Highly Accurate Determination of the Delay Volume between the MALS and Differential Refractometer in SEC

  • MATSUMOTO Yoshinori
    Department of Organic Materials Science, Graduate School of Organic Materials Science, Yamagata University TOSOH ARC.
  • UEDA Kayo
    Department of Organic Materials Science, Graduate School of Organic Materials Science, Yamagata University
  • KASUGA Sho
    Department of Organic Materials Science, Graduate School of Organic Materials Science, Yamagata University
  • ENOMOTO Kazushi
    Institute for The Promotion of General Graduate Education, Yamagata University
  • KIKUCHI Moriya
    Faculty of Engineering, Yamagata University
  • NARUMI Atsushi
    Department of Organic Materials Science, Graduate School of Organic Materials Science, Yamagata University
  • KAWAGUCHI Seigou
    Department of Organic Materials Science, Graduate School of Organic Materials Science, Yamagata University

Bibliographic Information

Other Title
  • SECにおける多角度光散乱検出器と示差屈折率検出器との間の遅延体積の精密測定法

Abstract

<p>Size exclusion chromatography (SEC) equipped with a multi-angle light scattering (MALS) detector has widely been used as the standard analytical equipment for estimating the fundamental characteristics of polymers, such as the weight average molecular weight (Mw) and root-mean-squared radius of gyration. The interdetector delay volume (IDV) between the MALS and differential refractometer (RI) is an important parameter that strongly influences the reliability of the experimental value. However, a reliable determination method has not been published as yet. This paper reports a method for determining the IDV value with high reliability. SEC-MALS measurements were performed for polystyrene (PSt) standard with an Mw ranging from 1.0 × 104 to 110 × 104 at different flow rates (U) ranging from 0.1 to 1.0 cm3 min−1 to investigate the effects of U and Mw on IDV value. The band broadening effects within the SEC column are evaluated based on the van Deemter equation, and those occurring between the detectors are discussed. Reliable IDV values are obtained when the theoretical height of the column and the turbulence between the detectors are minimized. The SEC-MALS set up with the reliable IDV value accurately gives the absolute Mw and Mn and differential weight distribution curve for the PSt’s with the broad and narrow molecular weight distribution.</p>

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 71 (10.11), 579-588, 2022-10-05

    The Japan Society for Analytical Chemistry

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