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Optical Fiber Technology 47 (2019) 15–20

Contents lists available at ScienceDirect

Optical Fiber Technology


journal homepage: www.elsevier.com/locate/yofte

U-bent plastic optical fiber probes as refractive index based fat sensor for T
milk quality monitoring

Gowri Annasamy, Allwyn S. Rajamani, Ramakrishna Bandaru, Sai V.V.R.
Biomedical Engineering Group, Department of Applied Mechanics, Indian Institute of Technology Madras, Chennai 600 036, India

A R T I C LE I N FO A B S T R A C T

Keywords: Milk fat content is an important parameter for milk quality assessment in the dairy industry. This study reports
U-bent plastic optical fiber probe the development of a hand-held, highly sensitive fiber optic milk fat sensor using U-bent plastic optical fiber
Fiber optic sensor (POF) probes based on the refractive index (RI) of milk, an inherent physicochemical property of milk, which is
Evanescent wave absorbance significantly influenced by the milk fat content. The U-bent POF sensor probes facilitate dip type sensing and
Refractive Index
offer non-destructive assessment of milk quality in real-time. The sensor works on the principle of intensity
Milk fat
modulation technique by exploiting evanescent wave absorbance and refractive losses. The fiber optic probes
sense a change in RI of the medium as a result of attenuated total reflection by virtue of the evanescent wave
interactions of light at the fiber core/cladding interface with the surrounding medium. A relative change in the
refractive index property of milk as a result of variation in fat content and addition of water is investigated using
U-bent POF probes for milk quality assessment. The sensor shows an optical absorbance sensitivity of 0.15 ΔA/
Δ% fat for the variation of fat content in the milk. Besides, the response of the sensor to water addition in wide
concentration range was studied. Furthermore, a low cost portable optoelectronic device is reported for in-
stantaneous milk quality monitoring in farm fields. This sensor could be of huge potential in dairy industries,
milk collection centers as well as end-user applications for real-time milk quality monitoring.

1. Introduction desirable for process control in dairy industry. However, the Gerber
method, well established and widely used for quantification of milk fat,
Recently, the quality of milk has become a major concern, which led is laborious and involves use of hazardous chemicals leading to wastage
to a huge demand for a rapid, environment friendly, cost-effective and of milk. In most of the dairy collection centers, electronic milk tester
field-deployable handheld device for milk quality assessment [1–3]. In and lactometer are utilized for measuring fat content and corrected
addition, the inability to meet the growing demands for milk has led to lactometer reading to evaluate milk quality. However, these techniques
the severe problem of milk adulteration at least in the developing require large sample volume and do not facilitate online monitoring
countries which requires the use of sophisticated spectroscopic tech- and are limited by their efficiency and subjectivity in measurements.
niques for specific detection of adulterants in milk [4–8]. Although, the Recently, the biophysical properties of milk such as electrical im-
milk composition could be identified from the molecular absorption pedance and pH have been exploited for milk quality monitoring [16].
bands using spectroscopic technique, the abovementioned techniques Refractive index and optical extinction (absorption and scattering)
require expensive instrumentation and lengthy procedures which make properties of milk have also been extensively studied for evaluation of
them impractical for applications at point of sale/use. As an alternative, milk fat percentage and chemical composition [17,18]. Refractive index
a few low-cost milk testing kits for specific detection of multiple adul- (RI) property of milk as a measure for its quality monitoring has several
terants have been explored and commercialized [9–12]. advantages including non-destructive evaluation by optical phe-
The key parameters considered for evaluating the quality of milk are nomena, low interference from bulk solution and possibility for online
fat, solid not fat percentage, protein content and appearance. Among monitoring. Fiber optic RI sensors have been explored as an alternative
these parameters, milk fat is responsible for the properties and sensory to the conventional prism based refractometers, mainly due to higher RI
attributes of milk and other dairy products [13,14]. The complex re- sensitivity, simpler instrumentation, wide operating range, remote
fractive index value of the milk is known to vary with its fat content monitoring and multiplexing [19]. A variety of fiber optic sensors based
[15]. Ability to monitor the milk fat content in real-time is highly on evanescent wave absorbance with simple decladded and


Corresponding author.
E-mail address: vvrsai@iitm.ac.in (V.V.R. Sai).

https://doi.org/10.1016/j.yofte.2018.11.019
Received 19 September 2018; Received in revised form 5 November 2018; Accepted 9 November 2018
1068-5200/ © 2018 Elsevier Inc. All rights reserved.
A. Gowri et al. Optical Fiber Technology 47 (2019) 15–20

geometrically modified fiber core [20] have been reported to achieve 2.3. Milk sample preparation
an enhanced RI sensitivity, in addition to use of specialty fibers and
microfabricated waveguides such as microstructured optical fibers Commercial packaged pasteurized milk including toned, standar-
(MOFs) [21], fiber bragg gratings (FBGs) [22], cladding stripped fiber dized and full cream (with 3%, 4.5% and 6% of fat respectively) and
tapers [23] and ring resonators [24]. Over the past decade, plastic fresh unpasteurized cow and buffalo milk were selected in this study.
optical fiber (POF) based RI sensors have been widely explored due to The fat and SNF values of fresh and packaged milk samples were
several advantages including low-cost, less fragility and robustness, quantified using standard gravimetric and Werner Schmidt methods
ease in handling and optical coupling. POF can be easily decladded and [28]. In this method, Conc. HCl is used to digest milk proteins and
modified into various geometries including U-shape or coiled as re- released fat is extracted using ethers. The residue left behind after
ported in our earlier studies [25]. These sensor geometries enable im- evaporation of ether is weighed to determine the milk fat content. The
proved light-matter interactions at the fiber core-medium interface by influence of water addition to milk on the response of the probes was
virtue of evanescent wave phenomenon, thereby allowing development carried out by adding known quantities of water to standardized milk
of intensity-modulated RI sensors. Recently, coiled POF probes samples. All experiments were carried out at room temperature and
(2–3 mm fiber diameter) have been exploited for detection of pre- utilized DI water as reference.
servatives in milk based on RI changes [26].
Here, we present a compact, dip-type U-bent plastic optical fiber 2.4. Experimental set-up
sensor with high refractive index sensitivity for milk fat sensing. U-bent
fiber geometry is chosen in this study mainly due to enhanced sensi- The optical set-up consists of the U-bent POF probe with either of its
tivity because of improved evanescent wave interactions and ergonomic distal ends connected to a halogen light source and a fiber optic spec-
design compared to other fiber geometries [27]. Our previous study trometer (HL2000 and USB4000-XR1-ES respectively, Ocean Optics
shows optimal design of U-bent POF probes for development of highly Inc., USA) with the help of bare fiber adaptors and SMA connectors
sensitive RI sensors [25]. In this study, U-bent probes with fiber and (BFT1 and B10510A respectively, Thorlabs Inc., USA) as shown in
bend diameters of 0.5 mm and 1.5 mm respectively are subjected to Fig. 1B. The U-bent POF sensor response to various milk samples was
commercial milk samples of varying fat content (toned, standardized recorded using SpectraSuite software. For each spectral recording, 100
and full cream) to realize a sensitive real-time milk fat sensor. In ad- spectra were averaged to achieve better signal to noise ratio. Reference
dition to milk fat sensing, the application of these probes for milk spectrum was taken while the decladded sensing portion of the U-bent
quality monitoring is investigated by testing the response of the probes probes was dipped in DI water, before subjecting the probes to various
subjected to milk samples diluted with different percentages of water, a milk samples (100 µL in a PCR tube) to record the respective absor-
common adulterant added to milk in a day-to-day life. Further, a bance spectra in real time. All the experiments were done in triplicate.
handheld optoelectronic device suitable for field applications is devel-
oped in-house and tested with fresh unpasteurized and various com- 3. Results and discussion
mercial packaged milk samples. This highly sensitive fiber optic sensor
for milk fat sensing could offer several advantages including rapid re- 3.1. Characterization of milk samples using standard technique
sponse with real-time monitoring ability, minimum sample volume
down to 100 µL and non-destructive analysis. The milk fat percentage and RI of the milk samples used in this
study are evaluated using standard Werner Schmidt technique and re-
2. Materials and methods fractometer. Fig. 2A shows the milk fat content estimation in which
there is an increasing trend observed for milk samples with increase in
2.1. Materials and reagents fat percentage. However, the huge standard deviation could be attrib-
uted to the manual intervention in handling the samples. Fig. 2B shows
The plastic optical fiber (SK20) was procured from Mitsubishi the increasing trend in the RI of the samples with an increase in milk fat
Rayon Pvt. Ltd., Japan. Ethyl acetate was purchased from Merck. Fresh content. This is in correlation with the reported literature stating the
cow and buffalo milk obtained from local farms and packaged milk with influence of fat content on the RI changes of the milk [13].
different fat percentages (toned (T) - 3%, standardized (S) - 4.5% and
full cream (FC) - 6%) sold under different brands obtained from local 3.2. U-bent fiber probes as milk fat sensors
ISO certified milk centers. LED and photodetector (PD) were purchased
from Digikey Electronics. Fat percentage is one of the important parameters for the milk
quality assessment [13]. The complex refractive index value of the milk
2.2. U-bent POF probe design is known to vary with its fat content. Ability to monitor the milk fat
content in real-time is highly desirable for process control in dairy in-
The plastic optical fiber consists of polymethylmethacrylate dustry. Here, experiments were carried out to investigate the ability of
(PMMA) core and fluorinated polymer cladding with refractive indices the U-bent POF probes to distinguish milk samples with different fat
of 1.49 and 1.41 respectively. The POF of 0.5 mm diameter was bent content. Commercial packaged milk samples with different fat percen-
into U-shape by means of glass capillary technique as discussed in our tages (toned, standardized and full cream) were considered for this
earlier studies [25]. Briefly, a 20 cm long POF was bent to bring the two study. The absorbance response from the probe in presence of the milk
ends close to each other and pushed into a glass capillary having inner samples with respect to DI water as reference was recorded. The ab-
diameter of 2 mm such that the bend portion of the fiber is within the sorbance is calculated as the logarithmic ratio of the initial light in-
capillary. Subsequently, the glass capillary loaded with POF was placed tensity to the final light intensity while subjecting the probes to DI
in a hot air oven and heated at 80 °C for 20 min in order to deform the water followed by various milk samples. Fig. 3A shows the absorbance
POF to obtain a permanent U-shape with a desired bend diameter of response in which the probes showed almost a flat trend in the visible
1.5 mm, which is close to the optimum value for highest RI sensitivity wavelengths. The absorbance response at 530 nm is considered for
(Fig. 1A). The calculation of fiber bend diameter is shown in Fig. 1C. further experiments because of the availability of low cost green light
Then, the U-bend region of the probe was dipped in ethyl acetate for sources. The increase in absorbance could be attributed to the sig-
2 min to remove the cladding over a probe length of 5 mm. The U-bent nificant variation of RI with increasing fat percentages which is in
sensing portion was wiped with a lint free tissue to remove the flakes correlation with the reported literature [29,30]. Hence, it confirms the
over the bent portion and cleaned with DI water. higher influence of fat on the RI sensitivity of the sensor probes in

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A. Gowri et al. Optical Fiber Technology 47 (2019) 15–20

DGC BD

RF
DGC = BD + 2*RF
Fig. 1. (A) U-bent POF probe (0.5 mm fiber diameter with 1.5 mm bend diameter) (B) Experimental setup consisting of U-bent POF probe (UPOF) coupled to a
halogen light source (LS) and a fiber optic handheld spectrometer (FS) (C) The bend diameter (BD) of the probes obtained from glass capillary method is calculated by
subtracting twice the fiber radius (RF) from the diameter of the glass capillary (DGC).

comparison to protein and other solid-not-fat (SNF) content. ∼0.2174 abs. units was obtained from the U-bent POF sensor for dif-
Fig. 3B shows the real-time response of the probe to the milk sam- ferent percentage of water dilution up to 50%. No significant absorption
ples with different fat percentages. The probe shows an instantaneous bands except scattering by milk solids were observed through the U-
increase in absorbance upon subjecting it to milk. No considerable rise bent POF probes. The probes show a reduction in absorbance with an
in absorbance was observed during incubation of a probe in water, increase in the water dilution from 1% to 90% due to reduction in their
indicating a negligible influence of adsorption of protein or fat, if any, refractive index value (Fig. 5B). More importantly, a significant drop in
to the probe surface. The response of U-bent probes is shown in Fig. 4. absorbance with respect to pure milk was observed with water dilutions
An approximately 3-fold increase in absorbance with an increase in % between 1% and 20%, which is the most probable range of water
fat was achieved demonstrating a sensitivity of 0.15 ΔA/Δ% fat. The adulteration. A measurable change in absorbance of 0.08 units was
probes are cleaned with mild handwash following by DI wash for obtained for addition of DI water as low as 5% v/v. The U-bent probes
2–3 min to remove any adsorbed constituents on the probe surface. demonstrate an ability to efficiently monitor as low as 1% v/v of water
dilution, which is five times better than that of a study based on mea-
3.3. Influence of water addition to milk on sensor response surement of change in electrical conductivity of milk reported else-
where [16].
Addition of adulterants to milk is likely to alter its RI [14]. The The results demonstrate the ability of the probes to respond to the
common practice for milk adulteration is addition of water to increase changes in the RI of the milk upon adulteration with water. However, it
the volume to meet the increased consumers demand. The U-bent POF is important to realize that identification of adulteration in milk could
probe (0.5 mm fiber diameter) was exploited to test the change in re- be more challenging as a combination of various adulterants, such as
fractive index of the milk upon addition of water to milk in different water and urea, could be utilized to trick the property of milk. Hence,
ratios. The milk samples were prepared by diluting standardized milk measurement of a single parameter of milk, such as the RI alone, might
with DI water to obtain samples with 1% to 90% dilution. The re- not be sufficient to identify the adulteration in milk. Similar observa-
fractive index values of these milk samples were measured using a tions have been made by Tripathy et al. 2017 [16] while proposing
handheld refractometer (Atago, PAL1) before subjecting them to U-bent electric impedance and pH of milk as a measure for the identification of
POF probes. The sensor was connected between halogen light source adulteration in milk.
and fiber optic spectrometer. The absorbance spectra of milk samples
diluted with water was recorded by dipping the U-bent POF probe in
packaged and water diluted milk samples (Fig. 5A). A change of

Fig. 2. (A) Milk fat content estimation using standard Werner Schmidt method (B) Measurement of milk refractive index using refractometer for milk samples with
varying fat percentages.

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Fig. 3. (A) Absorbance response from U-bent POF probe while subjecting to milk samples with different fat percentages (B) Temporal response from a U-bent POF
sensor upon exposure to commercial milk samples with different fat content demonstrating almost instantaneous response Note: The fat percentages mentioned in the
plot are calculated using standard technique.

3.4. Portable U-bent POF milk fat sensor for field applications

The transformation of U-bent POF probes as milk fat sensor for field
applications is achieved by developing a compact, battery-powered
hand-held device. The handheld optoelectronic device consisting of a
pair of LED and PD in a plastic casing, relevant electronic circuitry and
a digital voltmeter was built in-house (costs less than US $5) as a read-
out device (inset of Fig. 6). U-bent POF probes were connected between
LED and PD housed in the hand-held device. The output of PD response
was obtained in terms of voltage. The performance of the handheld
fiber optic sensor as a fat sensor is evaluated by subjecting it to three
full-cream milk samples sold under different commercial brand names
as well as fresh cow and buffalo milk samples. The fat and SNF values of
fresh and different brand packaged milk samples were quantified using
standard gravimetric and Werner Schmidt methods [28]. Cow and
buffalo milk samples show a fat percentage of 4.56% and 5.33% re-
spectively. The voltage output of the sensor subjected the above sam-
ples was measured and normalized with respect to that of DI water
reference (Fig. 6). The U-bent POF probes show an increase in the
voltage drop with increasing fat content as they are subjected to cow
Fig. 4. Sensor response to milk samples of different fat content (n = 3). The followed by buffalo and full cream milk samples. These results are in
probes gave a statistically distinguishable response with p < 0.1 (as indicated agreement with the absorbance response recorded for milk with dif-
by ‘*’). (For interpretation of the references to colour in this figure legend, the ferent fat content (Section 3.2). These results demonstrate the ability of
reader is referred to the web version of this article.) the sensor to detect the difference in milk composition of each brand,

Fig. 5. (A) Absorbance response of U-bent POF probe to milk sample diluted with different percentage of water (1% to 90%). (B) Refractive index values of milk
samples diluted with water as measured using a commercial refractometer (red) and respective absorbance response at 530 nm wavelength from U-bent POF probes
(blue). (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

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A. Gowri et al. Optical Fiber Technology 47 (2019) 15–20

quality from the cattle in the farm, as a highly sensitive fat sensor at
milk collection centers for valuation of milk from farmers (specific to
Indian conditions), real-time process monitoring in milk products
manufacturing units and consumer needs to assess the milk quality.

Acknowledgments

The authors thank National Agro Foundation Lab, Anna University


for extending their help in validation of milk samples. AG thank
Hariharan M, Divagar M, Ms. Ranjani and Prof. A. Kannan, Head, Dept.
of Chemical Engineering, IIT Madras for their help in milk sample
collection and refractometer facility. AG acknowledges the financial
support by Ministry of Human Resources Development (MHRD),
Government of India.

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