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<p>Solvent gradient interaction chromatography (SGIC) coupled to size exclusion chromatography (SEC), commonly referred to as 2D-LC, typically provides Three-dimensional data. Represented as contour plots, one axis shows the variation in molar mass (MM), and the other axis shows the comonomer (CM) content, while the detector intensity is color-coded. Currently, however, the accuracy of these systems is limited and provides only a qualitative understanding of these plots. In our previous work, we developed a single-sample integral calibration (SSIC) to mitigate current limitations and improve the accuracy of the molar mass measurements for metallocene-catalyzed polyethylene (mPE). In this current work, we addressed converting SGIC elution volumes (EV) to comonomer content across the molar mass distribution (MMD) of mPE samples using SEC-IR5 data as the calibrant.</p><p>Our results showed that a linear calibration of the SGIC EV axis can be achieved for a single sample using 2D-LC data acquired for the whole polymer, independent of branch type, CM content, or skewness of the CM distribution (CMD). Moreover, the same methodology was used to calibrate the CM content at each MM slice (and concurrently for each SGIC fraction) for the 2D-LC analysis of a 1-butene mPE copolymer. Furthermore, we showed that the resulting contour plot was successfully calibrated to &lt; 0.5&#xa0;mol% CM content for &gt; 95% of the MMD, and numerical matrix data had an estimated quantitation limit for MM (<i>z</i> axis) of ~ 2 wt.%. Using these calibration methods now allows us to evaluate 2D-LC data using statistical methods to better understand the SGIC separation process and to predict physical properties.</p>

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The Use of SEC-IR for Modeling and Calibrating the Comonomer Content from the 2D-LC Analysis Across the Molar Mass Distributions of LLDPE Samples

  • 期刊论文

  • 发表日期：

    2026年2月11日

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  • Paul DesLauriers,
  • Jan-Hendrik Arndt,
  • Guru Geertz,
  • Subrajeet Deshmukh,
  • Robert Brüll

摘要

Solvent gradient interaction chromatography (SGIC) coupled to size exclusion chromatography (SEC), commonly referred to as 2D-LC, typically provides Three-dimensional data. Represented as contour plots, one axis shows the variation in molar mass (MM), and the other axis shows the comonomer (CM) content, while the detector intensity is color-coded. Currently, however, the accuracy of these systems is limited and provides only a qualitative understanding of these plots. In our previous work, we developed a single-sample integral calibration (SSIC) to mitigate current limitations and improve the accuracy of the molar mass measurements for metallocene-catalyzed polyethylene (mPE). In this current work, we addressed converting SGIC elution volumes (EV) to comonomer content across the molar mass distribution (MMD) of mPE samples using SEC-IR5 data as the calibrant.

Our results showed that a linear calibration of the SGIC EV axis can be achieved for a single sample using 2D-LC data acquired for the whole polymer, independent of branch type, CM content, or skewness of the CM distribution (CMD). Moreover, the same methodology was used to calibrate the CM content at each MM slice (and concurrently for each SGIC fraction) for the 2D-LC analysis of a 1-butene mPE copolymer. Furthermore, we showed that the resulting contour plot was successfully calibrated to < 0.5 mol% CM content for > 95% of the MMD, and numerical matrix data had an estimated quantitation limit for MM (z axis) of ~ 2 wt.%. Using these calibration methods now allows us to evaluate 2D-LC data using statistical methods to better understand the SGIC separation process and to predict physical properties.