Analysis of ?-CH2 signals in the13C NMR spectra of the methyl methacrylate-ethyl acrylate copolymer as a tool for microstructure determination

Matlengiewicz, Marek; Nguyen, Giao T.M.; Nicole, D.; Henzel, N.

doi:10.1002/(sici)1099-0518(20000615)38:12<2147::aid-pola30>3.0.co;2-b

Cited by 21 publications

(9 citation statements)

References 12 publications

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“…The copolymerizations and microstructures of various methacrylates with other vinyl monomers have been reported by various researchers 15–17. Nicole and coworkers18, 19 reported the sequence distribution of methyl methacrylate (M)/ethyl acrylate (E) copolymers by 13 C{ 1 H} NMR spectroscopy. They calculated the intensities and chemical shifts of different sequences based on Markov–Bernoulli statistics with carbonyl carbon and β‐CH 2 resonance signals.…”

Section: Introductionmentioning

confidence: 99%

Compositional and configurational sequence determination of methyl methacrylate/ethyl acrylate copolymers by one‐ and two‐dimensional nuclear magnetic resonance spectroscopy

Brar

Hooda

Kumar

2002

J. Polym. Sci. A Polym. Chem.

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Ethyl acrylate (E)/methyl methacrylate (M) copolymers of different compositions were prepared, and their compositions were determined with 1 H NMR spectra. The complete spectral assignments, in terms of the compositional and configurational sequences of these copolymers, were made with the help of distortionless enhancement by polarization transfer and two-dimensional heteronuclear single quantum coherence spectroscopy. The ␣-(CH 3 ) M , OCH (E), OCH 2 , and ͘CAO carbons of both M and E units were found to be sensitive to various compositional and configurational sequences.

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Section: Introductionmentioning

confidence: 99%

Compositional and configurational sequence determination of methyl methacrylate/ethyl acrylate copolymers by one‐ and two‐dimensional nuclear magnetic resonance spectroscopy

Brar

Hooda

Kumar

2002

J. Polym. Sci. A Polym. Chem.

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“…Spectral assignments for the 13 C-NMR signals of the carbon centers in the terpolymers were primarily made on the basis of literature information reported for various polymers containing the three momomers. 4,5,[13][14][15][16][17] Thus, spectral assignments for most of the carbon centers in all three monomers could be defined for the 13 C spectra of the terpolymer products (see Table II and Fig. 1).…”

Section: Resultsmentioning

confidence: 99%

“…200 vs 12 ppm). There have been numerous studies that have used this fact to determine the microstructure of polymers 4, 5. The power of 13 C‐NMR for microstructural analysis is such that it has been used in the past to confirm microstructures predicted by different types of copolymerization models 6…”

Section: Introductionmentioning

confidence: 99%

“…There have been numerous studies that have used this fact to determine the microstructure of polymers. 4,5 The power of 13 C-NMR for microstructural analysis is such that it has been used in the past to confirm microstructures predicted by different types of copolymerization models. 6 Therefore, to support the analysis of BA/MMA/ AMS terpolymers made with 1 H-NMR, 13 C-NMR was used both to assign characteristic signals for the different monomers and to obtain quantitative data that confirmed the results from 1 H-NMR.…”

Section: Introductionmentioning

confidence: 99%

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NMR analysis of butyl acrylate/methylmethacrylate/α‐methyl styrene terpolymers

McManus

Penlidis

2006

J of Applied Polymer Sci

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Composition analysis for butyl acrylate (BA)/ methyl methacrylate (MMA)/a-methyl styrene terpolymers was carried out by NMR spectroscopy methods. 1 H-NMR was used primarily for this analysis, but because the method did not provide independent measurements for the BA and MMA fractions, the terpolymer composition analysis was open to higher than normal levels of uncertainty. Supplementary analyses were made with quantitative

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“…The program changes the parameter until it finds the best-fit between theoretical and experimental MS intensities. The procedure bears some resemblance to a method developed by Matlengiewicz et al [47] for NMR spectra. In this case, the experimental mass spectrum is memorized in a large vector (LV exp ).…”

Section: Theorymentioning

confidence: 92%

Mass spectra of copolymers which display compositional drifts or sequence constraints

Montaudo¹

2004

J. Am. Soc. Mass Spectrom.

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The spectral features appearing in mass spectra of random and block copolymers which display a drift in composition are discussed along with features appearing in mass spectra of terpolymers and tetrapolymers with sequence constraints. It is shown that previous models cannot account for these features. A new model is presented and a compact equation is derived which yields MS intensities. The prediction of the model is compared with some literature data, namely mass spectrometric data concerning a block copolymer sample containing units of alpha-methyl styrene and of methylmethacrylate which display a strong drift in composition, the molar fraction of methylmethacrylate units changing from 0.99 to 0.80 when passing from short to long macromolecular chains. The agreement between theory and experiment is good. A hyperbranched polymer obtained by condensing 4,4'-bis[p(acetoxy)phenyl] valeric acid (referred to as diphenolic acid, DPA) was then considered. The polymer turned out to be a copolymer with regular DPA units and modified DPA units (possessing a phenol group). The molar fraction of regular DPA units changes from 0.80 to 0.95 when passing from low masses to high masses. Copolymers with sequence constraints are considered, such as ABC copolymers in which AA cannot be found along the chain or ABCD copolymers in which A cannot follow A, B cannot follow B, etc. The novel method is applied to an exactly alternating copolymer with units of styrene (St) and maleic anhydride (MAH). The St-MAH sample turned out to be a complex mixture and the presence of a small amount of units of maleic acid (MAC) is detected. The abundance of MAC, estimated by the chain statistical method, is 5%. The method is applied to the copolymer obtained by reactive blending of poly(butylene terephthalate) and poly(bisphenolA carbonate). In this case, the theoretical spectra are generated and spectral features are discussed.

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Analysis of ?-CH2 signals in the13C NMR spectra of the methyl methacrylate-ethyl acrylate copolymer as a tool for microstructure determination

Cited by 21 publications

References 12 publications

Compositional and configurational sequence determination of methyl methacrylate/ethyl acrylate copolymers by one‐ and two‐dimensional nuclear magnetic resonance spectroscopy

Compositional and configurational sequence determination of methyl methacrylate/ethyl acrylate copolymers by one‐ and two‐dimensional nuclear magnetic resonance spectroscopy

NMR analysis of butyl acrylate/methylmethacrylate/α‐methyl styrene terpolymers

Mass spectra of copolymers which display compositional drifts or sequence constraints

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