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Updated: Jun 1, 2026

Characterization of Synthetic Polymers via Matrix Assisted Laser Desorption Ionization Time of Flight (MALDI-TOF) Mass Spectrometry
Published on: June 10, 2018
Polymer Analysis by Liquid Chromatography/Electrospray Ionization Time-of-Flight Mass Spectrometry
1General Analytical and Environmental Chemistry Department, Akzo Nobel Central Research, P.O. Box 9300, 6800 SB Arnhem, The Netherlands.
Combining liquid chromatography (LC) with mass spectrometry (MS) offers detailed polymer analysis. This study explores size-exclusion chromatography (SEC/MS), gradient polymer elution chromatography (GPEC/MS), and liquid chromatography at the critical point of adsorption (LCCC/MS) for polymer characterization.
Area of Science:
- Polymer Chemistry
- Analytical Chemistry
- Chromatography
Background:
- Polymer analysis requires both structural and quantitative data.
- Traditional methods may lack comprehensive characterization capabilities.
- Hyphenated techniques offer enhanced analytical power.
Purpose of the Study:
- To investigate the combined use of three liquid chromatography (LC) modes with electrospray ionization orthogonal acceleration time-of-flight mass spectrometry (ESI-oa-TOF-MS) for polymer analysis.
- To demonstrate the capabilities of SEC/MS, GPEC/MS, and LCCC/MS in characterizing polymer structure and composition.
- To highlight the advantages of time-of-flight mass analyzers in polymer science.
Main Methods:
- Interfacing size-exclusion chromatography (SEC) with ESI-oa-TOF-MS (SEC/MS).
- Interfacing gradient polymer elution chromatography (GPEC) with ESI-oa-TOF-MS (GPEC/MS).
- Interfacing liquid chromatography at the critical point of adsorption (LCCC) with ESI-oa-TOF-MS (LCCC/MS).
Main Results:
- SEC/MS enabled absolute mass calibration and determination of monomers and end groups.
- GPEC/MS provided detailed insights into polymer chemical heterogeneity and oligomer composition.
- LCCC/MS demonstrated that retention is governed by chemical heterogeneities, facilitating quantitative end group analysis.
Conclusions:
- The hyphenation of LC techniques with ESI-oa-TOF-MS provides powerful tools for comprehensive polymer analysis.
- Each LC mode (SEC/MS, GPEC/MS, LCCC/MS) offers unique advantages for structural and quantitative characterization.
- Time-of-flight mass spectrometry significantly benefits polymer analysis by providing detailed structural information.
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