UV-Vis quantification of the iron content in iteratively steam and HCl purified single-walled carbon nanotubes

PLoS One. 2024 May 10;19(5):e0303359. doi: 10.1371/journal.pone.0303359. eCollection 2024.

Abstract

As-produced carbon nanotubes contain impurities which can dominate the properties of the material and are thus undesired. Herein we present a multi-step purification treatment that combines the use of steam and hydrochloric acid in an iterative manner. This allows the reduction of the iron content down to 0.2 wt. % in samples of single-walled carbon nanotubes (SWCNTs). Remarkably, Raman spectroscopy analysis reveals that this purification strategy does not introduce structural defects into the SWCNTs' backbone. To complete the study, we also report on a simplified approach for the quantitative assessment of iron using UV-Vis spectroscopy. The amount of metal in SWCNTs is assessed by dissolving in HCl the residue obtained after the complete combustion of the sample. This leads to the creation of hexaaquairon(III) chloride which allows the determination of the amount of iron, from the catalyst, by UV-Vis spectroscopy. The main advantage of the proposed strategy is that it does not require the use of additional complexing agents.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Hydrochloric Acid* / chemistry
  • Iron* / analysis
  • Iron* / chemistry
  • Nanotubes, Carbon* / chemistry
  • Spectrophotometry, Ultraviolet*
  • Spectrum Analysis, Raman* / methods
  • Steam*

Substances

  • Nanotubes, Carbon
  • Iron
  • Hydrochloric Acid
  • Steam

Grants and funding

Ministerio de Ciencia e Innovación, PID2020-113805, Dr. Gerard Tobías-Rossell Ministerio de Ciencia e Innovación, CEX2019-000917-S European Commission, 290023, Dr. Gerard Tobías-Rossell.