Holzforschung, Vol. 59, pp. 59–64, 2005 • Copyright  by Walter de Gruyter • Berlin • New York. DOI 10.1515/HF.2005.

010

Changes in color and structure of birch wood (Betula

pendula) caused by bleaching with hydrogen peroxide
solution

Kirsi Mononen*, Leila Alvila and Tuula T. transition metals or by light/heat (Kishimoto et al. 2003).
Pakkanen Furthermore, H2O2 bleaching of chips is used as a pre-
treatment prior to mechanical pulping (Xu and Hodden-
University of Joensuu, Department of Chemistry,
bagh 2003). In the woodworking industry, the potential
Joensuu, Finland
of bleaching with H2O2 to remove fungal stain from pon-
*Corresponding author. derosa pine (Pinus ponderosa Laws.) or to change color
University of Joensuu, Department of Chemistry, P.O. Box 111, effects and adhesion strength of varnishes as well as the
FI-80101 Joensuu, Finland surface gloss of pine (Pinus sylvestris L.), oriental beech
E-mail: kirsi.a.mononen@joensuu.fi
(Fagus orientalis Lipsky), ash (Fraxinus excelsior), and oak
(Quercus petraea) have been studied by Lee et al. (1995),
Ozcifci et al. (1999) and Uysal et al. (1999).
Abstract Recently, a new industrial scale method, Wood-Brite,
based on the bleaching of solid wood surfaces to
The effect of bleaching with a hydrogen peroxide (H2O2)
improve wood color, has been developed (Malvaranta
solution on coloring of secondary xylem of kiln-dried
2003; Möttönen et al. 2003). In an earlier study on
birch wood (B. pendula) was investigated with CIELAB
bleaching wood pieces with H2O2 using Wood-Brite, it
color measurements. Structure of unbleached and
has been shown that bleaching changes the color (CIE-
bleached wood pieces was studied by light microscopy
LAB) of semi-finished wood pieces. After peroxide
(LM), environmental scanning electron microscopy
bleaching, the lightness, L*, of several hardwood species,
(ESEM), and transmission electron microscopy (TEM). In
namely, teak (Tectona grandis), oak (Quercus robur), birch
addition, hardness and surface roughness of unbleached
(Betula pendula), and maple (Acer platanoides), and one
and bleached wood pieces were characterized with
softwood species, namely, spruce (Picea abies),
Brinell hardness and contact angle measurements. The
increased while their redness, a*, and yellowness, b*,
results indicated that surface bleaching with H2O2 solu-
changed. However, little information is available on how
tion changed the color of birch wood toward white and
bleaching with hydrogen peroxide affects the structure of
less red, simultaneously increasing the porosity and
solid wood pieces (Möttönen et al. 2003).
roughness of the uppermost surface as well as decreas-
The aim of this study was to investigate the effect of
ing the hardness of bleached wood pieces. With embed-
bleaching with H2O2 on the structure of the secondary
ding bleaching for 24 h with H2O2, the color of the wood
xylem of kiln-dried birch (B. pendula). Our objective was
pieces could be changed further; however, microscale
to study whether bleaching with aqueous acidic H2O2
defects were detected in fiber secondary cell walls. Con-
solution changes the structure and properties of the
sequently, complementary to results obtained from
uppermost surface of birch boards; therefore, a labora-
microscopic studies, lower hardness values supported
tory-scale surface bleaching method was used. In addi-
the degradation of fiber secondary cell wall in bleached
tion, in order to investigate the extreme effect of H2O2
wood pieces. In addition, contact angle measurements
bleaching on the structure of birch wood, an embedding
indicated increased surface roughness of wood pieces
bleaching method was used.
after embedding bleaching with H2O2.

Keywords: Betula pendula; birch; bleaching; Brinell

Materials and methods
hardness; contact angle; electron microscopy; hydrogen
peroxide.
Wood samples

Introduction
Treatment with acidic or alkaline hydrogen peroxide
(H2O2) is a rapidly increasing technique in the pulp and
paper industry (e.g., Gierer 1990; Kadla et al. 1997) where
H2O2 is used as a brightening agent for mechanical pulp.
However, delignifying properties of H2O2 are limited since
neither acidic nor alkaline H2O2 is able to degrade all
structures of lignin network unless auxiliary substances
or high temperatures are used (Kadla et al. 1999). In addi-
tion, H2O2 also decomposes easily in the presence of
The samples were obtained from three planted silver birch (Betu-
la pendula) trees (denoted as trees 1, 2, and 3) grown in natural
state on a plantation with rich grass-herb vegetation (OMT, Oxa-
lis-Myrtillus type) located in Hollola, Ilomantsi, Finland. The trees
were healthy, relatively fast-grown, 33 years old and with stem
heights of 22.4, 19.5, and 18.4 m, and their diameters at breast
height (1.3 m above ground level) were 24.3, 20.2, and 20.0 cm,
respectively. After felling, the logs were cut into butt and top
logs and then into boards without storage. The boards were
dried conventionally at 37–708C according to the formula
described by Mononen et al. (2002) in a 1.5-m3 laboratory-scale
kiln (Brunner Trockentechnik GmbH, Germany) to about 5%
moisture content of dry weight of wood. One kiln-dried surface

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60 K. Mononen et al.
board from a top log of each stem (1–3) was used as specimen
for this study. In order to investigate the wood material as uni-
formly as possible while studying parallel wood individuals, care
was taken to select only light-colored sample boards that had
the least number of knots and no defects affecting the timber
quality.
Surface bleaching with H2O2 solution
The boards were planed down and smoothed mechanically to a
size of 350=60=10 mm3 to prepare a semi-finished wood
piece. Half of each board was used as untreated reference sam-
ple and was covered with aluminum foil before the surface
bleaching treatment. The other half of the board was exposed
to surface bleaching with 50% aqueous H2O2 solution, pH 3.5
(PP Finnish Peroxides, Voikkaa, Finland). A PMP150 diaphragm
pump equipped with a sprayer (Kremlin, Stains, France) was
used to spray H2O2 solution onto the tangential surface of the
boards placed on an Eta-K conveyor (Danfoss Inc., Baltimore,
MD, USA) at the conveyor velocity vcs0,19 m sy1, followed by
rapid drying (ts10 s, vcs0.06 m sy1, Tsabout 80 8C) under an
infrared dryer (14.5 kW, Solaronics IRT, Vänersborg, Sweden)
using a laboratory-scale device and method similar to Wood-
BriteTM (Malvaranta 2003). The amount of H2O2 solution applied
on the board surface amounted to 48 g my2 in average.
Embedding bleaching with H2O2 solution
Pieces of wood (10=50=50 mm3) cut from the unbleached
parts of the boards used above were placed in an aqueous 35%
H2O2 solution, pH 3.5 (Oy FF-Chemicals Ab, Yli-Ii, Finland) for
24 h at ambient temperature. After the embedding H2O2 treat-
ment, the pieces were oven-dried at 50 8C for 24 h and stabilized
in a desiccator for 24 h. An unbleached wood piece of the same
origin and size was used as a reference sample.
Color measurement
Reflectance spectra, R%(l), were measured on tangential sur-
faces of unbleached and bleached (surface bleaching and
embedding bleaching) wood pieces (boards 2 and 3) about
2 days after the bleaching treatments with a Lambda 900 UV/
VIS spectrophotometer (Perkin Elmer Instruments, Norwalk, CT,
USA) at wavelengths from 190 to 780 nm. The spectra were
analyzed with Lambda 900 UV/VIS/NIR software (Perkin Elmer),
and the color of wood pieces was reported as L*a*b* (CIELAB)
color coordinates using standard observer and illumination of 28
and D65, respectively.
Light microscopy (LM)
Semi-thin cross sections (1 mm) of unbleached and bleached
(embedding bleaching) specimens (boards 1–3) were cut from
the resin-embedded blocks prepared for TEM analysis (see
below) and stained with Toluidine blue O (Merck, Darmstadt,
Germany). The sections were analyzed in bright-field mode with
an Olympus BX51 microscope (Olympus Optical Co., Tokyo,
Japan) equipped with an Olympus C-3030 digital camera.
Environmental scanning electron microscopy
(ESEM)
The surface morphology of tangential surfaces of unbleached
and bleached (surface bleaching) specimens (boards 1–3) was
studied by ESEM with XL30 ESEM TMP environmental scanning
electron microscopy (FEI Co., Eindhoven, The Netherlands)
equipped with a gaseous secondary electron detector (GSE) at
15.0 kV. Three parallel sample pieces (1=5=5 mm3) cut from
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each board were analyzed as such without a coating in a cham-
ber saturated with aqueous vapor at 120 Pa.
Transmission electron microscopy (TEM)
Small pieces of wood (1=0.5=0.5 mm3) from earlywood section
were cut from unbleached and bleached (embedding bleaching)
wood pieces (boards 1–3). The samples were fixed (60 h) with
glutaraldehyde (Electron Microscopy Sciences, Fort Washington,
PA, USA) 2.5% in 0.1 M phosphate buffer, pH 7.0, mixed from
NaH2PO4=H2O (Merck, Darmstadt, Germany) and Na2HPO4 (J.
T. Baker, Deventer, The Netherlands). Prior to fixation, a short
vacuum treatment was applied (max 100 kPa, 5 min). The sam-
ples were then placed in a Lynx EM tissue processor (Reichert-
Jung/Leica Co., Vienna, Austria), washed with 0.1 M phosphate
buffer, pH 7.0, and fixed again with osmium tetroxide, 1% in
phosphate buffer, pH 7.0 (Electron Microscopy Sciences). After
washing out the fixing solution, the samples were dehydrated in
an increasing series (50%, 70%, 94%, abs.) of aqueous ethanol
(Primalco Ltd., Rajamäki, Finland) and then with propylene oxide
(Fluka, Buchs, Switzerland), followed by successive infiltration in
an increasing series (1:0, 3:1, 1:1, 1:3, 0:1 v/v) of propylene oxide
and LX-112 resin (Ladd Research Industries, Williston, VT, USA).
The samples were embedded in a mixture containing LX-112,
nadic methyl anhydride, dodecenyl succinic anhydride, and
2,4,6-tri(dimethylaminoethyl)phenol DMP-30 (Ladd Research
Industries) and polymerized at 37 8C and 60 8C for 24 h and
72 h, respectively. After trimming (Ultratrim, Reichert-Jung/Leica
Co.) and cutting with a diamond knife (Diatome U.S., Fort Wash-
ington, PA, USA) ultrathin cross sections were collected on cop-
per-coated grids (Agar Scientific, Essex, England) and
contrasted with uranyl acetate (Ultrostain I, Leica Co.) and lead
citrate (Ultrostain II, Leica Co.). A total of 148 TEM micrographs
were acquired at 60 kV with a JEM 1200 EX transmission elec-
tron microscope (JEOL Ltd., Tokyo, Japan) equipped with a
charge-coupled device (CCD).
Brinell hardness (HB)
Brinell hardness (HB) of tangential surfaces of unbleached and
bleached (surface bleaching and embedding bleaching) wood
pieces (boards 2 and 3) was measured with a Matertest FMT-
Mec 100 kN test apparatus with FMT ProgSys WIN software
(Matertest Co., Helsinki, Finland). According to the standard
method prEN 1534:1999(E), HB is calculated as follows:
2F
HBs w 1z
x |
gpDyDy(D2yd2) 2 ~
where HB is Brinell hardness in kg mmy2; g, the acceleration of
gravity in m sy2; F, the nominal force in N; D, the diameter of
the ball, 10 mm; d, the diameter of the residual indentation in
mm.
The diameter of the residual indentation d is calculated from
two diameters (d1 and d2) measured at 908 to each other, using
the formula
d1qd2
ds
2
The results were obtained from two parallel samples (average).
Contact angle measurement
Contact angle measurement was used to study the effect of
bleaching on surface roughness of unbleached and bleached
wood surfaces (boards 2 and 3). Dynamic and static contact
 Peroxide bleaching of birch wood 61

Table 1 L*a*b* (CIELAB) color coordinates of unbleached and bleached (surface bleaching and embedding bleaching) birch wood
(average of boards 2 and 3).

Unbleached Surface bleaching Embedding bleaching

L* 83.21 84.37 90.73

a* 3.74 3.02 1.05
b* 17.62 19.16 19.22

angles uc(t) of water droplet placed on tangential surfaces of
unbleached and bleached (embedding bleaching) wood pieces
were measured with a CAM 200 optical contact angle meter
equipped with CCD and an automatic dispenser (KSV Instru-
ments Ltd. Helsinki, Finland) at ambient temperature similar to
the method described by Scheikl and Dunky (1996) using deio-
nized water (Ultra Pure). In order to measure the dynamic con-
tact angle, the needle of the syringe was lowered down near the
surface of the wood specimen and the droplet was dispensed
at a rate of 0.2 ml/s to 4 ml. Advancing contact angles were
recorded at intervals of 1 s on either side of the droplet begin-
ning with the first contact with the liquid and the solid (ts0 s)
without removing the needle from the droplet during dynamic
contact angle measurements. After 20 s, the needle was care-
fully removed from the droplet, and static contact angles of the
sessile drop were recorded, however, with simultaneous wicking
of the liquid into solid wood. Both advancing and static contact
angles were calculated using circular fitting. Because moisture
content, structure, orientation, and semi-finishing procedures of
wood pieces may have a great influence on contact angles (e.g.,
Gardner et al. 1991; Scheikl and Dunky 1998; de Meijer et al.
2000; Stehr et al. 2001; Wålinder and Ström 2001; Pétrissans et
al. 2003), all measurements were made on earlywood sections.
For each specimen, five parallel measurements were completed
to obtain average graphs.
Results
Bleaching with peroxide solution caused a change of col-
or in both types of bleaching processes, that is, surface
bleaching and embedding bleaching (Table 1). After sur-
face bleaching, the lightness, L*, and yellowness, b*, of
the wood pieces increased subtly, contrary to the red-
ness, a*, which decreased slightly. With embedding
bleaching, however, the lightness, L*, of the wood pieces
increased notably and the redness, a*, decreased con-
siderably. On the other hand, the yellowness, b*, of
bleached wood pieces (embedding bleaching) increased
only slightly compared to unbleached wood pieces.
Generally, the cell wall of hardwoods consists of pri-
mary wall (P), secondary wall (S), and intercellular layer
(I) located between adjacent cells (e.g., Côté, Jr. 1984;
Harada and Côté, Jr. 1985; Fujita and Harada 1991). The
secondary wall of lignified fiber cells is composed of an
outer layer, S1, a relatively thick middle layer, S2, and a
thin innermost layer. The tissues of unbleached and
bleached (embedding bleaching) wood pieces were stud-
ied by LM (Figure 1). The fiber cell walls of unbleached
wood pieces of the section remained relatively unbroken
in the cutting of samples, demonstrated in Figure 1a.
However, the effect of bleaching on the structure of fiber
cells is shown in Figure 1b, indicating the fragmentation
and separation of secondary cell wall layer, S2, and the
thin innermost layer in fiber cells. On the other hand, the
outer secondary cell wall layer, S1, the primary wall, P,
and intercellular layer, I, of fiber cells of bleached
(embedding bleaching) wood samples showed no deg-
radation, indicating that under the prevailing conditions,
bleaching with H2O2 solution does not degrade the entire
cell wall structure in wood tissue.
Structural changes caused by bleaching (surface
bleaching) on the surface morphology of the birch boards
were characterized by ESEM (Figure 2). The structure of
the uppermost surface of unbleached boards is demon-
strated in Figure 2a. The pores present in wood, that is,
vessels and pits, had been closed up because of the
mechanical surface treatment. However, with bleaching
(surface bleaching), the pores of the tangential surface
were opened, causing the surface to become more
porous and rough, which is demonstrated in Figure 2b.

Figure 1 Light microscopy image of semi-thin sections (1 mm) of (a) unbleached and (b) bleached (embedding bleaching) birch
wood with rays (R), vessels (V), and fibers (F) stained with Toluidine Blue O (cell walls: bluish red; cytoplasm and RNA: bluish red;
DNA and most tannins: bluish green). The arrow indicates the partial fragmentation and separation of the inner secondary cell wall
layer, S2, of fiber cells.

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62 K. Mononen et al.

Figure 2 Scanning electron microscopy image of tangential planed surface of (a) unbleached and (b) bleached (surface bleaching)
birch wood with 100= magnification showing the open rays (R), vessels (V), and fibers (F) of bleached (surface bleaching) wood
surface.

Figure 3 Transmission electron micrograph of the fiber cell wall of (a) unbleached and (b) bleached (embedding bleaching) birch
with 30,000= magnification showing the rupture of fiber secondary cell wall. P, primary wall; I, intercellular layer; S1, S2, secondary
walls with different microfibrillar orientation. The arrow indicates the innermost layer of the secondary cell wall.

Table 2 Brinell hardness (HB) for unbleached and bleached The ultrastructure of unbleached and bleached
(surface bleaching and embedding bleaching) pieces of wood (embedding bleaching) cell walls was studied with TEM
(average of boards 2 and 3).
(Figure 3). Figure 3a demonstrates the intact structure of
the fiber secondary cell wall and its sublayers, S1 (about
Unbleached Surface Embedding
bleaching bleaching
0.5 microns thick) and S2 (about 2 microns), and the thin
innermost layer of unbleached specimen. With bleaching
HB (embedding bleaching), however, the S2 layer has
(kg mmy2) 3.08 2.53 2.24
become substantially more porous, revealed by the stain-
ing agents uranyl acetate and lead citrate, which have
penetrated into nanoscale ruptures less than 200 nm in
size (Figure 3b). In addition, microscale ruptures have
occurred in the secondary cell wall of fiber cells (Figure
3b). Furthermore, the thin innermost layer has changed.
However, under the conditions of this study, the S1 layer
as well as the primary wall, P, and intercellular layer, I,
have remained unaltered.
The effect of bleaching (surface bleaching and embed-
ding bleaching) on the physical properties of tangential
surfaces of wood pieces was tested by Brinell hardness
(HB) measurements. According to Kollman (1984), the
xylem of birch wood is considered to be soft compared
with several European, North American, and tropical
hardwood species. The results indicate that surface
Figure 4 Dynamic and static contact angles of water on the
surface of birch wood. (a) Continuous line denotes unbleached bleaching decreases the Brinell hardness of pieces of
wood, (b) dashed line indicates bleached (embedding bleaching) birch wood (Table 2). With embedding bleaching, the Bri-
wood. nell hardness of birch wood decreased further, indicating

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that the xylem of birch wood becomes softer with H2O2
bleaching.
Contact angle analysis was made to characterize the
roughness of tangential surfaces of unbleached and
bleached (embedding bleaching) specimens. The results
show that the contact angle of a water droplet placed on
the surface of unbleached wood differs from that of
bleached wood (embedding bleaching; Figure 4). Curves
(a) and (b) in Figure 4 demonstrate the advancing
(dynamic section) and static (static section) contact
angles of water on the surface of wood specimens,
respectively. In the beginning of the dynamic section, that
is, just after contact of liquid with wood surface,
increased values of the advancing contact angle were
measured for bleached wood (embedding bleaching),
indicating that the droplet spread at a slower rate along
the surface, possibly because of a higher surface rough-
ness. In a few seconds, however, the advancing contact
angles of water placed on bleached wood (embedding
bleaching) decreased more rapidly than those recorded
on unbleached wood, possibly because of a higher rate
of liquid penetration into bleached wood surface. Simi-
larly, in the static section, the static contact angle of
water placed on bleached wood (embedding bleaching)
decreased at a higher rate, indicating stronger wicking
with possibly higher porosity of the bleached specimen.
Discussion and conclusion
The results show that bleaching with H2O2 solution (sur-
face bleaching and embedding bleaching) changes the
color of kiln-dried birch boards toward white and less
red. However, the yellowness changes only slightly with
bleaching (surface bleaching and embedding bleaching).
The results are in good accordance with those obtained
by Möttönen et al. (2003).
The current study provides evidence of microscale
changes in the surface structure of birch wood occurring
with surface bleaching with a H2O2 solution combined
with rapid infrared drying. Scanning electron microscopic
studies show that after surface bleaching, the tangential
surface of wood became more porous. Besides the color
changes caused by peroxide bleaching (surface bleach-
ing), the increase in roughness probably resulted from the
wetting of the bleaching solution followed by an imme-
diate drying under an infrared dryer. Furthermore, images
obtained by light microscopy and transmission electron
microscopy indicate that embedding bleaching with H2O2
solution does not destroy basic anatomical features of
wood tissue, but changes can be observed in interior
sublayers of fiber secondary cell wall, namely in the S2
layer and in the thin innermost layer, after the embedding
bleaching treatment. With embedding bleaching, the
structure of the S2 layer in fiber cells is slightly collapsed,
including ruptures, and in places the S2 layer is partially
torn, thus increasing the inner porosity of wood material.
Meanwhile, the innermost layer was possibly degraded
because of embedding bleaching with H2O2.
The results indicate that the Brinell hardness of wood
subjected to H2O2 bleaching (surface bleaching and
embedding bleaching) is lower than that of unbleached
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Peroxide bleaching of birch wood 63
wood. The lower hardness values for bleached wood are
probably due to weaker secondary cell walls and
increased porosity. In addition, contact angle measure-
ments imply that embedding bleaching with H2O2
increases the surface roughness of birch wood. In earlier
investigations on the relation between the structure of
surface of wood and the contact angle, it was found that
the rough-sawn samples of oak (Quercus robur L.), pine
(Pinus sylvestris L.), and meranti (Sorea spp.) displayed
a slightly higher level of contact angle than the corre-
sponding planed samples (Winfield et al. 2001).
The information obtained in this study could be of
great importance in finishing wooden products bleached
with H2O2. Besides changed coloring properties, micro-
scale changes in wood structure as well as increased
porosity and surface roughness may supply a more
favorable surface accessible to finishing agents. Using
adequate surface finishing agents, color, hardness, and
durability of bleached surfaces could be improved.
In summary, the color of the wood pieces could be
changed with H2O2 bleaching. On the other hand, bleach-
ing with H2O2 solution affects the microscale structure of
wood tissue, thus decreasing the hardness and increas-
ing the surface roughness of the bleached part of the
wood. However, more knowledge is required on chemical
reactions between wood constituents and peroxide rad-
icals causing the partial degradation of secondary cell
wall, altering the surface properties as well as the color
change.
Acknowledgements
The authors would like to thank Alpo Pelttari and Virpi Miettinen
(University of Kuopio) for kind cooperation with electron micro-
scopic analyses, Pertti Malvaranta (Altonic Ldt.) for his valuable
help with the surface bleaching method, Katri Luostarinen (Uni-
versity of Joensuu, Faculty of Forestry), who was of great assis-
tance in interpreting wood anatomy, and Veikko Möttönen
(University of Joensuu, Faculty of Forestry) for sampling the
trees and performing kiln drying of the boards. This research
was funded by Academy of Finland.
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Received March 1, 2004