Nuclear Magnetic Resonance Study of Thermodynamic Interaction between Cellulose Acetate and Solvent

Kamide, Kenji; Okajima, Kunihiko; Saito, Masatoshi

doi:10.1295/polymj.13.115

Cited by 44 publications

(16 citation statements)

References 12 publications

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“…This is in agreement with IR and 1 H NMR data of CAs in organic solvents; the magnitude of interaction depends on the acidity of the latter (Kamide et al 1981). …”

Section: Solvatochromism In the Model Systemssupporting

confidence: 90%

Probing the dependence of the properties of cellulose acetates and their films on the degree of biopolymer substitution: use of solvatochromic indicators and thermal analysis

et al. 2010

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“…This is in agreement with IR and 1 H NMR data of CAs in organic solvents; the magnitude of interaction depends on the acidity of the latter (Kamide et al 1981). …”

Section: Solvatochromism In the Model Systemssupporting

confidence: 90%

Probing the dependence of the properties of cellulose acetates and their films on the degree of biopolymer substitution: use of solvatochromic indicators and thermal analysis

et al. 2010

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“…Then the three peaks appearing at about 169.8, 169.4, and 168.7ppm seem to be derived from C 6 -, C 3 -, and C 2 -mono-substituted glucopyranose units. These spectra for CA obtained here are much better resolved than those reported by Kamide and Okajima 9 and Miyamoto et a/. 10 The lower resolution of the spectra in these papers might have given basis to roughly divide the carbonyl carbon peak region into three major peaks.…”

Section: Peaks Was Adjusted To Givecontrasting

confidence: 43%

“…9 The former is just the reverse of the latter in the C 2 and C 3 · positions. In Kamide and Okajima's earlier work, the overlapping of the acetyl methyl proton peaks and the 0-acetyl carbon peaks are significantly large and in consequence, in both 1 H and 13 C NMR spectra, the peaks located at the middle position were unavoidably overestimated, leading to erroneous assignment.…”

Section: Peaks Was Adjusted To Givementioning

confidence: 97%

Further Study on the Distribution of Substituent Group in Cellulose Acetate by 13C{1H}NMR Analysis: Assignment of Carbonyl Carbon Peaks

Kowsaka¹,

Okajima²,

Kamide³

1986

Polym J

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ABSTRACT:An attempt was made to determine an unsolved problem in peak assignment of carbonyl carbon region in 13 C NMR spectra for cellulose acetate. For this purpose, Kamide and Okajima's method for determination of the distribution of acetyl group among three hydroxyl groups in a glucopyranose unit was reexamined carefully using a 200 MHz FT-NMR spectrometer, adequate and the most reasonable assignment at present was made on the carbonyl carbon peaks in NMR spectra, applying a low-power selective decoupling method to acetyl methyl proton located at specific carbon position. All three NMR peaks in the carbonyl carbon region were assigned to be attributed to the acetyl groups located at C6 , C3, and C2 positions, from the low magnetic field side. The previous Kamide and Okajima's assignment on C3 and C2 peaks was found to be erroneoulsy made by neglecting an overlapping of the three peaks due to low resolving power in the 1 H and 13 C NMR spectrometer used by them. The new and complete assignments were in good agreement with those by Miyamoto eta/.

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“…Recently Kamide et a/. 3 with the unperturbed chain dimension A and the partially draining parameter X 4 -8 were experimentally demonstrated for CA with = 0.49-2.92 iii various solvents. These experimental facts indicate explicitly that the solvation plays predominant roles in the flexibility of the unperturbed chain together with the hydrodynamic interaction in CA solutions.…”

Section: Methyl Proton I Carbonyl Carbon Imentioning

confidence: 97%

“…In this article as an extension of our earlier work 3 we measure the chemical shift J and the relaxation time T 1 by FT-1 H and -13 C NMR for cellulose triacetate (CT A) in various solvents to disclose the solution structure of CT A-solvent system.…”

Section: Methyl Proton I Carbonyl Carbon Imentioning

confidence: 99%

A Further Study on Solvation in Cellulose Triacetate Solutions by Pulse-Fourier 1H and 13C NMR Method

Kamide¹,

Saito²,

Kowsaka³

et al. 1987

Polym J

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ABSTRACT:An attempt was made by pulse-Fourier 1 H and 13 C NMR to measure the chemical shift b of the 0-acetyl-methyl (AMH) and -<:arbonyl carbon (ACC) of cellulose triacetate (CTA, the total degree of substitution = 2.92) in various deuterated solvents and to determine whether the possibility of the solvation depends on the position (C2, C 3 , or C6) of the 0-acetyl group or not and if so, to evaluate the positions of the 0-acetyl group, to which the solvent molecules are preferentially solvated. Among N,N-dimethylsulfoxide (DMSO), pyridine (Py), trichloromethane (TCM) and acetone, the spin-lattice relaxation time of AMH at C2 carbon and that of ACC at C2 , C3, and C6 carbons were maximum in acetone, indicating that acetone molecules interact the most weakly with 0-acetyl group. The difference of b of AMH at each carbon position (C2, C3 , and C6) between DMSO or Py or TCM and acetone was positive in DMSO and negative in Py, TCM. The similar difference of b of ACC was always positive, except the case of ACC at C2 and C3 positions in Py, where the difference was zero. Assuming no specific interaction between acetone and CTA we can conclude that DMSO and TCM molecules solvate equally with 0-acetyl group at C 2 , C 3 , and C6 positions, but the pyridine molecule solvates only with 0-acetyl group at C6 position.KEY WORDS Cellulose Triacetate I FT-NMR I Chemical Shift I Solvation I Methyl Proton I Carbonyl Carbon IThe earliest study of the interaction between the cellulose derivative and the solvent molecule (i.e., the solvation) seems to have been that of Moore and his coworkers, 1 who in 1965 measured the adiabatic compressibility of solutions of cellulose acetate (CA), cellulose nitrate, ethylcellulose and so on, estimating the number of the solvent molecules solvated to a glucopyranose ring, s. Unfortunately, as Kamide and Saito 2 pointed out later, the accuracy and preciseness of their data on the sound velocity are not satisfactory. Recently

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Nuclear Magnetic Resonance Study of Thermodynamic Interaction between Cellulose Acetate and Solvent

Cited by 44 publications

References 12 publications

Probing the dependence of the properties of cellulose acetates and their films on the degree of biopolymer substitution: use of solvatochromic indicators and thermal analysis

Probing the dependence of the properties of cellulose acetates and their films on the degree of biopolymer substitution: use of solvatochromic indicators and thermal analysis

Further Study on the Distribution of Substituent Group in Cellulose Acetate by 13C{1H}NMR Analysis: Assignment of Carbonyl Carbon Peaks

A Further Study on Solvation in Cellulose Triacetate Solutions by Pulse-Fourier 1H and 13C NMR Method

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