Accurate and reproducible determination of lignin molar mass by acetobromination

J. Asikkala, Tarja Tamminen, D.S. Argyropoulos (Corresponding Author)

Research output: Contribution to journalArticleScientificpeer-review

71 Citations (Scopus)

Abstract

The accurate and reproducible determination of lignin molar mass by using size exclusion chromatography (SEC) is challenging. The lignin association effects, known to dominate underivatized lignins, have been thoroughly addressed by reaction with acetyl bromide in an excess of glacial acetic acid. The combination of a concerted acetylation with the introduction of bromine within the lignin alkyl side chains is thought to be responsible for the observed excellent solubilization characteristics acetobromination imparts to a variety of lignin samples. The proposed methodology was compared and contrasted to traditional lignin derivatization methods. In addition, side reactions that could possibly be induced under the acetobromination conditions were explored with native softwood (milled wood lignin, MWL) and technical (kraft) lignin. These efforts lend support toward the use of room temperature acetobromination being a facile, effective, and universal lignin derivatization medium proposed to be employed prior to SEC measurements.
Original languageEnglish
Pages (from-to)8968-8973
Number of pages3
JournalJournal of Agricultural and Food Chemistry
Volume60
Issue number36
DOIs
Publication statusPublished - 2012
MoE publication typeA1 Journal article-refereed

Fingerprint

Molar mass
Lignin
lignin
molecular weight
Size exclusion chromatography
derivatization
Gel Chromatography
Bromine
Acetylation
Softwoods
bromine
Acetic Acid
softwood
acetylation
Wood
bromides
solubilization
Association reactions
acetic acid
ambient temperature

Keywords

  • 31P NMR
  • acetobromination
  • acetyl bromide
  • acetylation
  • derivatization
  • kraft lignin
  • lignin
  • milled wood lignin
  • molar mass determination
  • size exclusion chromatography

Cite this

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title = "Accurate and reproducible determination of lignin molar mass by acetobromination",
abstract = "The accurate and reproducible determination of lignin molar mass by using size exclusion chromatography (SEC) is challenging. The lignin association effects, known to dominate underivatized lignins, have been thoroughly addressed by reaction with acetyl bromide in an excess of glacial acetic acid. The combination of a concerted acetylation with the introduction of bromine within the lignin alkyl side chains is thought to be responsible for the observed excellent solubilization characteristics acetobromination imparts to a variety of lignin samples. The proposed methodology was compared and contrasted to traditional lignin derivatization methods. In addition, side reactions that could possibly be induced under the acetobromination conditions were explored with native softwood (milled wood lignin, MWL) and technical (kraft) lignin. These efforts lend support toward the use of room temperature acetobromination being a facile, effective, and universal lignin derivatization medium proposed to be employed prior to SEC measurements.",
keywords = "31P NMR, acetobromination, acetyl bromide, acetylation, derivatization, kraft lignin, lignin, milled wood lignin, molar mass determination, size exclusion chromatography",
author = "J. Asikkala and Tarja Tamminen and D.S. Argyropoulos",
year = "2012",
doi = "10.1021/jf303003d",
language = "English",
volume = "60",
pages = "8968--8973",
journal = "Journal of Agricultural and Food Chemistry",
issn = "0021-8561",
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Accurate and reproducible determination of lignin molar mass by acetobromination. / Asikkala, J.; Tamminen, Tarja; Argyropoulos, D.S. (Corresponding Author).

In: Journal of Agricultural and Food Chemistry, Vol. 60, No. 36, 2012, p. 8968-8973.

Research output: Contribution to journalArticleScientificpeer-review

TY - JOUR

T1 - Accurate and reproducible determination of lignin molar mass by acetobromination

AU - Asikkala, J.

AU - Tamminen, Tarja

AU - Argyropoulos, D.S.

PY - 2012

Y1 - 2012

N2 - The accurate and reproducible determination of lignin molar mass by using size exclusion chromatography (SEC) is challenging. The lignin association effects, known to dominate underivatized lignins, have been thoroughly addressed by reaction with acetyl bromide in an excess of glacial acetic acid. The combination of a concerted acetylation with the introduction of bromine within the lignin alkyl side chains is thought to be responsible for the observed excellent solubilization characteristics acetobromination imparts to a variety of lignin samples. The proposed methodology was compared and contrasted to traditional lignin derivatization methods. In addition, side reactions that could possibly be induced under the acetobromination conditions were explored with native softwood (milled wood lignin, MWL) and technical (kraft) lignin. These efforts lend support toward the use of room temperature acetobromination being a facile, effective, and universal lignin derivatization medium proposed to be employed prior to SEC measurements.

AB - The accurate and reproducible determination of lignin molar mass by using size exclusion chromatography (SEC) is challenging. The lignin association effects, known to dominate underivatized lignins, have been thoroughly addressed by reaction with acetyl bromide in an excess of glacial acetic acid. The combination of a concerted acetylation with the introduction of bromine within the lignin alkyl side chains is thought to be responsible for the observed excellent solubilization characteristics acetobromination imparts to a variety of lignin samples. The proposed methodology was compared and contrasted to traditional lignin derivatization methods. In addition, side reactions that could possibly be induced under the acetobromination conditions were explored with native softwood (milled wood lignin, MWL) and technical (kraft) lignin. These efforts lend support toward the use of room temperature acetobromination being a facile, effective, and universal lignin derivatization medium proposed to be employed prior to SEC measurements.

KW - 31P NMR

KW - acetobromination

KW - acetyl bromide

KW - acetylation

KW - derivatization

KW - kraft lignin

KW - lignin

KW - milled wood lignin

KW - molar mass determination

KW - size exclusion chromatography

U2 - 10.1021/jf303003d

DO - 10.1021/jf303003d

M3 - Article

VL - 60

SP - 8968

EP - 8973

JO - Journal of Agricultural and Food Chemistry

JF - Journal of Agricultural and Food Chemistry

SN - 0021-8561

IS - 36

ER -