Characterization of a Poly(fluorooxetane) and Poly(fluorooxetane-co-THF) by MALDI Mass Spectrometry, Size Exclusion Chromatography, and NMR Spectroscopy
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- 作者：Chrys Wesdemiotis ; Francesco Pingitore ; Michael J. Polce ; Vernon M. Russell ; Yongsin Kim ; Charles M. Kausch ; Thomas H. Connors ; Robert E. Medsker ; Richard R. Thomas
- 刊名：Macromolecules
- 出版年：2006
- 出版时间：November 28, 2006
- 年：2006
- 卷：39
- 期：24
- 页码：8369 - 8378
- 全文大小：230K
- 年卷期：v.39,no.24(November 28, 2006)
- ISSN：1520-5835
文摘
An 
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-dihydroxypoly(fluorooxetane) was prepared from a fluorinated oxetane monomer andcharacterized by matrix-assisted laser desorption ionization mass spectrometric (MALDI MS) and gel permeationchromatographic (GPC) methods. Estimated molecular weights were compared to those derived from NMRspectroscopic end-group analysis. The results of 2-D NMR spectroscopic analysis agreed well with 1-D NMRend-group analytical results and MALDI MS experiments. Because of the small molecular weight of the product,the results from the mass spectroscopic and NMR methods compared favorably. The overestimated molecularweights obtained from GPC are explained by aggregation of the amphiphilic poly(fluorooxetane) in a relativelypoor solvent. The robustness of the methods was verified by fractionation of the polymer and subsequent analysisof the fractions by MALDI MS. In addition, information regarding product architecture and copolymerizationwith THF, which was used to complex the BF3 catalyst, was obtained using tandem mass spectrometry (MS/MS)methods.
,-dihydroxypoly(fluorooxetane) was prepared from a fluorinated oxetane monomer andcharacterized by matrix-assisted laser desorption ionization mass spectrometric (MALDI MS) and gel permeationchromatographic (GPC) methods. Estimated molecular weights were compared to those derived from NMRspectroscopic end-group analysis. The results of 2-D NMR spectroscopic analysis agreed well with 1-D NMRend-group analytical results and MALDI MS experiments. Because of the small molecular weight of the product,the results from the mass spectroscopic and NMR methods compared favorably. The overestimated molecularweights obtained from GPC are explained by aggregation of the amphiphilic poly(fluorooxetane) in a relativelypoor solvent. The robustness of the methods was verified by fractionation of the polymer and subsequent analysisof the fractions by MALDI MS. In addition, information regarding product architecture and copolymerizationwith THF, which was used to complex the BF3 catalyst, was obtained using tandem mass spectrometry (MS/MS)methods.