the quantification of surface functional groups on single-walled carbon nanotubes. A high-purity single-walled carbon nanotube sample was subjected to a rapid functionalization reaction that attached butyric acid moieties to the nanotube sidewalls. This sample was then subjected to thermal analysis under inert desorption conditions. Resultant infrared and mass spectrometric data were easily utilized to identify the desorption of the butyric acid groups across a narrow temperature range and we were able to calculate the degree of substitution of the attached acid groups within the nanotube backbone as 1.7 carbon atoms per hundred, in very good agreement with independent analytical measurements made by inductively coupled plasma optical emission spectrometry (ICP-OES). The thermal analysis technique was also able to discern the presence of secondary functional moieties on the nanotube samples that were not accessible by ICP-OES. This work demonstrates the potential of this technique for assessing the presence of multiple and diverse functional addends on the nanotube sidewalls, beyond just the principal groups targeted by the specific functionalization reaction.

3D contour map of the FTIR spectra of the species desorbed from the GAP-functionalized SWCNT sample as a function of temperature.

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Authors and Affiliations

  1. Molecular and Nanomaterial Architectures Group, Steacie Institute for Molecular Sciences, National Research Council Canada, Ottawa, ON, K1A 0R6, Canada

    Christopher T. Kingston, Yadienka Martínez-Rubí, Jingwen Guan, Michael Barnes & Benoit Simard

  2. Chemical Metrology Group, Institute for National Measurement Standards, National Research Council Canada, Ottawa, ON, K1A 0R6, Canada

    Christine Scriver & Ralph E. Sturgeon

Authors
  1. Christopher T. Kingston
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  2. Yadienka Martínez-Rubí
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  3. Jingwen Guan
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  4. Michael Barnes
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  5. Christine Scriver
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  6. Ralph E. Sturgeon
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  7. Benoit Simard
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Correspondence to Christopher T. Kingston.

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Kingston, C.T., Martínez-Rubí, Y., Guan, J. et al. Coupled thermogravimetry, mass spectrometry, and infrared spectroscopy for quantification of surface functionality on single-walled carbon nanotubes. Anal Bioanal Chem 396, 1037–1044 (2010). https://doi.org/10.1007/s00216-009-3205-y

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  • DOI: https://doi.org/10.1007/s00216-009-3205-y

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