Article

Clothing and Textiles

Research Journal

Colorimetric Study on 2014, Vol. 32(2) 124-135

The Author(s) 2014
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DOI: 10.1177/0887302X14525658
Weld and Pomegranate ctr.sagepub.com

Peel Natural Dyes

Ali Shams-Nateri1,2, Abbas Hajipour1,

Ehsan Dehnavi1, and Ehsan Ekrami3

Abstract
In this research, yellow color on nylon was produced by dyeing with weld (Reseda luteola) and
pomegranate peel as natural dyes. The aluminum potassium sulphate salt was used as mordanting agent
and four different methods of dyeing as non-mordanting, pre-mordanting, meta-mordanting, and after-
mordanting were applied. The dyeing behavior of dyes was assessed by colorimetric evaluations and
fastness properties. The spectrophotometric properties of dyed samples were also studied by
Principal Component Analysis (PCA). Based on colorimetric evaluations, weld in comparison with
pomegranate peel resulted in lighter and yellower colors. The rubbing fastness in all dyed samples was
excellent, while samples dyed with pomegranate peel showed better washing fastness properties. Also,
the best light fastness was obtained by the after-mordanting dyeing method. Overall, the best results of
fastness properties were obtained by using after-mordanting method.

Keywords
natural dyes, nylon, weld, pomegranate peel

Natural dyes have many advantages, such as low toxicity and allergic reactions, in addition to bio-
degradability, because they are taken from animal or plant matter without chemical processing.
However, the use of natural dyes declined to a great extent with the advent of synthetic dyes, which
have moderate-to-excellent color fastness properties, in 1865. During the decade of the 1990s, the
textile and apparel industries, particularly the coloration industry, have been widely criticized for
their role in polluting the environment. For these reasons, the use of carcinogenic dyes has been
restricted, and the use of natural dyes has increased (Bechtold & Mussak, 2009; Bechtold, Turcanu,
Ganglberger, & Geissler, 2003; Derksen et al., 2003; Farizadeh, Montazer, Yazdanshenas, Rashidi,

1
Textile Engineering Department, University of Guilan, Rasht, Iran
2
Center of Excellence for Color Science and Technology, Tehran, Iran
3
Textile Engineering Department, Amirkabir University of Technology, Tehran, Iran

Corresponding Author:
Ali Shams-Nateri, Textile engineering department, Faculty of engineering, University of Guilan, Rasht, Guilan, Iran.
Email: a_shams@guilan.ac.ir
Shams-Nateri et al. 125

Figure 1. Chemical structure of dyeing material in pomegranate peel (A) granatonine and (B) tannin (Bechtold
& Mussak, 2009; Keheyan & Giulianelli, 2006).

Figure 2. Reseda Luteola structure (Cristea et al., 2003).

& Malek, 2009; Gaspar, Moiteiro, Turkman, Coutinho, & Carnide, 2009; Ghoranneviss et al., 2011;
Ghouila, Meksi, Haddar, Mhenni, & Jannet, 2012; Lokhande & Dorugade, 1999; Nagia &
EL-Mohamedy, 2007; Sarkar & Seal, 2003).
The rapid changes in trends, fashion, and the demand for good fastness properties on different
substrates require a basic database describing possible applications of natural dyes; otherwise, too
much parallel optimization work has to be done by each dyehouse (Bechtold & Mussak, 2009; Haar,
Schrader, & Gatewood, 2013).
Pomegranate peel (Punica granatum, Pooste Anar in Persian) is a representative source for plant-
based yellow dyes. P. granatum is from the family Punicacea, which grows in Iran, India, Mediter-
ranean countries, and all warm countries of the world; it was originally been a native of Persia. The
main coloring agent in the pomegranate peel is granatonine (Figure 1), which presents in the alkaloid
form of N-methyl granatonine (C9H15NO; Bechtold & Mussak, 2009; Keheyan & Giulianelli, 2006;
Legua et al., 2012; Viuda-Martos, Fernandez-Lopez, & Perez-Alvarez, 2010). There is also a con-
siderable amount of tannin, about 19%, in the pomegranate peel (Figure 1).
Weld (Reseda luteola [Figure 2], Sparak in Persian), which grows widely around the world
(Europe, Western Asia, and North America) is another representative source for plant-based yel-
low dyes. It is a perennial plant that produces a yellow dye (luteolin) from its foliage and flowers
(Bechtold & Mussak, 2009; Cristea, Bareau, & Vilarem, 2003; Cristea & Vilarem, 2006; Gaspar
et al., 2009). Weld, luteolin, and its sugar derivatives are considered to produce the most stable
yellow shades and thus have been widely used for dyeing. The chemical structure of R. luteola
is given in Figure 2.
Nylon is a polyamide that is mostly manufactured through condensation polymerization of dia-
mine and diacid. Generally, nylon is dyed with acid dyes as well as reactive and disperse dyes (Baig,
2010; Broadbent, 2001). Some researchers have studied dyeing nylon with natural dyes such as
indigo, onion, lac, turmeric, kamala, and henna (Agrawal, 2012; Badri & Burkinshaw, 1993; Baig,
2010; Lokhande & Dorugade, 1999).
126 Clothing and Textiles Research Journal 32(2)

The literature survey indicates that there have been relatively few works investigating the dyeing of
nylon with weld and pomegranate peel. It has been previously shown that principal component anal-
ysis (PCA) technique can be used to study the colorimetric properties of colors in textile dyeing. PCA
is a useful statistical technique for finding patterns in data and expressing the data without much loss of
information. It does so in such a way as to highlight the similarities and differences in the data. The
other main advantage of PCA is that once patterns in the data, and we compress the data. Weld and
pomegranate are important natural sources for producing yellow shades on the textile samples. In addi-
tion, there have been relatively few research works on the dyeing of nylon with these yellow-coloring
natural dyes. On the other hand, in order to demonstrate the merits of the PCA technique for explana-
tion and comparison of the colorimetric properties of natural dyes, we selected natural dyes, weld and
pomegranate, with relatively similar shades and spectral shapes. In this research, the natural yellow
color on the nylon fabrics was obtained with pomegranate peel and weld dyes by using different meth-
ods of dyeing as non-mordanting, pre-mordanting, meta-mordanting, and after-mordanting. The dye-
ing behavior and colorimetric and fastness properties of dyed samples were extensively investigated.
The conventional methods of colorimetric evaluation and comparison in textile dyeing involve study-
ing the spectrophotometric data (i.e., reflectance spectra), K-M spectra, and color values. In the present
work, PCA was also carried out to provide sufficient information about the spectrophotometric and
colorimetric properties of dyed samples. The applicability of the PCA method and advantages of the
technique over the conventional methods have been reported in the literature.

Experimental Procedure
Material
Scoured nylon fabric (plain weave and medium weight) was purchased commercially. Weld (R. luteola)
flowers and pomegranate peels were obtained from Yazd province, Iran. Aluminum potassium
sulfate (KAl (SO4)2.12H2O) and acetic acid were purchased from Merck.

Method
Dye extraction. First, fine dried powders of natural dyes were wetted for 24 hr and then boiled for 1 hr.
The extracts were cooled and filtered, and subsequently the filtrate dye solutions were used for dye-
ing the nylon samples.

Dyeing. Four different methods were used for dyeing of nylon samples: (1) non-mordanting: The dye-
ing process was started at room temperature, and the temperature was raised to boil over 30 min;
dyeing continued at boil for 1 hr with a liquor-good ratio of 40:1. Finally, the dyed samples were
rinsed with tap water and dried at room temperature. (2) Pre-mordanting method: The samples were
first mordanted by treating them with aluminum potassium sulfate salt at boiling temperature for 45
min in a bath with the liquor-good ratio of 40:1. The concentration of mordant was 5% on the weight
of the sample, and the pH was adjusted at 5 using acetic acid. The fabrics were then rinsed with tap
water and dried at room temperature. Subsequently, the mordanted nylon samples were dyed with
solutions of natural dyes. The dyeing process was done similar to the non-mordanting method, and
the dyed samples were then washed with tap water and dried at room temperature. (3) Meta-
mordanting method: The mordant and dye were added to the dyeing bath simultaneously. Subse-
quently, the dyeing process was carried out by raising the temperature to boil and continued for 1
hr. After the dyeing, the samples were washed with tap water and dried. (4) After-mordanting
method: in this method, the samples were first dyed with weld or pomegranate dye, similar to the
non-mordanting method. The samples dyed were rinsed and dried and then the after-
mordantation process was carried out with mordants at boil for 45 min. At the end of the mordanting
Shams-Nateri et al. 127

Figure 3. The reflectance spectra of nylon dyed with different dyeing methods: (A) non-mordanting, (B) pre-
mordanting, (C) meta-mordanting, and (D) after-mordanting.

period, the mordant bath solution was removed and the rinsing procedure started. Finally, the sam-
ples were dried at room temperature.

Color measurements. The reflectance spectra of the dyed samples were measured using a Gretage
Macbeth Color Eye 7000A spectrophotometer within

the visible spectrum at 39 wavelengths with
10 nm interval from 380 nm to 760 nm. The KS values were determined using the KubelkaMunk
equation. (Equation 1; Lee, 2005)
 
K 1  Rl 2
; 1
S l 2  Rl
where K and S are the absorption and scattering coefficients, respectively, and R is the reflectance
spectra of dyed fabric at lmax.
CIELab coordinates (Kuehni, 2005; Lee, 2005; Schanda, 2007; Shams-Nateri, 2008; L*, a*, b*,
C*, h, where, L* describes lightness, a* represents redness-greenness, b* represents yellowness-
blueness, C* is the saturation, and h is the hue angle) were measured under 10 degrees standard
observer and D65 standard illuminant.

PCA. The PCA is the basis of a new statistical method used in data analyses and compression. It is a
simple, nonparametric method of extracting relevant information from confused data sets. PCA is a
quantitatively accurate method for achieving simplification. The method generates a new set of vari-
ables, called principal components, which are linear combinations of original variables. The first
128 Clothing and Textiles Research Journal 32(2)

Figure 4. The unit (K/S) of nylon dyed with different dyeing methods: (A) non-mordanting, (B) pre-mordanting,
(C) meta-mordanting, and (D) after-mordanting.

principal component is a single axis in space. When each observation has been projected on that axis,
the resulting value from a new variable and the variance of this variable is the maximum among all
possible choices of the first axis. The second principal component is another axis in space, perpen-
dicular to the first. Projecting the observations on this axis generates another new variable. The var-
iance of this variable is the maximum among all possible choices of this second axis. The full set of
principal components is as large as the original set of variables, but it is commonplace for the sum of
the variances of the first few principal components to exceed 80% of the total variance of the original
data. The first principal component accounts for as much of the variability in the data as possible,
and each subsequent component accounts for as much of the remaining variability as possible. By
grading the Eigen vectors for descending Eigenvalues so that the largest is first, an ordered ortho-
gonal method can be created with the first Eigen vector having the direction of largest variance of the
data. In this way, directions in which the data set has the most significant amounts of energy and
variation can be found (Mohtasham, Shams-Nateri, & Khalili, 2012; Shams-Nateri, 2011; Smith,
2002; Westland & Ripamonti, 2004).

Fastness properties. The dyed samples were tested according to International Organization for Standar-
dization standard methods. The washing- and rubbing-fastness properties of the dyed samples were
measured according to ISO 105-C02 (1989) and ISO 105-X12 (1987), respectively, and the changes
in the color were assessed by the gray scale. The light fastness properties of the samples were measured
according to ISO 105-B02 (1988), and the changes in the color were assessed by the blue scale.
Shams-Nateri et al. 129

Figure 5. The lightness of nylon dyed with different dyeing methods: (A) non-mordanting, (B) pre-mordanting,
(C) meta-mordanting, and (D) after-mordanting.

Result and Discussion

Reflectance Spectra
The reflectance spectra of the nylon dyed with 50% of weld and pomegranate peel are shown in
Figure 3. From this figure, it can be seen that the shape of reflectance spectra of samples dyed with
the two dyes are different, and the nylon dyed with weld dye in all methods of dyeing is lighter
than the nylon dyed with pomegranate peel. The K/S value of a dyed sample is directly propor-
tional to the concentration of dye present in the sample (Dev, Venugopal, Sudha, Deepika, &
Ramakrishna, 2009). Figure 4 shows the absorbance (K/S) spectra of the nylon dyed with weld and
pomegranate peel dyes in four different methods of dyeing: non-mordanting, bottom-mordanting,
meta-mordanting, and after-mordanting.
As shown in Figure 4, the unit (K/S) of the samples dyed with weld dye in all different methods of
dyeing is almost similar to the samples dyed with pomegranate peel dye. So it can be found that the
color strength of dyes is almost equal, and the difference in lightness was due to the difference in the
shade of samples.

Colorimetric Analysis
The absorption behavior of weld and pomegranate peel natural dyes on nylon is studied by analyzing
the color parameter such as lightness (L*), chroma (C*), and hue angle (h). The lightness of the
130 Clothing and Textiles Research Journal 32(2)

Figure 6. The chroma of nylon dyed with different dyeing methods: (A) non-mordanting, (B) pre-mordanting,
(C) meta-mordanting, and (D) after-mordanting.

samples dyed with weld and pomegranate peel dyes in all methods of dyeing is shown in Figure 5. It
can be seen that the sample dyed with weld dye is lighter than the samples dyed with pomegranate
peel dye, while the samples lightness values were decreased by mordanting. Figures 6 and 7 show
the chroma and hue of nylon dyed in the different dyeing methods of non-mordanting, bottom-
mordanting, meta-mordanting, and after-mordanting, respectively. As shown in these figures, the
chroma and hue of the dyed samples are different, and the chroma and hue of the samples dyed with
weld dye are higher.
In order to further investigate the color parameters of nylon dyed with weld and pomegra-
nate peel dyes, a* and b* were calculated. The chromaticity distribution of the samples dyed is
shown in Figure 8. In this figure, the vertical axis is b* (blueness-yellowness) and the horizon-
tal axis shows a* (greenness-redness). It is clearly indicated that the samples dyed with weld
dye are yellower than the samples dyed with pomegranate peel dye. Also, the samples dyed
with weld dye have a green shade, while the samples dyed with pomegranate peel dye have
a red shade.

PCA
The Eigenvalues of the principal components of reflectance spectra for the samples dyed using dif-
ferent dyeing methods of weld and pomegranate peel dyes are shown in Figure 9. As seen in this
figure, the Eigenvalues of the first principal components are the largest and most important values.
Consequently, only the first principal component was investigated. Figure 10 shows the first
Shams-Nateri et al. 131

Figure 7. The hue of nylon dyed with different dyeing methods: (A) non-mordanting, (B) pre-mordanting, (C)
meta-mordanting, and (D) after-mordanting.

principal component of the dyed samples. As shown in this figure, the principal component of the
samples dyed with weld and pomegranate peel dyes in all methods of dyeing is different. So, vari-
able reduction with PCA also shows the difference in reflectance spectra between the samples dyed
with weld and pomegranate peel dyes.

Fastness Properties
The fastness properties of nylon dyed with weld and pomegranate peel are shown in Table 1. As can
be seen, the rubbing fastness of samples dyed with weld and pomegranate peel dyes in all methods of
dyeing is excellent. The washing fastness of dyed nylon was improved by mordanting. In all meth-
ods of dyeing, the washing fastness of nylon dyed with pomegranate peel dye was better than sam-
ples dyed with weld. The light fastness of dyed samples ranges from very poor to good. Overall, the
best results were given by the after-mordanting method. However, the light fastness of after-
mordanting is better than some other types of natural dyes used for nylon dyeing (Agrawal, 2012;
Badri & Burkinshaw, 1993; Lokhande & Dorugade, 1999).

Conclusion
In this research, weld and pomegranate peel natural dyes, which produce yellow colors, were used
for dyeing nylon fabrics. The obtained result shows that the samples dyed with weld and pomegra-
nate peel have different reflectance spectra, unit (K/S), and shades of yellow color. The PCA method
132 Clothing and Textiles Research Journal 32(2)

Figure 8. The CIELab color values of nylon dyed with different dyeing methods: (A) non-mordanting, (B) pre-
mordanting, (C) meta-mordanting, and (D) after-mordanting.

Figure 9. Eigenvalues of principal components of nylon dyed with (A) weld and (B) pomegranate peel dyes.

also showed the difference between the color of samples dyed with weld and pomegranate peel. The
results of fastness properties of the samples dyed showed that the rubbing fastness is excellent for
both the natural dyes. The washing fastness of nylon dyed was improved with mordanting. The best
light-fastness was obtained by the after-mordanting dyeing method. Overall, the best results of fast-
ness properties were obtained by using after-mordanting method.
Shams-Nateri et al. 133

Figure 10. Principal component analysis of nylon dyed with different dyeing methods: (A) non-mordanting, (B)
pre-mordanting, (C) meta-mordanting, and (D) after-mordanting.

Table1. The Fastness Properties of Nylon Dyed With Weld and Pomegranate Peel Dyes With Different
Dyeing Methods.

Fastness Properties

Rubbing

No Dyeing Method Dye Light Washing Wet Dry

1 Non-mordanting Weld 5 3 45 5
2 Non-mordanting Pomegranate peel 3 4 5 5
3 Pre-mordanting Weld 12 34 45 45
4 Pre-mordanting Pomegranate peel 45 5 5 5
5 Meta-mordanting Weld 2 4 5 5
6 Meta-mordanting Pomegranate peel 2 5 5 5
7 After-mordanting Weld 6 4 45 5
8 After-mordanting Pomegranate peel 45 5 5 5

Acknowledgment
The authors would like to express the grateful thanks to Iran National Science Foundation (INSF) for supporting
this research.
134 Clothing and Textiles Research Journal 32(2)

Declaration of Conflicting Interests

The author(s) declared no potential conflicts of interest with respect to the research, authorship, and/or publi-
cation of this article.

Funding
The author(s) disclosed receipt of the following financial support for the research, authorship, and/or publica-
tion of this article: This research was funded by Iran National Science Foundation (INSF).

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Author Biographies
Ali Shams-Nateri was born in 1986, Iran. He received his BSc degree (1994), MSc degree (1996), and PhD
degree (2002) in Textile Chemistry Engineering from Amirkabir University of Technology of Iran. The subject
of his PhD thesis was color physics. He is a professor in textile engineering department at the University of
Guilan. His research interests are color physics and colorimetry, computer and mathematic application in tex-
tile, neural network, and fuzzy logic.
Abbas Hajipour is a PhD student in the department of textile engineering at University of Guilan, Rasht, Iran.
He received his BSc degree from Kar University, Qazvin, Iran in 2010 and earned his MSc degree from
University of Guilan in 2012. His current research interests include color physics, image processing, and
dyeing.

Ehsan Dehnavi received the BS and MSc degrees from Kar University of Qazvin, Iran, in 2010, and Guilan
University, Rasht, Iran, in 2012, respectively, both in Textile Engineering, dye chemistry, and fiber science
branch. His research interests include chemistry science and dyeing and its process especially the natural one.
The most important point that he considers is the environmental protection, in any field of research.

Ehsan Ekrami was born in 1981, Iran. He received his BSc and MSc degrees in textile chemistry and fiber
sciences from University of Guilan at Rasht, Iran (2007). He is currently a PhD student in the department of
textile engineering at Amirkabir University of technology, Iran. His research interests include color physics,
textile dyeing, and recycling of textile wastes.