Quantification of diffusion coefficient distribution (DCD) and correlation with molecular weight distribution (MWD) of polymers is still an issue in pulsed field-gradient nuclear magnetic resonance (PFG-NMR). The conventional scaling law utilized so far to relate diffusion coefficient and molecular weight only holds true for the determination of MWD at sufficiently low concentrations. To extend measurement limits and to get a good signal-to-noise ratio, an exponential correlation is introduced to describe the effect of polymer concentration on diffusion in PFG-NMR. Two model polymers (polystyrene and poly(methyl methacrylate)) dissolved in deuterated chloroform are studied at different concentrations in the range of 0.16-8 wt%. The DCDs are determined by modeling the measured signal attenuation with three methods (gamma distribution, log normal distribution, and tailored norm regularization). It is shown that the proposed method applies to the PFG-NMR measurements on polymer solutions over a wide concentration range, providing almost the same MWDs as those obtained at low concentrations. The MWDs retrieved from NMR experiments agree well with those by size exclusion chromatography.
We present a study of the radial structure of a spherical polyelectrolyte brushes by anomalous small-angle X-ray scattering. The spherical polyelectrolyte brushes consist of a solid poly(styrene) core of ca. 100 nm diameter onto which long linear chains of poly(acrylic acid) (PAA) are densely grafted. A sufficiently high pH, these polyelectrolyte chains are fully charged. Rubidium ions are used as counterions because their adsorption edge (15 199.6 eV) can be conventiently reached by synchrotron radiation. By performing small-angle X-ray scattering studies at different energies of the incident radiation, the contribution of the Rb + counterions can be analyzed separately. The scattering contribution of the counterions can be derived and compared to the scattering intensity of the entire particle. The distributions of the macro-ion and of the counterions are shown to be very similiar. This shows that the counterions must be confined within the brush.
A newly developed high frequency spark provides a green, sustainable and versatile platform for manufacturing diverse sub-10 nm particles with well-defined chemical composition that serve as key building blocks.
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