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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 ticated llamas and yield finer and stronger fibers than the
irreplaceable even in a market dominated by its inexpen- llamas [3]. These fibers, mostly obtained from animals
sive and abundantly available synthetic versions such as native to remote corners of 1the world, have a very small
acrylics. Wool constitutes a minor segment (1.98%) of the annual production, but capture the best markets in the
total textile fibers produced globally [1]. However, a signif- high fashion industry [4]. Therefore, in spite of a small
icant portion of the wool is consumed by the high-end quantitative contribution, the significance of wool and spe-
fashion market because of its warmth, resiliency, and cialty hair fibers in the apparel and textile industry cannot
handle. Within animal hair fibers, specialty hair fibers be under-rated.
are considered to be even more exquisite than sheep wool Animal hair fiber, especially sheep wool, has to pass
[2]. Specialty hair fibers are fibers, obtained from animals through various stages of processing and cleaning (to get
other than sheep, such as, mohair, alpaca, llama and rid of the dirt, grease, vegetable matter, and other impuri-
camel [3]. Mohair, obtained from the angora goat, is a ties in the raw state) before it can qualify as a marketable
long, white, and lustrous fiber, devoid of any crimp. Camel product [5]. Conventionally, some of these processes
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, 1
Corresponding author: fax: +1785-532-3796; e-mail: ramas-
which are also native to the Andes mountains, are domes- 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. 127 TRJ

require chlorination or application of chlorine-containing
polymer, such as Hercosett [6, 7], which results in high lev-
Experimental
els of organic halogens discharged in waste-water [8]. This
has been an issue of major environmental concern and has Treatments
encouraged a lot of research in alternative eco-friendly Two varieties of sheep wool (merino and rambouillet) and
processes such as enzyme treatment [6–8]. four varieties of specialty hair fibers (llama, alpaca, camel,
Enzymes are natural proteins which act as bio-catalysts and mohair) were used in this study. Three replications
[9]. Most of the enzymes used in textiles are hydrolases, from each of the six fiber types were subjected to four dif-
which catalyze cleavage reactions through hydrolysis [6]. ferent enzymes scouring treatments (with xylanase, pecti-
Examples are proteases, which break down proteins into nase, savinase, and resinase) and two control treatments
amino acids and smaller peptides, lipases that break down (with hot water and soap). Thus there were eighteen samples
lipids into fatty acids and glycerol, and cellulases that break for each of the six treatments, and each fiber sample con-
down cellulose into glucose [9]. sisted of 10 g of fiber selected at random from the respec-
Enzymes used in wet-processing treatments of cotton, tive bags of fibers obtained from different shearing stations.
such as scouring, desizing, and stonewashing have already Enzymes pectinase (Bioprep 3000L), xylanase (Novozym
been introduced in the textile industry [10] and the possi- 628) and savinase (Savinase 16L, TYPE EX) were obtained
bilities of enzyme treatment for other fibers, especially from Novo Nordisk Biochem North America Inc. and enzyme
wool, are under extensive research. Studies have been con- Resinase A 2X was obtained from Novozymes North Amer-
ducted on the effectiveness of proteolytic (6, 11, 12) and ica, Inc. All the treatments were conducted for 5 minutes at a
lipolytic [13] enzymes in improving wool properties such as temperature of 60°C. All four enzymes were used at a con-
shrink resistance, softness, and wettability. The review centration of 0.2% o.w.f. and the soap-scouring treatment
showed that extensive work has been done to determine was done using 2 g/mL of AATCC soap. For each treat-
the efficiency of enzymes in finishing treatments of wool, ment, 10 g of fiber samples were used with 300 mL of water
such as anti-felting treatments [6, 14, 15]. However, the for the hot water treatment and 298 mL of water for the
effectiveness of enzymes as scouring agents for wool fibers, enzyme and soap-scouring treatment, to get a material to
in comparison with conventional soap scouring treatments liquor ratio of 1 : 30. A pH of 9.32 for xylanase, pectinase,
has not been studied. Furthermore, most work on enzyme and soap scouring, 9.0 for savinase, and 7.0 for resinase
treatment of wool has been confined to studies of a single treatment were used (according to optimum conditions for
type of wool – mainly merino wool. Limited work has been each enzyme, obtained from literature). After each scour-
done on the enzyme treatment of specialty hair fibers [16]. ing treatment, the fiber samples were rinsed thoroughly in
As the grease content of these fibers are much less than in cold water and air dried. The physical, chemical and struc-
sheep wool [17–20], enzyme scouring of these fibers, under tural property, and grease content of all the treated, and
mild treatment conditions, for cleaning and improving untreated samples of each fiber type, were then evaluated
softness, would be a worthwhile treatment. The enzymes and compared.
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 Physical Analysis
a lipase enzyme used in the paper pulp industry [22]. Apart
from these the effects of using a xylanase, which breaks Moisture content, of the conditioned fibers, and fiber
down hemicellulose [23], and pectinase, which breaks down diameter were measured according to the standard proce-
pectins, which are complex mixtures of polysaccharides dures [25–27].
[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. Chemical Analysis
Therefore, the objective of this study was, to do a com- Amino acid analysis was performed on single replica-
parative study of two varieties of wool and four varieties of tions for each treated and untreated fiber type, using the
specialty hair fibers, scoured with the enzymes xylanase, ‘Model 420 A Derivatizer’. The samples were hydrolyzed
pectinase, savinase and resinase, and compare the results for 24 hours at 110°C in 6 N solution of HCl, under vac-
to plain hot-water-treated, soap-scoured, and untreated uum and then derivatized using phenylisothiocyanate
wool – for control. The enzyme-treated and control samples (PITC). Finally, the derivatives were analyzed in the high-
were evaluated for mechanical, structural, chemical and pressure liquid chromatography (HPLC) unit. Standard areas
biological properties. The grease content of the treated used were from 20 µL of a 25 nmol/mL standard solution.
and untreated fiber samples was also evaluated to measure Fourier transform infrared (FTIR) spectroscopy was
and compare the cleaning efficiencies of the various treat- performed on single replications for each treated and
ments. 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 Effect of fibre type

Properties tested F-value p-value F-value p-value
Moisture content 114.25 < 0.0001 12.00 < 0.0001
Tenacity 619.85 < 0.0001 62.53 < 0.0001
Elongation 12.06 < 0.0001 55.18 < 0.0001
Diameter 3.04 < 0.0097 44.59 < 0.0001
Grease content 3.20 < 0.0151 6.67 < 0.0003
*Degree of freedom for treatment type = 6 and fiber type = 5

One FTIR spectrophotometer. A single bounce Universal Table 1 shows the analysis of variance results of the main
Attenuated Total Reflectance (U-ATR) accessory was effects of treatment and fiber type on the properties of the
attached to the FTIR spectrophotometer. The U-ATR is treated and untreated fiber samples. Subjective evaluation
a diamond/ZnSe composite crystal with a pressure arm and comparisons were made for the scanning electron
that allows a close contact between the surface of the wool microscope images, and FTIR spectra of the different
pads and the crystal. The spectrophotometer was also untreated and treated fiber types.
interfaced to a computer and the scanned spectra were
analyzed on Perkin Elmer Spectrum® version 3.01 soft-
ware. Physical Properties
The interaction effect between treatment and fiber type on
Grease Content the moisture content of fibers was found to be statistically
significant (F = 1.99, p = 0.0077). Furthermore, both the
Cleaning efficiency of the enzyme and control treatments treatment (F = 114.25 and p < 0.0001) and the fiber type
were measured by evaluating the grease content of single (F = 12.0 and p < 0.0001) had a significant effect on the
replications of treated as well as untreated fiber samples moisture content of the fibers. Higher moisture content
(2 g), according to the procedures described in ASTM values (Figure 1) were observed for xylanase, pectinase,
D-584 [28]. 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
Structural Analysis the wool fiber, by these treatments, making the wool more
Surface structure of the fiber samples were studied using hydrophilic [29]. The moisture content of conditioned
the Hitachi S-3500N scanning electron microscope under merino wool was found to be the least (10.24%) in compar-
an accelerating voltage of 5 kV. 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-
Results and Discussion cated scoured, xylanase, and pectinase treated fibers as the
treatments that have higher tenacity values (4.5 g/denier)
According to the experimental design, there were two than those obtained for untreated, water, savinase, and resin-
independent variables, the treatment type, and the fiber ase treatments (Figure 2). Among fiber types, merino
type. Within treatment type there were seven levels. These and rambouillet wool had the lowest tenacity values
were the four enzyme treatments, two control treatments, (2.48 g/denier) as compared to the specialty hair fibers.
and the untreated stage. The fiber type comprised of the The percentage elongation values of the sheep wool, on
six different fiber varieties. The dependent variables were the other hand was higher then the specialty hair fibers.
the different properties (physical, chemical and grease con- Mohair had the highest tenacity of all the fiber types stud-
tent) measured. The simultaneous effect of the two inde- ied (3.67 g/denier) and in terms of elongation it had higher
pendent variables on the different dependent variables, values than the other specialty hair fibers. The effect of
were evaluated using SAS General Linear Model (SAS treatments on the elongation values of fibers (unlike in the
Institute Inc., Cary, NC) for two factor analysis of variance case of tenacity) was less significant in comparison with the
(ANOVA). Tukey’s Studentized range test was conducted effect of fiber types.
to separate the means of the different properties for From the results of mean fiber diameter it was observed
each fiber types and treatment types, at an α level of 0.05. 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 effect of treatment and fiber type on the cystein content
values was found to be quite significant. The sheep wool was studied with greater emphasis (Figure 3). It was
had the lowest fiber diameters (average of 25 µm), whereas observed that, the cystein content was lowered in the case
alpaca and mohair had the highest diameters (36.1 and of merino wool (by savinase and resinase), mohair (by xyla-
31.8 µm, respectively) among all the fiber types. Diameter nase, pectinase and savinase), and alpaca (by savinase) in
values of all the fiber types studied were close to the stand- comparison with the untreated fiber. This drop in cystein
ard values, except for alpaca which had a much higher values might be attributed to the cystein being used up in
value than the standard, which is 27 µm. This was due to the formation of lanthionine [29] under the effect of alka-
the large proportion of coarse guard hairs present in the linity that was present in all these treatment conditions.
alpaca fiber samples. 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-
Chemical Properties nase, pectinase and scoured fibers) in comparison with the
untreated fiber, might be due to the cystein residues set
With the exception of glycine, none of the other amino free in the course of the amino acid analysis.
acids seemed to vary noticeably more between the differ- From the FTIR analysis of the fiber samples, it was
ent fiber types, as compared with the variation between the observed from the shift in the C–H asymmetric and sym-
different treatments within the same fiber type. The gly- metric bands at 2920 cm–1 and 2850–2870cm–1, respectively,
cine content of the sheep wool was consistently greater that the treatments might have caused rearrangements
than the specialty hair fibers across all treatments. This, of the molecular chains resulting in a tighter packing in
however, is not expected to have any effect on the treat- the case of camel fibers and looser packing in the case
ments of these fibers since glycine is a non-reactive amino of mohair, alpaca, and llama fibers [30]. The lipid band
acid. Among all the reactive amino acids, cystein is consid- at around 1734 cm–1 appeared strongest in merino wool,
ered to be the most significant, since the disulfide linkages and progressively less prominent in rambouillet, alpaca,
affect the efficacy of various treatments. Therefore, the mohair, camel, and llama fibers. The lipid band became
Enzyme Treatment of Wool and Specialty Hair Fibers T. Das et al. 131 TRJ

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 ments affected the fiber structures, physically beyond the
treated merino wool, in xylanase-treated rambouillet cuticle. Xylanase, pectinase, savinase, and soap scouring
wool, and in all mohair fibers except the savinase-treated produced a clean fiber surface, however with slight peeling
fibers. 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
Cleaning Efficiency grease content values of resinase and water-treated fib-
From the results of grease content analysis of the treated ers.
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). Conclusion
Untreated fibers had the highest grease content (11.2%),
followed by resinase, water, and savinase treatments (aver- In this study, the effect of enzyme treatment (savinase,
age 6.3%). This is consistent with the results of moisture resinase, xylanase and pectinase) on the physical, chemical
content, fiber tenacity and lipid band intensity studied in and structural properties of wool and specialty hair fibers
FTIR analysis. Resinase and savinase did not remove grease were evaluated. It was observed that xylanase and pectinase
any better than hot water treatment alone. This implies treatments had as good a cleaning efficiency as conven-
that at the concentration used, neither resinase nor savi- tional soap scouring. Furthermore, at the concentrations
nase were effective scouring agents. Among fiber types the used, neither of these two enzymes caused any physical
sheep wool had significantly higher grease content than the damage to the fibers, as confirmed by the tenacity and
specialty hair fibers. diameter values, and SEM pictures. The effectiveness of
resinase as a scouring agent was, however, not very satisfac-
tory.
Fiber Structure
The results of this study have a lot of implication for the
The scanning electron micrographs of all the treated processing of wool and specialty hair fibers in the industry.
and untreated fiber types reveal that none of the treat- Enzymes xylanase and pectinase would be very effective as
TRJ 132 Textile Research Journal 76(2)

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