DETERMINATION OF DEGREE OF SUBSTITUTION (DS) AND MOLAR SUBSTITUTION (MS) OF CELLULOSE ETHERS BY SOLID-STATE 13C NMR SPECTROSCOPY

  • Сергей (Sergej) Геннадьевич (Gennad'evich) Кострюков (Kostriukov) National Research Mordovian State University. N.P. Ogaryova http://orcid.org/0000-0002-1774-0836 Email: kostryukov_sg@mail.ru
  • Сергей (Sergej) Валерьевич (Valer'evich) Арасланкин (Araslankin) National Research Mordovian State University. N.P. Ogaryova Email: araslankin@bk.ru
  • Павел (Pavel) Сергеевич (Sergeevich) Петров (Petrov) National Research Mordovian State University. N.P. Ogaryova Email: petrovps83@gmail.com
Keywords: hydroxyethyl cellulose, hydroxyethyl methyl cellulose, hydroxypropyl methyl cellulose, microcrystalline cellulose, solid-state 13C NMR spectroscopy, degree of substitution, molar substitution, spectral region, integrated intensity

Abstract

The work is devoted to determining the substitution parameters of some commercial cellulose ethers by solid-state 13C NMR spectroscopy. The substitution parameters are the degree of substitution (DS) and molar substitution (MS). The objects of study are commercial additives based on hydroxyethyl cellulose (HEC), hydroxypropyl methyl cellulose (HPMC) and hydroxyethyl methyl cellulose (HEMC). In this paper, the degree of substitution (DS) and molar substitution (MS) were determined, and the distribution of the substituents at positions C-2, C-3 and C-6 of the glucopyranose link was established. The calculation of the degree of substitution (DS) and molar substitution (MS) is based on an analysis of relative intensity values of the spectral regions in the solid-state NMR spectra of cellulose ethers and microcrystalline cellulose. Thus the degree of substitution and molar substitution was determined: MSHEC = 1,41 иDSHEC = 1,08; MSHPMC = 0,69 и DSHPMC = 1,78; MSHEMC = 0,74иDSHEMC = 2,19. Comparison of the results with the literature data shows the effectiveness of the method. The proposed method differs from other existing methods in that it is a simple and informative.

Downloads

Download data is not yet available.

Metrics

Metrics Loading ...

Author Biographies

Сергей (Sergej) Геннадьевич (Gennad'evich) Кострюков (Kostriukov), National Research Mordovian State University. N.P. Ogaryova
доцент кафедры органической химии, кандидат химических наук
Сергей (Sergej) Валерьевич (Valer'evich) Арасланкин (Araslankin), National Research Mordovian State University. N.P. Ogaryova
аспирант
Павел (Pavel) Сергеевич (Sergeevich) Петров (Petrov), National Research Mordovian State University. N.P. Ogaryova
заведующий межфакультетской  лабораторией ядерного магнитного резонанса, кандидат химических наук

References

Kryazhev V.N., Shirokov V.A. Khimiia rastitel'nogo syr'ia, 2005, no. 3, pp. 7–12. (in Russ.).

Roy C., Budtova T., Navard P. Biomacromolecules, 2003, vol. 4, no. 2, pp. 259–264. DOI: 10.1021/bm020100s

Michaeli G. Carbohydrate Polymers, 1988, no. 9, pp. 269–275. DOI: 10.1016/0144-8617(88)90045-8

Hodges K., Kester W., Wiederrich D., Grover J. Anal. Chem, 1979, vol. 51, no. 13, pp. 2172–2176. DOI: 10.1021/ac50049a028

Sachse K., Metzner K., Welsch T. The Analyst, 1983, vol. 108, pp. 597–602. DOI: 10.1039/AN9830800597

Ibbett R.N., Philp K., Price D.M. Polymer, 1992, vol. 33, no. 19, pp. 4087–4094. DOI: 10.1016/0032-3861(92)90610-9

Hiertberg T., Zadorecki P. Makromol. Chem, 1986, no. 181, pp. 899–911. DOI: 10.1021/ma9615967

Kono H., Oshima K., Hashimoto H., Shimizu Y., Tajima K.Carbohydrate Polymers, 2016, vol. 146, no.1, pp. 1–9. DOI: 10.1016/j.carbpol.2016.03.021

Brogly M., Fahs A., Bistac S.ARPN Journal of Engineering and Applied Sciences, 2016, vol. 11, iss.11, pp. 7188–7192.

Alvarez-Lorenzo, Lorenzo-FerreiraR.A., Gόmez-AmozaJ.L.,Martίnez-PachecoR., SoutoC., Concheiro A.J. Pharm. Bi-omed. Anal., 1999,vol. 20, iss. 1–2, pp. 373–383. DOI: 10.1016/S0731-7085(99)00066-7

Karrasch A., Jäger C., Saake B., Potthast A., Rosenau T. Cellulose, 2009, no. 16, pp. 1159–1166. DOI: 10.1007/s10570-009-9304-2

Mori T., Chikayama E., Tsuboi Yu., I. Nobuhiro, Sh. Noriko, N. Yoshiyuki, M. Shigeharu, K. Jun. Carbohydrate Pol-ymers, 2012, vol. 90, no. 3, pp. 1197–1203. DOI: 10.1016/j.carbpol.2012.06.027

Mischnick P., Momcilovic D. Advances in Carbohydrate Chemistry and Biochemistry, 2010, vol. 64, pp. 118–210. DOI: 10.1016/S0065-2318(10)64004-8

Rinaudo M., Auzely R., Mazeau K. Encyclopedia of Polymer Science and Technology, 2004, vol. 11, pp. 200–261. DOI: 10.1002/0471440264.pst287

Published
2017-04-12
How to Cite
1. Кострюков (Kostriukov)С. (Sergej) Г. (Gennad’evich), Арасланкин (Araslankin)С. (Sergej) В. (Valer’evich), Петров (Petrov)П. (Pavel) С. (Sergeevich) DETERMINATION OF DEGREE OF SUBSTITUTION (DS) AND MOLAR SUBSTITUTION (MS) OF CELLULOSE ETHERS BY SOLID-STATE 13C NMR SPECTROSCOPY // chemistry of plant raw material, 2017. № 4. P. 31-40. URL: http://journal.asu.ru/cw/article/view/1860.
Section
Biopolymers of plants