Environmental Science and Pollution Research (2022) 29:83810–83823

https://doi.org/10.1007/s11356-022-21450-0

RESEARCH ARTICLE

Sustainable eco‑friendly extraction of yellow natural dye from haar

singhar (Nyctanthes arbor‑tritis) for bio coloration of cotton fabric
Muhammad Yameen1 · Shahid Adeel2 · Hunaira Nasreen1 · Fazal‑ur‑Rehman3 · Abdul Ghaffar1 · Tanvir Ahmad4 ·
Asma Inayat5

Received: 4 April 2022 / Accepted: 10 June 2022 / Published online: 30 June 2022
© The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature 2022

Abstract
The revival of natural dyes in different walks of life is due to stringent environmental standards imposed by many associations. For
current studies, flowers of haar singhar (Nyctanthes arbor-tritis) has been chosen for bio-dyeing of cotton fabric using microwave
irradiation techniques. For this purpose, liquid extracts and fabrics were exposed to microwave for 5 min at various conditions.
These treated and un-treated dye extracts obtained in respective media were employed to dye the radiated and non-radiated cotton
fabrics. The characterization of extract and untreated and undyed irradiated fabrics samples was done through FTIR. Different dye-
ing variables were optimized under CCD response surface methodology as a statistical tool. With the introduction of new shades
and improvement of colorfastness properties, different concentrations of sustainable chemical and bio-mordant were employed. All
dyed cotton fabrics were exposed to CIE-color space system for estimation of color coordinates and color strength by using spectra
flash SF600 and to rate colorfastness properties using ISO standard methods for light, dry and wet rubbing, washing fastness. Cotton
fabric was dyed with haar singhar flower extract of 7 pH from 4 g of powder, using 1.5 g/100 mL salt solution at 60 °C for 30 min.
To get acceptable shades, aqueous extract after microwave treatment for 4 min provided excellent color strength. Pistachio (K/S =
3.6342) is a bio-mordant with great results, and aluminum (K/S = 4.8205) is a chemical mordant with outstanding results. It is found
that green methods for isolation of colorant and green mordants for getting new shades should be employed.

Keywords Nyctanthes arbor-tritis · Bio-mordants · Microwave · Cotton fabric · Sustainability

Introduction
Natural dyes are the colorants derived from natural sources
such as animals, plants, minerals, and insects that have the
potential to dye the matrix (Glogar et al. 2020; Adeel et al.
Responsible Editor: Philippe Garrigues
* Shahid Adeel
shahidadeelchemist@gmail.com
1
Department of Biochemistry, Government College
University Faisalabad, Faisalabad 38000, Pakistan
2
Department of Chemistry, Government College University
Faisalabad, Faisalabad 38000, Pakistan
3
Department of Applied Chemistry, Government College
University Faisalabad, Faisalabad 38000, Pakistan
4
Department of Statistics, Government College University
Faisalabad, Faisalabad 38000, Pakistan
5
Applied Chemistry Research Center, PCSIR Laboratories
Complex, Feruzepur Road Lahore, Lahore, Pakistan
2021). In ancient times, natural dyes were used to dye natural
textiles, leather, plastics, and food because these pigments
display excellent hue with soothing luster (Menegazzo et al.
2020). The use of synthetic dyes has increased in the last
century due to industrialization as well as the global trade
(Sharma et al. 2019; Mahdi et al. 2021). They have been
widely utilized in the textile industry because of their tre-
mendous properties such as anti-viral, antioxidants, and anti-
bacterial. These dyes have high stability to light, temperature,
and progression in color covering the whole spectrum of color
(Elsahida et al. 2019; Adeel et al. 2022a). When synthetic
dyes are used to dye fabric, it produce efficient color, but
wastewater has high chemical effluents (Khattab et al. 2020).
These effluents raise the pH of water, which influences the
environment’s balance. The fundamental drawback of syn-
thetic dye is the abundance of volatiles and suspended sol-
ids that when added to water destroy aquatic life (Atav et al.
2020). The discharge that develops from its usage or syn-
thesis not only harms the world’s health but also contributes
to global warming, which disrupts agricultural land, bodies

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Environmental Science and Pollution Research (2022) 29:83810–83823
of water, and human health (Affat 2021). These dyes raise
harmful elements in the environment, such as sulfur, phos-
phorus, nitrogen, and other heavy metals, which boost the
growth of microbial, and carcinogenic products (Yusuf 2019).
These extremely dangerous impacts of synthetic products have
driven people to rush to shift towards green products such as
natural dyes (Singh et al. 2019). Here is a need to replace them
(synthetic dyes) with products that not only promote global
health but also contribute directly or indirectly to environmen-
tal sustainability (Phan et al. 2020). Also, the natural dyeing
as state of the art tool should be revised as an excellent part
of our cultural heritage. Natural dyes are gaining worldwide
recognition for their ability to cover a wide range of colors to
produce vibrant shades (Fröse et al. 2019). These dyes have
a distinct place in textiles all around the world because these
dyes have no disposal issues and do not require specific han-
dling for their isolation and uses (Akhtar et al. 2019). The
limited color strength (K/S) concomitant with natural dyes
has led to the use of modern procedures such as irradiation
techniques in the textile industry to overcome this constraint
(Fierascu et al. 2020).
Researchers are attempting to overcome this disadvan-
tage by utilizing and modifying extraction technologies
that require a lot of energy and time (Bachtler and Bart
2021). Microwave-assisted extraction has more potential
for enhancing functional natural product yields (Ticha et al.
2021). As a high-speed treatment, the radiation sources
cause no alteration in the chemical composition of the cotton
fabric functional site or any physiological properties of the
plant (Chen et al. 2020). This treatment tunnes the fabric’s
surface so that it can effectively absorb the dye molecule
to achieve maximum dyeing rate. When compared to con-
ventional extraction processes, this treatment has shown to
(b)
(a)
CH2OH
C O
H OH
H HO
C C
OH
H
OH H
HC C
H OH
Fig. 1  Cellulosic unit (a), haar singhar flower extract (b), nyctanthin (c)
83811
vastly reduce the requirement for a large volume of solvent,
energy usage, and extraction time (Arain et al. 2021). These
rays are used to isolate natural compounds (colorants) from
plants and are regarded one of the cleanest, most sustainable,
and uniform heating systems available. These radiations dis-
integrate the outer wall of cell by allowing higher yield of
phytochemicals, particularly potentially active isolates (natu-
ral dyes), and by their promising mass transfer kinetics into
solvent better results are obtained (Buyukakinci et al. 2021).
The key advantage of microwave heating is that it reduces
the size of the equipment, waste, time, and cost (Majumder
et al. 2020). So these require metal salts to develop deep and
colorfast shade. But some salts are toxic and need replace-
ment, now plant-derived pigments have been considered
alternatives to their chemical compartments (Chakraborty
et al. 2020).
The present study has been focused on the practical
application of natural dye (nyctanthin) isolated from haar
singhar flower (HSF) for cotton fabric (Fig. 1). Its floral
extract contains a large number of phenolic compounds,
flavonoids, iridous, and carotenoids, where as many bio-
logical activities such as anticancer, anti-leishmania,
anti-inflammatory, anti-allergic, and antiviral (Singh and
sheikh 2020). This is a mythical plant with strong ayurve-
dic therapeutic potential. Its extract is used to cure parasitic
infections, pyrosis, dermal diseases, depression, osteoar-
thritis, and the treatment of sciatica. It imparts yellow
color on fabric such as cotton, wool, and silk. Cotton fab-
ric is soft and absorbent in nature, with terminal hydroxyl
groups (Fig. 1). These groups are used in crosslinking dyes
and finishes, as well as in substitution reactions to altering
cellulose fibers (Mansour and Ben Ali 2021).
(c)
COOCH3
HO
O
OH
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83812 Environmental Science and Pollution Research (2022) 29:83810–83823

Fig. 2  Effect of microwave

radiations on aqueous extraction NRE.NRCF
(a)
of colorant from Nyctanthes 5
arbor-tritis flower (a), effect NRE.RCF
of microwave radiations on 4.5
the basic extraction of color- 4
RE.RCF
ant from Nyctanthes arbor-
tritis flower (b), and effect of 3.5 RE.NRCF
microwave radiations on acidic
3 MAD
extraction of colorant from
Nyctanthes arbor-tritis flower

K/S
2.5
(c)
2
1.5
1
0.5
0
1 2 3 4 5
Microwave radiation time (min.)

NRE.NRCF
2.5 (b)
NRE.RCF

RE.RCF
2
RE.NRCF

1.5 MAD
K/S

0.5

0
1 2 3 4 5
Microwave radiation time (min.)

NRE.NRCF
2.5 (c) NRE.RCF

RE.RCF
2
RE.NRCF

1.5 MAD
K/S

0.5

0
1 2 3 4 5
Microwave radiation time (min.)

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Environmental Science and Pollution Research (2022) 29:83810–83823 83813

Table 1  Optimum color Medium Time (minutes) Sample code K/S L* a* b* c* h

strength of microwave-
irradiated cotton fabrics dyed Aqueous 0 min NRE/NRCF 2.6938 75.37 13.56 59.77 21.53 29.34
with aqueous, basic, and acidic
4.0 min RE/RCF 4.4964 49.45 15.59 65.57 51.78 30.53
extracts of haar singhar flower
Basic 0 min NRE/NRCF 1.02218 76.74 8.82 43.42 19.61 24.81
4.0 min RE/NRCF 2.0507 68.27 7.01 17.54 34.65 33.91
Acidic 0 min NRE/NRCF 1.3052 81.46 8.51 38.98 25.91 23.67
5.0 min RE/NRCF 2.0252 77.66 10.61 33.17 46.40 26.65

Fig. 3  FTIR analysis of irradi-

ated (a), un-irradiated cotton
fabric (b), and Nyctanthes
arbor-tritis flower (c)

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83814 Environmental Science and Pollution Research (2022) 29:83810–83823

Table 2  Optimization parameters of cotton irradiated aqueous extract Nyctanthes arbor-tritis a through response surface methodology (RSM)
Expno. A (pH) B (ml) C (min) D (°C) E (g/100 ml) F (K/s) Expno. A (pH) B (mL) C (min) D (°C) E (g/100 mL) F (K/s)

1 7 55 30 80 1 6.1849 17 9 55 40 70 1.5 4.0438

2 9 55 30 60 1 8.4505 18 7 55 40 70 1.5 8.1239
3 7 35 30 60 1 8.698 19 9 45 40 70 1.5 8.5144
4 9 35 30 80 1 6.0174 20 6 45 40 70 1.5 7.2664
5 7 55 30 60 2 6.8697 21 10 25 40 70 0.5 6.2144
6 9 55 30 80 2 6.1436 22 8 65 20 70 2.5 7.6532
7 7 35 30 80 2 3.363 23 8 45 60 70 1.5 5.1290
8 9 35 30 60 2 5.973 24 8 45 40 70 1.5 5.4738
9 7 55 50 60 1 6.2575 25 8 45 40 50 1.5 6.1204
10 9 55 50 80 1 5.9734 26 8 45 40 90 1.5 5.7402
11 7 35 50 80 1 6.2753 27 8 45 40 70 1.5 5.7689
12 9 35 50 60 1 3.7721 28 8 45 40 70 1.5 6.1806
13 7 55 50 80 2 3.8534 29 8 45 40 70 1.5 5.6872
14 9 55 50 60 2 6.2122 30 8 45 40 70 1.5 6.7061
15 7 35 50 80 2 6.6268 31 8 45 40 70 1.5 5.7032
16 9 35 50 70 2 6.3523 32 8 45 40 70 1.5 5.4960

A (pH), B (volume), C (time), D (temperature), E (salt), F (color strength)

There have been no comprehensive investigations on the Materials and methods

use of haar singhar for cotton dyeing too far. For the first
time, our researchers have investigated the use of microwave
radiations for the isolation of colorant from haar singhar and
medicinal-based bio-mordants to get colorfast shades and
to improve the colorfastness. Our researchers have aimed:
• To observe the effect of microwave irradiation on the
extraction of colorant for cotton dyeing.
• To observe a physiochemical change in irradiated and
un-radiated cellulosic fabric through FTIR and SEM.
• To find the effect of various chemical and bio mordants
on the dyeing attributes of cotton.
• To evaluate bio mordanted dyed cotton fabric’s colorfast-
ness and color strength.
Collection of material
Haar singhar flowers (HSF) were purchased from a nearby
market and washed thoroughly with distilled water and
dried in the shade. By finely grinding the dried flowers and
putting them through a 20 mesh filter (sieve), a uniform
particle size powder was obtained. Mill mercerized cotton
fabric was bought from the local textile market in Faisal-
abad, Punjab, Pakistan. All of the chemicals employed in
the extraction, dyeing process, including sodium hydrox-
ide (NaOH), concentrated hydrochloric acid (HCl), sodium
chloride (NaCl), and mordants such as salts of aluminum
­(Al2(SO4)3), iron ­(FeSO4), and sodium-potassium tartrate

Fig. 4  SEM analysis of un-

irradiated cotton fabric (a) and
SEM analysis of irradiated cot-
ton fabric (b) (RC = 4 min)

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Environmental Science and Pollution Research (2022) 29:83810–83823 83815

­(KNaC4H4O6·4H2O), used were of Pakistan made. Pistachio
shell (Pistacia vera), walnut shell (Juglans regia), and pine
nutshell (Pinus gerardiana) were also acquired from the
native market for bio-mordanting.
Extraction of colorant and radiation process
acidic. The extract and fabric irradiated for 1, 2, 3, 4, and 5 min,
using high power of microwave oven and were used to color
radiated and un-radiated fabric. The microwave radiated (RE)
and non-radiated (NRE) extracts were used to dye the micro-
wave radiated (RCF) and non-radiated cotton (NRCF) fabrics
for an hour at 80 °C, keeping the solid to extract ratio at 1:25.

The extraction experiments were conducted by heating 4 g of Optimization of dyeing and mordanting parameters
haar singhar flower powder (HSFP) with 100 mL of selected
media for 45 min. To extract the colorant from haar singhar Central composite design under response surface method-
flower (HSF), three media were used: aqueous, alkaline, and ology (RSM) has been used as a statistical tool to optimize

Fig. 5  Effect of pre chemical

mordants (a) and post chemi-
cal mordants (b) on the color 6 (a) Fe Al SPT
strength value of Nyctanthes
arbor-tritis flowers dyed on
cotton fabric 5

4
K/S

0
0.5 1 1.5 2 2.5
Pre chemical mordant conc.(g/100ml)

(b)
6 Fe Al SPT

4
K/S

0
0.5 1 1.5 2 2.5
Post chemical mordant conc.(g/100ml)

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83816 Environmental Science and Pollution Research (2022) 29:83810–83823

Fig. 6  Effect of pre-biomor-

dants (a) and post-biomordants
(b) on the color strength value
(a)
Walnut Pistachio Pine nut
of Nyctanthes arbor-tritis flow- 4
ers dyed on cotton fabric
3.5

2.5

K/S
2

1.5

0.5

0
0.5 1 1.5 2 2.5
Pre bio mordant conc.(g/100ml)

Walnut Pistachio Pine nut

4
(b)
3.5

2.5
K/S

1.5

0.5

0
0.5 1 1.5 2 2.5
Post bio mordant conc.(g/100ml)

dyeing variables such as time, pH, temperature, volume, and
salt amount. The selected extract was used to color irradiated
fabric at 50, 60, 70, 80, and 90 °C for 20, 30, 40, 50, and 60
min. The selected extracts of 6, 7, 8, 9, and 10 pH, 0.5, 1,
1.5, 2, and 2.5 g/100 mL of salts (NaCl) were also applied
to dye cotton through a series of 32 experiments.
­ e+2 i.e ­FeSO4, as well as bio-mordants such as walnut
salt of F
(Juglans regia), pistachio (Pistacia vera), and pine nut (Pinus
gerardiana) were used at optimum conditions to improve color
strength (K/S) and colorfastness properties. To extract bio-mor-
dants, the dry powders of these plants were boiled for 1 h with
distilled water at a solid to liquid ratio of 1:25.

Process of enhancing the shade Evaluation of characteristics of dyed and un‑dyed

Different chemical and bio-mordants were used to improve
the colors as well as to make the process more environmental
friendly. For pre- and post-mordanting, chemical mordants such
­ l+3 i.e., ­Al2 ­(SO4)3, SPT ­(KNaC4H4O6·4H2O), and
as salts of A
fabrics
ANOVA as statistical model was used to determine the effect
of microwave radiations and extract on cotton fabric. The FTIR
analysis of untreated and microwave-treated cotton fabric for 4

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Environmental Science and Pollution Research (2022) 29:83810–83823 83817

Fig. 7  Supposed interaction

of cotton fabric with color-
ant (nyctanthin) and chemical Chemical mordants
mordants

Al, Fe & SPT Mordant

OH interaction
OH
OH OH OH OH

Cotton fabric CM

CM
OH OH

Mordanted cotton fabric

Nyctanthin
(colorant)

min was used to examine for any changes in the functional peak
of the hydroxyl linkage using Perkin Elmer-based fourier trans-
formed infrared spectrometer (USA), where physical analysis
of fabric was done using scanning electron microscope (SEM-
model Tescan; 5 kV). The color strength (K//S), L*, a*, and b*
values of all dyed fabrics were investigated by spectra flash SF
600 at the Department of chemistry Govt. college university
Faisalabad, Punjab, Pakistan.
Results and discussion
Plant-based colorants are a good source for the textile
industry (Anand et al. 2018; Habib et al. 2021). Flowers of
haar singhar are a good source of primary and secondary
metabolites. Secondary metabolites act as a coloring agent.
Microwave treatment is well-known as a sustainable heat-
ing method for the extraction of useful components (color-
ants) from plants. Because of the high treatment speed, low
solvent depletion, and good solvent interaction with plant
material through mass transfer kinetics, microwave treatment
is extensively used (Sundhu et al. 2021). In this study, our
researcher has found that microwave irradiation to aqueous
extract of haar singhar flower (HSF) for 4 min has provided
the most efficient color strength (K/S = 4.4964) on irradiated
cotton fabric, as shown in (Fig. 2a). When the medium was
changed (Fig. 2b), it was discovered that basic extract after 4
min of microwaves has produced good color strength (K/S =
2.0507). When compared to an aqueous medium, the results
achieved under alkaline conditions were not so good. This

Fig. 8  Supposed interaction

of cotton fabric with colorant
(nyctanthin) and bio-mordants
Biomordants
Walnut, Pistachio,
& Pine nut Mordant
OH interaction
OH
OH OH H2O OH

Cotton fabric BM
BM

HO OH

Mordanted cotton fabric

Nyctanthin
(colorant)

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83818 Environmental Science and Pollution Research (2022) 29:83810–83823

Table 3  Statistical analysis of Term Effect Coef SE Coef T-value P-value VIF
dyeing parameter using central
composite design/RSM Constant 5.7008 0.0857 66.48 0.000
pH −1.444 −0.722 0.100 −7.22 0.000 1.18
Volume −0.229 −0.115 0.115 −0.99 0.344 1.29
Time −0.714 −0.357 0.106 −3.35 0.007 1.10
Temperature −3.937 −1.968 0.130 −15.16 0.000 1.57
Salt −0.530 −0.265 0.115 −2.30 0.044 1.29
pH*pH 4.461 2.231 0.179 12.49 0.000 1.04
Volume*volume 3.241 1.621 0.299 5.42 0.000 1.89
Temperature*temperature −2.988 −1.494 0.249 −6.00 0.000 1.34
pH*volume 6.700 3.350 0.254 13.17 0.000 1.27
pH*time −4.554 −2.277 0.254 −8.96 0.000 1.27
pH*temperature 6.403 3.202 0.276 11.61 0.000 1.37
Volume*time −4.138 −2.069 0.235 −8.79 0.000 1.09
Volume*temperature 2.294 1.147 0.268 4.27 0.002 1.32
Volume*salt −2.809 −1.404 0.214 −6.55 0.000 1.77
Time*salt 5.858 2.929 0.235 12.44 0.000 1.09
Temperature*salt −5.201 −2.601 0.268 −9.69 0.000 1.32

is because the side chain of cotton fabric is not easily acces-
sible for covalent bonding with a reactive group of the color-
ant in an alkaline solution. However, when using an acidic
medium (K/S = 2.0252), less color is imparted (Fig. 2c). The
color coordinates show that before irradiation in aqueous
medium, the shades are brighter (L* = 75.37) and reddish
yellow (a* = 13.56, b* = 59.77) in hue having good satura-
tion in color. Upon irradiation for 4 min aqueous medium,
the shade became darker (L* = 49.45), more reddish yellow
(a* = 15.59, b* = 65.57) with excellent saturation (Table 1).

Table 4  ANOVA: K/S versus Source DF ADJ SS ADJ MS F-value P-value

pH, volume, time, temperature,
and salt second-order Model 16 40.1185 2.5074 49.19 0.000
polynomial regression
5
pH 1 14.4188 2.8838 56.57 0.000
Volume 1 2.6550 2.6550 52.08 0.344
Time 1 0.0504 0.0504 0.99 0.000
Temperature 1 0.5736 0.5736 11.25 0.007
Salt 1 0.2705 0.2705 5.31 0.044
Square 3 11.7155 11.7155 229.81 0.000
pH*pH 1 7.9483 7.9483 155.91 0.000
Volume*volume 1 1.4959 1.4959 29.34 0.000
Temperature*temperature 1 1.8380 1.8380 36.06 0.000
2-way interaction 8 22.2760 2.7845 54.62 0.000
pH*volume 1 8.8477 8.8477 173.56 0.000
pH*time 1 4.0886 4.0886 80.20 0.000
pH*temperature 1 6.8703 6.8703 134.77 0.000
Volume*time 1 3.9381 3.9381 77.25 0.000
Volume*temperature 1 0.9306 0.9306 18.25 0.002
Volume*salt 1 2.1869 2.1869 42.90 0.000
Time*salt 1 7.8931 7.8931 154.83 0.000
Temperature*salt 1 4.7855 4.7855 93.87 0.000
Error 10 0.5098 0.0510 0.000
Lack-of-fit 5 0.1831 0.0366 0.56 0.000
Pure error 5 0.3267 0.0653 0.000
Total 26 40.6283 0.000

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Environmental Science and Pollution Research (2022) 29:83810–83823 83819

Table 5  Color coordinated of Mordanted cotton fabric Conc (g/100 ml) K/S L* a* b* c* h*
selected mordanted fabrics
Without mordant (0.0 g/100 mL 2.6938 75.37 13.56 59.77 21.53 29.34
Fe (1.5 g/100 mL (chemical pre) 3.7343 73.65 8.71 35.72 39.51 38.43
Fe (chemical post) 4.5304 71.36 3.23 58.28 43.87 42.78
Al (2 g/100 mL (chemical pre) 3.1526 75.82 3.16 54.74 32.45 31.79
Al (1.5 g/100 mL (chemical post) 4.8205 62.88 9.19 42.64 47.21 47.11
SPT (2 g/100 mL (chemical pre) 4.7318 77.59 0.21 47.16 46.61 45.81
SPT (2 g/100 mL (chemical post) 3.6159 86.77 0.91 11.98 34.91 33.88
Walnut (1.5 g/100 mL (bio pre) 3.1782 68.91 0.96 39.78 29.53 28.34
Walnut (1 g/100 mL (bio post) 1.6567 81.72 2.31 32.72 16.18 15.65
Pistachio (1.5 g/100 mL (bio pre) 3.7172 74.64 2.89 58.78 35.61 35.11
Pistachio (1 g/100 mL (bio post) 3.6342 81.58 2.63 22.57 34.65 33.91
Pine nut (1.5 g/100 mL (bio pre) 2.3319 73.21 4.55 39.24 22.63 21.83
Pine nut (2 g/100 mL (bio post) 2.7042 73.26 3.10 46.40 26.65 25.92

Before irradiation in basic medium, the shades are brighter
(L* = 76.74) and less reddish yellow (a* = 8.82, b* =
43.42) in shade. Upon irradiation for 4 min basic medium,
the shade became brighter (L* = 68.27), less reddish yellow
(a* = 7.01, b* = 17.54) with excellent saturation (Table 1).
Shades produced through an un-irradiated acidic extract on
to un-irradiated cotton fabric are brighter (L* = 81.46) and
less reddish yellow (a* = 8.51, b* = 38.98) in shade. Upon
irradiation for 5 min in acidic medium, the shade became
brighter (L* = 77.66), less reddish yellow (a* = 10.61, b*
= 33.17) with excellent saturation (Table 1).
Results in Fig. 3a and b show that following MW treatment
for up to 4 min, the characteristic peak of hydrogen bonding in
the cellulose unit of cotton fabric does not alter. FTIR spectral
images obtained from irradiated and un-irradiated cotton fab-
ric show that the -OH peak 3300 ­cm−1, CH 1200 ­cm−1 peak,
and C=O peak 1075 ­cm−1 were unchanged by microwave
treatment for up to 4 min. The presence of a characteristic
peak of hydroxyl linkage in cellulosic fabric indicates that
these rays have not altered their chemical composition, which
is highly beneficial in the textile processing industry.
The presences of distinct functional groups were
found by FTIR analysis of haar singhar flowers (Fig. 3c).
Bonded hydroxyl groups (–OH) or amine groups (–NH)
are indicated by the broad and strong bands at 3395–2950
­c m −1. Spectral peak displayed at 1330 ­c m −1 is compat-
ible with aliphatic CH stretching, and peak at 1005 c­ m−1
is most likely caused by an asymmetric and symmetric
stretch of the CO group. As a result, FTIR peaks reveal
the presence of nyctanthin, indicating that it is the col-
orant that is present in the floral extract of haar singhar
flower (HSF). The surface tunning of cotton fabric after
MW treatment upto 4 min shows that these rays have
enhanced the fiber uptake ability by peeling or scratch-
ing. The circled presented in SEM images (Fig. 4a
and b) show the peeled surface which reveal that the
cellulosic surface substantive behavior might have been
increased which was observed in terms of excellent color
strength. Previously, the work done by our researchers as
well as othothers have explained that fact (Akram et al.
2022).
Effect of powder and pH
Use of powder (haar singhar) below the optimum levels pro-
duces less color, and its use above the optimum levels may
incorporate other plant compounds during the process of
extraction, resulting in low color strength, the quantity of pow-
der determines the extent of extraction of colorant in terms of
shade production and color strength (Adeel et al. 2022b; Pun-
yachareonnon et al. 2021). Results in Table. 2 show that 4 g of
powder used for colorant extraction in 100 mL of the aqueous
medium of 4 min of microwave treatment gave outstanding color
strength onto irradiated cotton fabric. To absorb the colorant
more efficiently, the fabric must be dyed in an aqueous dye bath.
This is because hydroxyl linkage is a primary functional site of
cotton fabric that reacts with a colorant (nyctanthin) hydroxyl
group to give good shade. Aqueous extract of 35 mL volume
with a pH of 7 was found to have outstanding color strength on
irradiated cotton fabric (Table. 2).
Effect of time and temperature
To achieve firm colors, it is essential to optimize various
dyeing conditions. The impact of different time durations
(20–90 min) on the absorption of colorant molecules onto
fabric was demonstrated, and the fabric was dyed to provide
a greater color strength value. Dyeing for a shorter period
did not provide the colorant molecule with good sorption,
whereas colorant desorption or hydrolytic breakdown may
also be favored by high heating (>60 °C) due to which low
actual yield is found. At 60 °C, not only excellent dyeing is

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83820 Environmental Science and Pollution Research (2022) 29:83810–83823

Table 6  Fastness ratings of Mordanted fabric LF WF RF Dyed Mordanted Fabrics

dyed fabrics before and after Conc.(g/100ml) DRF WRF
mordanting. LF (light fastness),
Without mordant 4 ¾ 4 ¾
WF (wash fastness), DRF (dry
rubbing fastness), WRF (wet (0.0g/100ml)
rubbing fastness)

Fe (1.5g/100 mL) ( 5 4 5 4/5

Chemical Pre)

Fe (1.5g/100 mL) 5 4/5 5 4/5

(Chemical Post)

Al(2/100 mL) 5 4/5 5 4/5

(Chemical Pre)

Al (1.5/g100 mL) 5 4/5 5 4/5

(Chemical post)

SPT (2g/100 mL) 5 4/5 5 4/5

(Chemical pre)

SPT (2g/100 mL) 5 4/5 5 4/5

(Chemical post)

Walnut (1.5g/100 5 4/5 5 4/5

mL) ( bio pre)

Walnut (1g/100 mL) 5 4/5 5 4/5

( bio post)

Pistachio(1.5g/100 5 4/5 5 4/5

mL) ( bio pre )

Pistachio (1g/100 5 4/5 5 4/5

mL) ( bio Post)

Pine nut (1.5g/100 5 4/5 5 4/5

mL) ( bio Pre )

Pine nut(2g/100 mL) 5 4/5 5 4/5

( bio Post)

13
Environmental Science and Pollution Research (2022) 29:83810–83823
achieved but also it has enhanced color strength (Table 2).
The irradiated cotton fabric should be dyed at 60 °C using
irradiated aqueous extract of haar singhar flower for having
excellent color strength.
Effect of salt and volume of extract
Salt, as an exhausting agent, produces outstanding coloring
results in natural cotton dyeing. Salt aids in permeating the
colorant in close proximity to the fabric, allowing for bond-
ing through short attractive forces (Akhtar et al. 2018). A low
amount of electrolyte does not affect the ability of colorant to
approach the cotton fabric, whereas a large amount of salt can
result in overexertion and unevenness. Results in Table 2 indi-
cates that 1 g/100 ml of NaCl produced a high color strength
(K/S) through maximum exhaustion. Excellent color strength
was obtained by 35 ml of extract derived from 4 g of haar sin-
ghar flower powder (HSFP) in 100 ml of solvent. The volume
of extract used in the extraction of colorant from haar singhar
played crucial role (Table 2). A small amount of extract is inef-
fective, whereas a large amount of molecules forms clusters on
fabric, which, rather than sorption, stay on the surface of the
fabric, causing uneven dyeing. The statistical analysis give in
Table 3 show the significance of using salt.
ANOVA narrated results presented in Table 4 have five
quadratic effects such as pH, time, temperature, and salt
that are highly significant (P = 0.000), and volume is insig-
nificant. ANOVA two-way interaction showed that pH with
volume, time, and temperature and salt with time and tem-
perature are highly significant (P = 0.000).
Mordanting is a well-known technique for overcoming the
fastness issues of natural dyes. Salts of Al, Fe, Cu, Cr, etc., are
used but some salts such as Cu, Co, Ni, etc. are carcinogenic.
As an alternative, plant-based extracts have been employed. In
this study, sustainable chemical anchors (Fe, Al, and sodium
potassium tartrate) have been employed. The results given in
Fig. 5(a and b) show that 1.5 g/100 mL of Fe, 2 g/100 mL of
Al, and sodium potassium tartrate as pre-chemical, whereas
1.5 g/100 mL of walnut shell, pistachio shell, and pine nut
shell extracts as pre biomordants gave outstanding results on
to cotton fabric (Table 5). Application of post mordanting
(Fig. 6a and b) has given excellent results with 1.5 g/100 mL
of Fe, 1.5 g/100 mL of Al, and 2 g/100 mL of SPT as chemi-
cal, 1 g/100 mL of walnut shell, 1 g/100 mL of pistachio shell,
and 2 g/100 mL of pine nut shell. These high fastness ratings
are based on the production of stable colors, either by chemi-
cal mordants in the case of metal dye complexes or by the bio
mordanting process in the case of additional hydrogen bond-
ing (Gong et al. 2020). Experimentation demonstrated that
Pistachio shell as a natural biomordant and Al as a chemical
mordant were greatly substantial in achieving a deeper color
onto the colored fabric by developing strong bonds with cot-
ton fabric and colorant, resulting in a more sustainable and
83821
environmentally friendly approach. Biomordanting is cost-
effective in terms of excellent yield. Results showed that the
colors produced by varying chemical and bio mordant con-
centrations are brighter and yellowish in tone. Pre- and post-
mordanted samples that were optimized exhibited good rating
fastness. Colorfastness qualities of pre- and post-biomordanted
samples demonstrated that these sustainable mordants yielded
firm colors (Table 5).
The development of a metal-dye complex onto cot-
ton fabric gives the fabric high color strength and an
enhanced fastness rating. A low amount will not form a
stable complex, whereas high amount of the above-men-
tioned mordant will form a complex and sorb onto fabric
as aggregates. The overloaded complex is torn away dur-
ing washing, resulting in a low color strength and a low
fastness rating. The colorant functional site (-OH linkage)
reacts with the hydroxyl linkage of the cellulosic fabric
(Fig. 7) and the hydroxyl linkage of the bio-mordant to
produce fixed colors through extra hydrogen bonding (Fig.
8) when utilizing bio-mordants (Sadeghi-Kiakhani et al.
2020). The bio-mordanted colored fabrics exhibit high
resistance to fade after rubbing, light exposure and wash-
ing (Rehman et al. 2021). Results in Table 6 shows that
after being tested according to ISO standards, bio- and
chemical-mordanted dyed cotton fabrics were found good
to outstanding in ratings at grey scale of fastness. It has
resulted that the coloring of cotton fabric with natural col-
orant haar singhar is appealing, colorfast, and environment
friendly (Table 6).
Conclusions
Ecofriendly isolation techniques such as microwave radia-
tions have subjected the universe of green products for
the global community because of their peculiar mode of
action, which uses less time, solvent, energy, and cost.
The results reveal that nyctanthin isolated from the haar
singhar flower and microwave irradiated for 4 min pro-
vided good natural yellow coloring effects on radiated
cotton fabric. Improved tint firmness and new colors with
exceptional fastness capabilities have emerged from the
employment of sustainable bio and chemical mordants.
As a result, microwave radiations can be used to acceler-
ate the extraction of natural colorants from plants to dye
fabric, accompanied by a contamination-free mordanting
technique to produce new, colorfast shades.
Author contribution Dr. Muhammad Yameen has supervised where
Dr. Shahid Adeel has co-supervised the work of M.Phil studies. Ms.
Hunairara Nasreen has performed experiments and Ms. Nimra amin,
Ms. Asma Inayat has analyzed fabrics through FTIR and SEM tech-
niques. Dr. Fazal-ur-Rehman and Dr. Abdul Ghaffar have technically
13
83822
and scientifically guided the work for smooth running of experiments.
The significance of the method utilized in this study was statistically
analyzed by Dr. Tanvir Ahmad.
Funding This work has not been funded by any agency.
Data availability The whole data is present in M.Phil. thesis.
Declarations
Ethics approval We approve that this manuscript is part of M.Phil
studies.
Consent to participate and publish We give consent to publish our
work of M.Phil studies and is jointly contributed by all authors.
Competing interests The authors declare no competing interests.
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