Characterisation and determination of fullerenes: A critical review

Abstract

Highlights Methodologies for fullerene aggregate characterization are discussed.  Chromatographic and electrophoretic techniques for fullerene analysis are presented.  Accurate identification and detection of fullerenes by LC-MS is critically reviewed. Graphical abstract AbstractA prominent sector of nanotechnology is occupied by a class of carbon-based nanoparticles known as fullerenes. Fullerene particle size and shape impact in how easily these particles are transported into and throughout the environment and living tissues. Currently, there is a lack of adequate methodology for their size and shape characterisation, identification and quantitative detection in environmental and biological samples. The most commonly used methods for their size measurements (aggregation, size distribution, shape, etc.), the effect of sampling and sample treatment on these characteristics and the analytical methods proposed for their determination in complex matrices are discussed in this review. For the characterisation and analysis of fullerenes in real samples, different analytical techniques including microscopy, spectroscopy, flow field-flow fractionation, electrophoresis, light scattering, liquid chromatography and mass spectrometry have been reported. The existing limitations and knowledge gaps in the use of these techniques are discussed and the necessity to hyphenate complementary ones for the accurate characterisation, identification and quantitation of these nanoparticles is highlighted.

Basic hydrolysis of fullerene-based esters: a tiny step away from nucleophilic addition to fullerene

“…Namely, although LC-MS methods are a powerful tool for the quantization of fullerenes in complex samples, these techniques alone cannot provide detailed qualitative information. 25 Due to the presence of six malonic addends on the C 60 skeleton, one may expect that the number of -OH groups will be smaller than in the case of pure fullerenol (i.e., 26). 19 Furthermore, the presence of residual water molecules and possible partial decarboxylation 9 additionally increases uncertainty of the molecular mass calculations from the measured hydrogen quantity.…”

Towards better understanding of C60organosols

“…[8][9][10][11][12][13][14] While in low-polar aromatic solvents, fullerenes are well solvated and relatively well dissolved, 14,15 in water they generate hydrosols and suspensions. 5,11,[16][17][18][19][20][21][22][23][24][25][26][27][28][29][30] In highly polar organic solvents, the molecular solubility of fullerenes is negligible, 14,15 but they readily form colloidal solutions. [9][10][11][12][13][14][31][32][33][34][35] The state of fullerenes, either molecular or colloidal, in the so-called 'good' or 'strong' solvents, such as CS 2 , toluene, and benzene, is still a matter of discussion.…”

Nanomaterials as stationary phases and supports in liquid chromatography

“…A number of nanomaterials have been explored for use as supports and stationary phases in column, capillary or planar LC methods. As is indicated in Table , both carbon‐based nanomaterials and inorganic nanomaterials have been used in LC applications . Much of this work was been done through the use of columns, however, nanomaterials have also been employed in packed capillaries and in planar techniques such as thin‐layer chromatography (TLC) and ultrathin‐layer chromatography (UTLC) (see Sections –).…”

“…The figures shown for the inorganic nanomaterials are (top) nanostructured columns coated with a material such as aluminum oxide and (bottom) gold nanoparticles coated on graphene‐modified silica. These figures were adapted with permission from .…”