Aqueous SEC–MALS Characterization of Hydrophilic Azolium-Based Poly(ionic liquid)s in Their Native Halide Form

Abstract

The molar-mass characterization of hydrophilic poly(ionic liquid)s (PILs) is challenging due to strong polymer–column interactions and low refractive-index contrast, which limit detector sensitivity. To address these limitations, we analyzed five imidazolium-based PILs using both aqueous and organic (THF/LiTFSI) size-exclusion chromatography (SEC) with polystyrene calibration or multi-angle light-scattering detection (SEC-MALS). In THF/LiTFSI, the low dn/dc values compromised sensitivity, hindering reliable molar-mass determination. We therefore screened various aqueous mobile phases to identify optimal elution conditions. Among those tested, 0.3 M formic acid yielded well-resolved polymer peaks for all five PILs, with significantly higher dn/dc values than THF/LiTFSI. Mass recoveries ranged from 60.5% to 78.5%, enabling accurate molarmass determination. The method was also qualitatively validated for poly(vinylimidazole), partially quaternized poly(vinylimidazole), and a poly(thiazolium). Overall, aqueous SEC with 0.3 M formic acid emerges as a simple, general, and efficient alternative for the SECMALS characterization of hydrophilic azolium-based homo- and co-PILs. Unlike organic SEC, this approach requires no prior counteranion exchange, thus streamlining the analytical workflow.

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BibTeX RIS

BibTeX

@misc{xu2026aqueous,
  title = {{Aqueous SEC–MALS Characterization of Hydrophilic Azolium-Based Poly(ionic liquid)s in Their Native Halide Form}},
  author = {Zhengxin Xu and Christophe Velour and Sylvain Bourasseau and Christophe Schatz and Joan Vignolle},
  howpublished = {ChemRxiv},
  year = {2026},
  month = oct,
  doi = {10.26434/chemrxiv.15010921/v1},
  url = {https://chemrxiv.org/doi/full/10.26434/chemrxiv.15010921/v1},
  note = {CC BY},
}

RIS

TY  - UNPB
TI  - Aqueous SEC–MALS Characterization of Hydrophilic Azolium-Based Poly(ionic liquid)s in Their Native Halide Form
AU  - Zhengxin Xu
AU  - Christophe Velour
AU  - Sylvain Bourasseau
AU  - Christophe Schatz
AU  - Joan Vignolle
PY  - 2026
DA  - 2026/10/22
PB  - ChemRxiv
DO  - 10.26434/chemrxiv.15010921/v1
UR  - https://chemrxiv.org/doi/full/10.26434/chemrxiv.15010921/v1
AB  - The molar-mass characterization of hydrophilic poly(ionic liquid)s (PILs) is challenging due to strong polymer–column interactions and low refractive-index contrast, which limit detector sensitivity. To address these limitations, we analyzed five imidazolium-based PILs using both aqueous and organic (THF/LiTFSI) size-exclusion chromatography (SEC) with polystyrene calibration or multi-angle light-scattering detection (SEC-MALS). In THF/LiTFSI, the low dn/dc values compromised sensitivity, hindering reliable molar-mass determination. We therefore screened various aqueous mobile phases to identify optimal elution conditions. Among those tested, 0.3 M formic acid yielded well-resolved polymer peaks for all five PILs, with significantly higher dn/dc values than THF/LiTFSI. Mass recoveries ranged from 60.5% to 78.5%, enabling accurate molarmass determination. The method was also qualitatively validated for poly(vinylimidazole), partially quaternized poly(vinylimidazole), and a poly(thiazolium). Overall, aqueous SEC with 0.3 M formic acid emerges as a simple, general, and efficient alternative for the SECMALS characterization of hydrophilic azolium-based homo- and co-PILs. Unlike organic SEC, this approach requires no prior counteranion exchange, thus streamlining the analytical workflow.
ER  -

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