Measurement 148 (2019) 106936

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Measurement
journal homepage: www.elsevier.com/locate/measurement

Physicochemical properties of Iranian ziziphus honey and emerging

approach for predicting them using electronic nose
Saeed Faal ⇑, Mohammad Loghavi, Saadat Kamgar
Department of Biosystems Engineering, School of Agriculture, Shiraz University, Shiraz 71441-65186, Iran

a r t i c l e i n f o a b s t r a c t

Article history: The aim of this paper is development and evaluation of an electronic nose as a non-destructive system for
Received 29 May 2019 predicting the physicochemical parameters of honey including ash content (AC), free acidity (FA), mois-
Received in revised form 27 July 2019 ture content (MC) and pH based on its aroma. To verify the authenticity of the honey samples the HPLC
Accepted 8 August 2019
analysis carried out. Artificial neural network (ANN) and Support Vector Machine (SVM) models were
Available online 12 August 2019
applied to the features extracted from the sensors responses to predict AC, FA, MC and pH. The developed
models for prediction of the physicochemical parameters showed high performance based on the honey
Keywords:
headspace gases and the best results for predicting the AC, FA, MC and pH obtained from the ANN model
Electronic Nose
Honey
which the R2 values were 0.838, 0.918, 0.926 and 0.933, respectively. The results proved feasibility and
Metal oxide semiconductor applicability of using the developed e-nose as a non-destructive system for predicting the physicochem-
Physicochemical attributes ical properties of honey.
Ó 2019 Elsevier Ltd. All rights reserved.

1. Introduction
Usually, the sweet taste of honey makes it easy to forget about
the health benefits of that and its replacement with white sugar as
a natural alternative. Honey has a wide range of health benefits for
people who consume it consistently and it contains wonderful
properties that can significantly enhance the overall health [1].
Honey quality is a complex concept referring to chemical com-
pounds that make honey acceptable for global standards. The
chemical compounds and specific aroma of honey are affected by
many different factors, such as geographical origin, environmental
conditions, botanical and climate. Basically, food quality evaluation
performs by using the conventional methods such as testing its
structure (moisture content, color, flavor and texture) or by means
of advanced analytical techniques such as gas chromatography
(GC), atomic absorption spectrophotometry, high performance liq-
uid chromatography (HPLC) and gas chromatography-mass spec-
trometry (GC-MS) analysis with solid phase micro extraction [2–
5]. Usually the honey quality parameters are measured by the con-
ventional analytical techniques and there are many studies report-
ing on the measurement of physicochemical properties of honey,
such as moisture content, pH, ash content, enzyme activities of
invertase, electrical conductivity, acidity, sugar composition
⇑ Corresponding author.
E-mail addresses: s.faal@shirazu.ac.ir (S. Faal), Loghavi@shirazu.ac.ir
(M. Loghavi), Kamgar@shirazu.ac.ir (S. Kamgar).
(sucrose, glucose and fructose), color and hydroxyl methyl furfural
(HMF) [6,7] which have been used to differentiate between differ-
ent species of honey or adulteration detection. The precise of these
techniques have been proven but these techniques are expensive,
time-consuming and destructive which they can’t be used in the
real time sorters. In the industrial quality control applications,
managers should utilize the type of test procedures that can handle
the large number of samples with low price. E-nose is one of the
analytical tool, that recently proposed by numerous researchers
for evaluating the food quality in the food industry [8]. E-nose is
a device that identifies the specific components of an odor coupled
with pattern recognition methods to extracts sample specifications
and characterizations.
For the sensory properties of foods, aroma plays an important
role and several studies are reporting the potential utilization of
the e-nose in food industry such as identifying the geographical
origin of the virgin olive oil [9], microbial contamination in pro-
cessed tomatoes [10], detecting the adulteration in milk [11], esti-
mating the saffron adulteration [12], prediction of rapeseed quality
[13], Real-time aroma monitoring of mint (Mentha spicata L.) [14],
predicting the peach freshness [15] tracing the tomato-juice qual-
ity [16], identification of tea quality [17], detecting the adulter-
ation in honey [18], discriminating the honey based on their
geographical and botanical [19], apple quality control [20] and pre-
dicting the banana quality properties [21].
Considering the successful reports researchers have been
reported on using the e-nose in the food industry the aim of this

https://doi.org/10.1016/j.measurement.2019.106936
0263-2241/Ó 2019 Elsevier Ltd. All rights reserved.
2 S. Faal et al. / Measurement 148 (2019) 106936
paper was to evaluate the potential of an e-nose for finding the
relationships between AC, FA, MC, pH and honey headspace gases
and utilizing the chemometric methods to predict AC, FA, MC and
pH.
2. Materials and methods
2.1. Honey samples and chemical materials
Ziziphus honey is one of the best and most desirable honey in
the southern regions of Iran. One hundred eleven different honey
Samples directly collected from beekeepers from major ziziphus
honey producing regions (Zahedan (S1), Bushehr (S2), Abadan
(S3), Ahvaz (S4), Bandar Abbas (S5), Iran Shahr (S6), Jahrom (S7),
Jiroft (S8), Shiraz (S9) and Kerman (S10)) in the summer season
of 2016. All chemicals and solvents used for analysis were pur-
chased from a reputable company: Sodium hydroxide, Phenolph-
thalein and HPLC-grade water were obtained from Merck
(Darmstadt, Germany).
2.2. Physicochemical analysis
2.2.1. HPLC analysis
To verify the authenticity of the honey purchased from bee-
keepers, the analysis of detecting glucose, fructose and sucrose
contents were performed by using the Knauer HPLC equipped with
the 1000 pump, a manual chromatographic valve, an on-line vac-
uum degasser and a thermostatic column compartment. The col-
umn was a Eurocat PB column (300–8 mm, 10 lm). The mobile
phase was HPLC-grade water and the flow-rate was maintained
at 0.5 ml min
1 and the column was operated at 75 °C. Every injec-
tion was performed by injecting 40 lL of the prepared sample and
it took twenty minutes between the two injections for re-
equilibration.
2.2.2. pH
For measuring the pH, it was evaluated in a solution of 10 g of
honey in 75 ml of CO2 free distilled water, using a FisherbrandTM
accumetTM AE150 pH Meter with custom buffers, all the experi-
ments were repeated in ten replications.
2.2.3. Moisture content
The moisture content was measured by refractometry, using a
WYA-2S Digital Abbe refractometry. All the measurements were
carried out at the 20 °C and all the experiments were repeated in
ten replications. For each measurement, two grams of sample
was poured on the glass surface of refractometry.
2.2.4. Ash content
To determine the ash content, a crucible was weighed with a
±0.0001 g scale and after it reached the constant weight, 5 g of
honey samples were weighed and then samples burned on the
direct flame. After samples were completely burned and they did
not produce any smoke they were placed in a furnace (Model
LEF-304P, Lab Tech, South Korea) and were calcined overnight at
600 °C. All the experiments were repeated in ten replications.
2.2.5. Free acidity
Free acidity was determined by potentiometric titration and
according to the harmonized methods of the European Honey
Commission [22]. 10 g sample was solved in 75 ml of CO2 free dis-
tilled water in a 250 ml beaker and it was titrated with 0.1 M NaOH
to pH 8.30 (operator have to wait 120 s of starting the titration to
determine that the read number is constant). The free acidity of
honey is the content of all free acids, expressed in milliequivalents
kg
1. All the experiments were repeated in ten replications.
2.3. E-nose system
The main components of the developed e-nose system are: sen-
sor chamber, gas sensors, pumps and pipes for circulating the air
and aroma, sample chamber, data preprocessing program written
in LabVIEW software and data acquisition system (Fig. 1a). For
designing sensor array about twenty different MOS gas sensors
available in Iran market were purchased and each of them evalu-
ated by means of different honey samples and finally eight sensors
which were more sensitive to the honey head space gases were
selected and were assembled inside the sensor chamber. The sen-
sor array contains two TGS sensors made in by Figaro Engineering
(Osaka, Japan) and six MQ sensors made in HANWEI Electronics
Co., Ltd. (Henan, China). Table 1 shows the sensors specifications.
A digital temperature and humidity sensor (DHT-11) were added
inside the sensor chamber to check up the conditions of the sensor
chamber. A scheme of the test station is presented in Fig. 1b that
shows how the system works. The experimental conditions for E-
nose are given as follows it is divided into two phases: (1) purging
and (2) saturation and measurement. About 250 g of the honey was
poured in an Erlenmeyer flask (500 ml) at the temperature of
25 °C ± 3 °C and was sealed by plastic for the headspace generation.
A computer program was wrote to control the solenoid valves to
circulate the air through different paths based on the system oper-
ation stage. Before the sensor chamber was exposed to sample
volatiles it was cleaned with the flow of fresh dry air. In this stage,
solenoid valves 1, 2 and 4 were opened and the solenoid valve 3
was closed and all the pumps were running. During this stage
the dry air flowed through the sample and sensor chambers to
clean them and at the end was exhausted from air outlet pipe to
the atmosphere. This operation takes about 600 (s). In the next
stage, pump 1 was turned off but the pumps 2 and 3 were still run-
ning and solenoid valves 1 and 4 were closed and solenoid valves 2
and 3 were opened. During this stage the honey volatiles became
saturated and were circulated throw the sensor chamber. The sen-
sors were exposed to sample volatiles and the changes in sensors’
responses were acquired by the data acquisition system for 600 (s),
within this time not only the headspace gasses were circulated
through the sensor chamber they also became saturated. The
steady-state sensor responses occurred at around 550 (s) and this
time was considered as the response time. After this phase again
the sensors and sample chambers that were saturated with the
honey headspace gases were cleaned by the fresh dry air for
600 s so the sensors response return to their baseline value.
2.4. LabVIEW program
Sensors output signals were acquired using an Arduino Mega
2560 microcontroller. The program, for communicating the data
with the computer was NI LabVIEW 2017 to acquire data from
the Arduino and convert the analog output to digital for prepro-
cessing them and a user-friendly graphical user interface (GUI)
was designed inside the LabView program. Fig. 2(a and b) show
the designed GUI and the algorithm of the LabVIEW program that
includes: A) Read count (ms) to determine the reading intervals. B)
VIZA COM port to select and activate the serial port. C) Start button
to start reading data from Arduino. D) Raw data from Arduino
which displays raw information. E) Data array which represents
data after converting from string to array. F) Real-time chart and
measurement gauges (these two parts display simultaneously the
values of the data on the chart and measurement gauges). G) Stop
button to stop the processing and storing all the data as an excel
file on the system.
 S. Faal et al. / Measurement 148 (2019) 106936 3

Fig. 1. a) The developed e-nose system b) schematic of developed e-nose system.

Table 1
Specifications of the sensors utilized in the sensor chamber.

Sensor Detection range (PPM) Detect

TGS-2610 500–10000 High sensitivity to LP and its component gases
TGS-2620 500–5000 For toluene, alcohol, xylene, other volatile organic vapors
MQ-2 200–5000 Butane, Methane, LPG, smoke
MQ-3 0.05–10 Ethanol, Alcohol, smoke
MQ-4 200–10000 CNG Gas, Methane
MQ-5 200–10000 LPG, Natural gas
MQ-6 200–10000 butane gas, LPG
MQ-136 1–200 Hydrogen Sulfide gas

2.5. Signal preprocessing
The purpose of data preprocessing is to extract useful informa-
tion from the sensors responses and using them as input data for
pattern recognition analysis. The preprocessing technique usually
depends on the sensors type, three general stages can be identified:
baseline manipulation, normalization and compression [23].
2.5.1. Baseline manipulation
Three baseline manipulation methods are commonly used: dif-
ferential, relative, and fractional. In this study the fractional
method was chosen as the baseline manipulation because the out-
put of sensor responses (Ys (t)) became dimensionless and normal-
ized [23]. Eq. (1) represents the fractional method, in this equation
Xs (0) (sensors minimum responses when they exposed to dry air)
was subtracted from the Xs (t) (sensor responses while exposed
with honey headspace gases) and then the calculated value was
divided by the Xs (0).
xs ðtÞ
xs ð0Þ
ys ðtÞ ¼ ð1Þ
xs ð0Þ
2.5.2. Compression
The sensor-array response should be compressed down to a few
descriptors. In Parameter-extraction methods, two features of the
signal obtained from particular sensors were extracted: the maxi-
4 S. Faal et al. / Measurement 148 (2019) 106936

Fig. 2. a) GUI designed in LabVIEW b) diagram of the Code written in the LabVIEW.

mum value of response time for each sensor (MVRT) and the area
under the response time curve for each sensor (AURTC). Each mea-
surement was described by sixteen parameters (i.e., 8 sensors  2
parameters per sensor) and all the measurements repeated ten
time for each sample.
2.5.3. Normalization
Normalization operates across the entire database for a single
sensor, and are generally employed to compensate for differences
ðkÞ
in sensor scaling. It means it will denote by xs the response of sen-
sors to the k-th example in the database. After data normalization,
 S. Faal et al. / Measurement 148 (2019) 106936
the value for each individual sensor normalized between [0, 1]
ðkÞ
(ys ). This is simply done by subtracting the minimum and dividing
by the range of the sensor across the entire database (Eq. (2)) [23].
ðkÞ ðkÞ
xs
min8k ½xs 
yðkÞ
s ¼
h i
ðkÞ ðkÞ
max8k xs
min8k ½xs 
2.6. Prediction and classification using machine learning techniques
In this study, artificial neural network (ANN) and support vector
machine (SVM), was utilized for predicting the physicochemical
parameter of honey samples and finally, all the results were com-
pared to find the best classifier. For both SVM and ANN classifiers
10-fold cross-validation technique was performed to compare the
accuracy of the models.
2.6.1. Support vector machine (SVM)
In the SVM analysis, a hyper plane is designed and all the train-
ing vectors classify into different classes and the best result accurse
when the hyper plane has the maximum margin from each class
and least error. In machine learning, one of the known branches
of SVM is the kernel method that is a class of algorithms for pattern
recognition analysis [24]. In this study different types of kernels
have been used in SVM and compared with each other to recognize
which kernel is better for prediction physicochemical properties.
2.6.2. Artificial neuron network (ANN)
In this study two features: MVRP and AURTC were utilized for
the input layer neurons and they were used to predict the AC,
FA, MC and pH. In the hidden layer for choosing the most efficient
number of neurons, the training step started with one neuron and
was stopped at fifteenth neurons. According to the results, the low-
est root mean square error value (RMSE) was expressed the best
number of nodes in the hidden layer. All the SVM and ANN analysis
were performed using Weka version 3.9 software.
3. Results and discussion
3.1. Physicochemical parameters
The physicochemical parameters obtained from the experi-
ments are presented in Table 2. The pH is a significant factor that
affects the acidity, texture (since acidity can influence its stability).
pH of honey can be changed by the storage and harvesting condi-
tions and effects to the shelf-life of honey [25]. The limitation for
pH has not yet been discussed by any regulatory committees [7],
the results of pH analysis showed that the pH value was between
3.83 and 5.06 (mean value = 4.28). These values are similar with
the pH values (3.34–5.33) reported by Silva, Sousa and Taveira
[26].
Free acidity is one of the important compounds of honey and it’s
effected by the presence of lactone, inorganic ions, organic acids
and internal esters [7], although the climatic factors, harvesting
season and botanical origin effect on the physicochemical proper-
ties of honey, these can explain the difference in acidity between
different samples [27]. According to the Codex Alimentarius Com-
mission [28], the maximum value permitted for the acidity is
50 meq kg
1 and the results of free acidity measurement of all
honey samples ranged from 17.24 meq kg
1 to 35.78 meq kg
1
(mean value = 28.37) and according to the results all of the tested
honey samples had the lower value comparing to the permitted
level (50 meq kg
1). Similar results for honey free acidity were
reported by Silva, Sousa and Taveira [26].
5
Moisture content like other physicochemical properties is
related to botanical origin, climatic conditions and the season of
the year. In the summer season the climate of Bushehr (S2), Aba-
dan (S3), Ahvaz (S4) and Bandar Abbas (S5) are sultry and other
cities (Zahedan (S1), Iran Shahr (S6), Jahrom (S7), Jiroft (S8), Shiraz
ð2Þ
(S9) and Kerman (S10)) have warm-dry climate, according to the
results presented in Table 2 the moisture content has affected by
climate change and the moisture content of sultry cities are higher
than the cities with warm-dry climate. The values of moisture con-
tent analysis were between 15.68% and 21.3% (mean
value = 17.87), the obtained values are similar with those obtained
by [29] who found the range of moisture content between 16.6%
and 23.3% for thirty different honey samples. According to the
Codex Alimentarius Commission [28], the moisture content of
honey should be less than specific value (>21%) because of safety
and shelf-life of honey. By increasing the moisture content the
probability of yeast fermentation during the storage time
increases, therefore, the amount of acidity increases [26]. Accord-
ing to the moisture content results presented in Table 2 some sam-
ples (one sample in the group of S2, and three samples in the group
of S5) exceeded the limitation suggested by Codex Alimentarius
Commission [28].
It can be seen from the results of ash content, all the results are
within 0.07% and 0.29% (mean value = 0.182) that are lower than
the limit allowed for floral honey (0.6%), and indicate originality
of honey samples [30]. The similar values were reported by [26],
who found the range of 0.02–0.46% for the ash content.
Although the sugar content of honey samples measured with
HPLC experiment are presented in Table 2, the values of summa-
tion of glucose and fructose were between 70.55% and 79.13%
(mean value = 75.22) and the sucrose values were between 2.94%
and 5.14% (mean value = 4.20). The similar values were reported
by [31,32], who found the range of 29.80–65.50%, 25.93–35.98%
and 0.4–8.80% for fructose, glucose and sucrose respectively.
According to the Codex Alimentarius Commission the summation
of fructose and glucose should be above 65% and the sucrose values
should be below 5%, the minimum amount of fructose and glucose
content for honey samples was 70.55% that was in the standard
range but for the sucrose results there were some samples (three
samples in the group of S6) which exceeded the limitation sug-
gested by Codex Alimentarius Commission [28].
On the basic of the results discussed above it concluded to elim-
inate the samples which exceeded the limitation suggested by
Codex Alimentarius Commission [28], so the final dataset consisted
of 104 samples.
3.2. Honey aroma and its relationship with AC, FA, MC and PH
The relationships (Pearson correlation coefficients) between
honey aroma and AC, FA, MC and PH are presented in the Table 3.
In this case, two features MVRT and AURTC were analyzed. Accord-
ing to the results, all the sensors outputs showed significant corre-
lations between aroma and AC, FA, MC and pH except MQ-3 gas
sensor that showed no significant correlations between honey
aroma and MC and pH for MVRT feature and no significant corre-
lations between honey aroma and AC, MC and pH for AURTC fea-
ture. On the basis of the above results it can be concluded that in
the sensor array, the MQ-3 gas sensor considering the fabrication
cost and reduction in computational process time can be elimi-
nated from the sensor array in further researches.
3.3. Predicting physicochemical parameters by e-nose response
The main goal of this research was to demonstrate the applica-
bility of the developed e-nose system as a simple and non-
destructive tool for honey aroma measurement and prediction
6 S. Faal et al. / Measurement 148 (2019) 106936

Table 2
Results of physicochemical parameters of pure honey samples (mean ± standard deviation).

Sample Sucrose Glucose Fructose pH Moisture Free acidity (meq/kg) Ash

(g 100 g
1) (g 100 g
1) (g 100 g
1) (g 100 g
1) (g 100 g
1)
S1 (n = 12) Mean ± SD 3.98 ± 0.2 27.57 ± 1 48.84 ± 0.88 4.03 ± 0.1 16.57 ± 0.04 20.17 ± 0.53 0.12 ± 0.02
MIN 3.5 25.84 47.51 3.94 16.52 19.68 0.1
MAX 4.21 28.22 49.82 4.23 16.65 21.57 0.14
Samples exceeding limits – – – – – – –
S2 (n = 11) Mean ± SD 4.64 ± 0.23 27.31 ± 0.92 47.44 ± 0.81 4.47 ± 0.07 19.43 ± 0.52 33.83 ± 0.72 0.15 ± 0.01
MIN 4.23 25.49 45.44 4.38 19.38 32.99 0.12
MAX 4.72 28.15 48.39 4.63 21.09 35.18 0.18
Samples exceeding limits – – – – 1 – –
S3 (n = 11) Mean ± SD 4.53 ± 0.27 30.33 ± 0.8 44.54 ± 0.85 4.56 ± 0.09 19.49 ± 0.04 24.43 ± 0.79 0.14 ± 0.01
MIN 4.09 28.77 42.67 4.46 19.44 23.51 0.12
MAX 4.74 31.16 45.18 4.71 19.55 25.84 0.16
Samples exceeding limits – – – – – – –
S4 (n = 13) Mean ± SD 4.15 ± 0.26 24.9 ± 0.82 49.34 ± 0.7 4.71 ± 0.09 19.88 ± 0.05 30.87 ± 0.69 0.18 ± 0.01
MIN 3.82 22.95 47.51 4.63 19.86 29.97 0.15
MAX 4.22 25.87 49.58 4.9 19.98 31.91 0.21
Samples exceeding limits – – – – – – –
S5 (n = 12) Mean ± SD 3.61 ± 0.27 28.45 ± 0.9 45.34 ± 0.64 4.86 ± 0.09 20.07 ± 0.48 30.17 ± 0.83 0.21 ± 0.02
MIN 3.24 27.56 43.35 4.8 20.02 29.23 0.18
MAX 3.91 29.41 46.3 5.06 21.3 31.05 0.24
Samples exceeding limits – – – – 3 – –
S6 (n = 12) Mean ± SD 4.86 ± 0.21 33.5 ± 0.81 44.04 ± 1.05 3.95 ± 0.11 16.06 ± 0.05 33.2 ± 0.64 0.23 ± 0.02
MIN 4.54 32.43 42.91 3.97 16.02 32.36 0.21
MAX 5.14 34.46 44.93 4.13 16.15 34.7 0.26
Samples exceeding limits 3 – – – – – –
S7 (n = 10) Mean ± SD 3.84 ± 0.27 26.37 ± 0.89 46.18 ± 0.86 3.91 ± 0.07 17.67 ± 0.04 34.7 ± 0.82 0.26 ± 0.02
MIN 3.45 24.4 44.58 3.83 17.64 33.88 0.24
MAX 4.09 27.29 46.63 4.03 17.77 35.78 0.29
Samples exceeding limits – – – – – – –
S8 (n = 10) Mean ± SD 4.41 ± 0.28 33.28 ± 0.96 43.62 ± 0.92 4.13 ± 0.08 17.27 ± 0.05 26.9 ± 0.66 0.19 ± 0.02
MIN 3.96 31.57 41.76 4.08 17.23 26.07 0.16
MAX 4.68 34.19 43.74 4.27 17.37 28.12 0.21
Samples exceeding limits – – – – – – –
S9 (n = 11) Mean ± SD 3.35 ± 0.16 26.73 ± 0.93 50.8 ± 0.9 4.15 ± 0.1 15.73 ± 0.03 18.21 ± 0.72 0.1 ± 0.02
MIN 2.94 24.76 49.02 4.07 15.68 17.24 0.07
MAX 3.56 27.22 51.4 4.33 15.83 19.27 0.13
Samples exceeding limits – – – – – – –
S10 (n = 9) Mean ± SD 4.66 ± 0.1 28.04 ± 0.95 45.62 ± 0.98 4.02 ± 0.08 16.3 ± 0.06 31.23 ± 0.67 0.24 ± 0.03
MIN 4.16 26.67 44.24 3.95 16.28 30.26 0.21
MAX 4.79 28.96 45.94 4.2 16.4 31.92 0.27
Samples exceeding limits – – – – – – –
Total (n = 111)

the AC, FA, MC and pH based on the data obtained from the honey structure obtained by using the best results for predicting the
aroma. Accordingly, ANN and SVM machine learning techniques pH, AC, FA and MC features.
were used for Prediction and classification.

3.3.1. Artificial neural network results
In the input layer of the ANN analysis the preprocessed data
were utilized in order to predict the physicochemical parameters
of honey. In the hidden layer for choosing the most efficient num-
ber of neurons, the training step started with one neuron and was
stopped at fifteenth neurons, each training step was repeated ten
times and at the end the mean value was calculated. The results
of ANN structures using the MVRT and AURTC features as input
data for predicting the physicochemical parameters are presented
in Table 4. According to the results the hidden layer with 2, 7, 13
and 10 neurons utilizing MVRT feature and hidden layer with 10,
5, 2 and 6 neurons utilizing AURTC feature had the lowest RMSE
and highest accuracy with best performance for predicting the
AC, FA, MC and pH, respectively. Comparing the best result of both
features showed that prediction of the AC, FA, MC and pH utilizing
MVRT feature have lower RMSE and higher accuracy against the
AURTC feature and suggests better performance for predicting
the physicochemical parameters of honey, Fig. 3 shows the ANN
3.3.2. Support vector machine results
It is important to select the right kernel of SVM analysis which
enhances SVM’s performance for honey classification. In this study,
four common types of kernel functions were used including poly-
nomial, normalized polynomial, Pearson VII universal kernel
(PUK) and radial basis function (RBF) [33]. For analyzing the data
set each training set repeated ten times and the mean value was
calculated, the results of SVM analyzed with the different kernel
using the MVRT and AURTC features as input data for prediction
of the physicochemical parameters are presented in Table 5. The
results of SVM for MVRT feature reveals that the RBF function pre-
sents lowest RMSE (0.195 ± 0.06), and highest accuracy
(88.85 ± 0.73) for prediction of AC, also the PUK function compar-
ing to the other kernels offers the lowest RMSE (1.272 ± 0.4,
0.752 ± 0.28) and the highest accuracy (94.8 ± 1.02, 94.72 ± 0.94)
for predicting the FA and MC, respectively and the normalized
polynomial function presents the lowest RMSE (0.75 ± 0.15), and
the highest accuracy (94.2 ± 1.07) for predicting the PH.
 S. Faal et al. / Measurement 148 (2019) 106936 7

Table 3
The correlation between eight sensors and physicochemical parameters for different features.

The maximum value of response time for each sensor (MVRT)

pH MC FA AC MQ 6 MQ 2 MQ 3 MQ 5 MQ 136 MQ 4 TGS 2610 TGS 2620
pH 1 0.871**
0.956**
0.936** 0.765** 0.713** 0.169 0.865** 0.849** 0.825** 0.856** 0.864**
MC 0.871** 1
0.813**
0.804** 0.674** 0.635** 0.273 0.767** 0.755** 0.720** 0.748** 0.746**
FA
0.956**
0.813** 1 0.911**
0.802**
0.754**
0.528*
0.887**
0.878**
0.851**
0.884**
0.884**
AC
0.936**
0.804** 0.911** 1
0.693**
0.657**
0.381*
0.794**
0.781**
0.755**
0.781**
0.789**
MQ 6 0.765** 0.674**
0.802**
0.693** 1 0.963** 0.804** 0.864** 0.954** 0.850** 0.957** 0.853**
MQ 2 0.713** 0.635**
0.754**
0.657** 0.963** 1 0.814** 0.764** 0.923** 0.744** 0.883** 0.747**
MQ 3 0.169 0.273
0.528*
0.381* 0.804** 0.814** 1 0.511** 0.673** 0.491** 0.697** 0.533**
MQ 5 0.865** 0.767**
0.887**
0.794** 0.864** 0.764** 0.511** 1 0.940** 0.995** 0.958** 0.987**
MQ 136 0.849** 0.755**
0.878**
0.781** 0.954** 0.923** 0.673** 0.940** 1 0.925** 0.977** 0.935**
MQ 4 0.825** 0.720**
0.851**
0.755** 0.850** 0.744** 0.491** 0.995** 0.925** 1 0.943** 0.979**
TGS 2610 0.856** 0.748**
0.884**
0.781** 0.957** 0.883** 0.697** 0.958** 0.977** 0.943** 1 0.962**
TGS 2620 0.864** 0.746**
0.884**
0.789** 0.853** 0.747** 0.533** 0.987** 0.935** 0.979** 0.962** 1
The area under the response time curve (AURTC)
pH 1 0.87**
0.95**
0.93** 0.74** 0.60** 0.19 0.83** 0.80** 0.79** 0.82** 0.83**
MC 0.871** 1
0.813**
0.804** 0.633** 0.556** 0.04 0.729** 0.715** 0.677** 0.694** 0.717**
FA
0.956**
0.813** 1 0.911**
0.795**
0.666**
0.295*
0.880**
0.848**
0.839**
0.865**
0.870**
AC
0.936**
0.804** 0.911** 1
0.670**
0.562**
0.15
0.772**
0.740**
0.729**
0.748**
0.764**
MQ 6 0.749** 0.633**
0.795**
0.670** 1 0.903** 0.733** 0.834** 0.958** 0.802** 0.940** 0.870**
MQ 2 0.609** 0.556**
0.666**
0.562** 0.903** 1 0.796** 0.626** 0.913** 0.578** 0.760** 0.664**
MQ 3 0.19 0.04
0.295*
0.15 0.733** 0.796** 1 0.316* 0.615** 0.291* 0.519** 0.376**
MQ 5 0.839** 0.729**
0.880**
0.772** 0.834** 0.626** 0.316* 1 0.879** 0.995** 0.966** 0.991**
MQ 136 0.800** 0.715**
0.848**
0.740** 0.958** 0.913** 0.615** 0.879** 1 0.846** 0.940** 0.904**
MQ 4 0.795** 0.677**
0.839**
0.729** 0.802** 0.578** 0.291* 0.995** 0.846** 1 0.952** 0.983**
TGS 2610 0.822** 0.694**
0.865**
0.748** 0.940** 0.760** 0.519** 0.966** 0.940** 0.952** 1 0.980**
TGS 2620 0.831** 0.717**
0.870**
0.764** 0.870** 0.664** 0.376** 0.991** 0.904** 0.983** 0.980** 1

*Correlation is significant at the 0.05 level (2-tailed).

**Correlation is significant at the 0.01 level (2-tailed).

Table 4
Results of ANN analysis of different number of nodes in the hidden layer (NHL) for predicting the different physicochemical parameters of honey (mean ± standard deviation).

NHL RMSE R (%)

pH MC FA AC pH MC FA AC
MVRT feature
1 0.535 ± 0.13 0.736 ± 0.06 1.372 ± 0.3 0.194 ± 0.07 96.12 ± 1.35 94.83 ± 1.36 95.64 ± 0.92 87.24 ± 1.36
2 0.461 ± 0.13 0.593 ± 0.11 1.184 ± 0.36 0.144 ± 0.06 96.26 ± 1.03 95.63 ± 1.18 95.72 ± 0.73 91.57 ± 1.41
3 0.438 ± 0.08 0.613 ± 0.08 1.493 ± 0.27 0.155 ± 0.05 96.36 ± 0.97 95.46 ± 1.48 95.84 ± 0.96 90.76 ± 1.41
4 0.411 ± 0.13 0.595 ± 0.12 1.157 ± 0.36 0.147 ± 0.05 96.5 ± 0.88 95.49 ± 1.27 95.75 ± 0.54 91.43 ± 1.68
5 0.4 ± 0.15 0.477 ± 0.1 1.112 ± 0.21 0.152 ± 0.06 96.42 ± 1.2 96.09 ± 1.17 95.82 ± 0.94 91.08 ± 1.66
6 0.436 ± 0.1 0.459 ± 0.1 1.163 ± 0.27 0.165 ± 0.04 96.29 ± 1.24 96.06 ± 1.3 95.75 ± 0.63 89.88 ± 1.17
7 0.405 ± 0.06 0.467 ± 0.09 1.099 ± 0.3 0.147 ± 0.07 96.39 ± 1.13 96.05 ± 1.56 95.85 ± 1.08 91.42 ± 1.5
8 0.397 ± 0.11 0.457 ± 0.13 1.101 ± 0.25 0.149 ± 0.06 96.46 ± 0.96 96.07 ± 1.19 94.91 ± 0.67 91.24 ± 1.71
9 0.413 ± 0.13 0.445 ± 0.12 1.109 ± 0.31 0.151 ± 0.06 96.45 ± 1.47 96.21 ± 0.98 94.86 ± 0.86 91.1 ± 1.78
10 0.389 ± 0.08 0.448 ± 0.13 1.174 ± 0.28 0.147 ± 0.06 96.64 ± 1.06 95.26 ± 0.79 95.75 ± 0.7 91.44 ± 1.02
11 0.399 ± 0.08 0.465 ± 0.11 1.129 ± 0.3 0.156 ± 0.06 96.54 ± 1.24 96.14 ± 1.27 95.65 ± 0.66 90.75 ± 1.47
12 0.423 ± 0.09 0.508 ± 0.13 1.187 ± 0.32 0.147 ± 0.04 96.48 ± 1.01 96.1 ± 1.2 95.75 ± 0.93 91.43 ± 1.39
13 0.403 ± 0.14 0.434 ± 0.15 1.117 ± 0.31 0.163 ± 0.05 96.47 ± 0.94 96.26 ± 0.94 95.35 ± 0.84 90.07 ± 1.15
14 0.406 ± 0.14 0.457 ± 0.11 1.134 ± 0.35 0.166 ± 0.06 96.56 ± 1.19 96.11 ± 1.09 95.82 ± 0.7 89.9 ± 1.64
15 0.405 ± 0.11 0.474 ± 0.14 1.159 ± 0.21 0.146 ± 0.07 96.48 ± 1.29 96.07 ± 1.27 95.83 ± 0.85 91.46 ± 1.66
AURTC feature
1 0.496 ± 0.2 0.713 ± 0.15 2.668 ± 0.37 0.242 ± 0.05 93.73 ± 0.97 93.75 ± 1.01 93.61 ± 1.2 85.74 ± 1.94
2 0.515 ± 0.17 0.549 ± 0.18 1.63 ± 0.46 0.195 ± 0.08 93.62 ± 0.88 94.08 ± 0.48 94.35 ± 1.02 88.53 ± 2.48
3 0.477 ± 0.22 0.571 ± 0.21 2.015 ± 0.37 0.169 ± 0.07 93.82 ± 1.13 93.99 ± 0.72 94.55 ± 0.82 90.42 ± 1.75
4 0.483 ± 0.15 0.634 ± 0.14 1.784 ± 0.35 0.194 ± 0.05 93.8 ± 0.92 93.91 ± 0.82 94.61 ± 1.13 89.27 ± 2.08
5 0.479 ± 0.16 0.554 ± 0.21 1.477 ± 0.53 0.202 ± 0.08 92.83 ± 1.06 93.08 ± 0.93 94.72 ± 1.19 88.87 ± 1.9
6 0.476 ± 0.13 0.684 ± 0.22 1.532 ± 0.35 0.203 ± 0.04 93.83 ± 1.15 93.57 ± 1 94.67 ± 1.03 88.82 ± 1.86
7 0.515 ± 0.15 0.734 ± 0.18 1.669 ± 0.33 0.206 ± 0.06 93.63 ± 1.09 93.55 ± 0.83 94.66 ± 1.08 88.66 ± 1.9
8 0.48 ± 0.19 0.556 ± 0.17 1.604 ± 0.37 0.204 ± 0.05 93.81 ± 0.67 94.06 ± 0.93 94.68 ± 0.86 89.4 ± 1.91
9 0.496 ± 0.21 0.602 ± 0.23 1.574 ± 0.44 0.174 ± 0.06 93.72 ± 0.98 93.86 ± 0.63 94.12 ± 0.9 90.94 ± 2.02
10 0.552 ± 0.12 0.787 ± 0.17 1.635 ± 0.41 0.166 ± 0.06 93.45 ± 1.07 93.28 ± 0.87 94.67 ± 0.89 91.1 ± 2.14
11 0.521 ± 0.18 0.713 ± 0.22 1.54 ± 0.43 0.172 ± 0.06 93.59 ± 0.77 93.52 ± 1.04 94.71 ± 1.04 90.64 ± 2.08
12 0.522 ± 0.18 0.674 ± 0.18 1.745 ± 0.27 0.178 ± 0.07 93.58 ± 1.26 93.77 ± 0.98 94.68 ± 1.11 89.52 ± 2.14
13 0.496 ± 0.15 0.617 ± 0.19 1.625 ± 0.36 0.171 ± 0.06 93.72 ± 0.71 93.91 ± 1.01 94.7 ± 1.06 90.92 ± 1.88
14 0.481 ± 0.18 0.581 ± 0.2 1.669 ± 0.51 0.179 ± 0.06 93.8 ± 0.98 93.99 ± 0.77 94.7 ± 1.29 90.88 ± 1.48
15 0.499 ± 0.23 0.627 ± 0.19 1.842 ± 0.27 0.181 ± 0.06 93.71 ± 0.92 93.78 ± 0.48 94.66 ± 1.05 90.45 ± 1.67
8 S. Faal et al. / Measurement 148 (2019) 106936

Fig. 3. The ANN structure obtained by using the best results for predicting the pH, AC, FA and MC features.

Table 5
Results of SVM analysis with different kernel functions for predicting the physicochemical parameters of honey (mean ± standard deviation).

Kernel Parameter-extraction methods

MVRT feature AURTC feature
pH MC FA AC pH MC FA AC
Polynomial R (%) 93.03 ± 1.13 90.1 ± 1.17 93.67 ± 1.66 87.28 ± 1.27 91.94 ± 1.29 87.09 ± 1.35 91.34 ± 1.27 86.87 ± 1.33
RMSE 0.971 ± 0.18 1.265 ± 0.21 2.152 ± 0.49 0.238 ± 0.05 0.88 ± 0.24 1.376 ± 0.31 2.249 ± 0.22 0.228 ± 0.04
Normalized polynomial R (%) 94.2 ± 1.07 93.71 ± 0.82 94.29 ± 1.09 86.41 ± 0.68 92.99 ± 0.9 88.82 ± 0.81 92.06 ± 1.14 87.66 ± 1.34
RMSE 0.75 ± 0.15 0.928 ± 0.24 1.849 ± 0.44 0.242 ± 0.07 0.714 ± 0.18 1.209 ± 0.29 2.149 ± 0.26 0.215 ± 0.07
RBF R (%) 90.99 ± 0.56 82.15 ± 0.76 92.46 ± 0.66 88.85 ± 0.73 90.7 ± 0.8 81.71 ± 0.78 90.15 ± 0.69 88.04 ± 0.59
RMSE 1.111 ± 0.19 2.02 ± 0.21 2.664 ± 0.39 0.195 ± 0.06 1.056 ± 0.18 2.024 ± 0.32 2.763 ± 0.37 0.2 ± 0.06
PUK R (%) 94 ± 0.98 94.72 ± 0.94 94.8 ± 1.02 87.7 ± 0.87 92.42 ± 0.96 92.52 ± 1.18 93.05 ± 1.21 87.21 ± 1.34
RMSE 0.811 ± 0.19 0.752 ± 0.28 1.272 ± 0.4 0.226 ± 0.05 0.789 ± 0.16 0.881 ± 0.23 1.92 ± 0.28 0.215 ± 0.05

For the AURTC feature, kernels have the same treatment as
MVRT feature. In the AURTC feature, the RBF function showed
the lowest RMSE (0.2 ± 0.06) and highest accuracy (88.04 ± 0.59)
for predicting the AC, but for FA and MC prediction, the PUK func-
tion has better results, the lowest RMSE (1.920 ± 0.28, 0.881 ± 0.23)
and highest accuracy (93.05 ± 1.21, 92.52 ± 1.18), respectively. For
pH prediction, the Normalized polynomial kernel offers lower
RMSE (0.714 ± 0.18) and higher accuracy (92.99 ± 0.9) in compar-
ison with other kernels. In the previous study Huang, Liu, Zhang
and Wu [34] have investigated the application of electronic nose
with multivariate analysis for botanical origin identification and
quality determination of honey. They have concluded that the
quality of honey can be predicted with high accuracy utilizing
the SVM method.
3.3.3. Comparing SVM and ANN results
Both SVM and ANN classifiers offer good accuracy for predicting
the physicochemical parameters of honey utilizing both MVRT and
AURTC features, but in comparison of both classifier the ANN clas-
sifier using the MVRT feature as input data has lower RMSE
(0.144 ± 0.06, 1.099 ± 0.3, 0.434 ± 0.15 and 0.389 ± 0.08) and higher
accuracy (91.57 ± 1.41, 95.85 ± 1.08, 96.26 ± 0.94 and 96.64 ± 1.06)
for prediction of AC, FA, MC and pH attributes, respectively. For the
ANN analysis utilizing the MVRT feature, the correlations between
the predicted and experimental AC, FA, MC and pH values for the
test sets are shown in Fig. 4. As seen in the figure the prediction
of the AC, FA, MC and pH values of honey samples utilizing the data
extracted from developed e-nose (MVRT feature) have reasonable
R2 value (0.838, 0.918, 0.926 and 0.933), respectively. The results
showed the effectiveness of the ANN model for honey properties
measurement. Previous studies have shown the efficiency of
chemo metric methods for fruit properties measurement utilizing
the e-nose. Zhang, Wang, Ye and Chang [35] have investigated
the potential of using an e-nose for predicting the quality proper-
ties of peach. They reported that the partial least-squares regres-
sions and principal component regression models show excellent
ability in describing the quality indices of the peaches also the
results demonstrate that the e-nose has the potential for measur-
ing fruit quality properties. Similar results were obtained by Su,
Zhang, Ye, Chen, Guo, Gu and Shen [36] for predicting the quality
properties of pulp by an electronic nose. They reported that the
e-nose utilizing the discriminant factor analysis is capable to pre-
 S. Faal et al. / Measurement 148 (2019) 106936
Fig. 4. Correlation between the measured and predicted physicochemical parameters of honey for ANN analysis using the MVRT feature (test mode).
dict the quality properties of pulp. Our study results were showed
that the developed e-nose is a reliable device for predicting the
honey ash content, free acidity, moisture content and pH as a fast,
cheap and non-destructive instrument that can be handled by any-
one and has the advantage of eliminating the need for specialist
operators in comparison with the other traditional methods.
4. Conclusion
This study was carried out to investigate the capabilities of an e-
nose for non-destructive prediction of physicochemical properties
of honey. Two aroma features of each sensor including the maxi-
mum value of response time for each sensor (MVRT) and the area
under the response time curve (AURTC) were extracted and after
preprocessing were utilized for prediction of ash content (AC), free
acidity (FA), moisture content (MC) and pH. The results showed
that the developed e-nose can be a reliable technic for predicting
the physicochemical parameters of honey. The best result for pre-
dicting the AC, FA, MC and pH was found for the artificial neural
network method applied to the MVRT feature data. The results
demonstrated that the developed e-nose linked with the artificial
neural network was able to predict AC, FA, MC and pH with high
regression coefficients. The results demonstrate that the developed
e-nose has the potential for assessing other food products such as
rosewater, saffron and other volatile products that their quality is
associated with their aroma.
Acknowledgements
This research was jointly supported by the scholarship from Shiraz
University. Funding for HPLC analysis was provided by the Depart-
ment of Food Science and Technology of Shiraz University.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared to
influence the work reported in this paper.
9
Appendix A. Supplementary data
Supplementary data to this article can be found online at
https://doi.org/10.1016/j.measurement.2019.106936.
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