2011Analytical ChemistryRequires access

A More Informative Approach for Characterization of Polymer Monolithic Phases: Small Angle Neutron Scattering/Ultrasmall Angle Neutron Scattering

Kathleen Ford, Brian G. Konzman, Judith F. Rubinson

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Abstract

Neutron scattering techniques have been used frequently to characterize geological specimens and to determine the structures of glasses and of polymers as solutions, suspensions, or melts. Little work has been reported on their application in determining polymers' structural properties relevant to separations. Here, we present a comparison of characterization results from nitrogen porosimetry and from combined small angle neutron scattering (SANS) and ultrasmall angle neutron scattering (USANS) experiments. We show that SANS is extremely sensitive to the pore characteristics. Both approaches can provide information about porosity and pore characteristics, but the neutron scattering techniques provide additional information in the form of the surface characteristics of the pores and their length scales. Fits of the scattering data show that cylindrical pores are present with diameters down to 0.6 μm and that, for length scales down to approxmately 20 Å, the material shows self-similar (fractal) slopes of -3.4 to -3.6. Comparison of these characteristics with other examples from the scattering literature indicate that further investigation of their meaning for chromatographic media is required.

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What this paper is about

Neutron scattering techniques have been used frequently to characterize geological specimens and to determine the structures of glasses and of polymers as solutions, suspensions, or melts. Little work has been reported on their application in determining polymers' structural properties relevant to separations. Here, we present a comparison of characterization results from nitrogen porosimetry and from combined small angle neutron scattering (SANS) and ultrasmall angle neutron scattering (USANS) experiments. We show that SANS is extremely sensitive to the pore characteristics. Both approaches can provide information about porosity and pore characteristics, but the neutron scattering techniques provide additional information in the form of the surface characteristics of the pores and their length scales. Fits of the scattering data show that cylindrical pores are present with diameters down to 0.6 μm and that, for length scales down to approxmately 20 Å, the material shows self-similar (fractal) slopes of -3.4 to -3.6. Comparison of these characteristics with other examples from the scattering literature indicate that further investigation of their meaning for chromatographic media is required.

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Available abstract

Neutron scattering techniques have been used frequently to characterize geological specimens and to determine the structures of glasses and of polymers as solutions, suspensions, or melts. Little work has been reported on their application in determining polymers' structural properties relevant to separations. Here, we present a comparison of characterization results from nitrogen porosimetry and from combined small angle neutron scattering (SANS) and ultrasmall angle neutron scattering (USANS) experiments. We show that SANS is extremely sensitive to the pore characteristics. Both approaches can provide information about porosity and pore characteristics, but the neutron scattering techniques provide additional information in the form of the surface characteristics of the pores and their length scales. Fits of the scattering data show that cylindrical pores are present with diameters down to 0.6 μm and that, for length scales down to approxmately 20 Å, the material shows self-similar (fractal) slopes of -3.4 to -3.6. Comparison of these characteristics with other examples from the scattering literature indicate that further investigation of their meaning for chromatographic media is required.

Key concepts: Chemistry, Small-angle neutron scattering, Neutron scattering, Characterization (materials science), Small-angle scattering, Scattering, Neutron, Neutron reflectometry

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