Impact of mechanical and enzymatic pretreatments on softwood pulp fiber wall structure studied with NMR spectroscopy and X-ray scattering

Tommi Virtanen (Corresponding Author), Paavo A. Penttilä, Thaddeus C. Maloney, Stina Grönqvist, Taina Kamppuri, Marianna Vehviläinen, Ritva Serimaa, Sirkka Liisa Maunu

Research output: Contribution to journalArticleScientificpeer-review

3 Citations (Scopus)

Abstract

Dissolution of wood pulp can be enhanced by applying certain pretreatments before exposing the fibers to solvents. We have analyzed effect of mechanical and enzymatic pretreatments on softwood fiber wall structure using nuclear magnetic resonance (NMR) spectroscopic methods, small and wide angle X-ray scattering (SAXS, WAXS). NMR diffusometry was used to estimate the effect of pretreatments on average pore sizes at micrometer size scale and for the connectivity of the porous network. A proton NMR experiment was used to quantify the nonfreezing water content inside the fiber wall, and solid state NMR (Formula presented.) cross polarization (CP) magic angle spinning (MAS) spectroscopy was used to observe the effect of pretreatments on crystallinity and lateral fibril dimensions of cellulose fibrils, and in combination with fiber saturation point measurement to calculate the average pore size at nanometer size scale. Both WAXS and CP-MAS NMR experiments confirmed that there were no changes in crystallinity nor in fibril lateral dimensions due to pretreatments. The pretreatments caused an increase in the amount of nonfreezing water, suggesting an opening of the pore system. According to diffusion experiments there are only minor changes in micrometer scale pore network due to pretreatments. SAXS results indicated that enzymatic treatment increased the microfibrillar distance, and there was also an increase in cross relaxation rate of magnetization from water to cellulose protons as observed by NMR. These were interpreted to be due to opening of microfibrillar bundles, leading to an increased accessibility of water.
Original languageEnglish
Pages (from-to)1565-1576
JournalCellulose
Volume22
Issue number3
DOIs
Publication statusPublished - 2015
MoE publication typeA1 Journal article-refereed

Fingerprint

Softwoods
X ray scattering
Nuclear magnetic resonance spectroscopy
Pulp
Nuclear magnetic resonance
Fibers
Magic angle spinning
Cellulose
Pore size
Water
Polarization
Experiments
Water content
Protons
Magnetization
Wood
Dissolution
Spectroscopy

Keywords

  • softwood pulp
  • NMR spectroscopy
  • diffusion
  • enzymatic hydrolysis
  • SAXS
  • WAXS

Cite this

@article{8892307994ae4eba8fbaad5eb1e557d6,
title = "Impact of mechanical and enzymatic pretreatments on softwood pulp fiber wall structure studied with NMR spectroscopy and X-ray scattering",
abstract = "Dissolution of wood pulp can be enhanced by applying certain pretreatments before exposing the fibers to solvents. We have analyzed effect of mechanical and enzymatic pretreatments on softwood fiber wall structure using nuclear magnetic resonance (NMR) spectroscopic methods, small and wide angle X-ray scattering (SAXS, WAXS). NMR diffusometry was used to estimate the effect of pretreatments on average pore sizes at micrometer size scale and for the connectivity of the porous network. A proton NMR experiment was used to quantify the nonfreezing water content inside the fiber wall, and solid state NMR (Formula presented.) cross polarization (CP) magic angle spinning (MAS) spectroscopy was used to observe the effect of pretreatments on crystallinity and lateral fibril dimensions of cellulose fibrils, and in combination with fiber saturation point measurement to calculate the average pore size at nanometer size scale. Both WAXS and CP-MAS NMR experiments confirmed that there were no changes in crystallinity nor in fibril lateral dimensions due to pretreatments. The pretreatments caused an increase in the amount of nonfreezing water, suggesting an opening of the pore system. According to diffusion experiments there are only minor changes in micrometer scale pore network due to pretreatments. SAXS results indicated that enzymatic treatment increased the microfibrillar distance, and there was also an increase in cross relaxation rate of magnetization from water to cellulose protons as observed by NMR. These were interpreted to be due to opening of microfibrillar bundles, leading to an increased accessibility of water.",
keywords = "softwood pulp, NMR spectroscopy, diffusion, enzymatic hydrolysis, SAXS, WAXS",
author = "Tommi Virtanen and Penttil{\"a}, {Paavo A.} and Maloney, {Thaddeus C.} and Stina Gr{\"o}nqvist and Taina Kamppuri and Marianna Vehvil{\"a}inen and Ritva Serimaa and Maunu, {Sirkka Liisa}",
year = "2015",
doi = "10.1007/s10570-015-0619-x",
language = "English",
volume = "22",
pages = "1565--1576",
journal = "Cellulose",
issn = "0969-0239",
publisher = "Springer",
number = "3",

}

Impact of mechanical and enzymatic pretreatments on softwood pulp fiber wall structure studied with NMR spectroscopy and X-ray scattering. / Virtanen, Tommi (Corresponding Author); Penttilä, Paavo A.; Maloney, Thaddeus C.; Grönqvist, Stina; Kamppuri, Taina; Vehviläinen, Marianna; Serimaa, Ritva; Maunu, Sirkka Liisa.

In: Cellulose, Vol. 22, No. 3, 2015, p. 1565-1576.

Research output: Contribution to journalArticleScientificpeer-review

TY - JOUR

T1 - Impact of mechanical and enzymatic pretreatments on softwood pulp fiber wall structure studied with NMR spectroscopy and X-ray scattering

AU - Virtanen, Tommi

AU - Penttilä, Paavo A.

AU - Maloney, Thaddeus C.

AU - Grönqvist, Stina

AU - Kamppuri, Taina

AU - Vehviläinen, Marianna

AU - Serimaa, Ritva

AU - Maunu, Sirkka Liisa

PY - 2015

Y1 - 2015

N2 - Dissolution of wood pulp can be enhanced by applying certain pretreatments before exposing the fibers to solvents. We have analyzed effect of mechanical and enzymatic pretreatments on softwood fiber wall structure using nuclear magnetic resonance (NMR) spectroscopic methods, small and wide angle X-ray scattering (SAXS, WAXS). NMR diffusometry was used to estimate the effect of pretreatments on average pore sizes at micrometer size scale and for the connectivity of the porous network. A proton NMR experiment was used to quantify the nonfreezing water content inside the fiber wall, and solid state NMR (Formula presented.) cross polarization (CP) magic angle spinning (MAS) spectroscopy was used to observe the effect of pretreatments on crystallinity and lateral fibril dimensions of cellulose fibrils, and in combination with fiber saturation point measurement to calculate the average pore size at nanometer size scale. Both WAXS and CP-MAS NMR experiments confirmed that there were no changes in crystallinity nor in fibril lateral dimensions due to pretreatments. The pretreatments caused an increase in the amount of nonfreezing water, suggesting an opening of the pore system. According to diffusion experiments there are only minor changes in micrometer scale pore network due to pretreatments. SAXS results indicated that enzymatic treatment increased the microfibrillar distance, and there was also an increase in cross relaxation rate of magnetization from water to cellulose protons as observed by NMR. These were interpreted to be due to opening of microfibrillar bundles, leading to an increased accessibility of water.

AB - Dissolution of wood pulp can be enhanced by applying certain pretreatments before exposing the fibers to solvents. We have analyzed effect of mechanical and enzymatic pretreatments on softwood fiber wall structure using nuclear magnetic resonance (NMR) spectroscopic methods, small and wide angle X-ray scattering (SAXS, WAXS). NMR diffusometry was used to estimate the effect of pretreatments on average pore sizes at micrometer size scale and for the connectivity of the porous network. A proton NMR experiment was used to quantify the nonfreezing water content inside the fiber wall, and solid state NMR (Formula presented.) cross polarization (CP) magic angle spinning (MAS) spectroscopy was used to observe the effect of pretreatments on crystallinity and lateral fibril dimensions of cellulose fibrils, and in combination with fiber saturation point measurement to calculate the average pore size at nanometer size scale. Both WAXS and CP-MAS NMR experiments confirmed that there were no changes in crystallinity nor in fibril lateral dimensions due to pretreatments. The pretreatments caused an increase in the amount of nonfreezing water, suggesting an opening of the pore system. According to diffusion experiments there are only minor changes in micrometer scale pore network due to pretreatments. SAXS results indicated that enzymatic treatment increased the microfibrillar distance, and there was also an increase in cross relaxation rate of magnetization from water to cellulose protons as observed by NMR. These were interpreted to be due to opening of microfibrillar bundles, leading to an increased accessibility of water.

KW - softwood pulp

KW - NMR spectroscopy

KW - diffusion

KW - enzymatic hydrolysis

KW - SAXS

KW - WAXS

U2 - 10.1007/s10570-015-0619-x

DO - 10.1007/s10570-015-0619-x

M3 - Article

VL - 22

SP - 1565

EP - 1576

JO - Cellulose

JF - Cellulose

SN - 0969-0239

IS - 3

ER -