Skip to main content

13C NMR of Crosslinked Poly(Methacrylic Anhydride)

  • Chapter
Solid State NMR of Polymers

Abstract

Solution and solid state 13C nuclear magnetic resonance (13C NMR) spectra for poly(methacrylic anhydride) (PMAH) polymers with various tacticities and thermal histories were correlated with infrared spectra and gel permeation chromatographs to detect anhydride crosslinks. Under most baking conditions, thin films of isotactic poly(tert-butyl methacrylate) (PtBMA) formed spherulitic crystals upon conversion to isotactic PMAH (i-PMAH), whereas PMAH prepared from 83% syndiotactic PtBMA or by the free-radical cyclopolymerization of methacrylic anhydride remained amorphous. Amorphous polymers gave broad solid state 13C NMR peaks, but crystalline i-PMAH yielded multiple carbonyl and α-methyl peaks. The i-PMAH spectra were compared to those for amorphous PMAH and a model compound to assign chemical shifts to PMAH crosslink α-methyl and carbonyl carbons.

This is a preview of subscription content, log in via an institution to check access.

Access this chapter

Chapter
USD 29.95
Price excludes VAT (USA)
  • Available as PDF
  • Read on any device
  • Instant download
  • Own it forever
eBook
USD 129.00
Price excludes VAT (USA)
  • Available as PDF
  • Read on any device
  • Instant download
  • Own it forever
Softcover Book
USD 169.99
Price excludes VAT (USA)
  • Compact, lightweight edition
  • Dispatched in 3 to 5 business days
  • Free shipping worldwide - see info
Hardcover Book
USD 169.99
Price excludes VAT (USA)
  • Durable hardcover edition
  • Dispatched in 3 to 5 business days
  • Free shipping worldwide - see info

Tax calculation will be finalised at checkout

Purchases are for personal use only

Institutional subscriptions

Preview

Unable to display preview. Download preview PDF.

Unable to display preview. Download preview PDF.

References

  1. Tiers, G. V. D.; Bovey, F. A., J. Polym. Sci., 47, 479, 1960.

    Article  CAS  Google Scholar 

  2. Hwa, J. G H.; Miller, L., J. Polym. Sci., 55, 197, 1961.

    Article  CAS  Google Scholar 

  3. Grant, D. H.; Grassie, N., Polymer, 1, 125, 1960.

    Article  CAS  Google Scholar 

  4. Miura, A.; Hideyama, S., J. Vac. Sci. Technol., 16(6), 199. 1979.

    Article  Google Scholar 

  5. Miller, L. J.; Granger, D. D., Hughes Research Laboratories, Malibu, CA (unpublished results).

    Google Scholar 

  6. Elias, H. G., Macromolecules, Vol. 2, Plenum: New York, pp 815–818, 1977.

    Google Scholar 

  7. Grant, D. H.; Grassie, N., Polymer, 1, 445, 1960.

    Article  CAS  Google Scholar 

  8. Lai, J. H., Macromolecules, 17(5), 1010, 1984.

    Article  CAS  Google Scholar 

  9. Fyfe, G A.; McKinnon, M. S., Macromolecules, 19(7), 1909, 1986.

    Article  CAS  Google Scholar 

  10. Heyboer, J.; Staverman, A. J., Recueil, 69, 787. 1950.

    Article  CAS  Google Scholar 

  11. Azimov, Z. A.; Korotkov, A. A.; Mitsengendler, S. P., Izv. Akad. Nauk SSSR, Ser. Khim., 1, 55 (Russ.), 1964; Bull. Acad. Sci., USSR Div. Chem. Sci., 46 (Eng. transi.), 1964.

    Google Scholar 

  12. Fox, T. G.; Garrett, B. S.; Goode, W. E.; Gratch, S.; Kincaid, J. F.; Spell, A.; Stroupe, J. D., J. Am. Chem. Soc., 80, 1768, 1958.

    Article  CAS  Google Scholar 

  13. Fox, T. G.; Schnecko, H. W., Polymer, 3, 575, 1963.

    Article  Google Scholar 

  14. Hwa, J. G H.; Fleming, W. A.; Miller, L., J. Polym. Sci., 2(5), 2385. A 1964.

    CAS  Google Scholar 

  15. Suzuki, T.; Yamada, O.; Watanabe, Y.; Takegami, Y., Polym. J., 14(5), 343, 1982.

    Article  CAS  Google Scholar 

  16. Hatada, K.; Kitayama, T.; Okamoto, Y.; Ohta, K.; Umemura, Y.; Yuki, H., Makromol. Chem., 179, 485, 1978.

    Article  CAS  Google Scholar 

  17. “Deuterated Solvents — Handy Reference Data”, Isotope Div., Merck & Co.

    Google Scholar 

  18. Eckert, H.; Yesinowski, J. P.; Sandman, D. J.; Valazquez, C. S., J. Am. Chem. Soc., 109, 761, 1987.

    Article  CAS  Google Scholar 

  19. Gray, Jr., T. F.; Butler, G. B., J. Macromol. Sci., Chem., A9(1), 45, 1975.

    Google Scholar 

  20. Miller, L. J.; Brault, R. G.; Granger, D. D.; Jensen, J. E.; van Ast, C. A.; Lewis, M. L., J. Vac. Sci. Technol., B7(1), 68, 1989.

    Google Scholar 

  21. Butler, G. B.; Matsumoto, A., J. Polym. Sci., Polym. Lett. Ed., 19, 167, 1981.

    Article  CAS  Google Scholar 

  22. Brouwer, H.; Stothers, J. B., Can. J. Chem., 50, 601, 1972.

    Article  CAS  Google Scholar 

  23. Ouano, A. C., Prepr. Pap.-Am. Chem. Soc, Div. Ctgs. and Plstcs., 48, 42, 1983.

    CAS  Google Scholar 

  24. Billmeyer, F.W., Textbook of Polymer Science, 2nd ed., Wiley-Interscience, New York, 1971, p 24.

    Google Scholar 

  25. Veregin, R. P.; Fyfe, C. A.; Marchessault, R. H., Macromolecules, 19, 2379, 1986.

    Article  CAS  Google Scholar 

  26. Ryan, C. F.; Heischer, P. C. Jr., J. Phys. Chem., 69(10), 3384, 1965.

    Article  CAS  Google Scholar 

Download references

Author information

Authors and Affiliations

Authors

Editor information

Editors and Affiliations

Rights and permissions

Reprints and permissions

Copyright information

© 1991 Springer Science+Business Media New York

About this chapter

Cite this chapter

Granger, D.D. (1991). 13C NMR of Crosslinked Poly(Methacrylic Anhydride). In: Mathias, L.J. (eds) Solid State NMR of Polymers. Springer, Boston, MA. https://doi.org/10.1007/978-1-4899-2474-2_10

Download citation

  • DOI: https://doi.org/10.1007/978-1-4899-2474-2_10

  • Publisher Name: Springer, Boston, MA

  • Print ISBN: 978-1-4899-2476-6

  • Online ISBN: 978-1-4899-2474-2

  • eBook Packages: Springer Book Archive

Publish with us

Policies and ethics