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Comprehensive Analysis of Oxidized Waxes by Solvent and Thermal Gradient Interaction Chromatography and Two-Dimensional Liquid Chromatography

Cite this: Anal. Chem. 2018, 90, 12, 7626–7634
Publication Date (Web):May 29, 2018
https://doi.org/10.1021/acs.analchem.8b01480
Copyright © 2018 American Chemical Society
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    Abstract

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    This report addresses the comprehensive analysis of oxidized/functionalized polyethylene waxes according to chemical composition and molar mass by selective chromatographic methods. For the first time, tailored high-temperature interaction chromatography in solvent gradient (HT-SGIC) and thermal gradient (HT-TGIC) modes are used for the chemical composition separation of these materials. Separation protocols are developed using three model wax samples with different degrees of oxidation. For the chromatographic separations polar silica gel is used as the stationary phase. Solvent gradients of decane and cyclohexanone are used in HT-SGIC at 110 °C to separate the bulk waxes into several heterogeneous fractions according to polarity and the type of functionality. Column temperature and gradient manipulation are shown to influence chromatographic resolution and retention. The HT-SGIC investigations are complemented by HT-TGIC separations where a solvent mixture of decane and cyclohexanone is used as the mobile phase in isocratic mode. It is shown that HT-SGIC and HT-TGIC provide different types of separation, however, both are predominantly based on differences in functionality. To provide comprehensive information on chemical composition (functionality) and molar mass, HT-SGIC and HT-TGIC are coupled to HT-SEC, using ortho-dichlorobenzene as the second dimension mobile phase. Clear differences between oxidized and nonoxidized waxes are detected in HT-2D-LC providing comprehensive information on the molecular heterogeneity of these materials.

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    The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.analchem.8b01480.

    • Detailed experimental methods for size exclusion chromatography, Fourier-transform Infrared spectroscopy, differential scanning calorimetry, crystallization analysis fractionation, diagram of temperature profile and flow rate used in TGIC, bulk analyses of the three waxes by DSC, CRYSTAF and SEC, tabular information for peak elution volumes and peak areas of wax No. 3 as influenced by column temperature, and peak area comparisons of wax Nos. 1, 2, and 3, ATR-FT-IR spectra of wax Nos. 1, 2, and 3, HT-SGIC-FT-IR, and HT-TGIC-FT-IR analysis of wax No. 3 (PDF)

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    Cited By

    This article is cited by 10 publications.

    1. David M. Meunier, James H. Wade, Miroslav Janco, Rongjuan Cong, Wei Gao, Yongfu Li, Dibyaranjan Mekap, Grace Wang. Recent Advances in Separation-Based Techniques for Synthetic Polymer Characterization. Analytical Chemistry 2021, 93 (1) , 273-294. https://doi.org/10.1021/acs.analchem.0c04352
    2. Laura Plüschke, Anthony Ndiripo, Robert Mundil, Jan Merna, Harald Pasch, Albena Lederer. Unraveling Multiple Distributions in Chain Walking Polyethylene Using Advanced Liquid Chromatography. Macromolecules 2020, 53 (10) , 3765-3777. https://doi.org/10.1021/acs.macromol.0c00314
    3. Anthony Ndiripo, Andreas Albrecht, Harald Pasch. Advanced Liquid Chromatography of Polyolefins Using Simultaneous Solvent and Temperature Gradients. Analytical Chemistry 2020, 92 (10) , 7325-7333. https://doi.org/10.1021/acs.analchem.0c01095
    4. Bob W. J. Pirok, Dwight R. Stoll, Peter J. Schoenmakers. Recent Developments in Two-Dimensional Liquid Chromatography: Fundamental Improvements for Practical Applications. Analytical Chemistry 2019, 91 (1) , 240-263. https://doi.org/10.1021/acs.analchem.8b04841
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    6. Laura Plüschke, Anthony Ndiripo, Robert Mundil, Jan Merna, Harald Pasch, Albena Lederer. Fractionation of chain walking polyethylene and elucidation of branching, conformation and molar mass distributions. International Journal of Polymer Analysis and Characterization 2021, 26 (1) , 47-59. https://doi.org/10.1080/1023666X.2020.1840865
    7. Muhammad Imran Malik, Harald Pasch. Characterization of polyolefins. 2021, 173-222. https://doi.org/10.1016/B978-0-12-819768-4.00016-6
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    9. Anthony Ndiripo, M.-M. Pornwilard, Thipphaya Pathaweeisariyakul, Harald Pasch. Multidimensional chromatographic analysis of carboxylic acid-functionalized polyethylene. Polymer Chemistry 2019, 10 (43) , 5859-5869. https://doi.org/10.1039/C9PY01191A
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