Characterization of glycidyl methacrylate/styrene copolymers by one- and two-dimensional NMR spectroscopy

Brar, A. S.; Yadav, Anil Kumar; Hooda, Sunita

doi:10.1016/s0014-3057(02)00030-7

Cited by 15 publications

(28 citation statements)

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“…[5][6][7][8] In continuation of our earlier work, in this paper we report the complete compositional and configurational assignments of Glycidyl methacrylate/vinylidene chloride copolymers. The high-resolution 1D-and 2D-NMR spectroscopy has proved to be an informative technique for the investigation of microstructure of the polymers.…”

Section: Introductionmentioning

confidence: 73%

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Glycidyl Methacrylate and Vinylidene Chloride Copolymers. Nuclear Magnetic Resonance Characterisation

Brar

Yadav

2003

Polym J

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ABSTRACT:The copolymers of glycidyl methacrylate/vinylidene chloride (G/C) were synthesized and the quantitative 13 C{ 1 H} NMR spectrum was used to determine the copolymer composition. The comonomer reactivity ratios as determined by Kelen-Tudos (KT) and non-linear least squares error in variable method (EVM) are r G = 2.55 ± 0.56, r c = 0.26 ± 0.06 and r G = 2.7, r c = 0.27, respectively. The Distortionless Enhancement by Polarization Transfer (DEPT), heteronuclear single quantum coherence (HSQC) and Total Correlation Spectroscopy (TOCSY) were used for the complete spectral assignments of 13 3 have investigated the microstructure of vinylidene/vinyl halide copolymers. The microstructure of vinylidene chloride/trans-4-methacryloyloxyazobenzene were investigated by Brar and Thiyagarajan 4 using one-and two-dimensional NMR spectroscopy.In our earlier publications, the microstructure determination of glycidyl methacrylate with acrylonitrile, vinyl acetate, methacrylonitrile and styrene copolymers have been reported. [5][6][7][8] In continuation of our earlier work, in this paper we report the complete compositional and configurational assignments of Glycidyl methacrylate/vinylidene chloride copolymers. The high-resolution 1D-and 2D-NMR spectroscopy has proved to be an informative technique for the investigation of microstructure of the polymers. 9, 10 Comonomers reactivity ratios were calculated using the Kelen-Tudos (KT) 11 and non-linear error in variable (EVM) 12 methods, using compositional data obtained from 13 C{ 1 H} NMR quantitative spectrum. EXPERIMENTALGlycidyl methacrylate (Merck) and vinylidene chloride (Merck) were purified by distillation under reduced pressure and both the monomer were then stored be- † To whom correspondence should be addressed. low 5 • C. A series of G/C copolymers containing different mol-fraction of G-in feed were prepared by solution polymerisation in benzene at 60 • C using benzoyl peroxide as an initiator. The conversion was kept below 10% by timely precipitating the copolymer in methanol. The copolymers were further purified using chloroform/methanol system. All the NMR spectra were recorded in CDCl 3 solvent at 25 • C as reported in our earlier publications. [5][6][7][8] RESULTS AND DISCUSSION Copolymer Composition and Reactivity Ratios DeterminationThe composition of G/C copolymers was determined from quantitative 13 C{ 1 H} NMR spectrum. The mol fractions of monomers in feed and in copolymer and their molecular weight distribution data are given in Table I. The copolymer composition data was used to determine the terminal model reactivity ratio (KT method). These initial estimates of reactivity ratios, along with the copolymer composition data were used for the calculation of the reactivity ratios by non-linear error in variable method. The value of reactivity ratios as obtained from Kelen-Tudos (KT) 11 and non linear error in variable method (EVM) 12 r G = 2.55 ± 0.56, r c = 0.26 ± 0.06 and r G = 2.7, r c = 0.27, respectively.

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Section: Introductionmentioning

confidence: 73%

“…All the NMR spectra were recorded in CDCl 3 solvent at 25 • C as reported in our earlier publications. [5][6][7][8] …”

Section: Methodsmentioning

confidence: 99%

Glycidyl Methacrylate and Vinylidene Chloride Copolymers. Nuclear Magnetic Resonance Characterisation

Brar

Yadav

2003

Polym J

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“…In the precipitation polymerization, since the molecular weight of the product is not sufficiently small, which is necessary for the measurement of reactivity ratio, due to crosslinking, it was not possible to measure the reactivity ratio. Thus, the reactivity ratios measured in the free radical polymerization are referenced; r st =0.26, r DVB =1.18 for r st =styrene, r DVB =p-divinylbenzene 17 and r st =0.48, r GMA =0.6 for r st =styrene, r GMA =GMA, 18 respectively. From these two results, the reactivity ratios of GMA and DVB can be induced to r DVB =2.18, r GMA =0.6.…”

Section: Methodsmentioning

confidence: 99%

Verification of core/shell structure of poly(glycidyl methacrylate-co-divinyl benzene) microspheres

et al. 2009

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The core/shell type structure of the highly crosslinked poly(glycidylmetharylate-co-divinylbenzene) microspheres prepared in the precipitation polymerization in acetonitrile was thoroughly verified by means of swelling, 1 H NMR, XPS, TEM and TGA measurements. In the XPS measurement, the higher the GMA content, the higher the oxygen content was observed, implying that the higher content of GMA is observed in the particle surface. The further verification of the core/shell structure of the poly(GMA-co-DVB) particles was carried out using 1 H NMR and TEM techniques, resulting in the poly(GMA-co-DVB) particles with the GMA rich-phase and DVB richphase. In overall, the poly(GMA-co-DVB) microspheres consist of a highly crosslinked DVB rich-phase in the core and slightly or non-crosslinked GMA rich-phase in the shell part due to the different reaction ratios between two monomers and self-crosslinking density of DVB.

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“…The relative composition of the copolymers was determined by means of 1 H NMR [40], although the 1 H NMR spectra of the polymers showed a signal broadening. The mole fraction of CS units in the copolymer poly(CS-GMA) was found to be equal to 0.69, while it was 0.80 in the feeding composition.…”

Section: Preparation Andmentioning

confidence: 99%

“…NMR (CDCl 3 ), d (ppm): 7.08 (broad s, aromatic, CS), 6.55 (m, aromatic, CS), 4.06-3.13 (m overlapped, -OCH 2 -in GMA, pCH-of epoxy ring in GMA), 2.73-2.24 (m, -CH 2 -of epoxy ring of GMA), 1.82 (m, pCH-of CS), 1.56-1.25 (m, -CH 2 -in backbone), 0.89-0.49 (m, -CH 3 of GMA)[40].…”

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confidence: 99%

Covalent attachment of chromophores to chlorinated copolymers for optical waveguides: Synthesis and optical characterization

Cerruti

Borbone

Carella

et al. 2009

Polymer

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Characterization of glycidyl methacrylate/styrene copolymers by one- and two-dimensional NMR spectroscopy

Cited by 15 publications

References 16 publications

Glycidyl Methacrylate and Vinylidene Chloride Copolymers. Nuclear Magnetic Resonance Characterisation

Glycidyl Methacrylate and Vinylidene Chloride Copolymers. Nuclear Magnetic Resonance Characterisation

Verification of core/shell structure of poly(glycidyl methacrylate-co-divinyl benzene) microspheres

Covalent attachment of chromophores to chlorinated copolymers for optical waveguides: Synthesis and optical characterization

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