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Liquid chromatography at critical conditions (LCCC): Capabilities and limitations for polymer analysis

Molnar, Kristof and Helfer, Carin A. and Kaszas, Gabor and Krisch, Eniko and Chen, Dongjie and McKenna, Gregory B. and Kornfield, Julia A. and Puskas, Judit E. (2021) Liquid chromatography at critical conditions (LCCC): Capabilities and limitations for polymer analysis. Journal of Molecular Liquids, 322 . Art. No. 114956. ISSN 0167-7322. https://resolver.caltech.edu/CaltechAUTHORS:20201208-105039049

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Abstract

This paper investigates liquid chromatography at critical condition (LCCC) for polymer analysis. Based on controversial claims on the separation of cyclic polymers from linear analogues in the literature, the efficiency of LCCC for separation and purity analysis is questioned. Polyisobutylene (PIB) and poly(3,6-dioxa-1,8-octanedithiols) (polyDODT) were used for the study. The structure of low molecular weight cyclic and linear polyDODT was demonstrated by MALDI-ToF. NMR did not show the presence of thiol end groups in higher molecular weight PIB-disulfide and polyDODT samples, so they were considered cyclic polymers. When a low molecular weight polyDODT oligomer with only traces of cycles, as demonstrated by MALDI-ToF, was mixed with an M_n = 27 K g/mol cyclic sample, LCCC did not detect the presence of linear oligomers at 6 wt%. Based on the data presented here, it can be concluded that the LCCC method is not capable of measuring <6 wt% linear contamination so earlier claims for cyclic polystyrene (PS) samples purified by LCCC having <3% linear contaminants are questioned.


Item Type:Article
Related URLs:
URLURL TypeDescription
https://doi.org/10.1016/j.molliq.2020.114956DOIArticle
ORCID:
AuthorORCID
Molnar, Kristof0000-0002-5393-2130
Helfer, Carin A.0000-0003-4550-4942
McKenna, Gregory B.0000-0002-5676-9930
Kornfield, Julia A.0000-0001-6746-8634
Puskas, Judit E.0000-0001-5282-5256
Additional Information:© 2020 Published by Elsevier. Received 8 September 2020, Revised 27 October 2020, Accepted 2 December 2020, Available online 5 December 2020. The Authors would like to thank Dr. Prajakatta Mulay, Mauricio Azevedo de Freitas and Andres Munoz Salgado for their contribution to this work. This work was supported by the U.S. Department of Energy, Office of Science, Basic Energy Sciences under Award #DE-SC0018891. Author Contributions: Kristof Molnar – Investigation, formal analysis, Writing - Original Draft, Writing - Review & Editing Carin A. Helfer – Investigation, formal analysis, Writing - Original Draft, Gabor Kaszas - Investigation, formal analysis Eniko Krisch - Writing - Original Draft, Writing - Review & Editing, Visualization Dongjie Chen – Writing - Original Draft, Writing - Review & Editing Gregory B. McKenna – Writing - Original Draft, Writing - Review & Editing, Funding aquisition, Supervision Julia A. Kornfield - Writing - Original Draft, Writing - Review & Editing, Supervision, Funding aquisition, Judit E. Puskas - Writing - Original Draft, Writing - Review & Editing, Funding aquisition, Supervision.
Funders:
Funding AgencyGrant Number
Department of Energy (DOE)DE-SC0018891
Subject Keywords:Liquid chromatography; Sensitivity; Poly(3,6-dioxa-1,8-octanedithiol); Critical conditions; Polyisobutylene; Disulfide cyclic polymers
Record Number:CaltechAUTHORS:20201208-105039049
Persistent URL:https://resolver.caltech.edu/CaltechAUTHORS:20201208-105039049
Official Citation:Kristof Molnar, Carin A. Helfer, Gabor Kaszas, Eniko Krisch, Dongjie Chen, Gregory B. McKenna, Julia A. Kornfield, Judit E. Puskas, Liquid chromatography at critical conditions (LCCC): Capabilities and limitations for polymer analysis, Journal of Molecular Liquids, Volume 322, 2021, 114956, ISSN 0167-7322, https://doi.org/10.1016/j.molliq.2020.114956. (http://www.sciencedirect.com/science/article/pii/S0167732220371981)
Usage Policy:No commercial reproduction, distribution, display or performance rights in this work are provided.
ID Code:106967
Collection:CaltechAUTHORS
Deposited By: George Porter
Deposited On:09 Dec 2020 15:49
Last Modified:16 Dec 2020 19:13

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