Solid-State 13C CP/MAS NMR for Alkyl-O-Aryl Bond Determination in Lignin Preparations

Standard

Solid-State ¹³C CP/MAS NMR for Alkyl-O-Aryl Bond Determination in Lignin Preparations. / Evstigneyev, Edward I.; Mazur, Anton S.; Kalugina, Aleksandra V.; Pranovich, Andrey V.; Vasilyev, Aleksander V.

In: Journal of Wood Chemistry and Technology, Vol. 38, No. 2, 04.03.2018, p. 137-148.

Research output: Contribution to journal › Article › peer-review

Author

Evstigneyev, Edward I. ; Mazur, Anton S. ; Kalugina, Aleksandra V. ; Pranovich, Andrey V. ; Vasilyev, Aleksander V. / Solid-State ¹³C CP/MAS NMR for Alkyl-O-Aryl Bond Determination in Lignin Preparations. In: Journal of Wood Chemistry and Technology. 2018 ; Vol. 38, No. 2. pp. 137-148.

BibTeX

@article{39c5aa4eec074644b97338a91c13645a,

title = "Solid-State 13C CP/MAS NMR for Alkyl-O-Aryl Bond Determination in Lignin Preparations",

abstract = "Several lignin preparations (Freudenberg lignin, Bj{\"o}rkman lignin, and Pepper lignin), technical lignins (soda, soda-AQ, Kraft, Kraft-AQ, and hydrolysis), dimeric lignin model compounds, and different polysaccharides (galactoglucomannan, arabinogalactan, xylan, and arabinan) were analyzed by means of solid-state 13C CP/MAS NMR. Signals assignment in solid-state NMR lignin spectra was performed on the basis of the conducted studies and earlier published data. It was established that there exists strong linear correlation (r = 0.985) between Alkyl-O-Aryl inter-unit bond content in lignin and integral signals intensity in NMR spectra in the range of chemical shifts of 96–68 ppm. The integral signals intensity was measured in correlation with the reference integral signals in the range of chemical shifts of 162–102 ppm, typical for aromatic carbon atoms. To eliminate the effect, caused by carbohydrates contained in lignin, the correction factor of 0.67% of the area of integration per 1% of carbohydrates was determined. It was shown that the solid-state 13C CP/MAS NMR method allowed to determine Alkyl-O-Aryl bond content in both soluble and insoluble lignin preparations, and also to determine methoxyl groups content in soluble preparations.",

keywords = "Alkyl-O-Aryl bonds, lignins, methoxyl groups, Solid-state C CP/MAS NMR",

author = "Evstigneyev, {Edward I.} and Mazur, {Anton S.} and Kalugina, {Aleksandra V.} and Pranovich, {Andrey V.} and Vasilyev, {Aleksander V.}",

year = "2018",

month = mar,

day = "4",

doi = "10.1080/02773813.2017.1393436",

language = "English",

volume = "38",

pages = "137--148",

journal = "Journal of Wood Chemistry and Technology",

issn = "0277-3813",

publisher = "Taylor & Francis",

number = "2",

}

RIS

TY - JOUR

T1 - Solid-State 13C CP/MAS NMR for Alkyl-O-Aryl Bond Determination in Lignin Preparations

AU - Evstigneyev, Edward I.

AU - Mazur, Anton S.

AU - Kalugina, Aleksandra V.

AU - Pranovich, Andrey V.

AU - Vasilyev, Aleksander V.

PY - 2018/3/4

Y1 - 2018/3/4

N2 - Several lignin preparations (Freudenberg lignin, Björkman lignin, and Pepper lignin), technical lignins (soda, soda-AQ, Kraft, Kraft-AQ, and hydrolysis), dimeric lignin model compounds, and different polysaccharides (galactoglucomannan, arabinogalactan, xylan, and arabinan) were analyzed by means of solid-state 13C CP/MAS NMR. Signals assignment in solid-state NMR lignin spectra was performed on the basis of the conducted studies and earlier published data. It was established that there exists strong linear correlation (r = 0.985) between Alkyl-O-Aryl inter-unit bond content in lignin and integral signals intensity in NMR spectra in the range of chemical shifts of 96–68 ppm. The integral signals intensity was measured in correlation with the reference integral signals in the range of chemical shifts of 162–102 ppm, typical for aromatic carbon atoms. To eliminate the effect, caused by carbohydrates contained in lignin, the correction factor of 0.67% of the area of integration per 1% of carbohydrates was determined. It was shown that the solid-state 13C CP/MAS NMR method allowed to determine Alkyl-O-Aryl bond content in both soluble and insoluble lignin preparations, and also to determine methoxyl groups content in soluble preparations.

AB - Several lignin preparations (Freudenberg lignin, Björkman lignin, and Pepper lignin), technical lignins (soda, soda-AQ, Kraft, Kraft-AQ, and hydrolysis), dimeric lignin model compounds, and different polysaccharides (galactoglucomannan, arabinogalactan, xylan, and arabinan) were analyzed by means of solid-state 13C CP/MAS NMR. Signals assignment in solid-state NMR lignin spectra was performed on the basis of the conducted studies and earlier published data. It was established that there exists strong linear correlation (r = 0.985) between Alkyl-O-Aryl inter-unit bond content in lignin and integral signals intensity in NMR spectra in the range of chemical shifts of 96–68 ppm. The integral signals intensity was measured in correlation with the reference integral signals in the range of chemical shifts of 162–102 ppm, typical for aromatic carbon atoms. To eliminate the effect, caused by carbohydrates contained in lignin, the correction factor of 0.67% of the area of integration per 1% of carbohydrates was determined. It was shown that the solid-state 13C CP/MAS NMR method allowed to determine Alkyl-O-Aryl bond content in both soluble and insoluble lignin preparations, and also to determine methoxyl groups content in soluble preparations.

KW - Alkyl-O-Aryl bonds

KW - lignins

KW - methoxyl groups

KW - Solid-state C CP/MAS NMR

UR - http://www.scopus.com/inward/record.url?scp=85042094319&partnerID=8YFLogxK

U2 - 10.1080/02773813.2017.1393436

DO - 10.1080/02773813.2017.1393436

M3 - Article

AN - SCOPUS:85042094319

VL - 38

SP - 137

EP - 148

JO - Journal of Wood Chemistry and Technology

JF - Journal of Wood Chemistry and Technology

SN - 0277-3813

IS - 2

ER -

ID: 15199450