Textile Research Journal Article

Enzyme Treatment of Wool and Specialty Hair Fibers

Trina Das and Gita N. Ramaswamy1
Abstract Enzyme treatment is one of the most Department of Apparel, Textiles, and Interior Design
prospective eco-friendly processes, for treating Kansas State University, Manhattan, KS 66502, USA
wool. Although, extensive research has been con-
ducted on the effectiveness of enzymes as anti-
felting agents for wool, the use of enzymes as
scouring agents for wool, versus conventional
soap-scouring has not been studied. Furthermore,
limited studies have been conducted on enzyme
treatment of specialty hair fibers. This study eval-
uated the efficiency of enzymes (xylanase, pecti-
nase, savinase, and resinase) in scouring wool,
(merino and rambouillet) and specialty hair fibers
(llama, alpaca, mohair and camel), in comparison
with control treatments with hot water, and con-
ventional soap. Various physical, chemical, and
structural properties of the treated and untreated
fibers were evaluated. Xylanase, and pectinase
were found to clean the fibers as efficiently as soap,
but without causing any physical damage to the
fibers. Resinase was however, not an efficient scour-
ing agent.

Key words enzyme processing, wool, speciality

hair fibers, scouring, protein fibers

The unique aesthetic quality of pure wool has made it
irreplaceable even in a market dominated by its inexpen-
sive and abundantly available synthetic versions such as
acrylics. Wool constitutes a minor segment (1.98%) of the
total textile fibers produced globally [1]. However, a signif-
icant portion of the wool is consumed by the high-end
fashion market because of its warmth, resiliency, and
handle. Within animal hair fibers, specialty hair fibers
are considered to be even more exquisite than sheep wool
[2]. Specialty hair fibers are fibers, obtained from animals
other than sheep, such as, mohair, alpaca, llama and
camel [3]. Mohair, obtained from the angora goat, is a
long, white, and lustrous fiber, devoid of any crimp. Camel
hair, shed by the two-humped Bactrian camel, is golden-
tan in color. Llama fibers, obtained from the ‘llamas’ of
the Andes mountains, are fine and lustrous. Alpacas,
which are also native to the Andes mountains, are domes-
ticated llamas and yield finer and stronger fibers than the
llamas [3]. These fibers, mostly obtained from animals
native to remote corners of 1the world, have a very small
annual production, but capture the best markets in the
high fashion industry [4]. Therefore, in spite of a small
quantitative contribution, the significance of wool and spe-
cialty hair fibers in the apparel and textile industry cannot
be under-rated.
Animal hair fiber, especially sheep wool, has to pass
through various stages of processing and cleaning (to get
rid of the dirt, grease, vegetable matter, and other impuri-
ties in the raw state) before it can qualify as a marketable
product [5]. Conventionally, some of these processes
1
Corresponding author: fax: +1785-532-3796; e-mail: ramas-
wam@humec.ksu.edu

Textile Research Journal Vol 76(2): 126–133 DOI: 10.1177/0040517506063387 www.trj.sagepub.com © 2006 SAGE Publications
Figures 1-4 appear in color online: http://trj.sagepub.com
 Enzyme Treatment of Wool and Specialty Hair Fibers T. Das et al.
require chlorination or application of chlorine-containing
polymer, such as Hercosett [6, 7], which results in high lev-
els of organic halogens discharged in waste-water [8]. This
has been an issue of major environmental concern and has
encouraged a lot of research in alternative eco-friendly
processes such as enzyme treatment [6–8].
Enzymes are natural proteins which act as bio-catalysts
[9]. Most of the enzymes used in textiles are hydrolases,
which catalyze cleavage reactions through hydrolysis [6].
Examples are proteases, which break down proteins into
amino acids and smaller peptides, lipases that break down
lipids into fatty acids and glycerol, and cellulases that break
down cellulose into glucose [9].
Enzymes used in wet-processing treatments of cotton,
such as scouring, desizing, and stonewashing have already
been introduced in the textile industry [10] and the possi-
bilities of enzyme treatment for other fibers, especially
wool, are under extensive research. Studies have been con-
ducted on the effectiveness of proteolytic (6, 11, 12) and
lipolytic [13] enzymes in improving wool properties such as
shrink resistance, softness, and wettability. The review
showed that extensive work has been done to determine
the efficiency of enzymes in finishing treatments of wool,
such as anti-felting treatments [6, 14, 15]. However, the
effectiveness of enzymes as scouring agents for wool fibers,
in comparison with conventional soap scouring treatments
has not been studied. Furthermore, most work on enzyme
treatment of wool has been confined to studies of a single
type of wool – mainly merino wool. Limited work has been
done on the enzyme treatment of specialty hair fibers [16].
As the grease content of these fibers are much less than in
sheep wool [17–20], enzyme scouring of these fibers, under
mild treatment conditions, for cleaning and improving
softness, would be a worthwhile treatment. The enzymes
used in this research are savinase, resinase, xylanase and
pectinase. Savinase is a proteolytic enzyme, used in laundry
detergents to remove protein-based stains [21]. Resinase is
a lipase enzyme used in the paper pulp industry [22]. Apart
from these the effects of using a xylanase, which breaks
down hemicellulose [23], and pectinase, which breaks down
pectins, which are complex mixtures of polysaccharides
[24], were also studied. Xylanase, and pectinase were cho-
sen to observe the efficiency of these enzymes in breaking
down the waxes and sugar, present in the wool grease.
Therefore, the objective of this study was, to do a com-
parative study of two varieties of wool and four varieties of
specialty hair fibers, scoured with the enzymes xylanase,
pectinase, savinase and resinase, and compare the results
to plain hot-water-treated, soap-scoured, and untreated
wool – for control. The enzyme-treated and control samples
were evaluated for mechanical, structural, chemical and
biological properties. The grease content of the treated
and untreated fiber samples was also evaluated to measure
and compare the cleaning efficiencies of the various treat-
ments.
127 TRJ
Experimental
Treatments
Two varieties of sheep wool (merino and rambouillet) and
four varieties of specialty hair fibers (llama, alpaca, camel,
and mohair) were used in this study. Three replications
from each of the six fiber types were subjected to four dif-
ferent enzymes scouring treatments (with xylanase, pecti-
nase, savinase, and resinase) and two control treatments
(with hot water and soap). Thus there were eighteen samples
for each of the six treatments, and each fiber sample con-
sisted of 10 g of fiber selected at random from the respec-
tive bags of fibers obtained from different shearing stations.
Enzymes pectinase (Bioprep 3000L), xylanase (Novozym
628) and savinase (Savinase 16L, TYPE EX) were obtained
from Novo Nordisk Biochem North America Inc. and enzyme
Resinase A 2X was obtained from Novozymes North Amer-
ica, Inc. All the treatments were conducted for 5 minutes at a
temperature of 60°C. All four enzymes were used at a con-
centration of 0.2% o.w.f. and the soap-scouring treatment
was done using 2 g/mL of AATCC soap. For each treat-
ment, 10 g of fiber samples were used with 300 mL of water
for the hot water treatment and 298 mL of water for the
enzyme and soap-scouring treatment, to get a material to
liquor ratio of 1 : 30. A pH of 9.32 for xylanase, pectinase,
and soap scouring, 9.0 for savinase, and 7.0 for resinase
treatment were used (according to optimum conditions for
each enzyme, obtained from literature). After each scour-
ing treatment, the fiber samples were rinsed thoroughly in
cold water and air dried. The physical, chemical and struc-
tural property, and grease content of all the treated, and
untreated samples of each fiber type, were then evaluated
and compared.
Physical Analysis
Moisture content, of the conditioned fibers, and fiber
diameter were measured according to the standard proce-
dures [25–27].
Chemical Analysis
Amino acid analysis was performed on single replica-
tions for each treated and untreated fiber type, using the
‘Model 420 A Derivatizer’. The samples were hydrolyzed
for 24 hours at 110°C in 6 N solution of HCl, under vac-
uum and then derivatized using phenylisothiocyanate
(PITC). Finally, the derivatives were analyzed in the high-
pressure liquid chromatography (HPLC) unit. Standard areas
used were from 20 µL of a 25 nmol/mL standard solution.
Fourier transform infrared (FTIR) spectroscopy was
performed on single replications for each treated and
untreated fiber types, using the Perkin Elmer Spectrum
TRJ 128 Textile Research Journal 76(2)
Table 1 ANOVA test results showing the effects of treatment and fiber type on all the properties tested on processed wool
fibers.
Effect of treatment
Properties tested F-value
Moisture content 114.25
Tenacity 619.85
Elongation 12.06
Diameter 3.04
Grease content 3.20
*Degree of freedom for treatment type = 6 and fiber type = 5
One FTIR spectrophotometer. A single bounce Universal
Attenuated Total Reflectance (U-ATR) accessory was
attached to the FTIR spectrophotometer. The U-ATR is
a diamond/ZnSe composite crystal with a pressure arm
that allows a close contact between the surface of the wool
pads and the crystal. The spectrophotometer was also
interfaced to a computer and the scanned spectra were
analyzed on Perkin Elmer Spectrum® version 3.01 soft-
ware.
Grease Content
Cleaning efficiency of the enzyme and control treatments
were measured by evaluating the grease content of single
replications of treated as well as untreated fiber samples
(2 g), according to the procedures described in ASTM
D-584 [28].
Structural Analysis
Surface structure of the fiber samples were studied using
the Hitachi S-3500N scanning electron microscope under
an accelerating voltage of 5 kV.
Results and Discussion
According to the experimental design, there were two
independent variables, the treatment type, and the fiber
type. Within treatment type there were seven levels. These
were the four enzyme treatments, two control treatments,
and the untreated stage. The fiber type comprised of the
six different fiber varieties. The dependent variables were
the different properties (physical, chemical and grease con-
tent) measured. The simultaneous effect of the two inde-
pendent variables on the different dependent variables,
were evaluated using SAS General Linear Model (SAS
Institute Inc., Cary, NC) for two factor analysis of variance
(ANOVA). Tukey’s Studentized range test was conducted
to separate the means of the different properties for
each fiber types and treatment types, at an α level of 0.05.
Effect of fibre type
p-value F-value p-value
< 0.0001 12.00 < 0.0001
< 0.0001 62.53 < 0.0001
< 0.0001 55.18 < 0.0001
< 0.0097 44.59 < 0.0001
< 0.0151 6.67 < 0.0003
Table 1 shows the analysis of variance results of the main
effects of treatment and fiber type on the properties of the
treated and untreated fiber samples. Subjective evaluation
and comparisons were made for the scanning electron
microscope images, and FTIR spectra of the different
untreated and treated fiber types.
Physical Properties
The interaction effect between treatment and fiber type on
the moisture content of fibers was found to be statistically
significant (F = 1.99, p = 0.0077). Furthermore, both the
treatment (F = 114.25 and p < 0.0001) and the fiber type
(F = 12.0 and p < 0.0001) had a significant effect on the
moisture content of the fibers. Higher moisture content
values (Figure 1) were observed for xylanase, pectinase,
and scoured treatments (12.5%) in comparison with other
treatments (9.5 to 10%). This might be attributed to the
greater removal of surface lipid layer from the epicuticle of
the wool fiber, by these treatments, making the wool more
hydrophilic [29]. The moisture content of conditioned
merino wool was found to be the least (10.24%) in compar-
ison to other fibers (11.6 to 11%). The overall range of
moisture content values between fiber types was, however,
quite small.
The effect of treatments on fiber tenacity also demar-
cated scoured, xylanase, and pectinase treated fibers as the
treatments that have higher tenacity values (4.5 g/denier)
than those obtained for untreated, water, savinase, and resin-
ase treatments (Figure 2). Among fiber types, merino
and rambouillet wool had the lowest tenacity values
(2.48 g/denier) as compared to the specialty hair fibers.
The percentage elongation values of the sheep wool, on
the other hand was higher then the specialty hair fibers.
Mohair had the highest tenacity of all the fiber types stud-
ied (3.67 g/denier) and in terms of elongation it had higher
values than the other specialty hair fibers. The effect of
treatments on the elongation values of fibers (unlike in the
case of tenacity) was less significant in comparison with the
effect of fiber types.
From the results of mean fiber diameter it was observed
that the treatment did not have any noticeable effect on
 Enzyme Treatment of Wool and Specialty Hair Fibers T. Das et al. 129 TRJ

Figure 1 Moisture content (%) of all wool/specialty hair fiber types (merino, rambouillet, llama, camel, alpaca, and mohair)
subjected to various treatments (untreated, scoured, water treated, xylanase, pectinase, savinase and resinase enzyme
treatments).

Figure 2 Tenacity at break in g/den of all wool/specialty hair fiber types (merino, rambouillet, llama, camel, alpaca, and
mohair) subjected to various treatments (untreated, scoured, water treated, xylanase, pectinase, savinase and resinase
enzyme treatments).
TRJ 130 Textile Research Journal 76(2)
Figure 3 The mole % of cystein in all wool/specialty hair fiber types (merino, rambouillet, llama, camel, alpaca, and
mohair) subjected to various treatments (untreated, scoured, water treated, xylanase, pectinase, savinase and resinase
enzyme treatments.
the fiber diameters. The effect of fiber types on diameter
values was found to be quite significant. The sheep wool
had the lowest fiber diameters (average of 25 µm), whereas
alpaca and mohair had the highest diameters (36.1 and
31.8 µm, respectively) among all the fiber types. Diameter
values of all the fiber types studied were close to the stand-
ard values, except for alpaca which had a much higher
value than the standard, which is 27 µm. This was due to
the large proportion of coarse guard hairs present in the
alpaca fiber samples.
Chemical Properties
With the exception of glycine, none of the other amino
acids seemed to vary noticeably more between the differ-
ent fiber types, as compared with the variation between the
different treatments within the same fiber type. The gly-
cine content of the sheep wool was consistently greater
than the specialty hair fibers across all treatments. This,
however, is not expected to have any effect on the treat-
ments of these fibers since glycine is a non-reactive amino
acid. Among all the reactive amino acids, cystein is consid-
ered to be the most significant, since the disulfide linkages
affect the efficacy of various treatments. Therefore, the
effect of treatment and fiber type on the cystein content
was studied with greater emphasis (Figure 3). It was
observed that, the cystein content was lowered in the case
of merino wool (by savinase and resinase), mohair (by xyla-
nase, pectinase and savinase), and alpaca (by savinase) in
comparison with the untreated fiber. This drop in cystein
values might be attributed to the cystein being used up in
the formation of lanthionine [29] under the effect of alka-
linity that was present in all these treatment conditions.
However, the amino acid analysis did not show any levels
of lanthionine. On the other hand, the increase in cystein
content in the case of rambouillet wool (in savinase, xyla-
nase, pectinase and scoured fibers) in comparison with the
untreated fiber, might be due to the cystein residues set
free in the course of the amino acid analysis.
From the FTIR analysis of the fiber samples, it was
observed from the shift in the C–H asymmetric and sym-
metric bands at 2920 cm–1 and 2850–2870cm–1, respectively,
that the treatments might have caused rearrangements
of the molecular chains resulting in a tighter packing in
the case of camel fibers and looser packing in the case
of mohair, alpaca, and llama fibers [30]. The lipid band
at around 1734 cm–1 appeared strongest in merino wool,
and progressively less prominent in rambouillet, alpaca,
mohair, camel, and llama fibers. The lipid band became
 Enzyme Treatment of Wool and Specialty Hair Fibers T. Das et al.
Figure 4 The grease content percentage of all wool/specialty hair fiber types (merino, rambouillet, llama, camel, alpaca,
and mohair) subjected to various treatments (untreated, scoured, water treated, xylanase, pectinase, savinase and resin-
ase enzyme treatments).
less intense in the case of xylanase, pectinase, and resinase
treated merino wool, in xylanase-treated rambouillet
wool, and in all mohair fibers except the savinase-treated
fibers.
Cleaning Efficiency
From the results of grease content analysis of the treated
as well as untreated fibers, it was observed that xylanase,
pectinase and scoured fibers had much less grease content
(average 1%) than the other treatment types (Figure 4).
Untreated fibers had the highest grease content (11.2%),
followed by resinase, water, and savinase treatments (aver-
age 6.3%). This is consistent with the results of moisture
content, fiber tenacity and lipid band intensity studied in
FTIR analysis. Resinase and savinase did not remove grease
any better than hot water treatment alone. This implies
that at the concentration used, neither resinase nor savi-
nase were effective scouring agents. Among fiber types the
sheep wool had significantly higher grease content than the
specialty hair fibers.
Fiber Structure
The scanning electron micrographs of all the treated
and untreated fiber types reveal that none of the treat-
131 TRJ
ments affected the fiber structures, physically beyond the
cuticle. Xylanase, pectinase, savinase, and soap scouring
produced a clean fiber surface, however with slight peeling
in the case of xylanase and pectinase. Resinase, as well as
hot water treatment, could not effectively clean the sur-
face of any of the fibers, which accounts for the high
grease content values of resinase and water-treated fib-
ers.
Conclusion
In this study, the effect of enzyme treatment (savinase,
resinase, xylanase and pectinase) on the physical, chemical
and structural properties of wool and specialty hair fibers
were evaluated. It was observed that xylanase and pectinase
treatments had as good a cleaning efficiency as conven-
tional soap scouring. Furthermore, at the concentrations
used, neither of these two enzymes caused any physical
damage to the fibers, as confirmed by the tenacity and
diameter values, and SEM pictures. The effectiveness of
resinase as a scouring agent was, however, not very satisfac-
tory.
The results of this study have a lot of implication for the
processing of wool and specialty hair fibers in the industry.
Enzymes xylanase and pectinase would be very effective as
TRJ 132 Textile Research Journal 76(2)
scouring agents, especially for fibers such as llama, alpaca,
camel, and mohair. Since specialty hair fibers possess very
little impurities compared with sheep wool, the mild treat-
ment conditions used in this study would be very appropri-
ate for the treatment of these fibers. Moreover, at the
extremely low concentrations used in this study, the use of
enzymes is expected to result only in a limited increase in
the cost of treatments. In future studies it would be inter-
esting to observe the softness and shrinkage properties of
fabric woven from enzyme-scoured wool/specialty hair fib-
ers. Such studies might help realize the objective of attaining
a non-felting, clean, and soft woolen product by subjecting
the raw fiber to a single and mild enzyme scouring treat-
ment at the fiber stage.
Acknowledgement
We acknowledge helpful suggestions from Dr.Barbara
Gatewood, and Dr.Sherry Haar. We are grateful to Jenni-
fer Rogers and Renee for their assistance, and Kent
Hampton, for providing technical assistance with SEM. We
would also like to thank the Kansas State Agricultural
Experiment Station for funding the project, and the Depart-
ment of Entomology, and the Department of Biochemistry
for letting us use their facilities. This research was also a
part of the Southern Regional Research Project S-1002.
This is contribution 04-105-J from the Kansas Agricultural
Experiment Station.
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