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Ultrasonic Assessment of Olive Oil Mixtures

Properties

Besma Alouache, Tarek Boutkedjirt Didier Laux


Physics of Ultrasoud Research Team, Physics of Materials University of Montpellier, IES, UMR 5214, F-34000
Laboratory, Faculty of Physics, University of Sciences and CNRS, IES, UMR 5214, F-34000 Montpellier, France
Technology Houari Boumediene, U.S.T.H.B., BP32 El- 860 Rue Saint Priest. 34095 Montpellier
Alia, DZ-16111 Algiers, Algeria

Abstract Mainly produced in the Mediterranean countries, acoustic impedance from velocity measurements by an
olive oil excels by its nutritional and medicinal benefits. However, ultrasonic multifrequency interferometer. The determination of
olive oil available in the market is not always authentic. It can be the ultrasonic attenuation coefficient in oil can also be
altered by inadequate storage conditions or if it is mixed to other considered. For this, Benedito et al. [8] have used both velocity
kinds of oils. The objective of this work is to use ultrasonic and attenuation to characterize frying oil degradation. Gradwell
methods for a possible quick detection of olive oil adulteration et al. [9] have correlated them to rheological properties of
from the characterization of its ultrasonic properties. In this many edible oils.
context, ultrasonic longitudinal propagation velocity and
attenuation were measured for pure olive oil and for its mixtures The aim of this work is the characterization of olive and
with soya oil at different proportions, at 20 C and using a 5 MHz soya oils and their mixtures in order to determine in which
ultrasonic transducer. Then, the longitudinal viscosity of the extend ultrasonic waves can be used to control the olive oil
different oil samples has been deduced on the whole bandwidth adulteration with soybean oil.
of the transducer (3-7 MHz) thanks to frequential analysis of the
rough data. Thanks to the measurement of the shear viscosity
with a Couette viscosimeter, we also deduced the bulk viscosity. II. MATERIALS AND METHODS
Propagation velocity starts from 1458 m.s-1 for pure olive oil and Olive and soya oils were acquired from a local retailer and
increases with percentage of soya oil in the mixture up to 1464 used without treatment. The characterizations are performed
m.s-1. The corresponding longitudinal viscosity decreases with on olive oil and mixtures of soya oil in different weight
percentage of soya oil from 161.4 mPa.s, for pure olive oil, to
proportions: 0%, 10%, 20%, 30%, 40%, 50%, 60%, 80%, and
136.7 mPa.s, for pure Soya oil. As a function of frequency,
longitudinal and bulk viscosities decrease, for all proportions of
100%.
soya oil, indicating that ultrasonic relaxation may take place. A. Viscosity Measurement
Thanks to the high level of accuracy of the method proposed in
this communication, the results show the ability of ultrasonic The shear viscosity measurements were performed with a
methods to be an efficient tool, which allows distinguishing Physica MCR301 rotational rheometer (Anton Paar France,
mixtures of oils and thus detecting adulterated olive oil. Courtaboeuf, France) with a Couette type flow measuring cell
(Ref. DG27 / T2000 / SS). This rheometer was equipped with a
Keywords Olive oil, Quality control, Ultrasonic velocity, sample temperature control system (Pt100 sensor). The tests
Ultrasonic attenuation, Longitudinal viscosity. were carried out at (20.0 0.1) C.

I. INTRODUCTION B. Ultrasonic measurements


Ultrasound is a noninvasive technique that, in addition to its The ultrasonic measurements were carried out by a pulse
applications in non-destructive testing (NDT) of materials and echo method. The experimental device (Fig.1) comprises a
in medical applications, has recently been used in food Panametrics plane sensor with a central frequency of 5 MHz.
industry. Its bandwidth ranges from 3 to 7 MHz. The sensor was excited
with a Panametrics 5800 pulse generator. All displacements
In literature, many applications of this technique can be were achieved with a Microcontrol stepper motor, with an
found for different types of food products, ranging from liquids accuracy of 1 m. The obtained echoes were displayed on a
to solids [1,2]. As complementary to classical physico- Lecroy LT374M oscilloscope. The entire system (sample -
chemical analysis methods [3], ultrasound can also be applied container - motor-transducer) was placed in a Binder KB 53
to solve some problems found in the oil related industries. To chamber, to ensure good temperature control (20.0 0.1) C.
this respect, this technique was used for the determination of
solid fat content in solidifying fat oils [4] and of the oil content The measuring principle of the propagation velocity and
in a homogeneous solution of crude palm oil and hexane [5] ultrasonic attenuation coefficient consists in placing the
and to determine the ultrasonic properties of palm oil and other ultrasound sensor at an initial distance z0 (along the vertical
vegetable oils [6]. Mahammad and Basharath [7] calculated the axis) from the bottom of the sample holder containing the oils

978-1-4673-9897-8/16/$31.00 2016 IEEE 2016 IEEE International Ultrasonics Symposium Proceedings


mixture. This distance is progressively reduced by using the with VL and L the longitudinal propagation velocity and
stepping motor. At each position, the ultrasonic echo reflected attenuation respectively.In this expression is the mass
from the bottom of the container is acquired by using a density.
Labview Software after its propagation in oil. As the wave path
is gradually reduced, the time required for its propagation in The detailed calculation of this expression is given in [13].
the oil is also reduced. In addition, the amplitude of the For Newtonian fluids, the longitudinal viscosity can also be
acquired echo at each position increases during the experiment. written as:
The direct processing of data, allowed us to calculate the (2)
propagation velocity in (m/s) and the attenuation coefficient in
(dB/m) at the nominal frequency of the transducer, f0. This was with S the shear viscosity and B the bulk viscosity.
done by plotting the evolution of the time of flight and
20. versus the displacement z (A is the signal This implies that:
amplitude).
(3)
The calculation of the Fast Fourier Transform (FFT) for
each acquired echo (for frequencies of the sensor bandwidth) The bulk viscosity is related to S by a factor K, as:
allows us to determine the phase velocity and the attenuation (4)
coefficient. The amplitude 'A (f )' of the FFT of the signal has
been used to deduce the attenuation coefficient from the curve
20.Log (A (f )) as a function of the displacement z. The slope is III. EXPERIMENTAL RESULTS
equal to -2 (f ), with (f ) the attenuation coefficient in dB/m. Figure (2) illustrates the variation of the propagation
In addition, the slope of the curve of the phase divided by 2f, velocity measured for the different oil samples on the whole
versus z is equal to 2/c (f ) with c (f ) the phase velocity (m/s). bandwidth of the transducer, without FFT treatment, according
the percentage of soya oil in olive oil. This curve shows an
The ultrasound attenuation is a phenomenon caused by
increase in the propagation velocity with the percentage of the
many factors such as losses due to viscosity and thermal
soya oil.
conductivity, the effect of the diffraction due to the dimensions
of the transducers and eventually scattering by any small The evolution of the phase velocity for different
particles in suspension [10][11][12]. In our case, the losses due frequencies (in the frequency range around 5 MHz) for the
to thermal conductivity are negligible and those due to different oil samples is shown in Figures (3). The curves in this
scattering by small particles are null. Furthermore, as oil figure show a linear increase of this parameter for the chosen
viscosities are high, diffraction losses can also be neglected. frequencies, with the percentage of the added soya oil.
Regarding these figures it is clear that for velocity analysis, as
The accuracy of the viscosity measurements using the
no FFT treatment is needed, a simpler signal processing is
viscometer described in II.A is about 3%. The ultrasonic
suffucient.
velocity measurements were made with an accuracy of 0.5 m/s.
1465
1464 y = 0.0634x + 1457.6
1463
1462
V (m/s)

1461
1460
1459
1458
1457
1456
0 20 40 60 80 100 120
Soya Oil Percentage

Fig. 2. Ultrasonic propagation velocity according to the percentage of added


soya oil in olive oil (whole bandwidth).
Fig. 1. Schematic diagram of the experimental set-up.

From the classical thermo-viscous model [13, 14, 15], the


longitudinal viscosity related to ultrasonic waves propagation
can be written as:

(1)
The variation of the shear viscosity measured with the
1465 viscometer described in II.A, depending on the percentage of
1464 soybean oil mixed with olive oil, is shown in Fig. 6. The high
1463 value of the olive oil viscosity is probably due to the strong
1462 interaction between its triglycerides. The low viscosity of the
Vph (m/s)

1461
soya oil could be due to the fact that it contains little
triglycerides compared to olive oil.
1460
1459 Figure (7) illustrates the variation of the longitudinal
1458
3 MHz 5 MHz 6.7 MHz viscosity versus the percentage of soya oil, calculated from the
attenuation coefficient and the measured phase velocity (Eq. 4).
1457
0% 20% 40% 60% 80% 100% 120%
The trend is decreasing. This figure shows the sensitivity of
Soya Oil percentage
this parameter to the addition of Soya oil.
The evolution of the Bulk viscosity, calculated from the
equation (6), is shown in Fig. 8. The K factor deduced from
Fig. 3. Phase velocity versus the percentage of added soybean oil in olive oil (at equation (7) is given by the figure (9).
different frequencies in the bandwidth of the 5 MHz transducer).
0.085
The curve giving the attenuation coefficient (on the whole 0.08
bandwidth) is illustrated in Fig. 4. It shows a quasilinear
decrease according to the percentage of added soya oil. The 0.075
attenuation coefficient increases by 30 Np/m, when the

S (Pa,s)
0.07
frequency varies from 3 to 7 MHz (Fig. 5).
0.065

35 0.06
33 0.055
31
29 0.05
y = -0.0592x + 28.835 0 10 20 30 40 50 60 70 80 90 100 110
(Np/m)

27
Soya oil percentage
25
23
Fig. 6. Shear Viscosity as a function of percentage of added soya oil in olive
21
oil.
19
17
15
0.245
0 20 40 60 80 100 120
Soya oil percentage 0.225
0.205
0.185
3 MHz
L (Pa.s)

Fig. 4. Ultrasonic attenuation coefficient according to the percentage of the


added soya oil in olive oil (whole bandwidth). 0.165
0.145 5 MHz
0.125
0.105
50 7 MHz
0.085
45
y = -0.0932x + 42.925 0 10 20 30 40 50 60 70 80 90 100 110
40
7 MHz Soya oil percentage
35
(Np/m)

30
Fig. 7. Longitudinal viscosity as a function of the percentage of added soya oil
25 5MHz
in olive oil (at different frequencies in the bandwidth of the 5 MHz
20
y = -0.0503x + 27.422 transducer).
15 3 MHz
10
5
y = -0.0328x + 14.028
0
0 20 40 60 80 100 120
Soya oil percentage

Fig. 5. Ultrasonic attenuation coefficient according to the percentage of added


soya oil in olive oil (at different frequencies in the bandwidth of a 5 MHz
transducer).
0.16
amount increase. The K factor is constant for all Soya oil
percentage in olive oil.
0.14
0.12 This ultrasonic method is sensitive since it can identify the
0.1
3 MHz mixtures with a content of 10% soya oil. This method allowed
B (Pa.s)

0.08
us to determine some mechanical properties of our oils.
0.06 5 MHz These results show the ability of ultrasound methods to
0.04 characterize olive oil and to detect its possible adulteration by
0.02
soya oil. Furthermore, they show that these methods may be a
7 MHz non-invasive, useful tool in addition to classical physico-
0
0 10 20 30 40 50 60 70 80 90 100 110
chemical analysis used in the quality control of food oils.
Soya oil percentage Works are now going on to enlarge the frequency range in
order to see if the sensitivity is better for high frequencies (for
Fig. 8. Volume viscosity according to the percentage of added soya oil in olive instance 20 MHz transducer).
oil (at different frequencies in the bandwidth of the 5 MHz transducer).

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