Issue 10, 2020

Insights into the internal structures of nanogels using a versatile asymmetric-flow field-flow fractionation method

Abstract

Poly(N-isopropylacrylamide) (pNIPAM) nanogels are a highly researched type of colloidal material. In this work, we establish a versatile asymmetric-flow field-flow fractionation (AF4) method that can provide high resolution particle sizing and also structural information on nanogel samples from 65–310 nm in hydrodynamic diameter and so different chemical compositions. To achieve this online multi-angle light scattering and dynamic light scattering detectors were used to provide measurement of the radius of gyration (Rg) and hydrodynamic radius (Rh) respectively. Two different eluents and a range of cross-flows were evaluated in order to provide effective fractionation and high recovery for the different nanogel samples. We found that using 0.1 M NaNO3 as the eluent and an initial cross-flow of 1 mL min−1 provided optimal separation conditions for all samples tested. Using this method, we analysed two types of samples, pNIPAM nanogels prepared by free radical dispersion polymerisation with increasing diameters and analysed poly(acrylic acid)-b-pNIPAM crosslinked nanogels prepared by reversible addition–fragmentation chain transfer dispersion polymerisation. We could determine that the differently sized free radical nanogels possessed differing internal structures; shape factors (Rg/Rh) ranged from 0.58–0.73 and revealed that the smallest nanogel had a homogeneous internal crosslinking density, while the larger nanogels had a more densely crosslinked core compared to the shell. The poly(acrylic acid)-b-pNIPAM crosslinked nanogels displayed clear core–shell structures due to all the crosslinking being contained in the core of the nanogel.

Graphical abstract: Insights into the internal structures of nanogels using a versatile asymmetric-flow field-flow fractionation method

Supplementary files

Article information

Article type
Paper
Submitted
21 Apr 2020
Accepted
17 Aug 2020
First published
18 Aug 2020
This article is Open Access
Creative Commons BY license

Nanoscale Adv., 2020,2, 4713-4721

Insights into the internal structures of nanogels using a versatile asymmetric-flow field-flow fractionation method

E. Niezabitowska, A. R. Town, B. Sabagh, M. D. Morales Moctezuma, V. R. Kearns, S. G. Spain, S. P. Rannard and T. O. McDonald, Nanoscale Adv., 2020, 2, 4713 DOI: 10.1039/D0NA00314J

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