Original article

Textile Research Journal

0(00) 1–9

Rapid identification of plant- and ! The Author(s) 2020

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chemical-dyed cotton fabrics using DOI: 10.1177/0040517520912036
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the near-infrared technique

Mingxia Li1,2, Guangting Han1,2 , Wei Jiang1,2,

Chengfeng Zhou1,2, Yuanming Zhang1,2, Sishe Wang3,
Jianjun Su3 and Xianbo Li1,2

Abstract
Plant dye is a promising dyestuff to be used in textiles due to its unique environmental compatibility. However, currently
there is no effective method for the identification of plant-dyed and chemical-dyed textiles. In this study, near-infrared
(NIR) spectroscopy combined with three kinds of pattern recognition methods, namely soft independent modeling of
class analogy (SIMCA), partial least squares (PLS) regression and principal component regression (PCR), were applied to
identify cotton fabrics dyed with plant and chemical dyes. A total of 336 plant dye and chemical dye dyed cotton fabrics
were prepared and the NIR spectra were collected; 267 samples were used as the calibration set, while the remaining
69 samples were used as the validation set. After pretreatment with the Savitzky–Golay first derivative, the calibration
model was constructed. In the SIMCA model, the correct recognition rate values of the calibration and prediction sets
were 100% and 98.55%, respectively. The PLS model showed that the number of principal components (PCs) and the
correlation coefficient (R2) were 8 and 0.9978, respectively, and the results of PCR were PC ¼ 10, R2 ¼ 0.9937. Both
methods were satisfactory for the predicted results. The overall results indicated that NIR spectroscopy could be used
for rapid and nondestructive identification of plant-dyed cotton fabrics and chemical-dyed cotton fabrics.

Keywords
near-infrared, plant dye, chemical dye, cotton fabric, identification

Chemical dyes are obtained by reacting primary chem-
ical substances separated from petroleum derivatives
with high temperature and high pressure, which has
been developed for more than 160 years since its inven-
tion. Chemical dyes are attractive as textile colorants
due to their complete spectrum, low cost and high col-
orfastness, providing colorful fabrics and garments for
human beings and occupying an important position in
the national economy.1–4 Natural dyes imply and refer
to all the coloring materials derived or extracted from
nature, that is, of plant, animal, mineral and microbial
origins.5,6 Nowadays, along with the social develop-
ment and the improvement of people’s living standards,
the significance of textiles has been from warmth to
fashion, environmental protection and other functions.
The pollution of chemical dyes to the environment has
become increasingly prominent, and its potential harm
to the human body has also begun to attract
attention.7–9 With the public’s enhanced cognizance to
eco-safety and health concerns, plant dyes are favored
and respected by people for their excellent environmen-
tal compatibility and health care functions and are
widely used in the preparation of a variety of high
value-added textiles.5,10,11 Textiles dyed with plant
dyes retain the unique medicinal and aromatic
1
State Key Laboratory of Bio-Fibers and Eco-Textiles, Qingdao University,
China
2
College of Textile & Clothing, Qingdao University, China
3
Dezhou Hengfeng Textile Co., Ltd, China
Corresponding author:
Xianbo Li, Qingdao University, Ningxia Road NO.308, Qingdao,
Shandong 266071, China.
Email: fann@public.qd.sd.cn
2 Textile Research Journal 0(00)
components of plants, which have superior human and
environmental safety.12
Due to the massive price difference between chemical
and plant dyes, textiles using chemical dyes to fake
plant dyes dyed fabrics can be found in the market,
leading to an active demand to distinguish fabrics
dyed with chemical and plant dyes.13 Since both chem-
ical- and plant-dyed fabrics are similar in their compos-
ition and physical texture, the identification of the two
fabrics is currently still a problem, and there is no
standard in this area. Some studies have been per-
formed to establish an identification method in the
recent years. The chemical stripping method was used
to determine yellow plant-dyed wool fabrics.14 Raman
spectroscopy successfully identified natural indigo dyed
silk fabrics and chemical indigo dyed silk fabrics.15
However, the methods are not adaptable to other
dyed fabrics and market quality supervision because
of the disadvantages of being time-consuming, destroy-
ing samples and lacking of versatility. Therefore, effect-
ive and reliable analytical technologies that can identify
plant-dyed and chemical-dyed fabrics are demanded
urgently.
The near-infrared (NIR) technique is a modern tech-
nique that provides fast quantitative and qualitative
analysis, which has the advantages of easy operation,
high speed, low cost and no sample consumption.16–18
NIR spectroscopy has recently gained popularity in
many fields, such as pharmaceutical and clinical medi-
cine, environmental science, food industry, wood testing
and the petrochemical industry.19–22 Principal compo-
nent analysis (PCA), partial least squares discriminant
analysis (PLS-DA), soft independent modeling of class
analogy (SIMCA), linear discriminant analysis (LDA),
the support vector machine (SVM) and artificial neural
networks (ANNs) have all been used to deal with clas-
sification issues. Our previous study successfully used
the NIR modeling technique to classify natural
fibers,23 different fabrics that are constructed using dif-
ferent fibers.24 The quantitative analysis of different
wood chemical composition was also studied.16,25–27
Therefore, using NIR spectroscopy to classify chemical-
and plant-dyed fabrics is feasible and should be
investigated.
The objective of this study is to explore the feasibil-
ity of the identification of cotton fabrics dyed with
plant dyes and chemical dyes using NIR spectroscopy
combined with pattern recognition methods. In particu-
lar, we choose three primary colors respectively for the
two dyes in order to verify the universality of our
models. Therefore, we adopt SIMCA, partial least
squares (PLS) regression and principal component
regression (PCR) methods to build qualitative and
quantitative models. The correct recognition rate
(CRR) of the models for the calibration sets and the
prediction sets sample was used for the evaluation of
the model.
Materials and methods
Sample preparation
The samples were all obtained by dyeing bleached
cotton fabrics with six types of dyes. The bleached
cotton fabrics and chemical dyes were provided by
Fuyuan Textile and Dyeing Company (Weifang,
Shandong, China). The plant dyes were obtained
from Dezhou Hengfeng Textile Co., Ltd (Dezhou,
Shandong, China); the red, yellow and blue dyes were
extracted from sappan, turmeric and radix isatidis,
respectively. The bleached cotton fabrics underwent
the dyeing process using the standard dyeing method.
There were 45 chemical-dyed red fabrics (CR), 45 che-
mical-dyed yellow fabrics (CY), 45 chemical-dyed blue
fabrics (CB), 72 red plant-dyed cotton fabrics (PR), 72
yellow plant-dyed cotton fabrics (PY) and 57 blue
plant-dyed cotton fabrics (PB) prepared in this study.
Each sample was obtained from different dyeing condi-
tions to ensure the diversity and independence of the
sample. In the modeling process, 36 CR samples, 36 CY
samples, 36 CB samples, 57 PR samples, 57 PY samples
and 45 PB samples were used for constructing the
models. The remaining samples were used to validate
the performances of the established models.
Infrared spectra and near-infrared spectra collection
The bleached and six different dyed cotton fabrics were
investigated with Fourier transform infrared spectros-
copy (FT-IR, Thermo Fisher Scientific NICOLET
5700, Waltham, MA, USA) in a wavenumber range
of 4000–500 cm1. Each spectrum was an average of
16 scans. The NIR spectra were collected using a
PerkinElmer Frontier spectrometer. The wavenumber
range was selected as 10,000–4000 cm1 and the spec-
tral resolution was 4 cm1. Each spectrum was mea-
sured from an average of 32 scans with air as the
internal reference. Three reduplicative spectra were col-
lected for each sample and averaged as the final spec-
trum of the sample. In total, 336 spectra of six different
sample species were acquired. Before analysis and
during the measurements, constant relative temperature
(25  2 C) and humidity (57  2%) were maintained.
Spectral pretreatment and classification method
In addition to the sample information, the raw NIR
spectra also had baseline drift and a large noise in the
spectra. Prior to modeling, all of the spectra collected
were pretreated using the Savitzky–Golay first
Li et al.
derivative (SG 1st-Der). The pretreatment can effect-
ively eliminate the influence of baseline drift, reduce
noise and enhance the spectral features. SIMCA,
PCR and PLS regression were applied to all the pre-
processed data.
SMICA is a supervised discriminant analysis method
based on PCA. For each class of sample, a PCA model
is established and then the residual variance of the
model class with the residual variance of the unknown
samples is compared to determine which category the
sample belongs to.28,29 The internal recognition rate
represents the identification capability of the model
for the calibrating samples. The recognition rate and
rejection rate refer to the number of samples in and
out the area of the model.
PCR and PLS are both data description and dimen-
sion reduction methods,30,31 which are widely used to
deal with large datasets, such as spectra data. The per-
formance of established models is evaluated using two
prime parameters, which are the correlation coefficient
(R2) and the root mean square error of prediction
(RMSEP).18,32 R2 indicates the relationship between
the actual results and the predicted values, which rep-
resents the prediction performance of the model. In
addition, the RMSEP values show the prediction accur-
acy of the models. To classify the different species of
our samples by PCR and PLS regression, some rules
were set up as described in Table 1. The samples that
come from different species were assigned to different
values (1, 2, 3, . . ., n). Then PLS and PCR models were
constructed based on these values. If the predicted
value of the sample was inside the 0.5 error area
(0.5) of one number, this sample was identified to
the relevant species.
In this study, the values of the six species were assigned
as follows: 1: CR; 2: CY; 3: CB; 4: PR; 5: PY; 6: PB.
Results and discussion
Spectra of plant- and chemical-dyed samples
Figure 1 shows images of the bleached and six different
dyed cotton fabrics (a) and their FT-IR spectra (b).
Table 1. Algorithm for classifying samples of different species using partial least squares/principal component regression
Sample CR CY
Sample size N1 N2
Assigned value 1 2
Classification value 0.5–1.5 1.5–2.5
Prediction value A1 – AN1 B1 – BN2
Recognition no. Nrg ¼ the number of samples that predict
Recognition rate Nrg/Nx  100% (x ¼ 1, 2, 3, . . . ,n)
CR: chemical-dyed red fabrics; CY: chemical-dyed yellow fabrics; CB: chemical-dyed blue fabrics; PB: blue plant-dyed cotton fabrics.
3
The colors of the six samples were different, but it
was hard to identify the chemical-dyed and plant-
dyed samples visually. Traditionally, FT-IR is used to
distinguish different samples with different chemical
bonds and functional groups. In our research, it was
obviously to find that the main peaks of the FT-IR
spectra of the six samples were similar to those of the
bleached samples, and there were no characteristic
peaks for dyes with either chemical and plant species
in the spectra. Theoretically speaking, the dye informa-
tion should be presented in the spectra. However, the
contents of the dyes in the fabric were very low (the
concentration was lower than 0.1% in many cases33)
leading to no visible difference in the FT-IR spectra
as a result of a weak absorption of the dyes, which is
shown in Figure 1. The above results indicated that it
was difficult to use infrared spectroscopy to identify the
chemical- and plant-dyed fabrics.
As the dye information has been included in the IR/
NIR spectra, the NIR modeling method has the poten-
tial to classify the different dyed fabrics. The raw NIR
spectra of the six different dyed cotton fabrics and the
spectra after SG 1st-Der pretreatment are shown in
Figure 2. The SG 1st-Der preprocessed spectra retain
and strengthen the information of the raw spectra.
There were also no obvious differences between the
six spectra, which indicated the dyed cotton fabrics
could not be identified directly from this figure. To
solve the problem, classification models based on
chemo-metrics were developed.
SIMCA classification
An optimized classification model was successfully con-
structed using the SIMCA method. Table 2 shows the
results of the calibration model for the six different
types of samples. The results showed a 100% internal
recognition rate and 100% rejection rate for CR, CY,
CB, PY and PB, while PR had a 100% recognition rate
and 99% rejection rate, demonstrating that the model
can identify the dyed fabrics with high accuracy.
Then 69 samples were used to validate the precision
of the model. Table 3 shows that all the CR, CY, CB,
CB ... PB
N3 ... Nn
3 ... n
2.5–3.5 ... (n – 0.5) – (n + 0.5)
C1 – CN3 ... Z1 – ZNn
the value inside the classification value
4 Textile Research Journal 0(00)

Figure 1. Photographs (a) and Fourier transform infrared spectra (b) of bleached and dyed cotton fabrics. CR: chemical-dyed red
fabrics; CY: chemical-dyed yellow fabrics; CB: chemical-dyed blue fabrics; PR: red plant-dyed cotton fabrics; PY: yellow plant-dyed
cotton fabrics; PB: blue plant-dyed cotton fabrics.

Figure 2. Raw near-infrared spectra (a) and Savitzky–Golay first derivative spectra (b) of six kinds of dyed cotton fabrics.
CR: chemical-dyed red fabrics; CY: chemical-dyed yellow fabrics; CB: chemical-dyed blue fabrics; PR: red plant-dyed cotton fabrics;
PY: yellow plant-dyed cotton fabrics; PB: blue plant-dyed cotton fabrics.

Table 2. Classification performance report using the soft independent modeling of class analogy method

Material CR CY CB PR PY PB

Recognition rate (%) 100 100 100 100 100 100

(36/36) (36/36) (36/36) (57/57) (57/57) (45/45)
Rejection rate (%) 100 100 100 99 100 100
(231/231) (231/231) (231/231) (208/210) (210/210) (222/222)
CR: chemical-dyed red fabrics; CY: chemical-dyed yellow fabrics; CB: chemical-dyed blue fabrics; PR: red plant-dyed cotton fabrics; PY: yellow plant-
dyed cotton fabrics; PB: blue plant-dyed cotton fabrics.
Li et al.
Table 3. Identification results of the soft independent modeling
of class analogy method
Sample Identification Identification
Sample no. no. rate (%)
CR 9 9 100
CY 9 9 100
CB 9 9 100
PR 15 15 100
PY 15 15 100
PB 12 11 91.67
CR: chemical-dyed red fabrics; CY: chemical-dyed yellow fabrics;
CB: chemical-dyed blue fabrics; PR: red plant-dyed cotton fabrics; PY:
yellow plant-dyed cotton fabrics; PB: blue plant-dyed cotton fabrics.
PY and PR samples were correctly identified using
the model. In addition, 11 PB samples were correctly
identified from the total 12 samples; the identifica-
tion rate was 91.67%. All results demonstrated that
coupled with NIR spectroscopy and SIMCA, the mod-
eling method can be effective for the identification of
dyed fabrics.
Inter material distance (IMD) values represent the
differences between the six types of dyed cotton fabrics
in the modeling analysis. If the IMD values are higher,
the two species have a large difference, and it is easier to
classify and identify. In contrast, when the two species
have closer relationships, the IMD will be small, and
they are more difficult to distinguish. In order to illus-
trate the accuracy and effectiveness of the identification,
the IMD between the six species was evaluated by using
the SIMCA method. As shown in Table 4, the IMD
among plant-dyed cotton fabrics (PR, PY, PB) and CR
were all higher than 3, indicating that the difference
between chemical dyes and plant dyes was prominent
and was easier to recognize. The average IMD value
between the plant-dyed cotton fabric (PR, PY, PB) was
2.55, revealing that the spectra of PR, PY and PB of the
plant-dyed cotton fabric were similar and difficult to
identify. The average IMD value between chemically
dyed cotton fabrics (CR, CY, CB) was also lower
than 3, demonstrating that they maybe misclassified
using the model.
PLS/PCR classification
PLS and PCR classification models were successfully
built based on the preprocessed spectra. The corres-
ponding relationship between the specified value and
the predicted value of the cotton fabric under the
two modeling methods is shown in Figure 3. The
x-coordinate represents the real value of cotton fabrics
dyed by plant dyes and cotton fabrics dyed by chemical
dyes, and the y-coordinate is the calculated value of the
5
Table 4. Inter material distance of the soft independent
modeling of class analogy model
Material CR CY CB PR PY PB
CR – 2.6 3.18 5.35 4.9 5.97
CY – – 1.86 4.28 3.59 5.31
CB – – – 3.9 3.13 5.21
PR – – – – 1.89 2.04
PY – – – – – 3.12
CR: chemical-dyed red fabrics; CY: chemical-dyed yellow fabrics; CB:
chemical-dyed blue fabrics; PR: red plant-dyed cotton fabrics; PY:
yellow plant-dyed cotton fabrics; PB: blue plant-dyed cotton fabrics.
model. The sample coordinates points were closely
around the fitting line, and the slope of the fitting line
under both models was close to 1. The results of the
quantitative analysis of the PLS method are as follows:
the number of principal components (PCs) was 8, the
correlation coefficient (R2) was 0.9978 and the root
mean square error (RMSEE) was 0.0779; the results
of the quantitative analysis of PCR were as follows:
the number of PCs was 10, R2 was 0.9937 and
RMSEE was 0.1332. Both of the methods were satis-
factory for the predicted results. By comparing the
evaluation indexes of the two models, it can be seen
that the model established based on the PLS method
had fewer PCs; R2 and RMSEE were both superior to
PCR. Therefore, the PLS model was relatively simple
with higher identification accuracy and stability.
To verify the accuracy of the models, 69 samples (the
number of CR was 9; CY was 9; CB was 9; PR was 15;
PY was 15 and PB was 12, respectively) were used to
validate the model. Figure 4 shows the correction of
predicted value and the specified value under the two
modeling methods in the prediction set. As shown in
Figure 4, the slope of the fitted line was 0.9641 and
0.9536, respectively, both of which were greater than
0.9, and the validation results of the two models were
acceptable. However, the R2 of the PLS model was
0.9940, which was larger than that of 0.9937 of PCR,
and the RMSEP of the PLS was also lower than that of
the PCR, so the prediction accuracy of the PLS model
was higher.
The classification results using PLS and PCR are
shown in Tables 5 and 6. It is found that the predicted
value of the sample was inside the 0.5 error area (0.5)
of the assigned value, and all the samples were identi-
fied to the relevant species. The six different types of
samples have a 100% recognition rate under the two
modeling methods in the prediction set.
Figure 5 gives the score values of all samples with
different PCs when establishing a quantitative identifi-
cation model based on the PLS algorithm. The score
values show clearly the similarity degree among the
6 Textile Research Journal 0(00)

Figure 3. Partial least squares (a) and principal component regression (b) model regression figure of calibration set. PC: principal
component; RMSEE: root mean square error.

Figure 4. The correlations between predicted value and specified value for partial least squares (a) and principal component
regression (b) models in the prediction set. RMSEP: root mean square error of prediction.

Table 5. Classification results using partial least squares

Sample CR CY CB PR PY PB

Sample size 9 9 9 15 15 12
Classification value 0.5–1.5 1.51–2.5 2.51–3.5 3.51–4.5 4.51–5.5 5.51–6.5
Prediction value 0.89–1.20 2.01–2.22 2.76–3.14 3.87–4.19 4.72–5.19 5.64–6.17
Recognition no. 9 9 9 15 15 12
Recognition rate 100% 100% 100% 100% 100% 100%
CR: chemical-dyed red fabrics; CY: chemical-dyed yellow fabrics; CB: chemical-dyed blue fabrics; PR: red plant-dyed cotton fabrics; PY: yellow plant-
dyed cotton fabrics; PB: blue plant-dyed cotton fabrics.
Li et al. 7

Table 6. Classification results using principal component regression

Sample CR CY CB PR PY PB

Sample size 9 9 9 15 15 12
Classification value 0.5–1.5 1.51–2.5 2.51–3.5 3.51–4.5 4.51–5.5 5.51–6.5
Prediction value 0.96–1.24 1.95–2.26 2.81–3.18 3.85–4.19 4.76–5.17 5.58–6.16
Recognition no. 9 9 9 15 15 12
Recognition rate 100% 100% 100% 100% 100% 100%
CR: chemical-dyed red fabrics; CY: chemical-dyed yellow fabrics; CB: chemical-dyed blue fabrics; PR: red plant-dyed cotton fabrics; PY: yellow plant-
dyed cotton fabrics; PB: blue plant-dyed cotton fabrics.

Figure 5. Score values of all samples with different principal components (PCs) using partial least squares regression: (a) PC ¼ 1;
(b) PC ¼ 2; (c) PC ¼ 3; (d) PC ¼ 8. CR: chemical-dyed red fabrics; CY: chemical-dyed yellow fabrics; CB: chemical-dyed blue fabrics;
PR: red plant-dyed cotton fabrics; PY: yellow plant-dyed cotton fabrics; PB: blue plant-dyed cotton fabrics.

different dyed cotton fabrics samples, and which PC
can choose to identify the species better. It was found
that plant-dyed cotton fabrics (PR, PY, PB) and che-
mical-dyed cotton fabrics (CR, CY, CB) can be sepa-
rated using PC 1. By choosing PC 2, the CR can be
separated from chemically dyed cotton fabric (CY,
CB). PR, PY and PB of plant-dyed cotton fabric were
also well separated, while CY and CB were the only two
that were still unseparated. CY and CB were well sepa-
rated when PC 8 was chosen, while the other samples
8 Textile Research Journal 0(00)
were mixed again. As a result, combining PC 8 was the
best for identifying all the samples.
Conclusion
In this study, six species of dyed cotton fabrics, namely
CR, CY, CB, PR, PY and PB, were qualitatively iden-
tified by using NIR spectroscopy and the SIMCA iden-
tification method. The model recognition rate and
rejection rate were both higher than 95%. PLS and
PCR were also created to classify the six species using
a quantitative analysis method. It was found that the
correlation coefficient between the calibration set and
the prediction set of the two models was greater than
99%; the PLS model was more accurate and concise.
The overall results indicated that it is feasible to iden-
tify cotton fabrics dyed with plant dyes and chemical
dyes using NIR spectroscopy combined with pattern
recognition methods.
Declaration of conflicting interests
The author(s) declared no potential conflicts of interest with
respect to the research, authorship, and/or publication of this
article.
Funding
The authors disclosed receipt of the following financial sup-
port for the research, authorship and/or publication of this
article: This work was supported by the National Natural
Science Foundation of China (51903131), the Natural
Science Foundation of Shandong Province (ZR2019Q
EM007 & ZR2017BEM045) and the Special Foundation of
‘‘Taishan Scholar’’ Construction Program.
ORCID iDs
Guangting Han https://orcid.org/0000-0002-5320-5400
Xianbo Li https://orcid.org/0000-0002-8904-3298
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