Multi-wall carbon nanotube aqueous dispersion monitoring by using A4F-UV-MALS

In this work, the potentiality of asymmetrical flow field-flow fractionation (A4F) hyphenated to UV detector and multi-angle light scattering (MALS) was investigated for accurately determining multi-walled carbon nanotube (MWCNT) length and its corresponding dispersion state in aqueous medium. Fractionation key parameters were studied to obtain a method robust enough for heterogeneous sample characterization. The main A4F conditions were 10(-5) mL min(-1) NH(4)NO(3), elution flow of 1 mL min(-1), and cross flow of 2 mL min(-1). The recovery was found to be (94 ± 2)%. Online MALS analysis of eluted MWCNT suspension was performed to obtain length distribution. The length measurements were performed with a 4% relative standard deviation, and the length values were shown to be in accordance with expected ones. The capabilities of A4F-UV-MALS to size characterize various MWCNT samples and differentiate them according to their manufacturing process were evaluated by monitoring ball-milled MWCNT and MWCNT dispersions. The corresponding length distributions were found to be over 150-650 and 150-1,156 nm, respectively. A4F-UV-MALS was also used to evaluate MWCNT dispersion state in aqueous medium according to the surfactant concentration and sonication energy involved in the preparation of the dispersions. More especially, the presence or absence of aggregates, number and size of different populations, as well as size distributions were determined. A sodium dodecyl sulfate concentration of 15 to 30 mmol L(-1) and a sonication energy ranged over 20-30 kJ allow obtaining an optimal MWCNT dispersion. It is especially valuable for studying nanomaterials and checking their manufacturing processes, size characterization being always of high importance.