peerreviewed

LowTemperature
AcidicPectinase
Scouringfor Enhancing
TextileQuality
By Umut Kivanc; Sahin and Nevin c;igdem GOrsoy, Istanbul Technical University, Turkey
Cotton may contain 4-12% by weight
waxes, proteins, pectins, ash, and other
substances such as pigments, hemicelluloses, and reducing sugars. These impurities create a physical hydrophobic barrier providing environmental protection
for the fiber throughout its growth cycle. 1
The waxes and pectins impede the wetting and wicking needed for aqueous
textile processing. Conventionally, scouring is done in a hot aqueous solution of
NaOH to remove hydrophobic components from the primary wall (pectin, protein, and organic acids) and the cuticle
(waxes and fats). However, the use of
high concentrations
quires wastewater

of NaOH also reneutralization.

Al-

though alkaline scouring is effective and

NaOH is inexpensive, the scouring process
is rather inefficient because it consumes
large quantities of water and energy. This
process needs considerable improvement
to meet current energy and environmental demands2 Recent research has been
directed towards replacing this process
with an enzymatic one.3-9
Pectinases can be used for alkaline-

ABSTRACT
Enzymes are increasingly being used in the textile industry to prepare textile goods. In this
study, knitted cotton fabric was scoured with
pectinase.

Treatment

conditions

mized by varying the amount

pectinase, and treatment

were opti-

of surfactant,

time. Treatment

ef-

fectiveness on fabric properties was determined

via water absorbency,

weight

loss, scanning

electron microscope, and qualitative analysis of

residual pectin on the fabric. The goal of this
research is to evaluate and optimize acidic pectinase scouring at 40C.

Key Terms
Cotton
Pectinase
Scouring
SEM
Water Absorbency

procedure. The liquor was raised to the

reaction temperature before surfactant,
pact of pectinase scouring is reduced enzyme, and fabric were added to the
compared to the traditional approach solution. At the end of each reaction, the
becausefewer harsh chemicals and less sample was rinsed in hot purified water
(> 60C) followed by tap water. The
rinse water are needed. Bio-scouring
leadsto approximately 50-65% lessCOD sample was then dried at 105C in an
in the wastewater compared to alkaline oven, cooled in a desiccatorfor 1 hr, and
scouring depending on the sourceof cot- weighed to determine weight loss. The
ton and the maturity of fiber. Because sampleswere placed in the conditioning
the bio-scouring processreducesboth ef- room for 24 hr, then tested for water
fluent load and water consumption, it is absorbency using AATCC Test Method
lessexpensivethan conventional chemi- 79-1986.10
cal treatments.
Residualpectin on the fabric was analyzed by staining with Ruthenium Red
EXPERIMENTAL
(stains pectins and proteins) using the
procedure of Rollinsand deGruy.ll
Materials
A JEOLJSM-840 scanning electron
microscope
(SEM) was usedfor microsThe fabric used in this study was a 30/1
copy
observations.
Care was taken not
Ne cotton knit with a unit area weight of
to
subject
the
specimens
to mechanical
152 g/m2 Beforescouring,fabric samples
were cut into rectangular shapes. Each damage when gluing. The specimens
samplewas dried in the oven at 105C for were coated with gold. The surface characteristicsof cotton sampleswere deter1 hr to determine weight loss, then
folded and a stirring bar was placedin the mined by summarizing numerous observations of individual fibers from a
fabric. The remaining three edges (besides the folded one) were handsewn specimen.
Experiments were conducted using,
using a polyester yarn.
Pectinaseused in this study was from first a two-level full factorial, which included three levels of each variable (-1,
Aspergillus niger and was in powder
form. The main component of the en- 0, + 1), and then a central composite exzyme is polygalacturonase. The specific perimental design, which included five
enzymeactivity is 1 unit/mg of protein at levelsof each variable (-a, -1, 0, + 1, +a)
pH 4.2 and 40C when polygalacturonic with a = 1.682. The central composite
acid is used as assaysubstrate. The non- design permits a more accurate mathionic surfactant used was Nonyl Phenol ematical model to be produced than the
10 EO (Tekpar).For all reactions, buffer full factorial and is appropriate for opsolutionswere used.All enzymereactions timization.12 Three variables of pectiwere performed in purified water. A stir- nase scouring were examined (Table I).
ring hot plate (YellowlineMSHbasic)was The other processparameters (40C, pH
used for enzymatic scouring. A cylindri- 4.2, 1:40 liquor ratio, and 1000 rpm
cal stirring bar (0.5 x 3 cm) was used at stirring speed) were kept constant. The
a stirring speed of 1000 rpm. The liquor criteria for assessingscouring effectiveratio was 1:40.
ness were water absorbency, microscopic appearance under SEM, weight
Methods
loss, and qualitative analysisof residual
All enzymetreatmentsfollowedthesame pectin on the fabric.
free enzymatic pretreatment, especially
for dark shades.The environmental im-

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peerreviewed

The interaction of the surfactant and

TABLEI.

pectinase on water absorbency time is

shown in Fig. 2. An increasedamount of
surfactant was shown to decrease the

Coded and Actual Design Factor Levels

Factor
Symbol
Xl
X2
X3

Factor
Surfactant(g/100 mL)
Pectinase(g/100 mL)
TreatmentTime (min)

-1.682
0.660
0.007
11.590

Levels of the Variables

-1
0
+1
1
1.500
2
0.015
0.010
0.020
15
20
25

+ 1.682
2.340
0.023
28.410

TABLE II.
Estimated and Measured Response Values for Optimum Recipe
Responses
Water absorbencytime (see)
Weight loss (%)
RESULTS

AND

Estimated Value
0.9
4.0

DISCUSSION

Baselevelswere adjustedfor the variables

taking into account of the preliminary
experiments (Table I). The full factorial
experimentaldesignand the central composite experimental design for three variableswere applied to investigate the parameter effects on responsevaluesand to
optimize processing conditions. Every
recipe was repeated three times and arithmetical averagesof measuredresponse
values were calculated.
The quadratic model that predicts
water absorbencytime in terms of actual
valuesat different factor levelswithin the
scope of the experiments is shown in Eq.
1. This model was usedfor prediction of
the water absorbency time (in seconds)
throughout the entire experimental volume evaluated.
Water absorbencytime =
9.95373 - 0.19348 . X,
- 92.29949 . X2 0.08666 . X3 - 4.82135
. X,2 + 299.23457 . xi 6.13899' xi - 0.29' X,
. X2 + 8.9 . X1 . X3 + 1.04 .
X2. X3

Eq. 1

Effecton WaterAbsorbency
The average water absorbency time at
plus and minus levels of variables are
shown in Fig. 1. The sizeof the difference
can be used as a measure of the size of
the effect. The amount of surfactant had
the largest effect on water absorbency
with an averagewater absorbencydifferAATCC REVIEW

28

Measured Value
0.8
3.94

ence of 2.1, followed by treatment time

at 0.5, and pectinase amount at 0.3. If
boiling water pretreatment had been used
- levels

prior to the enzymereaction' the effect would

havebeen different. YouLo reported that boiling
water pretreatment prior
to enzyme reaction enhanced accessibility of
enzymes to the other
non cellulosics beneath
the waxes, thus improving the enzymatic scouring effect on cotton.4
However, it requires an
extrastep aswell as more
energy and water. Since
this was thought not to
be convenient for industrial work, this step was
not included in the
present study. In the authors'
opinion,
the
surfactant's effect on
water absorbency depends on the amount of
hydrophobic substances
presenton the surface of
the cotton fibers. Nonionic surfactants reduce
the surfaceenergyof cotton, allow enzymes to
penetrate micropores or
cracks,and help enzymes
maintain the proper orientation for catalysis to
occur.7

water absorbency time, thereby improving the water absorbency,at all pectinase
levels. It was also apparent that the water absorbencyability increasedwhen the
enzyme concentration was between
0.01-0.013 g/100 mL, although at higher
enzyme concentrations, an increase in
water absorbencytime occurred.
The use of surfactant is important for
ensuring good contact between the enzyme and the cotton fabric. The surfactant can be applied before or together
with the enzyme, but application to the
fabric before enzyme addition is recomof the variables

0 + levels of the variables

3
2,6

12,5

..~

()'
c

1,5

-fa

g
...

~ 0,5
0

Pectinase

Surfactant

Treatment
time

I
Fig. 1.Averagewater absorbencytime values at + and - levels of
variables.

Water Absorbency l1me (see)

0.020

:J

0.017

0
0

Ct!
c

O.oJS

~ 0.013

a.

0.010
1.00

1.25

Surfactant

1.50

1.75

2.00

(gI100mL)

Fig. 2. The effects of pectinase and surfactant amount on water

absorbency time of pectinase scoured fabrics. Contour lines represent water absorbency time (sec) and the level of parameters not
shown for each plot were at their center point (0 level in Table I).
JANUARY 2005

peerreviewed

. - levels of the variables 0 + levels of the variables

Water Absorbency lime (see)

25.00

4,4
4,35
...... 22.50
.Iii

g
i=

;
i

4,375

4,3

~en 4,25

20.00

4,2

.E 4,15
0>
'Q5 4,1

I!:!

I- 17.50

15.00

~
I

1.00

1.25

1.50

4,05
4
3,95

1.75

2.00

Surfactant

Pectinase

Surfactant (gI1OOmL)
Fig. 3. The effects of treatment time and surfactant amount on

Fig. 4. Average weight loss (%) at + and -levels

Treatment
time

of variable.

water absorbency time of pectinase scoured fabrics. Contour lines

represent water absorbency time (sec) and the level of parameters not shown for each plot were at their center point (0 level in

Optimization

TableI).

To obtain an optimized scouring recipe,

an ideal water absorbencytime of 1 sec
and a weight loss of 4% was proposed.
To optimize the recipe, the water absorbency time was assumedto be lessthan
1 secand the weight lossto be between
4-4.3%. A total of 4913 points were
studied and the optimized process parameterswere estimatedto be asfollows:

mended, considering the possible reaction of the surfactant with the enzyme. In
this study, the surfactant and enzyme
were added to the scouring bath just before adding the fabric. It isthought, in this
case,that the useof pectinasein concentrations greater than 0.013 g/100 mL inactivated the surfactant over time, resulting in decreasedenzyme penetration and
subsequent lower wettability.
The interaction effect of surfactant and

siderablysmaller effect on
weight loss within the
ranges studied. Weight
loss was within the range of the estimated noncellulosicweight. The conclusion, confirmed by microscopic observations, was that the waxes, proteins, and
pectin of the cuticle were removed by
pectinase scouring without damage to
the cellulose portion of the cotton fiber.

pectinase,0.011 g/100 mL; surfactant, 1

g/l 00 mL; treatment time, 25 min; treatRuthenium Red stains pectic substances ment temperature, 40(; pH, 4.2; liquor
and proteins due to the presenceof car- ratio, 1:40; and stirring speed, 1000 rpm.
boxyl groups in the molecules.8
The software-estimated responsevalUnscoured cotton had poor absorbency ues used for the optimized scouring
for the dye solution. For this reason, hot recipe,along with the measuredresponse
water pretreatment was performed prior values obtained by applying the estito staining. Hot water pretreatment does mated scouring recipe, are given in Table
not remove pectin, it just lets the dye 11.13The measured and estimated repenetrateinto unscouredfabric. All of the sponses were very close to each other
pectinase digested specimens stained and the desirability,defined asa measure
very faintly, indicating removal of pectic of how well the combination of experiand proteinaceous substancesfrom cot- mental variablesmeets a responsespeciton, while unscoured cotton was stained
fication, at the optimum point was 1.
to a dark shade.
CONCLUSION

Staining

treatment time on water absorbencytime

is given in Fig. 3. The increase in the
amount of surfactant improved the water
absorbencyat all treatment times studied.
The water absorbency improved as the
treatment time increasedto 17.5 min, but
wettability was found to decreaseat treatment times longer than this. It is thought
that 17.5 min is long enough to decompose the pectin-releasing oil and wax in
the multilayer cotton structure. At treatment times longer than 17.5 min, some
releasedoil and wax may stick on the fiber surfaceinsteadof staying in the scour- SEM
ing bath, causinga decreasein wettability. Theeffect of enzymatictreatmentson cellulosicstructurewas evaluatedby comparEffecton Weight Loss
ing the micrographsof unscouredcotton
Theaverageweightloss(%)valuesat plus fibers with pectinase-scouredcotton fiand minuslevelsof variablesareshown bers.As seenin Figs.5 and 6, the celluloin Fig.4. Thesurfactanthad the largest sic surface structure of the cotton fiber

of the fiber. Scouring results in a much

more water absorptive fiber that is ready
for wet processing.The conventional system, using hot solutions of sodium hy-

effecton weightloss.Theamountof pec- doesn't changeafter enzymatictreatment.

tinaseandalsotreatmenttime hada con-

tends to be a major source of environ-

The aim of cotton scouring is to remove

noncellulosic materials from the surface

droxide,is effective in this regard,but

JANUARY 2005

29
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peerreviewed

Fig. 5. Scanning electron microscopy of the surface of unscoured cotton fiber.

mental pollution. Therefore, it was useful

to examine an alternative method to the
traditional scouring of cotton.
In this study, the effects of acidic pectinase enzyme on improving the water
absorbency of unscoured knitted cotton
fabric were investigated. The variable
base levels were first determined, then a
full-factorial experimental design was prepared to investigate the effects of the
parameters on response values. The central-composite experimental design was
then applied to optimize the processing
conditions. To obtain a software-optimized scouring

recipe, an ideal water

absorbency time (1 sec) and weight loss

(4%) was chosen. For recipe optimization, a water absorbency time less than
1 sec and weight loss of 4-4.3% were
assumed. Using 4913 data points, the
estimated optimized process parameters
were determined. Staining results with
Ruthenium Red confirmed that pectinase
treatment removed the pectins and proteins when compared to unscoured fab-

Fig. 6. Scanning electron microscopy of the surface of pectinase scoured

cotton fiber that gives the best water absorbency (pectinase = 0.011 g/
100 mL, surfactant = 1 g/100 mL, treatment time = 25 min, pH = 4.2,
liquor ratio = 40:1, stirring speed = 1000 rpm).

rie. Microscopy observations showed

that the cellulosic
structure of cotton fiber did not change
after enzymatic treatment. The resultsof
this researchshowed that acidicpectinase
can be used as a scouring agent at 40C
for cotton in the textile industry.
References

1. Shore,J., CellulosicsDyeing, Alden Press,

Oxford,U.K., 1995,pp82-83.
2. Etters,J. N., NovoNordiskBulletin,1998,
ppl-9.
3. Bach,E.and E.Schollmeyer,TextilPraxisInternational,Vol.3, March 1993, pp220-224.
4. Hartzell, M. M. and Y.-L. Hsieh, Textile
Research Journal, Vol. 68, No.4, April
1998, pp233-241.
5. Hsieh,Y.-L. and L. Cram, TextileResearch
Journal, Vol. 69, No.8, August 1999,
pp590-597.
6. Karmakar, S. R., ColourageAnnual/99B,
pp75-86.
7. Li,Y. and I. R.Hardin, TextileChemistand
Colorist, Vol. 30, No.9, September 1998,
pp23-29.

8. Li,Y. and I. R.Hardin, TextileChemistand

Colorist, Vol. 29, No.8, August 1997,
pp71-76.
9. Rossner,U., Melliand Textilberichte, Vol.
74, No.2, February 1993, pp144-"148.
10. AA TCCTechnicalManual, Vol. 66, 1991,
p106.
11. Rollins,M. L. and I. V. deGruy, Instrumental Analysisof Cotton Celluloseand Modified Cotton Cellulose,Marcel Dekker,New
York, N.Y., 1972, p145.
12. Montgomery, D. c., Design and Analysis
of Experiments, John Wiley & Sons,
Singapore, 1991, pp391-395, 533-551.
13. Design Expert Software, Stat-EaseInc.

Author's Address
Nevin<::igdemGursoy,Dept. of TextileEngineering, Istanbul Technical University,
80191 Inonu Cad, No. 87 Gumussuyu/
Taksim, Istanbul, Turkey; telephone +90
212 292 13 22; fax +90 212 292 13 22;
e-mail gursoyne@itu.edu.tr.

unifSCALE

This scale is used in conjunction with

AATCC Test Method 178, Barre: Visual Assessment and Grading. Barre

is the optical resultof physicalor dye

differencesin the yarns,geometric

differencesin thefabricstructureor

6T
:&
:&

P,0. Box 12215

any combination of these differences. The Uniformity Reference Scale is a 9 step'vi-

Research Triangle Park

sual scale used in evaluating the intensity of the barrEL The number from the scale that
most nearly matches the barre intensity of the test specimen or the number midway between whole-number standards are assigned to the test specimens. Order No. 08358.

N~rt~ca;~I~:-:;;~9
Fe., ~~9/~49/8933
ax.
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