Cellulose (2014) 21:607–614
DOI 10.1007/s10570-013-0104-3
ORIGINAL PAPER
The effect of eucalypt pulp xylan content on its bleachability,
refinability and drainability
Valéria J. Gomes • Dalton Longue Jr. •
Jorge L. Colodette • Robisnéa A. Ribeiro
Received: 24 April 2013 / Accepted: 5 November 2013 / Published online: 21 November 2013
Ó Springer Science+Business Media Dordrecht 2013
Abstract Currently, bleached eucalypt pulps are
largely used for printing and writing (P&W) and
sanitary (tissue) paper grades. Among the many pulp
quality requirements for P&W and tissue paper
production the xylan content is one of the most
significant. For P&W papers, increasing xylans
improve pulp refinability and strength properties but
negatively affect bulk and drainability. For tissue
paper, xylans are purportedly advantageous during
paper drying in the Yankee cylinder but negatively
affect paper bulk and may increase dusting during
paper manufacture. On the other hand, bleachability is
a very important parameter for both P&W and tissue
grade pulps since bleaching cost is the second most
significant in eucalypt bleached kraft pulp production.
The aim of this study was evaluating the influence of
eucalyptus pulp xylan content on its bleachability,
refinability and drainability. A sample of industrial
unbleached eucalyptus kraft pulp containing 15.6 %
xylans was treated with various alkali charges at room
temperature in order to obtain materials with different
xylan contents. The pulps were bleached to 90 % ISO
brightness with the O–DHT–(EP)–D sequence and
evaluated for their refinability and drainability. By
increasing the alkali concentration in the range of
V. J. Gomes
D. Longue Jr. (&)

J. L. Colodette
R. A. Ribeiro
Pulp and Paper Laboratory, Federal University of Viçosa,
Viçosa, MG CEP 36570-000, Brazil
e-mail: daltonufv@yahoo.com.br
10–70 g/L pulps of 14.5–5.9 % xylans were produced
with no significant impact on cellulose crystallinity.
The decrease of xylan content significantly decreased
pulp bleaching chemical demand, water retention
value and refinability and increased pulp drainability.
Keywords Eucalypt
Alkali extraction

Xylans
Bleaching
Refinability
Drainability
Introduction
The two most important applications of eucalypt kraft
pulps are for P&W and tissue paper grades. Because
P&W and tissue paper grade pulps are made from fully
bleached fibers, bleaching represents an important
fraction of the manufacturing cost of these pulps.
Several studies on bleaching of eucalyptus pulps
aimed to these grades have been published recently
(Colodette et al. 2007; Pedrazzi et al. 2010).
The O-acetyl-4-O-methylglucuron-xylans are the
most important eucalyptus hemicelluloses. Acetyl
groups and 4-methylglucuronic acids are responsible
for increasing the alkali consumption during pulp
production (Magaton et al. 2011). In addition, the
4-methylglucuronic acids are the precursors of hex-
enuronic acids (HexA), substances that negatively
impact pulp brightness stability (Buchert et al. 1997).
Eucalyptus pulp bleachability is affected by the kappa
number composition. At a given kappa number,
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608 Cellulose (2014) 21:607–614

different chemical consumptions are observed for
different pulps depending upon their contents of
HexA, lignin and other oxidizable structures (Costa
and Colodette 2002, 2007; Buchert et al. 1997; Jiang
et al. 2000). Since pulp HexA content is largely
affected by its xylan content, the removal of the latter
may have significant impact on bleachability.
The xylan content can be decreased by pulp
treatment with alkali under controlled conditions,
since xylans are alkali soluble (Liu et al. 2011; Sum
et al. 2000; Bjerre et al. 1996; Gabrielii et al. 2000; Al-
Dajani and Tschirner 2008). The alkali concentration
must be well controlled to avoid cellulose crystallinity
disturbance, which can limit pulp use for paper grade
products (Gehmayr and Sixta 2011).
Pulp xylan content affects its application in the
paper manufacturing processes. For P&W paper
grades xylans are desirable for improving pulp refin-
ability and bonding related strength properties (Ped-
razzi et al. 2010). Among the many pulp quality
requirements for tissue grade paper production, the
xylan content has been the most controversial.
Purportedly, xylans are advantageous during paper
drying in the Yankee cylinder but negatively affect
paper bulk and may increase dusting during paper
manufacture (Magaton et al. 2009). On the other hand,
xylan depleted pulps presents low bonding and
consolidation capacity and produce bulkier papers.
This study aimed at developing a technique to
prepare several levels of xylan depleted eucalyptus
unbleached kraft pulps in order to understand their
influence on pulp bleachability, refinability, and
drainability.
time (30 min), a sample of liquor was squeezed out
and the pulp was washed with excess distilled water.
The four alkali treated and the reference pulps were
subjected to analysis of viscosity (SCAN cm-15:99),
gravimetric yield and xylans content (HPAEC–PAD)
after acid hydrolysis according to TAPPI T249). The
filtrates collected after extractions were analyzed for
COD (Standard Methods 5220D). All experiments
were performed in duplicate.
The pulps were pre-delignified with oxygen in a
reactor/mixer, Mark V model (Quantum Technologies
Inc.) and bleached with the DHT–(EP)–D sequence
under the conditions presented in the Table 1. The
DHT, (EP) and D stages stand for hot chlorine dioxide,
alkaline extraction reinforced with hydrogen peroxide
and chlorine dioxide bleaching, respectively. After
each bleaching stage, carried out in polyethylene bags,
the pulps were washed with the equivalent of 9 m3 of
distilled water per ton of pulp. All stages were
performed in duplicate. The bleached pulps were
evaluated for their kappa number (TAPPI T236 cm-
85), brightness (TAPPI T525 om-92), brightness
reversion (TAPPI UM200—4 h, 105 ± 3 °C) and
hexenuronic acid content (TAPPI T282 pm-07).
The bleached pulps were refined in a PFI mill and
evaluated for their drainability according to TAPPI
248 om-00 and TAPPI 200 sp-01 standard procedures,
respectively. The number of revolutions was varied in
order to obtain three levels of refining, allowing for
the development of refining curves in the range
15–50°SR. Paper sheets were formed using a TAPPI
former, with a grammage of approximately 60 g/m2,
according to TAPPI 205 sp-02 standard. The hand

Experimental Table 1 General oxygen delignification and bleaching

conditions
An industrial unbleached Eucalyptus urograndis kraft Conditions O DHT (EP) D
pulp with the following characteristics was used:
Consistency (%) 10 10 10 10
kappa number = 16.1, viscosity = 1,226 dm3/kg,
Time (min) 60 120 60 120
brightness = 42.1 % ISO, xylans content = 15.6 %
Temperature (°C) 100 75 82 76
and HexA content = 61.8 mmol/kg. Xylan removal
O2 pressure (kPa) 500 – – –
from the pulp was carried out in polyethylene bags by
O2 (kg/odt) 15 – – –
the so-called cold caustic extraction technique using
ClO2 as Cl2 – 17.4; 16.2; – 5; 10; 15
four sodium hydroxide concentrations (10, 30, 50 and
(kg/odt) 14.4; 11.4; 8.6
70 g/L NaOH), while the other operating conditions
H2O2 (kg/odt) – – 3.0 –
were kept constant (30 min, 30 °C, 10 % consis-
NaOH (kg/odt) 15 – –
tency). The pulp was thoroughly mixed with NaOH
End pH – 3.0 10.8 4.5
before reaction and after completion of the reaction

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Cellulose (2014) 21:607–614
sheets were placed in an environmentally controlled
room at temperature of 23 ± 1 °C and relative
humidity of 50 ± 2 %. Tensile index, a pulp strength
property, was measured according to Tappi T494 om-
06. The water holding capacity of the pulps was
evaluated using Water Retention Value—WRV,
according TAPPI um 256 standard procedure.
Wide-angle X-ray diffraction (WAXD) analyses
were carried out using a PANalytical X’pert PRO
diffractometer with a cobalt tube. The collected data
were prepared using the Origin 8.0 software. The use
of WAXD counts offers a simple and quick method for
determining cellulose crystallinity index. The mini-
mum between 101 peak (amorphous peak) and 002
peak (crystalline peak) indicates the reflection inten-
sity of the amorphous material (Iam) (Mwaikambo
and Ansell 2002).
Statistical analyses were carried out using the
Statistica software (version 7.0) using the 5 % signif-
icance level for variance analysis. The hypotheses
tested were: H0: all means are equal, i.e., there is no
significant difference between treatments, and Ha:
there is at least an average statistically distinct from the
others. Tukey test was applied to find out which
treatments were distinguished from each other. In
addition, the Curve Expert software (version 1.4) was
used to obtain the models for drainability and refin-
ability analysis of the pulp samples at different beating
levels. The adjusted equations were compared by
‘‘F-test’’, using the identity test models at 5 % signif-
icance level, according to the methodology for linear
(Regazzi 1993) and nonlinear models (Regazzi and
Silva 2004). The hypotheses tested were: H0: all
equations are equal and can be represented by a
reduced common equation, and Ha: the equations are
statistically different and cannot be reduced to a
common equation.
Results and discussion
Eucalypt kraft pulps containing variable amounts of
xylans were prepared by cold caustic extraction (CCE)
of the pulp with alkali concentrations of 10–70 g/L
NaOH. The main characteristics on the untreated (Ref)
and alkali treated pulps are presented in Table 2. It is
observed that a wide range of pulp xylan concentra-
tions were obtained by the CCE treatment, which is
explained by the xylans intrinsic solubility in alkali
609
(Al-Dajani and Tschirner 2008; Sjöström and Alén
1999; Hashimoto and Hashimoto 1975; Scott 1989;
Cunningham et al. 1986; Walton et al. 2010). Xylan
removal from pulp is less challenging then from wood
due to the low concentration of lignin in the former. As
the concentration of the NaOH solution increased,
increased xylan amounts were solubilized and
removed from the pulp, reaching 62 % removal when
the original pulp was treated with 70 g/L NaOH. The
xylan removal had a direct effect on pulp yield and
HexA content. HexA groups are directly attached to
the xylan chains, and are thus removed along with
these polymers. The yield drop was mainly caused by
the xylan weight loss but other materials such as
degraded cellulose and lignin also contributed to this
yield loss as has been reported elsewhere (Schild et al.
2010). Low molecular weight carbohydrates are
generally soluble under strong alkaline conditions
and potentially extractable by alkali. The decrease in
pulp kappa number with increasing alkali concentra-
tion demonstrates the partial removal of lignin and
HexA during the CCE treatment. The alkali treatment
with 70 g/L NaOH decreased pulp kappa number by
8.2 units and HexA content by 39 mmol/kg. Given
that one kappa number unit is equivalent to
11.6 mmol/kg HexA (Li and Gellerstedt 1997; Costa
and Colodette 2007), the HexA contribution amounted
to about 3.4 kappa units of the total 8.2 units removed
across the CCE treatment. Therefore, the amount of
lignin removed was about 0.7 %, assuming that each
kappa unit contains about 0.15 % lignin (Ventorim
et al. 2009). Pulp brightness increased slightly with
increasing alkali concentration above 50 g/L NaOH
due to removal of small amounts of lignin fragments,
which are the true pulp chromophores; the brightness
gains could have been higher but was likely offset by
lignin darkening that typically occurs when pulp is
exposed to strong alkaline conditions due to conver-
sion of lignin phenol moieties (leuco chromophores)
into quinones ones (chromophores). Darkening did
occur when the CCE treatment was run at low NaOH
concentrations (10 and 30 g/L). Pulp viscosity tended
to increase with increasing alkali concentration due to
removal of the low molecular weight carbohydrates,
which more than offset the normal viscosity losses
occurring when pulp is exposed to alkali. The only
exception was the treatment with 10 g/L NaOH that
caused a slight but not significant decrease on
viscosity. The potential viscosity increase caused by
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610 Cellulose (2014) 21:607–614

Table 2 Effect of NaOH concentration on the performance of Table 3 Performance of the oxygen delignification on refer-
the cold caustic extraction (CCE) treatment applied to an ence and xylan depleted eucalypts pulps
eucalypt kraft pulp
Results Xylans content (%)
Results NaOH concentration (g/L)
15.6 14.5 10.8 8.1 5.9
0 10 30 50 70
(Ref) Kappa number 10.9a 10.1a 9.0b 7.1c 5.4d
a a b c
HexA (mmol/kg) 59.8 59.8 48.1 33.1 22.0d
Xylans (%) 15.6a 14.5a 10.8b 8.1c 5.9d
Lignin (%) 0.9 0.7 0.7 0.6 0.5
Kappa number 16.1a 15.2b 13.3c 10.5d 7.9e
Viscosity (dm3/kg) 1101a 1071b 915c – 904c
HexA (mmol/kg) 61.8a 61.4a 50.0b 34.7c 22.8d
Brightness (% ISO) 49.2a 53.4b 54.0c 55.2d 57.8e
Lignin (%) 1.6 1.5 1.3 1.1 0.9
Kappa drop (%) 32.3 33.6 32.3 32.4 31.7
Kappa removedA – 0.9 2.8 5.6 8.2
HexA drop (%) 3.1 2.6 3.7 4.6 3.5
HexA removed – 0.4 11.8 27.1 39.0
Lignin drop (%) 46.7 50.1 46.0 43.4 41.0
(mmol/kg)A
Viscosity drop (dm3/ 125 133 330 – 404
Lignin – 0.1 0.3 0.5 0.7
kg)
removed (%)A
Brightness gain (% 7.1 13.3 12.6 12.0 14.9
Gravimetric – 98.5a 96.7b 89.2c 85.7d
ISO)
yield (%)
Brightness (%ISO) 42.1a 40.1b 41.4a 43.2c 42.9d Averages followed by the same letter in the same line do not
3
Viscosity (dm /kg) 1226 a
1204 a
1245 a
1278 a
1308 b differ by the Tukey test, at the 5 % significance level
COD of the filtrate – 6.3a 66.3b 196.4c 206.6d Oxygen delignification: 10 % consistency, 100 °C, 60 min, O2
(kg O2/t pulp) pressure 500 kPa, 15 kg of O2/odt and 15 kg of NaOH/odt

Averages followed by the same letter in the same line do not

differ by the Tukey test, at the 5 % significance level
CCE: 10 % consistency, 30 °C, 30 min
A
Difference between treatments and reference
the very low xylan removal at 10 g/L NaOH was not
sufficient to offset the normal pulp viscosity loss that
occurs when pulp is exposed to alkali (alkali induced
hydrolysis and peeling reactions). The CCE treatment
filtrate COD (chemical oxygen demand) confirmed the
xylan and yield loss data previously discussed. More
material was dissolved in the alkaline solution as the
NaOH concentration increased, thus increasing filtrate
COD. Note the COD is an important parameter to
indirectly measure the amount of organic matter in a
liquid stream.
The reference and alkali treated pulps were oxygen
delignified under similar conditions. The results of
Table 3 show kappa reductions across oxygen delig-
nification (O-stage) ranging from 31.7 to 33.6 % for
the CCE treated pulps, with the reference pulp also
falling in this range (32.3 %). The results suggest that
O-stage efficiency is not significantly affected by pulp
xylan removal. In fact, it was expected that the O-stage
efficiency would be higher for the xylan depleted
pulps because they contained less HexA, which
notoriously have a negative effect on O-stage
efficiency (Colodette et al. 2006). However, this effect
was masked by the fact that the xylan depleted pulps
had lower lignin contents than the reference one and
lignin positively affects O-stage efficiency. In other
words, pulps containing more lignin tend to show
higher kappa drops across the O-stage. The HexA
removal in the O-stage was very low (2.6–4.6 %). This
result was expected since HexA do not react with
oxygen (Vuorinen et al. 1996). The small HexA loss
across the O-stage is likely caused by slight xylan
dissolution under the alkaline conditions of this stage.
The pulp viscosities after O-stage were lower for the
CCE treated samples (904–1,071 dm3/kg) when com-
pared to the reference (1,101 dm3/kg), with the
negative effect being more pronounced with increas-
ing NaOH concentration in the CCE. The reference
and the 70 g/L NaOH treated pulp samples lost 125
and 404 dm3/kg viscosity, respectively, across the
O-stage. Pulps treated with NaOH are more suscep-
tible to degradation in the O-stage since they contain
less hemicellulose in the fiber surfaces. Hemicellu-
loses are known to protect the cellulose chains against
the attack of radical species which are present in the
O-stage (Colodette et al. 2011). The xylan depleted
pulp samples tended to gain more brightness
(12–14.9 % ISO) across the O-stage than the reference

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Table 4 Performance of the DHT–EP–DA bleaching on oxygen delignified reference and xylan depleted eucalypts pulps
Results Xylans content (%)
15.6 14.5 10.8 8.1 5.9

Total active chlorine (%)B 3.87a 3.75a 3.07b 2.27c 1.99d

a a a a
Bleachability (ud kappa/% active Cl) 2.8 2.7 2.9 3.1 2.7a
Brightness (%ISO) 89.8a 89.8a 89.9a 89.8a 90.1a
a a a a
Brightness reversion (%ISO) 2.7 2.6 2.4 2.5 2.2a
3 a a b
Viscosity (dm /kg) 926 911 813 – 767c
a b b c
HexA (mmol/kg) 6.6 7.3 7.3 9.4 5.5d
Average values followed by the same character in the same line do not differ by the Tukey least
A
DHT–EP–D bleaching sequence: DHT-stage: 10 % consistency, 75 °C, 120 min, 3.0 end pH and 17.4–8.6 kg ClO2 (as Cl2)/odt;
(EP)-stage: 10 % consistency, 82 °C, 60 min, 10.8 end pH and 3.0 kg H2O2/odt; D-stage: 10 % consistency, 76 °C, 120 min, 4.5 end
pH and 5–15 kg ClO2 (as Cl2)/odt
B
Total active chlorine = ClO2 (kg/odt) 9 2.63 ? H2O2 (kg/odt) 9 2.09; ClO2 9 2.63 = Cl2

(7.1 %). It is apparent that the strong alkaline condi-
tion in CCE treatment created certain lignin structures
which were more amenable to oxidation in the O-stage
then the untreated pulp, thus improving brightness.
The oxygen delignified pulps were bleached with
the DHT–(EP)–D sequence under similar conditions,
keeping a constant kappa factor (0.16) in the first
bleaching stage and varying the dose of chlorine
dioxide in the second stage. All the experiments were
aimed at achieving a final brightness of 90 ± 0.5 %
ISO. The most significant bleaching results are shown
in Table 4. The lowest value of total active chlorine
consumption was attained with the pulp having the
lowest xylan content. This result was anticipated given
that this pulp sample had the lowest kappa number
after the O-stage. There was a clear trend of decreased
total active chlorine consumption with decreasing
pulp xylan content. There was no statistical difference
among treatments for bleachability and brightness
reversion values. The bleached pulp HexA content
varied between 5.5 and 9.4 mmol/kg and although
statistical differences were detected among the values,
there was no clear trend on the effect of xylan removal
by the CCE treatment; the lack of a clear trend is
explained by the different total active chlorine charges
required for bleaching of the various pulps to *90 %
ISO. The bleached pulp viscosities ranged from 767 to
926 dm3/kg, with the highest value found for the
reference sample and lowest for the sample treated
with the highest concentration of NaOH solution. This
confirms the important role played by xylans in
protecting the cellulose chains against degradation
by the oxidizing bleaching reagents. Thus, by remov-
ing xylans, the cellulose chains become susceptible to
degradation (Gustavsson and Al-Dajani 2000). Also,
about the brightness reversion, it was no statistical
differences among the samples.
When treating kraft pulp with strong alkali there is
always the risk of converting native cellulose (cellu-
lose I) into cellulose II. Hence, it was necessary to
prove that the CCE treatments were not strong enough
to convert cellulose I in cellulose II. This conversion is
undesirable when producing pulp for paper applica-
tions although it may not be a big problem for
dissolving pulp applications. An easy way to deter-
mine whether or not cellulose I was converted into
cellulose II is by measuring cellulose crystallinity by
X-ray diffraction analysis for example. The pulp X-ray
diffractogram shows different patterns for cellulose I
and II. Earlier attempts to assess cellulose crystallinity
were actually done by treating pulp with strong NaOH
solution (Segal et al. 1959). The so-called peak height
method, developed by Segal and co-workers, is an
empirical method being the most common and simple
method to determine the degree of crystallinity
(Terinte et al. 2011). This method has been widely
used for the study of crystallinity of native cellulose.
Figure 1a–f shows X-ray diffractograms of the five
pulp samples, including pulp xylan content and
crystallinity indexes, plus an additional sample that
was treated with 18 % NaOH in order to intentionally
convert cellulose I into cellulose II. There were no
large variations among the crystallinity indexes
(58.3–63.2 %) of the various CCE treated samples of

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612 Cellulose (2014) 21:607–614

Fig. 1 X-ray
diffractograms and
crystallinity index for
reference and CCE treated
pulps of this study and of a
sample treated with high
NaOH concentration (18 %)
representing cellulose II

this study, confirming the absence of cellulose II.

However, the X-ray diffractogram of the pulp sample
treated with excess NaOH is totally different than the
others, indicating the presence of cellulose II.
Pulp refinability can be loosely defined as the
amount of energy required during refining to achieve a
given paper property such as tensile strength, sheet
density, etc. High pulp refinability is always desirable
because it means low energy consumption for refining.
Energy is a very important component of the produc-
tion cost for certain paper grades. Printing and writing
paper grades require significant amounts of energy to
achieve the required resistance to drainage of
30–35 °SR in order to achieve a minimum tensile Fig. 2 Effect of pulp xylan content on the energy consumption
required to achieve 20 Nm/g tensile index
index (TI) of about 60 Nm/g and benefit from pulps of
high refinability. Pulps that are used in the manufacture
of tissue paper are only slightly refined to about 20 °SR on the refining energy consumption to achieve a tensile
(TI about 20 Nm/g). An excess refining impairs tissue index at 20/60 Nm/g for tissue and P&W applications.
papers ability to absorb water and also retain water It is apparent that by increasing of the xylans content
through their capillaries (Vuorinen et al. 1996). from 6 to 16 % for both tissue and P&W application,
Figure 2 shows the effect of the pulp xylans content the energy consumption decreased by 100/74.6 %,

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Cellulose (2014) 21:607–614
Fig. 3 Effect of pulp xylan content on the resistance to
drainage degree (°SR) at 20 Nm/g tensile index
Table 5 Effect of xylan content on pulp water retention value
Xylans content (%) 15.6 14.5 10.8 8.1 5.9
WRV (%) 162a 161a 154b 141c 131d
Averages followed by the same letter in the same line do not
differ by the Tukey test, at the 5 % significance level
which corresponds to approximately 10/7 % energy
savings per each 1 % increase in xylans content,
respectively. It is known that xylans exert positive
influence on the swelling, hydration, and fiber flexi-
bility, which favors the pulp refining process (Vuori-
nen et al. 1996).
Pulp drainability affects the paper machine speed
and runnability. It is measured by the drainage
resistance value (°SR) at a given tensile index.
Figure 3 shows that pulps with lower xylan contents
have higher drainage resistance at a given tensile index
for both applications, mainly for P&W applications
that require higher tensile index (TI = 60 Nm/g) than
tissue paper (TI = 20 Nm/g). Therefore, low xylan
pulps for tissue applications will drain faster and
improve paper machine speed and runnability.
The water retention value (WRV) data for the five
bleached and unrefined pulps samples with different
amounts of xylan are shown in Table 5. The removal
of pulp xylans by CCE treatment to levels of 10.8 % or
lower significantly affected the water retention of the
fibers. The WRV is a combined property involving
chemical effects (hemicellulose content) and physical
effects (fiber population, total pore volume and
distribution of the capillaries in dimension). Pulps
with low levels of xylans tend to retain less water and
613
thus have lower levels of water retention (Foelkel
2007).
Conclusions
The CCE treatment with NaOH (10–70 g/L) was
effective in reducing eucalypt kraft pulp xylan content
from 15.6 % to levels in the range of 14.5–5.9 %.
The CCE treatment with 10–70 g/L NaOH dropped
pulp kappa number from 16.1 to levels in the range
15.2-7.9 and decreased total active chlorine demand
from 3.87 (ref) to 1.99 % (70 g/L NaOH) to bleach the
pulps to *90 % ISO brightness.
Pulp xylan content had no significant effect on
oxygen delignification efficiency and bleachability.
Pulp refinability was negatively affected by
decreasing xylan content at a given tensile index.
Pulp drainability was positively affected by
decreasing xylan content at a given tensile index.
Pulp water retention value was negatively
affected by decreasing xylan content.
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