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Microstructure determination of isobornyl methacrylate-styrene copolymer by NMR spectroscopy

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Abstract

An investigation of the microstructure of isobornyl methacrylate - styrene (I/S) copolymers prepared by the atom transfer radical polymerization (ATRP) using methyl-2-bromopropionate as an initiator and PMDETA copper complex as catalyst under nitrogen atmosphere at 70 °C has been done by two-dimensional NMR techniques. 2D- HSQC and TOCSY have been utilized to resolve the complex 1H NMR spectrum and to establish the compositional and configurational sequences of isobornyl methacrylate-styrene (I/S) copolymers. 2D HSQC and TOCSY spectra showed compositional and configurational sensitivity of α-methyl carbon of I unit and methine proton of S unit and are assigned up to the triad level. The methylene carbon (C10) also shows triad level of compositional sensitivity in 2D HSQC spectra. Heteronuclear multiple-bond correlation (HMBC) spectroscopy has been used to study carbonyl/quaternary carbon-proton coupling. The carbonyl and quaternary carbons showed compositional and configurational sensitivity upto the triad level. The values of reactivity ratios were determined by Kelen-Tudos (KT) and nonlinear error in variable method (RREVM) using copolymer composition data that were determined by 1H NMR spectrum. Reactivity ratios of co-monomers in I/S copolymer, determined from a linear Kelen-Tudos method (KT) and non-linear Error-in-Variable Method (EVM), are rI = 0.39 ± 0.09, rS = 0.44 ± 0.08 and rI = 0.42, rS = 0.47, respectively.

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Acknowledgments

One of the authors, Deepika, wants to thank University Grant Commission (UGC), New Delhi, India, for providing financial support and Indian Institute of Technology Delhi, New Delhi, India, for providing the space and facilities.

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Authors and Affiliations

  1. Department of Chemistry, Indian Institute of Technology Delhi, New Delhi, 110016, India

    Deepika Khandelwal, A. S. Brar & Ravi Shankar

  2. Department of Chemistry, Acharya Narendra Dev College, Govindpuri, Kalkaji, New Delhi, 110019, India

    Sunita Hooda

  3. Guru Nanak Dev University, Amritsar, Punjab, India

    A. S. Brar

Authors
  1. Deepika Khandelwal
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  2. Sunita Hooda
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  3. A. S. Brar
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  4. Ravi Shankar
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Correspondence to A. S. Brar.

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Khandelwal, D., Hooda, S., Brar, A.S. et al. Microstructure determination of isobornyl methacrylate-styrene copolymer by NMR spectroscopy. J Polym Res 21, 377 (2014). https://doi.org/10.1007/s10965-014-0377-8

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