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Standardization of Dyeing Process Variables for Dyeing of Cotton Khadi Fabric

with Aqueous Extract of Babul Bark (Acacia Nilotica L.)

Article in Journal of The Institution of Engineers (India) Series E · September 2018

DOI: 10.1007/s40034-018-0127-2

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J. Inst. Eng. India Ser. E
https://doi.org/10.1007/s40034-018-0127-2
ORIGINAL CONTRIBUTION
Standardization of Dyeing Process Variables for Dyeing of Cotton
Khadi Fabric with Aqueous Extract of Babul Bark (Acacia
Nilotica L.)
H. D. Sinnur1 • Ashis Kumar Samanta2 • Dileep Kumar Verma1
Received: 17 March 2018 / Accepted: 30 July 2018
Ó The Institution of Engineers (India) 2018
Abstract Study of dyeing process variables and its stan-
dardization is essential for establishing scientifically
reproducible standard method of dyeing cotton fabric with
specific natural dye like babul bark containing veg-
etable gallic/tannic acid residue besides natural color
component. Effects of different single and combined dou-
ble mordanting and dyeing process variables on surface
color strength and color fastness properties after dyeing
cotton khadi fabric with aqueous extract of Babul Bark
(Acacia Nilotia L.) as natural dye were studied in the
present work. Potash alum, aluminium sulphate and stan-
nous chloride were used as metallic salt mordant and Harda
(Myrobolan) was used as natural mordant assisting agent.
Relevant results indicate that application of overall 15%
dosages of Harda and aluminium sulphate in 75:25 ratio
offers maximum K/S value (5.44) and overall good color
fastness (3–4 or higher) than other combination studied.
After finalizing the mordants, dyeing process variables
were studied for standardization of the dyeing process
using babul bark extract. Relevant results indicate that this
particular natural dye (babul bark) renders better color
strength for optimized conditions of dyeing with dyeing
time: 60 min, dyeing temperature: 65 °C, at MLR: 1:30,
& H. D. Sinnur
hdsinnur.gouda@gmail.com
Ashis Kumar Samanta
ijtaksamanta@hotmail.com
Dileep Kumar Verma
dileephome@gmail.com
1
Mahatma Gandhi Institute for Rural Industrialization
(MGIRI), Maganwadi, Wardha, India
2
Department of Jute and Fibre Technology, IJT, Calcutta
University, Kolkata, India
dye bath pH: 5.0, optimum dye conc.: 30% (based on dry
weight of source materials) and common salt—5%. Study
of FTIR and Atomic absorption spectrophotometry (AAS)
for the said natural dyed cotton khadi fabric with babul
bark indicate presence of metallic mordant and tannin
content for explaining the observed results showing dye-
fibre-mordant complex formation besides hydrogen bond-
ing as well.
Keywords Babul bark  Cotton khadi fabric 
Dyeing process variables  Mordant  Natural dyes
Introduction
Successful ready commercial use of different natural dyes
for application on cotton to obtain reproducible shades,
moderate to good color fastness, the standardized recipe
and techniques for dyeing of that particular natural fibre
like cotton and any specific natural dye system like aque-
ous extract of babul bark need to be made available readily
in hand to the dyers/artisans with shade card for repro-
ducible dyeing. Therefore to obtain newer shade with
acceptable color fastness behaviour and reproducible color
yield, standardized dyeing process parameters need to be
established and be made available in the hand of the dyers
for regular use. The present work on standardization of
dyeing process variables for dyeing of cotton khadi fabric
with aqueous extract of babul bark (Acacia Nilotica L.) as
natural dye source is an endeavour towards this attempt for
natural dyeing of cotton khadi fabrics.
Hand loom woven fabrics made from hand-spun yarns
of cotton are widely popular to consumers as eco-friendly
sustainable textile starting from super fine muslin to coar-
ser type cotton khadi fabric (with heavy areal density and
123

handcrafted look).In the present market there is a specific
demand for cotton khadi fabrics for its special handcrafted
look and surface character as well as eco consideration
(free from industrial contaminants and pollution). The
value of this cotton khadi fabric may further be enhanced,
by dyeing with eco-friendly natural dyes at optimum dye-
ing conditions obtaining reproducible and more uniform
shade with acceptable color fastness properties.
Most of the natural dyes are usually environmental
friendly, low or non-toxic and less or no allergenic and also
have some medicinal value in some of the plants sources
from where natural dyes are extracted. Due to these
advantages, over the last decade, the use of natural dyes has
gained its revival in food, pharmaceutical, cosmetic and
textile industry [1]. For many years, scientists have
investigated the deodorizing/aroma [2], insect-repellent [3]
and UV protection against to sun rays [4], [5], [6]; and
antioxidant/antimicrobial finishing [7, 8] even with natural
dyes or with other natural agents obtained from plants for
either dyeing or finishing or both dyeing and finishing of
natural fibres like cotton, wool, silk and jute and other
natural fibres based textiles.
Babul (Acacia nilotica l) is a very common tree avail-
able in Punjab, Haryana, Rajasthan, Bihar and Uttar Pra-
desh and it is locally known as Kikar [9] and [10] or Babla
or Babul or Indian gum Arabic tree. There are more than 40
different species of this babul tree available in India. The
bark of babul tree contains some tannin made up of strong
and a stringent natural acid called gallic acid and hence it is
used in tanning and dyeing of textiles as well as manu-
facture of inks and also in pharmaceuticals [11]. Acacia is
the most significant genus of family: Leguminosae, first of
all described by Linnaeus in 1773. It is estimated that there
are roughly 1380 species of Acacia worldwide, about two-
third of them native to Australia and rest of spread around
tropical and subtropical regions of the world [12, 13]
including Africa and Indian subcontinent as per reports in
literature. Acacia species are commonly known as ‘Babul’
in India and ethno medicinally has long been used for the
treatment of skin, stomach and tooth problems. Acacia
Nilotica (L.) Del. syn. Acacia arabica (Lam.) Wild (Mi-
mosaceae). It is widely distributed throughout the semi-arid
zones of the world. Acacia arabica has been proved its
effective medicinal value in treatment of malaria; sore
throat (aerial part) and toothache (bark) [14–16] problem,
where the binder/action for adhesion property of babul, due
to high tannin contents in it, is advantageous in such
application.
Textile chemists and dyers or dyeing artisans are facing
day to day challenges for assuring reproducibility and
shade matching with natural dyes due to insufficient sci-
entific information and lack of optimised processes of
dyeing for specific fibre-mordant-dye system for any
123
J. Inst. Eng. India Ser. E
natural dye to achieve uniform and optimum color yield.
However, recently there are some reports available on
study of dyeing process variables and standardization of
dyeing process with few other natural dyes on Cotton, Jute,
Wool and Silk [6, 17–26], but this work has still not been
done with babul bark as natural dye source that too for its
application for dyeing of cotton and particularly Khadi
cotton fabrics. So an essential need was felt to standardize
dyeing process conditions for obtaining uniform and
reproducible brown shades by varying type and concen-
tration of mordants, concentrations of dye and other dyeing
process variables using babul bark extract as natural dye
for standardizing its dyeing process with suitable mordants
as well as to obtain correct and desirable shades.
So, in the present work, effects of different single and
combined double mordanting on dyeability and color
fastness properties for dyeing cotton khadi fabric with
standardized aqueous extract of babul bark i.e. Acacia
Nilotica (L.) as natural dye has been studied along with
study of optimization of conditions of aqueous extraction
method for extraction of color components of babul bark
and choice of suitable mordants. Before dyeing, selective
mordants like potash alum, aluminium sulphate and stan-
nous chloride as metallic salt mordant and harda (my-
robolan) from natural source as mordant assisting agent
were used for dyeing pre-mordanted khadi cotton fabric
with aqueous extract of babul bark to finally make a choice
of suitable mordanting system. After finalizing the mordant
type and concentration, dyeing process variables have been
standardized for dyeing cotton khadi fabric with aqueous
extract of babul bark powder applied on bleached cotton
khadi fabric. Study on dyeing process variables includes
variation in dyeing time, temperature, MLR, pH, mordant
conc., dye conc., and salt conc. for dyeing of cotton khadi
fabric with aqueous extract of babul bark after pre-mor-
danting with optimized combination and conditions of
suitable mordanting system for specific fibre-mordant–
natural dye system. Also color fastness to washing, rub-
bing, light and perspiration against use of different mor-
dants and also against different dyeing process variables
have been investigated and reported.
The present work thus has a high level of importance to
the dyers of decentralized khadi cotton sector for their
regular use of standardized dyeing process with babul bark
for obtaining reproducible and uniform shades with
acceptable color fastness to washing, uv light, rubbing
(crocking), and perspiration. The present work thus
involves optimization is needed for optimization of
extraction process, selection of right mordant and its
dosage and mordanting assistants and standardization of
dyeing process variables for achieving uniform and
reproducible shades with babul bark extract as a natural
J. Inst. Eng. India Ser. E

dye in brown tone for cotton khadi fabrics, which is not

Chemicals/Dyes Source Purpose
done earlier.
Myrabolan (harda/ Local supplier A complexing agent as a
haritaki, botanically in Nagpur, natural mordanting
Experimental known as Terminalia Maharashtra assitant used.
chebula containing
chebulinic acid
Fabric Babul (Acacia Nilotica Local supplier As a brownish colored
L.) bark as natural dye in Nagpur, natural dye source
Bleached cotton khadi fabric having following specifica- Maharashtra materials need
tion, obtained from Gram Sewa Mandal, Gopuri, Wardha, extraction
Maharashtra, India, was used in this work:

Parameter of the fabric Value As natural dye, to obtain brown color shade fresh and
dried bark of Babul (Acacia Nilotica L.) was used for the
Material Cotton
present study. Babul bark (Acacia Nilotica L. or Acacia
Warp yarn count 73 (Nm)
arabica L.) is the source of brown colored chemical con-
Weft yarn count 70 (Nm)
stituents along with reasonable quantity of tannins. Phy-
Ends per inch 76
tochemical analysis of babul bark reveals presence of
Picks per inch 53
polyphenolic complex (Fig. 1) present in the bark of babul
Aerial density (g/m2) 73.5
plant with presence of phenols, flavones, tannins and gly-
Thickness (mm) 0.075
coside. The total phenolic and tannin content in the dried
bark of babul is found to be 9.86 and 13.40%, respectively;
while the total flavonols and total O-dihydric phenols
including chlorogenic acid are 0.0025 and 0.013%
respectively [10–12]. The babul bark also contains some
Chemicals and Dyes
tannin in the form of gallic acid (Fig. 2) besides some
saponins [10–12]. So, the main color components of babul
Locally procured following chemicals and dyes were used
bark, obtained from its aqueous extract, is shown in Figs. 1
in the present work:
and 2 below:

Chemicals/Dyes Source Purpose

Lab. Grade aluminium E Marc-India As metallic Mordanting

sulphate, potash agent or dyeing
aluminium sulphate additives
(alum) and stannous
chloride, sodium
chloride/sodium
sulphate
Green-zyme DSZL GreenTex To desize, scour and
(Enzymatic desizing chemicals, bleaching of cotton
agent), Green scour Mumbai khadi fabric
RW (low foaming
rewetting agent), Green
scour FC (Conc.
scouring agent), Pero-
stab S.F (phosphate
based non silicate
peroxide stabilizer),
green-zyme POK
(enzymatic peroxide
killer)

Fig. 1 Poly-phenolic complex obtained from babul bark, as its colour

component

123

Fig. 2 Gallic acid from babul
bark
Experimental Methods
Optimization of Conditions of Aqueous Extraction
of Babul Bark and its Purification
Babul bark powder, prepared from the sun dried bark of
babul plant, by grinding it mechanically using a motorized
pulveriser cum grinding machine, in hot water was taken
for aqueous extraction of its color component under vary-
ing conditions (MLR 1:30–1:80, pH 4–10, time period
15–90 min and temperature 60–90 °C) for optimizing the
conditions of extraction. The pH of aqueous extract of
babul bark was normally found to be 4; which was either
acidified with acetic acid or alkalified with caustic soda
solution for altering or varying the pH during dyeing, as per
requirement of study of variation pH during dyeing.
Absorbance (optical density) at a particular maximum
absorbance–wavelength (kmax. 510 nm) for the aqueous
extract of the babul was estimated using Shimadzu –UV
2450 UV–Vis absorbance spectrophotometer for very
dilute solution of it. The wavelength scan of UV–Vis
spectrum (Fig. 3) of colored solution of aqueous extract of
babul bark indicates three characterized peaks at 510 nm
(visible regions) and at 270 and 240 nm (uv region) out of
the total scan wavelength at 200 nm to 900 nm.
For characterization the color components of babul bark
as natural dye, the concentrated aqueous extracts of babul
bark was filtered and the filtrates was evaporated to a semi-
solid mass under water bath. The semi-solid mass was then
Fig. 3 UV–VIS Spectrum of aqueous extract of Babul bark
123
J. Inst. Eng. India Ser. E
put in a cage of wrapped filter paper and further subjected
to in soxhlet apparatus using 1:1 ethyl alcohol/benzene
mixture for 10 cycles at 70 °C for 2 h. The alcohol-ben-
zene extract of the color component was finally subjected
to evaporation in a water bath at 50 °C to get semi-dry
mass of the pure color component. Finally, this dry mass of
the color component was washed with acetone followed by
methyl alcohol and finally dried in air to obtain the dry
powder of the pure color component of babul bark for
chemical analysis and characterization.
Preparation of Harda (Myrobolan) Gel and Solution
Myrobolan powder was allowed to swell in water medium
overnight. Thus, swollen myrobolan gel was obtained by
soaking harda (myrobolan) powder in water (MLR – 1:10)
for overnight (12 h) at ambient temperature (25 ± 5 °C).
A known volume of water was mixed to this aqueous gel of
harda to dilute it to required strength and heated at around
80 °C for 30 min. The solution was filtered in a 60 mesh
nylon cloth after cooling and the filtrate was used as harda
solution of varying concentration (10–40%)—as pre-mor-
danting assistant.
Single Mordanting of Cotton Khadi fabric
with Harda (Myrabolan)
For Initial pre-mordanting with harda bleached khadi cot-
ton fabric was treated with myrabolan (harda) filtered
solution in separate bath at 40–50 °C and then temperature
was raised to 80 °C [23]. The process was continued for
30 min. After the said first pre-mordanting with harda
solution using MLR of 1:20 at 80 °C for 30 min, the fabric
samples were then squeezed and dried in air without
washing for either subsequent dyeing or for second mor-
danting in sequence.
J. Inst. Eng. India Ser. E
Single Mordanting of Cotton Khadi fabric
with Metallic salts
Aqueous solution of metallic salts like aluminium sulphate
[Al2 (SO4)3], potash alum [KAl (SO4)2], and stannous
chloride [SnCl2] at varying concentrations 5–20% was used
for pre-mordanting of bleached khadi cotton fabric sepa-
rately with metallic salt mordants at 80 °C for 30 min
using MLR of 1:20. The fabric samples were squeezed
properly after metallic salt mordanting and dried in air
without washing for subsequent dyeing.
Sequential Double Pre-mordanting
The sequential double pre-mordanting was done following
our earlier work on natural dye already published [17] for
optimization of mordant and dyeing conditions for madder
as natural dye applied on cotton khadi fabric. In case of
sequential double pre-mordanting system adopted, the said
combination of double pre-mordanting was done by fol-
lowing method for applying the said different combination
of double mordants with different concentrations and also
in optimum concentrations, applied in sequence, as given
below:
Myrabolan/harda ‘gel’ prepared by soaking myrobolan
in water overnight (12 h) was diluted an appropriate con-
centration (15% or 11.25% w/w or other varying percent-
ages) and heated, cooled and filtered. Bleached khadi
cotton fabric was then first mordanted with 11.25% (i.e.
75% of 15% or other varying percentages) myrabolan
solution using 1:20 MLR at 80 °C for 30 min. After the
treatment, the fabric was dried in air without washing to
make it ready for second mordanting.
Then the myrobolan/harda pre-treated cotton fabric was
further treated with 3.75% (i.e. 25% of 15% or other
varying percentages) aluminium sulphate at 80 °C for
30 min using 1:20 MLR. After the second mordanting the
fabric samples were finally dried in air without washing to
make them ready for subsequent natural dyeing with babul
bark for the present work..
Thus, all single pre-mordanted [Harda, Al2(SO4)3,
KAl(SO4)2and SnCl2] and all combination of sequential
double pre-mordanted [Al2(SO4)3 ? KAl(SO4)2,-
Al2(SO4)3 ? SnCl2, Al2(SO4)3 ? Harda, KAl(SO4)2-
? SnCl2, KAl (SO4)2 ? Harda, SnCl2 ? Harda] cotton
khadi fabric samples were used for further study of dyeing
with aqueous extract of bark of babul to optimise the
mordanting process and later to optimise the dyeing pro-
cess variables with optimized pre- mordanted system.
Dyeing of Pre-mordanted Khadi Cotton Fabrics
with Aqueous Extract of Babul Bark
Peroxide bleached and pre-mordanted (single and double)
khadi cotton fabric samples were subjected to dyeing
separately using the aqueous extract of babul bark with
prefixed or varied concentrations. Initially the study was
carried out using varying concentrations (5–20%) of single
mordants and then with varying ratio of double mordants.
After optimization of mordant type and combination and
concentration of each of the said double premordanting
was finally done with overall 15% concentration of com-
bination of Harda ? Al2SO4 (75:25 ratio) at optimum
mordanting concentration which were dyed with specific
aqueous extract of babul bark as dye-liquor having specific
concentration (30% on the weight of dye source material)
of aqueous extract of Babul bark, using normal dyeing
conditions as—MLR, 1:20; pH, 6; dyeing temperature,
80 °C and dyeing time, 60 min. After optimization of
mordant concentrations and dyeing parameters, all such
dyeing was done with 30% babul bark extract at optimized
dyeing conditions after sequentially double pre mordanted
with overall 15% concentration of combination of
Harda ? Al2SO4 (75:25 ratio) at optimum mordanting
conditions.
In the next phase, the study of the effects of dyeing
process variables on color yield was carried out for opti-
mizing the dyeing conditions. The dyeing process vari-
ables/parameters were varied taking dyeing time
15–120 min, dyeing temperature 50–95 °C, material to
liquor ratio 1:10–1:50, conc. of aqueous extract of babul
bark (as natural dye) 10–50%, common salt conc, 0–15%
and pH 3–13 after double pre mordanted with optimized
double pre mordanting system with overall 15% concen-
tration of (Harda as first mordant ? Al2SO4 as second
mordant in 75: 25 ratio) applied in sequence on khadi
cotton fabric. The dyed khadi cotton fabric samples were
washed thrice with hot and cold water, after completion of
each dyeing cycle and then dried in air. Finally soaping of
the dyed samples was done with 2 gpl neutral soap solution
at 60 °C for 15 min, followed by repeated water wash
followed by drying under sun. Unless otherwise stated,
after optimization of the dyeing process variables, all
dyeing experiments using babul extract were carried out at
optimum dyeing conditions only for further analysis dyeing
results and characterization of color fastness properties
following our earlier series of studies on natural dyeing of
cotton khadi fabrics and jute fabrics with other natural dyes
already published [6, 17, 23].
123
 J. Inst. Eng. India Ser. E

Testing Methods of scattering; and Rkmax, is the Reflectance value at

maximum absorbance–wavelength.Whereas,
The following testing and characterization were done as
DE ¼ ½ðLÞ2 þ ðDaÞ2 þ ðDbÞ2 1=2 ð2Þ
per method mentioned respectively, after prior condition-
ing of the samples at 65 ± 2% RH and 27 ± 2 °C tem- Where,
perature for 48 h as per the IS: 6359-1971:
L* = 116 ðY/Yo Þ1=3 16 DL ¼ L1  L2 ð3Þ
h i
a ¼ 500 ðX/X0 Þ1=3  ðY/Y0 Þ1=3 Da = a1  a2
Testing Instrument Methods
parameter
h i ð4Þ
b ¼ 200 ðY/Y0 Þ1=3 ðZ/Z0 Þ1=3 Db ¼ b1  b2
Warp-way Paramount digi strength ASTM: D
breaking (Model no. 16509 2004T) 5035-11,2015 Chroma, (psychometric chroma) values in CIELAB color
tenacity tester, traverse speed of cut strip method space was calculated as follows:-
(CN/tex) and 100 ± 10 mm/min, pre- of tensile
 1=2
breaking tension of 0.050 N/mm., strength testing CðabÞ ¼ a2 + b2 ; DC ¼ C1ðabÞ  C2ðabÞ ð5Þ
extension gauge [27]
(%) values length = 25 mm 9 125 mm
Where, C*1(ab) and C*2(ab) are the chroma values for
Stiffness in Paramount fabric stiffness As per IS: 6490 –
standard and produced sample.
terms of tester (cantilever type) for 1971(Cantilever h
warp-way fabric samples of test) [28] 2  2 
DHab ¼ DEab  ðDL Þ2  Cab 1=2 ð6Þ
bending 200 mm 9 25 mm
length
UV–VIS scan Shimadzu –UV 2450 UV–Vis As per standard
RðDRX0 Þ2 RðDRY0 Þ2
Metamerism Index (MI) ¼ þ
of aqueous absorbance method of X2 Y2 ð7Þ
extract of spectrophotometer wavelength scan 2
RðDRZ0 Þ
natural dyes of dye solution þ
(Results of against distilled Z2
UV–Vis scan water as
Where, X0, Y0 and Z0 are the tri stimulus values of a
is shown in reference using
Fig. 3) 3 mm path standard white surface of MgO (or equivalent surface of
length standard standard white tile) and X, Y and Z are the tri stimulus
quartz cell values of the corresponding samples.
K/S, DE, DL, X-rite (Gretag Macbeth) As Per CIE-1976
Brightness Index
DC, DH, MI, portable reflectance method [29]
and related spectrophotometer with respectively Reflectance value of the substrate at 457 nm
¼  100:
color associated color-eye XTH using formulae Reflectance value of the standard diffuser/white tile at 457 nm
parameters, color measurement and given below ð8Þ
matching software
Brightness Same instrument as above As per ISO-2469 Determination of Color Difference Index Value
index (BI) and 2470 (CDI)
method [30]
After measuring the above said usual color parameters, the
magnitudes of respective DE, DC, DH and MI values
irrespective of their sign and direction was used to obtain a
single index called as Color Difference Index (CDI) as per
Measurement of Surface Color Strength (K/S) DE,
following empirical relationship [31]
DL, DC, DH, MI, BI and Related Other Color
Parameters DE  DH
Color Difference Index ðCDI) ¼ : ð9Þ
DC  MI
K/S value, DE, DL, DC, DH, Metamerism Index (MI) and This color difference index or CDI value is considered
Brightness Index (BI), etc. were measured by using X-rite to be a very important indicator for distribution of color
reflectance spectrophotometer using following standard across the plane of the surface area of the fabric and the
CIE formulae [31]: - same is established earlier published literature, which may
ð1  Rkmax Þ2 be used not only to understand overall variation of color
K=Skmax ¼ ¼ aCD ð1Þ across the plane of the fabric but also to understand the
2Rkmax
effect of any dependant variables on uniformity of dyeing
Where K is the coefficient of absorption; S, the coefficient (a higher value of CDI value indicate more criticality of
that dependant dyeing parameters for control of uniformity

123
J. Inst. Eng. India Ser. E
in dyeing by using this single index instead of measuring
DE, DC, DH and MI separately. Higher is the CDI value
less is dye uniformity across the surface of the textile
fabrics. Higher is the differences of CDI maximum vs CDI
minimum values, less are the dye uniformity across the
surface of the textile fabrics. Moreover for application of
binary mixture of colors/natural dyes, the compatibility
rating between any two dyes (used in combination as a pair
for developing compound shades) may be determined by
calculating differences between Maximum CDI and
Minimum CDI values for dyeing any textile fabric using
binary mixture of two dyes at different proportions. But in
this case of present study, this is more important to
determine CDI values against variation of each dyeing
parameters/process variables, as higher is the CDI value for
small variation of any one dyeing process variable, the
criticality of that variable is indicated to be more important
and need to control more to obtain uniform and
reproducible natural dyeing.
Evaluation of Wash, Light, Rubbing (Dry and Wet)
and Perspiration Fastness Properties
Color fastness to washing [28] of the dyed samples was
determined as per the IS: 764-1984 method following IS -3
(equivalent to ISO-III) wash fastness method using
Megatech Overseas India Launder-O-Meter and relevant
grey scale.
Color fastness to rubbing [28] (dry and wet) was
assessed as per the IS: 766-1984 method using an elec-
tronic crock meter and relevant grey scale.
Color fastness to light [28] was determined as per IS:
2454-1984 method using Microsal Fade-O-Meter and eight
blue wool standards with known light fastness grade 1–8.
Perspiration fastness tests for dyed cotton khadi fabric
samples were carried out as per IS method 971-1983: RA
2009 method [28] at two different pH levels i.e., pH - 5.5
and pH - 8 using freshly prepared perspiration liquor as
per standard recipe and method (As Human Perspiration
may be acidic or alkaline in nature depending on one’s
metabolism).
Metallic Element Content Analysis on Mordanted
and Dyed fabric by Atomic Absorption
Spectroscopy (AAS)
The contents of metallic element i.e., Suphur (S), Nitrogen
(N), were measured in a GBC 90.6 AA model Atomic
Absorption Spectrophotometer as per Alpha method.
Study of Changes in Chemical Functionality
by FTIR Analysis
Fourier transform infrared spectroscopy (FTIR) of pre-
mordanted and dyed cotton khadi fabric samples were
examined in a FTIR spectrophotometer (model—Perkin
Elmer spectrum version 10.03.09) using the KBr disc
technique and was analyzed following FTIR—spectro-
scopic Table [32]. Before sample preparation, each of the
samples was thoroughly washed in distilled water and
methanol before final drying and then it was subjected to
FTIR testing and scans.
Results and Discussion
Standardization of Conditions of Aqueous extraction
of Bark of Babul
The optimum conditions for aqueous extraction of the color
components from completely dried bark of babul have been
standardized prior to dyeing of bleached cotton khadi
fabric (control) with aqueous extract of bark of babul. The
maximum absorbance–wavelength kmax is found to be
510 nm for aqueous extract of babul bark from UV–Vis
scan (Fig. 3). This wavelength scan also show two pre-
dominant peaks at uv-region at 240 and 270 nm, showing
its good uv-absorbance character expecting to affect the
light fastness properties. Data in Table 1 indicates optical
density (i.e. Absorption) of aqueous extract of color com-
ponent extracted from babul bark. Data in bold letters
signifies maximum value of absorption/Optical density at
observed maximum absorbance–wavelength (kmax) at
510 nm and the conditions at which color yield/absorption
value is maximum, that condition is treated as optimum.
The final result from Table 1 reveals that the aqueous
extraction of color components from the bark of babul
gives maximum color yield when extraction is done under
MLR-1:30, Extraction time-45 min, Temperature-60 °C
and pH-6. However, as pH of aqueous extract of babul bark
(without any addition of alkali or acid) is normally 4, it
needs to alkalified to bring pH- 6 from pH -4for uniform
color yield.
Effects of Selective Single Pre-mordanting
for Dyeing with Extract of Babul Bark
Data available in Table 2 indicates the impact of usage of
aqueous solution of different mordants alone in varying
quantities (5–20%). Mordants applied were aluminium
sulphate [Al2 (SO4)3], potash alum [KAl (SO4)2], stannous
chloride [SnCl2] and harda using a MLR of 1:20 at 80 °C
for 30 min keeping all dyeing variables constant. There is a
123
 J. Inst. Eng. India Ser. E

Table 1 Optical density of aqueous extract of bark of Babul unusual that only harda, as a mordanting assistant without
extracted under various conditions of extraction any metallic mordant also gives good color strength, which
Extraction variables Absorbance/optical density of Babul is then further, analyzed by atomic absorption spec-
extract at kmax 510 nm trophotometry and is found that the extract of babul and
also babul dyed cotton fabric contains metallic impurities
Material-to-liquor ratio (MLR)
in babul bark and it helps harda to act so predominantly.
1:30 0.483
However, combination of harda with other metallic mor-
1:40 0.305
dant may give a better result which is examined later.
1:50 0.318
Based on the chemical structure, molecular weight and
1:60 0.113
no. of coordinated groups available etc., the giant complex
1:70 0.129
formation amongst fibre-mordant-dye system for particular
1:80 0.08
natural fibres vary and shows different results. In this case,
Temperature (°C)
10% single mordant concentrations of harda perhaps sat-
50 0.190
isfies the required stoichiometric ratio and gives good
60 0.194 result in terms of the surface color strength of the babul
70 0.193 dyed sample than other single metallic mordants. Hence
80 0.158 10% (on weight of fabric) mordant concentration of harda
90 0.114 as single mordanting assistant is advantageous though
Time (min) combination of harda with other metallic mordants has
15 0.08 even though better results as proven later.
30 0.129 Negative charges acquired by the cotton cellulose on
45 0.418 immersion in water needs to be neutralized before anionic
60 0.142 or mordantable natural dyes are absorbed on celluloses.
75 0.15 This can be achieved by pre-treatment with metallic
90 0.214 cationic salts (like alum or aluminium salts). Hence, cotton
pH fabric has been pre-treated with harda and metallic salts in
4 0.233 sequence by double pre-mordanting. This enables creation
5 0.173 of more and more cationic sites on pre-mordanted cotton
6 0.34 for more absorption of anionizable natural dyes like bark of
7 0.184 babul containing poly-phenolic color components and
8 0.157 vegetable gallic/tannic acid residue, as shown in Figs. 1
9 0.122 and 2.
10 0.085
Effects of Selective Double Pre-mordanting Applied
*Values in bold indicate the optimum values considered while
studying the effect of other extraction parameters in Sequence for Dyeing with Extract of Babul Bark

noticeable increase in the K/S values of the dyed sample,
when it is mordanted with 10% harda separately as single
mordant against application of same percent aluminium
sulphate [Al2 (SO4)3], potash alum [KAl (SO4)2] and
stannous chloride [SnCl2] on the same fabric at comparable
and similar conditions of treatment. Probably the chebu-
linic acid content in harda is expected to develop more
numbers of dye-mordant-fibre complexes, yielding higher
color yield. Enhancement of mordant concentration above
10% either do not show any further increase in K/S value
or reduce the tenacity of the mordanted fabric to a
noticeable extent and hence considering an overall balance
in all factors including costs, etc. pre-mordanting with 10%
harda as a single mordanting ambient, renders an accept-
able option in this case for dyeing with babul bark extract
than the effects of other single mordants used. This is
Changes in surface color strength and other color interac-
tion parameters due to application of different double
mordants applied in sequence (harda followed by other
metallic mordants or otherwise) on cotton khadi fabric
dyed with 30% (on the basis of dry weight of solid source
material) aqueous extract of bark of babul has been shown
in Table 3. Double pre-mordanting was done with 15%
overall combination of any two mordant concentrations
applied in sequence with varying ratio (0:100, 25:75,
50:50, 75:25 and 100:0) on cotton khadi samples. These
samples were further studied and subsequently dyed with
aqueous extract of bark of babul at comparable conditions
of dyeing. The sequential double mordanting was done
with—Al2 (SO4)3 ? KAl(SO4)2, Al2 (SO4)3 ? SnCl2,
Harda ? Al2 (SO4)3, KAl (SO4)2 ? SnCl2, Harda ? KAl
(SO4)2 and Harda ? SnCl2.

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J. Inst. Eng. India Ser. E

Table 2 Effects of selective single pre-mordanting for dyeing of cotton khadi fabric with Babul bark extract
Mordant and Warp-way tenacity Warp-way breaking elongation Warp-way bending length K/S at BI MI CDI CV
conc. cN/tex (%) (cm) kmax (%)

(Control fabric)a 1.58 11.52 1.43 0.11 69.13 – – –

Alum KAl2(SO4)a3
5% 1.55 16.37 1.32 2.41 19.66 0.38 4.35 5.96
10% 1.36 16.05 1.30 2.03 22.74 0.09 0.11 5.71
15% 1.29 14.28 1.36 1.44 27.68 0.35 4.78 2.66
20% 1.33 15.52 1.40 1.22 30.68 0.21 1.26 3.405
b
Aluminium Sulphate (Al2(SO4)3)
5% 1.35 12.30 1.21 2.03 22.79 0.46 3.65 4.58
10% 1.02 11.43 1.14 1.82 24.71 0.07 4.36 6.82
15% 1.41 14.78 1.38 1.69 26.74 0.27 0.77 5.36
20% 1.31 12.67 1.36 1.47 28.74 0.23 1.22 3.94
b
(SnCl2)
5% 1.54 15.69 1.62 1.50 26.51 0.69 0.64 1.45
10% 1.27 14.54 1.52 0.89 36.31 0.35 6.20 8.63
15% 1.28 12.70 1.41 1.39 31.42 0.31 0.55 6.37
20% 0.92 13.81 1.25 0.78 39.89 0.37 4.22 1.89
Harda
5% 1.44 14.60 1.24 5.24 14.64 0.10 1.82 22.69
10% 1.40 12.10 1.28 6.57 13.54 0.26 4.66 13.22
15% 1.28 11.63 1.29 3.05 17.00 0.21 6.08 8.61
20% 1.31 11.18 1.31 4.42 15.18 0.14 6.08 12.32

Data in Table 3 reveals that 15% overall application of
harda and aluminium sulphate in 75:25 ratios on bleached
cotton khadi fabric for dyeing with aqueous extract of bark
of babul shows maximum surface color strength (K/S
value) than any of the above said single pre-mordants or
other double pre-mordants. The reason behind this fact is
that myrobolan (harda) acts as pre-mordanting assistants/
additives when used in conjunction with metallic salts as
another mordant. Higher color yield is possible due to
presence of chebulinic acid (having mordantable–COOH/–
OH groups) present in myrobolan and tannin content in
babul extract. Insoluble metal tannates (for gallic/tannic
acids present in babul) or metal poly carboxylates (for
chebulinic acid in harda) are expected to be formed when
myrobolan is used along with the metal salts as second
mordant to fix well on the cellulosic fibres. Inspite of this,
fibre is still having enough free adjacent hydroxyl/car-
boxylic acid groups to form mordant-dye complex to fix
the anionizable/mordantable natural dyes like bark of babul
on the said double pre-mordanted cotton.
Further Table 4 shows the differences in shades gener-
ated with and without usage of harda as one among the pre-
mordanting assistant and later dyed with 40% of extract of
babool. Visual observation of the swatches in Table 4
clearly signifies that brighter shade can be seen in the
samples which contain harda as one among the mordanting
assistants during pre-mordanting.
A glance at Table 5 also signifies more surface color
strength (K/S) value for the cotton fabric samples which
are pre-mordanted with harda as one among mordanting
assistants.
The cotton khadi fabric acquires a light brown shade
after pre-mordanting with harda alone as a single mordant
and dyed with bark of babul extract, whereas both potash
alum and aluminium sulphate as single mordant give bright
shades of varying color ranging from light pinkish brown
to medium pinkish brown shades. Double pre-mordanting
with harda followed by aluminium sulphate (15% overall
application of two mordants i.e., harda and aluminium
sulphate in 75:25 ratio respectively show medium brown
(for babul dye extract concentration being 30%). Thus,
finally, a double pre-mordanting with harda and aluminium
sulphate applied in sequence with overall 15% application
in 75:25 ratio of harda and aluminium sulphate gives
overall balanced results of color strength with reddish
brown shade on cotton khadi fabric. Table 6 shows shades
obtained by cotton khadi fabric by dyeing with babool bark
without mordanting and after pre-mordanting with 15%
[Harda ? KAl2(SO4)2 (in 75:25 ratio)] and later dyed with
bark of babool. It indicates that the color content of babool

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Table 3 Effects of selective double pre-mordanting applied in sequence for dyeing of cotton khadi with Babul bark as natural dye
Mordant Warp Warp way Warp way K/S BI MI CDI CV Colour Colour Colour Perspiration (LOD)
and its way breaking bending at % fastness to fastness to fastness to
concn. tenacity elongation length kmax of washing light ISO- rubbing ISO
cN/tex (%) (cm) K/S ISO III 2454:1984 766-1984
Dry Wet Acidic Alkali

(Control 1.58 11.52 1.43 0.115 69.13 – – – – – – – – –

fabric)a
Al2(SO4)3 ?KAl2(SO4)3–overall 15%
0:100 1.29 14.28 1.36 1.44 27.68 0.35 4.78 2.66 3/4 1/2 4/5 4 1/2 1/2
25:75 1.35 10.06 1.53 1.72 0.14 0.14 2.92 3.92 3/4 2 4/5 3/4 1/2 1/2
50:50 1.31 10.69 1.43 2.15 22.77 0.11 2.54 6.94 3/4 2 4/5 4 1/2 1/2
75:25 1.39 9.75 1.53 2.21 22.93 0.08 0.38 8.41 2/3 2 4/5 4 1/2 1/2
100:0 1.41 14.78 1.38 1.69 26.74 0.27 0.77 5.36 2/3 1/2 5 4 1/2 1/2
Al2(SO4)3 ?SnCl2–overall 15%
0:100 1.28 12.70 1.41 1.39 31.42 0.31 0.55 6.37 2/3 2 4/5 4 1/2 1/2
25:75 1.19 10.58 1.34 2.56 20.64 0.29 4.77 6.36 4 3 4/5 3/4 2 2
50:50 1.15 9.87 1.26 2.15 23.23 0.29 5.39 4.30 3/4 2/3 4/5 4 1/2 1/2
75:25 1.40 9.73 1.28 1.77 25.50 0.45 1.61 6.38 3/4 2/3 5 4 1/2 1/2
100:0 1.41 14.78 1.38 1.69 26.74 0.27 0.77 5.36 2/3 1/2 5 4 1/2 1/2
Harda ? Al2(SO4)3–overall 15%
0:100 1.41 14.78 1.38 1.69 26.74 0.27 0.77 5.36 2/3 1/2 5 4 1/2 1/2
25:75 1.43 13.90 1.53 2.78 20.94 0.29 16.13 2.45 3/4 2 4/5 3/4 1/2 1/2
50:50 1.46 13.73 1.31 5.04 16.29 0.36 4.16 5.02 3/4 3 4/5 3/4 2 2
75:25 1.64 13.73 1.31 6.44 15.11 0.12 0.25 4.78 4 3/4 4 3/4 2/3 2/3
100:0 1.28 11.63 1.29 3.05 17.00 0.21 6.08 5.61 4 1/2 4/5 3/4 1/2 1/2
KAl2(SO4)3 ? SnCl2–overall 15%
0:100 1.28 12.70 1.41 1.39 31.42 0.31 0.55 6.37 2/3 2 4/5 4 1/2 1/2
25:75 1.36 9.68 1.45 2.21 22.48 0.20 11.04 5.55 3/4 3/4 4/5 4 2/3 2/3
50:50 1.07 7.84 1.35 2.06 23.54 0.60 3.12 4.90 4 3/4 4/5 4 1/2 1/2
75:25 1.22 10.50 1.5 2.38 21.20 0.11 2.61 6.14 3/4 2/3 4/5 3/4 1/2 1/2
100:0 1.29 14.28 1.36 1.44 27.68 0.35 4.78 2.66 3/4 1/2 4/5 4 1/2 1/2
Harda ? KAl2(SO4)3–overall 15%
0:100 1.28 11.63 1.29 3.05 17.00 0.21 6.08 8.61 3/4 1/2 4/5 4 1/2 1/2
25:75 1.08 14.36 1.38 3.58 20.44 0.39 4.08 9.28 3 3 4/5 3/4 1/2 1/2
50:50 1.24 17.86 1.73 5.41 16.01 0.37 8.26 8.47 3/4 3 4/5 3/4 2/3 2/3
75:25 1.47 13.90 1.36 4.61 15.59 0.19 8.60 7.06 3/4 3 4/5 3 2/3 2/3
100:0 1.29 14.28 1.36 1.44 27.68 0.35 4.78 2.66 4 1/2 4/5 3/4 1/2 1/2
Harda ? SnCl2–overall 15%
100:0 1.28 11.63 1.29 3.05 17.00 0.21 6.08 8.61 4 1/2 4/5 3/4 1/2 1/2
75:25 1.15 16.16 1.5 4.35 18.92 0.32 8.42 2.04 3/4 Above 4 4/5 4 1/2 1/2
50:50 1.19 13.70 1.41 3.75 21.18 0.72 5.33 0.48 3/4 3/4 4/5 4 2/3 2/3
25:75 1.41 15.60 1.33 3.09 20.82 0.05 9.98 2.18 4 Above 4 4/5 4 2/3 2/3
0:100 1.28 12.70 1.41 1.39 31.42 0.31 0.55 6.37 2/3 2 4/5 4 1/2 1/2

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J. Inst. Eng. India Ser. E
Table 4 Swatches showing shades generated with and without usage of harda as one among the pre-mordanting assistant and later dyed with
40% of extract of babool
Particulars of shade Shade image
Mordanted with 15% [Al2(SO4)3
?KAl(SO4)2 (in 50:50 ratio)]
and later dyed with 40%
Babool extract
Mordanted with 15%
[Al2(SO4)3 ? SnCl2 (in 50:50
ratio)] and later dyed with 40%
Babool extract
Mordanted with 15%
[KAl2(SO4)2 ? SnCl2 (in
50:50)] and later dyed with
40% Babool extract
bark is low. But, to get deep shades, cotton fabric has been
mordanted with Harda and then dyed with Babool bark.
Effect of variation of Types and Dosages
of Mordants on Color Fastness for Dyeing
with Extract of Babul bark
Data in Table 3 indicate color fastness properties of cotton
khadi fabric samples pre-mordanted with varying type of
single mordant and dyed with bark of babul as well as
double pre-mordanted in different ratio with Overall 15%
mordant application and subsequently dyed with extraction
of bark of babul.
It is clear from color fastness data from Table 3 that
both the use of either only harda or use of higher con-
centration of harda with any of the metallic mordant
combination shows better or higher color fastness to wash
than any other metallic mordant and in single without
harda. However, light fastness is independent on harda
concentration. Light fastness is also found to be better on
use of SnCl2, showing best results for Harda and SnCl2
combination followed by next good result for harda and
aluminium sulphate combination for 15% overall applica-
tion in 75:25 ratio. Fastness to dry rubbing (crocking
fastness) of the dyed samples remains good in all the cases,
whereas fastness to wet (crocking) becomes bit lower
irrespective of the concentration of harda or aluminium
sulphate and other metallic pre mordants used for pre-
mordanting the said samples, indicating more loose dye
absorption on the surface, anion is not faded in dry rubbing
but fades during wet rubbing for breaking of some tannin/
Particulars of shade Shade image
Mordanted with 15%
[Harda ? KAl2(SO4)2 (in
50:50 ratio)] and later dyed
with 40% Babool extract
Mordanted with 15%
[Harda ? Al2 (SO4)3 (in
50:50 ratio)] and later dyed
with 40% Babool extract
Mordanted with [15%
Harda ? SnCl2 (in 50:50
ratio)] and later dyed with
40% Babool extract
chebulinic acid based hydrogen bonding with phenoxy
group containing babul dye forming cordial/covalent
bonds/complex.
However, there is some clear difference on color fast-
ness grading when the double pre-mordanting system is
used, wherein there are no much differences in grade of
color fastness to washing, light and rubbing for the dif-
ferent double mordants used. 15% overall application of
harda followed by aluminium sulphate (in 75:25 ratio)
shows very good color fastness rating to wash and rubbing
amongst all different double mordanting systems tried.
This may be presumed to be due to some combined and
synergistic effect of the combination of aluminium sul-
phate along with harda as pre-mordanting assistant due to
additional coordinating power of chebulinic acid of harda,
which perhaps facilitates more number of strong complex
formation with more coordinated covalent bonds amongst
the said fibre-mordants-dye system in presence of both
myrobolan (harda) containing chebulinic acid residue and
aluminium sulphate in combination.
Perspiration fastness with respect to the loss in depth of
shade from babul dyed khadi cotton fabric samples dyed
with babul extract is found to be generally poor to mod-
erate for both acidic and alkaline perspiration for all the
four single mordants used. But, it is not the same with
double mordants. Use of double mordants shows some
improvement in it in few cases. Perspiration fastness with
respect to loss of depth is moderate to good for the babul
dyed samples prepared by using 15% overall application of
harda followed by aluminium sulphate (in 75:25 ratio) as
double mordants that anchors the color components of
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 J. Inst. Eng. India Ser. E

Table 5 Various color parameters of cotton fabric samples pre-mordanted with/without harda and dyed with bark of babool
Mordant and its concn. K/S at kmax DE DL Da Db DC DH BI MI CDI CV % of K/S

(Control fabric)a 0.115 – – – – – – 69.13 – – –

Al2(SO4)3 ? KAl(SO4)2, 15% combination
50:50% 2.15 0.38 - 0.08 0.05 - 0.37 - 0.30 - 0.22 22.77 0.11 2.54 6.94
Al2(SO4)3 ? SnCl2, 15% combination
50:50% 2.15 1.79 1.08 - 0.29 1.40 1.09 0.92 23.23 0.29 5.39 4.30
KAl2(SO4)2 ? SnCl2, 15% combination
50:50% 2.06 0.65 0.45 0.11 0.45 0.45 0.13 23.54 0.60 3.12 4.90
Harda ? KAl2(SO4)2, 15% combination
50:50% 5.41 1.33 0.87 - 0.78 0.63 0.40 0.92 16.01 0.37 8.26 8.47
Harda ? Al2(SO4)3, 15% combination
50:50% 5.04 1.07 0.29 - 0.61 0.83 0.60 0.84 16.29 0.36 4.16 11.02
Harda ? Sncl2, 15% combination
50:50% 3.75 1.86 - 0.42 - 1.35 1.20 0.79 1.63 21.18 0.72 5.33 0.48

Table 6 Comparison of shades obtained by dyeing cotton fabric dyed with babool with & without mordanting
Mordanted with 15% Cotton fabric dyed with
[Harda ? KAl2(SO4)2 (in 75:25 40% Babool without
ratio)] (K/S value - 1.33) Mordanting (K/S value
- 2.93)

Mordanted with 15%

[Harda ? KAl2(SO4)2 (in 75:25
ratio)] and later dyed with 30%
Babool (K/S value - 3.88)

babul extract in the Khadi cotton fabric often under acidic
or alkaline pH of perspiration solution. Hence, based on
both color yield (K/S value) and color fastness perfor-
mance of all double pre- mordanted samples, 15% overall
application of harda followed by aluminium sulphate (in
75:25 ratio) gives optimum results of dyeing (color yield
i.e., K/S Value) with 30% extract of dried babul bark
powder. Moreover, considering data for CV% varying
between 0.38 and 9.28% for different double mordants
used, the optimized mordant system show CV% within
4.78% (within 5%), which is considered to be accept-
able uniform shades. Moreover, CDI value is minimum in
this case compared to other mordants.
Studies on Dyeing Process Variables with Respect
to Color Strength and Color Fastness Properties
Bleached cotton khadi fabric mordanted with 15% overall
application of Harda ? Al2 (SO4)3 combination in 75:25
ratio, which was dyed with 30% (on the basis of dried
weight of solid plant materials) aqueous extract of babul
bark has been studied for effect of different dyeing process
variables to optimize the dyeing conditions so as to obtain
uniform and reproducible maximum color yield (in terms
of K/S value). Data in Tables 7, 8, 9, 10, 11, 12, 13 indi-
cates the effects of dyeing process variables on color yield
(K/S values) and data in Table 14 shows corresponding
color fastness properties with respect to variation in dyeing
process variables.
It is observed from the data in Table 10 that K/S value
gradually increases with the increase in time of dyeing
(15–120 min), when all other variables are kept constant.
This may be explained by increased amount of heat energy
(with higher dyeing time) leads to achieve dyeing equi-
librium with increase in dyeing time from 60 to 120 min,
depending on the rate of dye diffusion (being the slowest
step among adsorption, absorption, diffusion and fixation
of colorant molecule from Babul extract). However,

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Table 7 Effect of variation of dyeing time on colour strength, Harda ? Al2(SO4)3 (75:25) pre-mordanted Khadi cotton fabric sub-
brightness index, metamerism index, CDI value and related colour sequently dyed with specific percentage of extract of Babul bark
parameter for dyeing of 15% overall concentration of
Dyeing condns. K/S at kmax DE DL Da Db DC DH BI MI CDI* CV (%) CDImax - CDImin

Control mordanted 2.53 2.95 2.55 0.47 1.39 1.31 0.67 19.85 0.36 0.70 0.36
Time (min)
15 5.74 1.29 - 1.14 0.32 - 0.53 - 0.38 - 0.49 14.13 0.20 8.31 9.87 6.07
30 5.77 1.66 - 1.37 0.73 - 0.60 - 0.32 - 0.89 14.22 0.59 7.82 11.06
60 6.37 1.87 1.10 - 1.07 1.07 0.62 1.38 14.12 0.53 7.85 17.85
90 6.45 1.16 - 0.91 - 0.08 - 0.72 - 0.69 - 0.20 12.65 0.15 2.24 12.86
120 6.91 0.39 - 0.31 0.22 - 0.11 - 0.12 - 0.24 12.21 0.17 4.58 10.80

Table 8 Effect of variation of dyeing temperature on colour strength, Harda ? Al2(SO4)3 (75:25) pre-mordanted Khadi cotton fabric sub-
brightness index, metamerism index, CDI value and related colour sequently dyed with specific percentage of extract of Babul bark
parameter for dyeing of 15% overall concentration of
Dyeing condns. K/S at kmax DE DL Da Db DC DH BI MI CDI* CV % CDImax - CDImin

Control mordanted 2.53 2.95 2.55 0.47 1.39 1.31 0.67 19.85 0.36 0.70 0.36 12.09
Temp. (°C)
50 5.19 1.48 - 1.42 0.38 - 0.13 0.17 - 0.40 16.29 0.31 11.23 11.26
65 6.49 1.93 - 1.67 0.96 - 0.04 0.25 - 0.93 14.55 0.36 19.94 16.2
80 6.37 1.87 1.10 - 1.07 1.07 0.62 1.38 14.12 0.53 7.85 17.85
95 7.86 2.21 - 1.99 0.81 - 0.51 - 0.27 - 0.92 13.41 0.39 19.30 18.8

Table 9 Effect of variation of pH of dyeing liqour in dye bath on Harda ? Al2(SO4)3 (75:25) pre-mordanted khadi cotton fabric sub-
colour strength, brightness index, metamerism index, CDI value and sequently dyed with specific percentage of extract of babul bark
related colour parameter for dyeing of 15% overall concentration of
Dyeing condns. K/S at kmax DE DL Da Db DC DH BI MI CDI* CV % CDImax - CDImin

Control mordanted 2.53 2.95 2.55 0.47 1.39 1.31 0.67 19.85 0.36 0.70 0.36 8.16
pH
3 4.40 3.39 - 2.39 1.57 - 1.83 - 1.25 - 2.06 16.15 0.80 6.98 0.82
5 6.39 0.41 - 0.35 0.00 0.22 0.21 0.07 15.47 0.04 3.41 19.76
7 4.66 0.29 0.08 - 0.02 0.28 0.25 0.11 16.48 0.07 1.82 4.76
9 3.74 1.78 - 1.77 0.20 0.07 0.21 - 0.18 22.35 0.18 8.47 8.13
11 4.73 1.00 0.50 - 0.10 0.86 0.80 0.33 17.55 0.20 2.06 9.13
13 2.25 1.16 - 0.92 0.28 0.66 0.72 0.03 21.48 0.16 0.30 5.27

comparing color fastness properties (Table 8), it is
observed that 60 min dyeing time render the said dyed
fabric over all better balanced color fastness to wash, light,
rubbing and perspirations, while further increase in dyeing
time to 90–120 min, the color fastness are to some extent
reduced probably because of possibility of more unfixed
dyes adhered/deposited on the surface of the fibre for
higher dyeing time, which later causes lesser color fastness
grade. So, 60 min dyeing time may be considered as
optimum, out of all experiments of varying dyeing time
carried out in the present work.
The surface color strength (K/S values) is found to show
an increasing trend as per data in Table 8, up to 95 °C on
increase of dyeing temperature (50–95 °C), when all other
variables were kept constant. Increase in temperature of
dyeing inevitably supplies more heat energy for trans-
portation of dye molecule thus facilitating the higher rate
of dye sorption and diffusion up to a temperature of 95 °C

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Table 10 Effect of variation of MLR in dye bath on colour strength, Harda ? Al2(SO4)3 (75:25) pre-mordanted khadi cotton fabric sub-
brightness index, metamerism index, CDI value and related colour sequently dyed with specific percentage of extract of babul bark
parameter for dyeing of 15% overall concentration of
Dyeing condns. K/S at kmax DE DL Da Db DC DH BI MI CDI* CV % CDImax - CDImin

Control mordanted 2.53 2.95 2.55 0.47 1.39 1.31 0.67 19.85 0.36 0.70 0.36 10.87
MLR
1:10 6.60 0.45 - 0.22 - 0.12 - 0.37 - 0.39 - 0.02 13.45 0.10 0.23 14.67
1:20 6.37 1.87 1.10 - 1.07 1.07 0.62 1.38 14.12 0.53 7.85 17.85
1:30 6.73 0.67 0.18 - 0.49 0.41 0.20 0.61 13.68 0.24 8.51 17.5
1:40 9.10 5.30 - 4.26 3.01 - 0.94 1.03 - 3.13 11.02 1.45 11.10 39.9
1:50 7.80 0.21 0.19 0.05 - 0.08 - 0.05 - 0.07 12.95 0.05 5.88 34.2

Table 11 Effect of variation of Overall mordant concentration (5 to concentration of Harda ? Al2(SO4)3 (75:25) pre-mordanted Khadi
20%) on colour strength, brightness index, metamerism index, CDI cotton fabric subsequently dyed with specific percentage of extract of
value and related colour parameter for dyeing of 15% overall Babul bark
Mordant concn. K/S at kmax DE DL Da Db DC DH BI MI CDI* CV % CDImax - CDImin

Control mordanted 2.53 2.95 2.55 0.47 1.39 1.31 0.67 19.85 0.36 0.70 0.36 6.17
Mordant concentration i.e. Varying overall total concentration (5 to 20%) of combination of harda and aluminium sulphate in
75:25 ratio, applied in sequence with following overall mordant concentrations before dyeing with extract of Babul bark
5 6.02 0.82 - 0.25 0.16 0.77 0.75 0.21 11.60 0.18 1.27 55.9
10 6.03 1.33 - 0.29 0.51 120 1.30 - 0.01 13.72 0.27 0.03 5.67
15 6.37 1.87 1.10 - 1.07 1.07 0.62 1.38 14.12 0.53 0.35 4.85
20 7.20 1.59 - 1.47 0.09 - 0.59 - 0.52 - 0.30 12.53 0.12 7.44 17.25

Table 12 Effect of variation of dye concentration (on the basis of dry of 15% overall concentration of Harda ? Al2(SO4)3 (75:25) pre-
weight of source material) on colour strength, brightness index, mordanted Khadi cotton fabric subsequently dyed with specific
metamerism index, CDI value and related colour parameter for dyeing percentage of extract of Babul bark
Dyeing condns. K/S at kmax DE DL Da Db DC DH BI MI CDI* CV % CDImax - CDImin

Control mordanted 2.53 2.95 2.55 0.47 1.39 1.31 0.67 19.85 0.36 0.70 0.36 8.87
Dye conc. (%)
10 4.81 0.48 - 0.32 0.09 - 0.34 - 0.32 - 0.16 19.37 0.08 3.00 10.02
20 5.39 2.07 - 1.76 0.84 - 0.71 - 0.44 - 1.01 15.78 0.40 11.87 9.34
30 6.63 0.58 0.41 - 0.35 0.20 0.12 0.40 14.89 0.44 3.10 22.46
40 6.37 1.87 1.10 - 1.07 1.07 0.62 1.38 14.12 0.53 7.85 17.85
50 6.73 1.34 - 0.88 0.39 - 0.94 - 0.69 - 0.74 12.73 0.29 4.95 10.34

until equilibrium is reached. While comparison of corre-
sponding color fastness data in Table 14, it is observed that
overall color fastness data for different types/agency show
a better balance for dyeing temperature at 65 °C than those
obtained for 50 °C or 80 °C as dyeing temperature. Hence,
considering both K/S value and also color fastness prop-
erties, 65 °C temperature may be considered as better
choice for fixing optimum dyeing temperature for this
fibre-mordant-dye (babul) system.
Table 9 shows maximum dye up take in terms of surface
color strength (K/S value) with the variation of pH
(keeping other variables constant) from 3 to 5, while for pH
from 9 to 11, the surface color strength (K/S value) values
starts reducing and it further shows an increase at pH 11.
Considering, color fastness data Table 14, it is further
understood that pH 5 render batter balance of overall all
types of color fastness results even better than that obtained
at pH 11. So, pH 5 may be considered as optimum value in
this case of fibre-mordant—dye (Babul) system. It may be

123
J. Inst. Eng. India Ser. E

Table 13 Effect of variation of salt concentration on colour strength, Harda ? Al2(SO4)3 (75:25) pre-mordanted Khadi cotton fabric sub-
brightness index, metamerism index, CDI value and related colour sequently dyed with specific percentage of extract of Babul bark
parameter for dyeing of 15% overall concentration of
Dyeing condns. K/S at kmax DE DL Da Db DC DH BI MI CDI* CV % CDImax - CDImin

Control mordanted 2.53 2.95 2.55 0.47 1.39 1.31 0.67 19.85 0.36 0.70 0.36 13.00
Salt conc. (%)
0 6.23 1.68 - 1.26 0.99 - 0.52 - 0.34 - 1.11 13.00 0.54 10.15 15.88
3 7.12 5.01 - 3.87 1.59 - 2.75 - 1.88 - 2.57 11.15 1.03 6.64 8.91
5 7.25 1.26 - 0.77 0.53 0.85 0.99 - 0.16 11.92 0.21 0.96 13.2
10 6.03 0.27 - 0.07 0.25 - 0.09 0.32 - 0.27 14.36 0.10 2.27 13.49
15 6.18 1.32 1.01 - 0.86 0.07 - 0.25 0.82 14.24 1.32 13.96 8.98

presumed that at pH 5, i.e. in acidic conditions, there may
be higher chances of ionization of phenoxy hydroxyl
groups of color component of babul rendering better
chances of complex formation with harda and metallic
mordant (aluminium sulphate) forming higher anchoring of
Fibre—Mordant-Dye system in this case. Anchoring of the
color component from aqueous extract of bark of babul on
cotton khadi fabric is mainly due to formation of Fibre-
Mordant-Dye complex amongst Cotton Fibre—Harda
(chebulinic acid as mordanting assistant)—aluminium
sulphate (metallic mordant)—Gallic/Tannic acid residue—
Babul Color Component (as Dye) is shown in Fig. 4.
However formation of Hydrogen bonding between Fibre–
Mordant–Dye interactions cannot be excluded totally.
Keeping other variables constant, with the variation in
material-to-liquor ratio (MLR) from 1:10 to 1:50 as shown
in Table 10, indicates an increasing trend of K/S value
initially up to MLR of 1:40 and then there is a slow
decrease at MLR 1:50. Though MLR 1:40 shows highest
K/S value as compared to any other MLR used, but MLR
1:40 and MLR 1:50 gives very high CV% of K/S value and
thus excludes its acceptance. So, MLR 1:30 render lesser
CV% of K/S values than that of MLR 1:40 or 1:50. Con-
sidering all these, the optimum MLR may be considered to
be 1:30. Comparing corresponding color fastness data in
Table 14, it is observed that all MLR used here show
medium to good overall all types color fastness except for
1:50 MLR.
Thus, considering both color yield and color fastness
data, MLR 1:30 may be considered as optimum dyeing
conditions as it gives a better balance of color strength and
color fastness properties.
In earlier part of this study with effect of single vs
double mordanting, it is already observed that 15% overall
total application of harda (myrobolan) and aluminium
sulphate (in 75:25 ratio) applied in sequence as double
mordant, renders an overall balanced results considering its
tensile strength retention (Table 3) and K/S Value
(Table 3) after dyeing cotton with 30% babul bark extract.
However, further study of the same at comparable condi-
tions of dyeing, varying overall percentage (5–20%) of the
said selected double mordant system (i.e. harda and alu-
minium sulphate (with fixed 75:25 ratio) shows maximum
K/S values for 15–20% overall total application of harda
(myrobolan) and aluminium sulphate (75:25 ratio) with
CDI value 0.25 and CV% of K/S value as 4.78% (Table 3)
having moderate to good overall color fastness properties.
Data in Table 11 shows an increase in K/S value with the
increase in mordant concentrations for overall varying
percentages of application of harda and aluminium sul-
phate in sequence leading to optimum total concentrations
of mordants/mordant assistant in between overall 15% with
ratio of harda and aluminium sulphate 75:25 having CDI
value 0.35 and CV% 4.85 (Table 11). Though the K/S
value is slowly increasing with increase in mordant con-
centration from 5 to 20%, while 20% overall concentration
of these said two mordants, assumes higher dye non-uni-
formity showing higher value of CV% of K/S value i.e.,
17.25%. So, 15% overall concentration of harda ? Alu-
minium sulphate is considered as better. Considering cor-
responding color fastness properties (Table 14), it may be
said that both application of 10% to 20% overall concen-
tration of the said two double mordants (harda and alu-
minium sulphate in 75:25 ratio) applied in sequence, show
overall equal degree of a balanced all types of color fast-
ness properties studied here. But as 20% mordant also
reduces the tensile strength at higher extent as CV % of
K/S value is very high, CDI value is high (7.44), 20%
mordant concentration of harda ? aluminium sulphate and
is not recommended as acceptable. Thus considering all the
above facts, the optimum concentration of the mordant
system selected as optimum is 15% overall application of
Harda plus aluminium sulphate (applied in sequence with
75: 25 ratio).
Results of K/S value and other color parameters for
varying degree of dye concentration (based on oven dry

123

weight of source dye materials from plant) for selective dye
concentrations from 10 to 50% are shown in Table 12.
There is an increase in K/S value with increase in dye
conc., from 10% to 30% (on the basis of weight % of dry
Babul bark) and then it drops down slowly in 40% dye
concentration and finally increase in dye concentration at
50%. Finally 30% dye conc., is considered as the optimum
value for dye concentrations for good to very good overall
color fastness, as one of the important dyeing process
variables having lower to moderate differences between
CDI maximum and CDI minimum.
The addition of an electrolyte (common salt) to the
dyeing liquor expectedly increases the exhaustion of the
dye. Common salt is dissolved completely in the aqueous
dye liquor at different temperature of dyeing and increases
the force of repulsion between the dye molecules and
water, so that the dye molecules are more attracted towards
the cellulosic fibres. But the higher amount of salt above a
certain limit causes retardation effect in the dye absorption
vis-a-vis color yield and renders lower color strength. Data
in Table 13, it is observed that with the increase in
salt/electrolyte concentration from 0 to 5%, the color yield
in terms of K/S value increases and starts decreasing for
use of 10% salt concentration and then steadily increases
up to 15% salt concentration. However comparing over all
color fastness properties for corresponding part, the overall
all round color fastness properties are found best for 5%
salt concentrations. Considering all the above matter i.e.,
K/S value is found to be maximum at this 5% salt conc.,
rendering good all round color fastness properties, 5% salt
concentration is considered as the optimum concentration
for babul dyed cotton khadi fabric.
So, considering color fastness results in Table 14 and
results of Dyeing Uniformity in terms of CV % of K/S
values as well as CDI values obtained for each or all dyeing
parameters, as shown in Tables 7, 8, 9, 10, 11, 12, 13,
variation of Salt concentration (with difference of max and
min CDI value—13.0), Dyeing temperature (with differ-
ence of max and min CDI value–12.09) and MLR (with
difference of max and min CDI value—10.87) are found to
be considered as three most critical dyeing variables in this
case as it gives maximum dispersion of CDI value and
higher CV% of K/S Values for dyeing with babul bark.
Color Fastness results also show varying grades of fastness
for changes in these three dyeing parameters as critical. So,
It is understood that for dyeing of Cotton khadi fabric with
extract of Babul bark, these three variables are to be con-
trolled with utmost care for obtaining uniform and repro-
ducible dyeing results.
From this study, it may be summarized that the observed
optimum conditions of dyeing of the double pre-mordanted
(with overall 15% concentration of harda and Aluminium
Sulphate in 75:25 ratio in sequence) bleached cotton khadi
123
J. Inst. Eng. India Ser. E
fabric with aqueous babul bark extract are: dyeing time-
60 min, dyeing temperature-65 °C, MLR—1:30, pH-at 5,
mordant concentration-15% overall concentration of
harda ? aluminium sulphate in 75:25 ratio, dye concen-
tration—30%,(on weight percentage of dried color source
material) and common salt concentration is 5%, considered
as optimum.
Analysis of Color Differences and Related Color
Interaction Parameters for Application of Babul
Bark Extract Under Different Dyeing Conditions
As said earlier, data in Tables 7, 8, 9, 10, 11, 12, 13 shows
the effects of different process variables on K/S values
along with other color interaction parameters, including
total color difference (DE), change in hue (DH), change in
chroma (DC), general Metamerism index (MI), Brightness
index (BI) and color difference index (CDI) values. The
most important and predominating variables among the
dyeing conditions (time, temperature, pH, MLR, Mordant
concentration, dye concentration, and salt concentration)
varied are identified as salt concentration, dyeing temper-
ature and MLR as indicated by wide dispersion of CDI
values (higher value of differences of CDImaximum and
CDIminimum i.e. the ranges of CDI values are varying from
13.00 to 10.87 (For varying salt concentration it is found as
13.00, for dyeing temp—it is 12.09 and for MLR it is
10.87), while for all other dyeing process variables studied
here, the range of dispersion of CDI is B 9.00. The order of
increasing CDI values therefore appears to be as follows:
Time \ Mordant concentration \ pH \\ Dye concen-
tration \\ MLR \\\ Temperature \\\ Salt Concentra-
tionTherefore, for uniform dyeing of cotton khadi fabric
using babul bark extract, special care are to be taken for
control of Salt concentration, dyeing temperature & MLR.
Indication of the differences in color yield or surface
color strength for varying dyeing condition in each case, as
compared to standard un-dyed pre-mordanted control cot-
ton khadi fabric has been indicated by other color param-
eter data like DE, DL, Da and Db.
The DH value in Tables 7, 8, 9, 10, 11, 12, 13 reveals
that there is minor change in predominating hue as change
in hue in more cases is found to be negative and in very
few cases it is positive. However, the maximum DH value
is observed in case of the variation in salt concentration
from 0–15% which further indicates the high sensitivity of
color yield for this particular natural dye for salt concen-
tration of dyeing. Bark of babul contains a considerable
amount of tannin in the form of gallic acid and the main
coloring component i.e., poly phenolic complex is salt
sensitive for complex formation with mordant and mordant
assistants.
J. Inst. Eng. India Ser. E

Table 14 Colour fastness data against variation of dyeing process variables for dyeing 15% overall concentration of Harda ? Al2(SO4)3 (in
75:25 ratio) pre mordanted khadi cotton fabric subsequently dyed with Babul Bark extract as a natural dye
Dyeing conditions Colour fastness at 50 °C
Washing Light Rubbing Perspiration
Loss of depth Staining Dry Wet Acidic Alkali

Time (min)
15 4 4–5 3–4 4–5 3 4–5 4–5
30 4 4–5 3–4 4–5 3 4–5 4–5
60 4–5 4–5 3–4 4–5 3 4–5 4–5
90 4 4–5 3–4 4–5 3 4–5 4–5
120 3–4 4–5 3–4 4 2–3 4–5 4–5
Temp. (°C)
50 4 4–5 3–4 4–5 3–4 4–5 4–5
65 4 4–5 4 4–5 3–4 4–5 4–5
80 4 4–5 3–4 4–5 3–4 4–5 4–5
95 3–4 4–5 4 4–5 3–4 4–5 4–5
pH
3 3–4 4–5 3–4 4–5 3 4–5 4
5 4 4–5 3–4 4–5 3 4–5 4
7 4 4–5 3 4 3–4 4 4–5
9 3–4 4–5 2–3 4–5 4 4–5 4–5
11 4 4–5 3 4–5 3 4–5 4–5
13 3 4–5 1–2 5 4 4 4
M LR
1:10 4 4–5 3–4 4–5 3–4 4–5 4–5
1:20 4 4–5 3–4 4–5 3–4 4–5 4–5
1:30 4 4–5 3–4 4–5 3–4 4–5 4–5
1:40 4 4–5 3 4–5 3–4 4–5 4–5
1:50 3–4 4–5 3 4–5 3–4 4–5 4–5
Mordant concentration i.e. varying overall total concentration of harda and potash alum applied in sequence in 75:25 ratio with following overall
concentrations
5 4 4–5 3–4 4–5 3–4 4–5 4–5
10 4 4–5 3–4 4 3–4 4–5 4–5
15 4 4–5 3–4 4 3–4 4–5 4–5
20 4–5 4–5 3–4 4 3 4–5 4–5
Dye conc.(%)
10 4–5 4–5 2–3 4–5 3–4 4–5 4–5
20 4 4–5 3 4–5 3–4 4–5 4–5
30 4–5 4–5 3–4 4–5 3–4 4–5 4–5
40 4 4–5 3–4 4–5 3–4 4–5 4–5
50 4 4–5 3–4 4–5 3–4 4–5 4–5
Salt conc. (%)
0 4 4–5 3–4 4–5 3 4–5 4–5
3 4 4–5 3–4 4–5 3 4–5 4–5
5 4–5 4–5 3–4 4–5 3 4–5 4–5
10 4 4–5 3–4 4–5 3 4–5 4–5
15 4 4–5 3–4 4–5 3–4 4–5 4–5

123

Fig. 4 Reaction showing complex formation amongst aluminium sulphate mordanted cotton, polyphenolic dye -Babul and gallic acid present in
Babul bark applied on pre-mordanted cotton
Reflectance value of dye and its orientation along the
fibre axis after fixation is mainly dependant on Brightness
index of dyed products. As reported earlier [6] for other
natural dyes, there is an appreciable reduction in brightness
index also for babul dyed cotton khadi fabric irrespective
of dyeing conditions used. However, it may be noted that at
lower concentration of mordant (10–20%) and lower con-
centration of salt (0–15%), the reduction in brightness
index is lower than that observed in other conditions.
Expectedly, due to disorientation of dye molecules in case
of higher concentration of dye or higher MLR, the reduc-
tion in brightness index is found to be higher.
The metameric effect on the babul bark dyed cotton
khadi fabric for different conditions of dyeing is indicated
by the general metamerism index (MI). A glance at
Tables 7, 8, 9, 10, 11, 12, 13 reveals that the MI varies
from 0.04 to 0.80 in all the cases and data are not much
widely dispersed within a particular condition being varied,
but varies to a noticeable degree from one condition to
other, indicating its potent metameric nature from one
condition to other. Hence, it is recommended to use opti-
mized conditions of dyeing to minimize metamerism.
123
J. Inst. Eng. India Ser. E
FTIR Analysis
FTIR spectra of (a) bleached control cotton (b) mordanted
cotton and (c) mordanted & dyed cotton fabric as shown in
Fig. 5. The spectra shows the following common peaks and
trough (FTIR Peak Position in cm-1) mentioning specific
peak positions and corresponding chemical functional
groups/bonds vibration/stretching etc.:
Control cotton shows common peaks in all the FTIR
curves (a), (b), and (c) at 3351–3402 cm-1 for free OH
stretching, 2902–2919 cm-1 for C–H stretching,
2840–2850 cm -1 for C–H2 stretching (in association with
some –OH bending and stretching), 1744 cm-1 for –C = O
i.e. ketone or carboxylate ester or aldehyde –C(H) = O
group vibration, 1633–1638 cm-1 for Adsorbed
water/moisture, 1430 cm-1 for d(C–H); d(C–OH) primary
& secondary alcohol and also for some d(C–H) stretching,
*1372 cm-1 for d(C–H) stretching, 1337 cm-1 for d(CH2)
wagging, 1317 cm-1 for d(C–H) stretching, 1281 cm-1 for
d(CH2) twisting, 1235 cm-1 for d(C–OH) out-of-plane
bending, 1164 cm-1 for m(C–C) ring breathing, asym-
metric, 1113 cm-1 for (C–O–C) glycosidic vibration,
1059 cm-1 for (C–OH) secondary alcohol stretching,
1031 cm-1 for (C–OH) primary alcohol stretching,
J. Inst. Eng. India Ser. E

Fig. 5 FTIR spectra for

(a) bleached control cotton
fabric, (b) mordanted cotton and
(c) mordanted & dyed cotton
fabric

Table 15 Results of elemental analysis of untreated and treated cotton fabric by atomic absorption spectrophotometry (AAS)
Sample description Metal content (mg/kg)
By microwave digestion followed by ICP-
OES/AAS

Aluminium (Al) Sulphur (s) Zinc (Zn)

Control bleached cotton fabric 62.5 11.6 22.7

Cotton fabric mordanted with 15% (harda ? Al2(SO4)3) (75:25) 2728.0 69.7 41.3
Cotton fabric mordanted with 15% (harda ? Al2(SO4)3) (75:25) and dyed with 30% babul bark 1839.0 19.0 31.2

668 cm-1 and 616 cm-1 for cis distributed alkanes like –
C–H bending.
However, the small difference observed in FTIR peaks
between curve (a) and (b) is that there is small reduction of
peak height and width in (b) i.e. in mordanted cotton than
that of control cotton (a), indicating some form of chemical
interaction/association (expectedly complex formation)
occurring between chebulinic acid residue (from Harda)
and ketone/aldehyde group of Fibre in presence of alu-
minium metal (metallic response peak is not seen in FTIR
curve (b), as FTIR scan is not taken below 450 cm-1).
Moreover, FTIR curve (c) i.e. for mordanted and dyed
(with Babul as natural dye) cotton shows complete absence
of FTIR peak 1744 cm-1 and also absence of small peak at
2850 cm-1, after dyeing, which are probably due to further
complex formation with phenolic hydroxyl group of color

123

component of babul (as natural dye) in association with
both poly hydroxyl group of chebulinic acid of harda and
unsaturated metallic valence of aluminium to form fibre-
mordant-dye - coordinated complex and some hydrogen
bonding also associating –OH group in association with
CH2 stretching of cotton celluloses.
Study of Elemental Analysis by AAS
Further Results of elemental analysis of untreated and
mordanted and dyed (babul) Cotton fabric by Atomic
absorption Spectrophotometry (AAS)—vide data in
Table 15, also confirms presence of much higher amount of
aluminium in both mordanted and dyed fabrics (than that of
the control cotton fabric) confirming complex formation
amongst fibre –aluminium (from aluminium sulphate as
mordant) and babul natural dye powder along with pres-
ence of sulphur to some extent.
Conclusions
The optimized conditions for aqueous extraction of color
component from babul bark powder as natural dye are
Extraction time-45 min, Temperature-60 °C, MLR-1:30
and pH-6.
The observed results indicate that 15% overall concen-
tration of harda and aluminium sulphate in 75:25 ratio
applied in sequence at 65 °C for 60 min is the best and
better color yielding mordanting technique for bleached
cotton khadi fabric dyed with aqueous extract of babul
bark.
The observed optimum conditions of dyeing of the
double pre-mordanted (with overall 15% concentration of
harda and aluminium sulphate in 75:25 ratio in sequence)
for bleached cotton khadi fabric with aqueous extract of
babul bark are as follows:
Dyeing time-60 min, dyeing temperature-65 °C,
MLR—1:30, pH-at 5, mordant concentration—15%., dye
concentration—30% (on weight percentage of dried color
source material) and common salt conc., is 5%, considered
as optimum.
Interpretation from color difference index values clearly
reveals that salt conc., temperature of dye bath and MLR
are the three most critical dyeing process variables amongst
all other parameters of dyeing process variables in this
case.
Both FTIR and AAS study confirms complex formation
with harda and aluminum sulphate in babul dyed cotton
fabric confirming chemical interaction/complex forming
association amongst Fibre—Aluminium and phenolic
hydroxy group of color component of babul bark powder
(as natural dye).
123
J. Inst. Eng. India Ser. E
Acknowledgement Special Thanks are extended to the Ministry of
Micro, Small & Medium Enterprises (Govt. of India) for the relevant
R&D project grant-in-aid for the R & D project on Standardization of
process of dyeing Cotton Khadi with natural dyes. Thanks are also
due to BTRA lab manager for helping in FTIR analysis. Authors are
also thankful to the Director, Mahatma Gandhi Institute for Rural
Industrialization (MGIRI), Wardha for time to time encouragement
and all support to carry out the major part of R&D work at MGIRI,
Wardha–Maharashtra.
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