Chemometric determination of the length distribution of single walled carbon nanotubes through optical spectroscopy

Current synthesis methods for producing single walled carbon nanotubes (SWCNTs) do not ensure uniformity of the structure and properties, in particular the length, which is an important quality indicator of SWCNTs. As a result, sorting SWCNTs by length is an important post-synthesis processing step. For this purpose, convenient analysis methods are needed to characterize the length distribution rapidly and accurately. In this study, density gradient ultracentrifugation was applied to prepare length-sorted SWCNT suspensions containing individualized surfactant-wrapped SWCNTs. The length of sorted SWCNTs was first determined by atomic force microscope (AFM), and their absorbance was measured in ultraviolet–visible near-infrared (UV–vis-NIR) spectroscopy. Chemometric methods are used to calibrate the spectra against the AFM-measured length distribution. The calibration model enables convenient analysis of the length distribution of SWCNTs through UV–vis-NIR spectroscopy. Various chemometric techniques are investigated, including pre-processing methods and non-linear calibration models. Extended inverted signal correction, extended multiplicative signal correction and Gaussian process regression are found to provide good prediction of the length distribution of SWCNTs with satisfactory agreement with the AFM measurements. In summary, spectroscopy in conjunction with advanced chemometric techniques is a powerful analytical tool for carbon nanotube research.

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► Optical spectroscopy is used as a convenient tool to analyze the length distribution of single walled carbon nanotubes.
► Advanced multivariate chemometric methods are compared, and the best methods can satisfactorily predict the length distribution.
► The entire length distribution, not just the mean, is modelled and calibrated.