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Characterization of Synthetic Polymers via Matrix Assisted Laser Desorption Ionization Time of Flight MALDI-TOF Mass Spectrometry
Published on: June 10, 2018
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Matrix-assisted laser desorption/ionization sample preparation optimization for structural characterization of
Evgenia Tisdale1, Devin Kennedy1, Xiaodong Xu
1University of Arkansas, Department of Chemistry and Biochemistry, 119 Chemistry Building, Fayetteville, AR 72701, United States.
Analytica Chimica Acta
|December 28, 2013
Summary
Optimized matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) enables detailed characterization of poly(styrene-co-pentafluorostyrene) copolymers. Styrene monomer distribution is more sensitive to catalyst changes than pentafluorostyrene distribution.
Area of Science:
- Polymer Chemistry
- Analytical Chemistry
- Mass Spectrometry
Background:
- Poly(styrene-co-pentafluorostyrene) copolymers are synthesized via atom transfer radical polymerization.
- Accurate characterization of copolymer composition and molecular weight distribution is crucial for understanding structure-property relationships.
Purpose of the Study:
- To optimize sample preparation parameters for MALDI-TOF MS analysis of these copolymers.
- To apply the optimized method for detailed characterization of synthesized copolymers.
- To investigate the sensitivity of monomer distribution to polymerization conditions.
Main Methods:
- Investigated sample preparation parameters: matrix choice, matrix:analyte ratio, and salt:analyte ratio.
- Utilized 2,5-dihydroxybenzoic acid as the matrix for MALDI-TOF MS.
- Applied optimized MALDI-TOF MS to analyze three different copolymers.
Main Results:
- Established optimal conditions for MALDI-TOF MS analysis, achieving high ion yields.
- Successfully determined end-group identity, molecular weight distributions, and individual monomer length distributions.
- Demonstrated that styrene monomer distribution is more sensitive to catalyst composition (CuBr2 addition) than pentafluorostyrene distribution.
Conclusions:
- The optimized MALDI-TOF MS method provides a robust approach for copolymer characterization.
- Catalyst composition significantly influences styrene chain length distribution in these copolymers.
- MALDI-TOF MS is a powerful tool for elucidating the fine structure of complex copolymers.
Keywords:
Atom transfer radical polymerizationCopolymer compositional analysisMatrix-assisted laser desorption/ionization sample preparation optimizationPoly(styrene-copentafluorostyrene)
