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Two-Dimensional Liquid Chromatography Analysis of Polystyrene/Polybutadiene Block Copolymers

  • Sanghoon Lee
    Sanghoon Lee
    Division of Advanced Materials Science and Department of Chemistry, Pohang University of Science and Technology (POSTECH), Pohang, 37673, Korea
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    Orcidhttp://orcid.org/0000-0002-8367-1787
  • , 
  • Heejae Choi
    Heejae Choi
    Division of Advanced Materials Science and Department of Chemistry, Pohang University of Science and Technology (POSTECH), Pohang, 37673, Korea
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  • , 
  • Taihyun Chang*
    Taihyun Chang
    Division of Advanced Materials Science and Department of Chemistry, Pohang University of Science and Technology (POSTECH), Pohang, 37673, Korea
    *Tel.: +82-54-279-2787. Fax: +82-54-279-3399. E-mail: [email protected]
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    Orcidhttp://orcid.org/0000-0003-2623-1803
  • , and 
  • Bastiaan Staal
    Bastiaan Staal
    Competence Center Analytics, BASF SE, Ludwigshafen, 67056, Germany
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Cite this: Anal. Chem. 2018, 90, 10, 6259–6266
Publication Date (Web):April 20, 2018
https://doi.org/10.1021/acs.analchem.8b00913
Copyright © 2018 American Chemical Society
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    Abstract

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    A detailed characterization of a commercial polystyrene/polybutadiene block copolymer material (Styrolux) was carried out using two-dimensional liquid chromatography (2D-LC). The Styrolux is prepared by statistical linking reaction of two different polystyrene-block-polybutadienyl anion precursors with a multivalent linking agent. Therefore, it is a mixture of a number of branched block copolymers different in molecular weight, composition, and chain architecture. While individual LC analysis, including size exclusion chromatography, interaction chromatography, or liquid chromatography at critical condition, is not good enough to resolve all the polymer species, 2D-LC separations coupling two chromatography methods were able to resolve all polymer species present in the sample; at least 13 block copolymer species and a homopolystyrene blended. Four different 2D-LC analyses combining a different pair of two LC methods provide their characteristic separation results. The separation characteristics of the 2D-LC separations are compared to elucidate the elution characteristics of the block copolymer species.

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    The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.analchem.8b00913.

    • Figure S1: Overlap-injection of the second-D SEC. Figure S2: LCCC analyses of the Styrolux for second-D LCCC. Figure S3: SEC chromatogram of the Styrolux fractions. Figure S4: RP-TGIC chromatogram of the Styrolux fractions. Table S1: SEC-light scattering analysis results of the Styrolux fractions (PDF).

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