Optics & Laser Technology 153 (2022) 108246

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Optics and Laser Technology

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

State of the art in fiber optics sensors for heavy metals detection
Amit Kumar Shakya, Surinder Singh *
Department of Electronics and Communication Engineering, Sant Longowal Institute of Engineering and Technology, Sangrur, Punjab, India

A R T I C L E I N F O A B S T R A C T

Keywords: Several pollutants are getting added to the water content in today’s world, sometimes intentionally and some­
Fiber grating method times unintentionally. These pollutants, chemicals, and heavy metals can severely affect people’s health, causing
Fluorescence method cancer, tuberculosis, and even death. An optical sensor has tremendous potential to detect heavy metals ion.
Heavy metals
These sensors possess several properties like minute size, remote sensing monitoring, real-time investigation,
Modal interference method
Optical absorbance method
chemical inertness, non-reactiveness, etc., which are considered ideal for heavy metal detection. This work has
Surface-enhanced Raman scattering presented an exhaustive study of different optical methods like fiber grating method, modal interference method,
Surface plasmon resonance method fluorescence method, optical absorbance method, surface plasmon method, and surface-enhanced Raman scat­
tering method to detect heavy metals ions. Various advantages and shortcomings of these methods are analyzed,
along with details of the chemicals, structural formulas, and multiple setups developed to detect heavy metal
ions. Finally, the advancement in fiber optics sensors from future perspectives is also discussed.

1. Introduction standards [24]. In European Union, the “Drinking Water Directive

The world of the 21st century is continuously moving towards
modernization, industrialization, digitalization, etc. [1,2]. The mad race
of sustainable development for modernization has affected mother na­
ture significantly. As a result, today, drastic changes in air quality, at­
mosphere behavior, soil composition, and water purity are observed [3].
Especially water has to pay a high price in terms of quality which is
downgraded by several factors. Industrial pollutants having several
toxic materials are disposed of directly into the main rivers. Chemical
waste, domestic waste, and metal waste are some of the leading con­
taminants present in the river water [4]. Continuous use of fertilizers for
improving crop productivity not only degrades agricultural land but, at
the same time, also adds contaminants to the underground water [4].
One of the leading causes of polluting the underground water is exces­
sive use of fertilizers for agriculture purposes [5]. Heavy metals (HM)
are polluting agents which settle deep inside the Earth’s surface after
continuous use of fertilizers in the agriculture field [6]. HM have a
density greater than 4.5gm/cm3 . There are 60 types of metals that fall
under the category of HM from the point of density [7]. Some prominent
HM frequently found in the groundwater, and their physical appearance
and properties, are tabulated in Table 1.
Different countries follow their water quality standard for proper
water management; in Australia, the “Australian Government National
Health and Medical Research Council (NHMRC)” regulate water
(DWD)” is enforced by every country in the European Union [25].
Similarly, the “Safe Drinking Water Act (SDWA)” in the USA [26] and
the Bureau of Indian Standard (BIS), India [27], etc., are some govern­
ment bodies that regulate the water quality standards in their respective
countries and monitors the presence of HM ions and other impurities in
drinking water.
The HM in groundwater enters the human body when water is
consumed without purification. Besides direct consumption, HM can
enter the human body through skin contact, the digestive tract, and
sometimes even the respiratory tract. HM affects human organs and gets
deposited in the brain, kidney, liver, stomach, etc. [28 29]. HM are also
essential for human health and proper metabolic activity of the human
body but strictly prescribed for maintaining healthy life and health.
Excessive and daily consumption of these HM intentionally or unin­
tentionally leads to the growth of harmful and hazardous diseases in
human beings [30]. Some of the most common HM present in the
groundwater are lead (Pb2+ ), mercury (Hg2+ ), chromium (Cr2+ ), cad­
mium (Cd2+ ), nickel (Ni2+ ), and arsenic (As2+ ) [31]. These HM are
extremely dangerous to human beings, even at low concentrations.
Table 2 presents a brief study of the toxicity caused by various HM in the
human body.
Thus, HM content in the groundwater is hazardous from a health
point of view. It has been observed that HM consumption is one of the
main reasons for cancer in human beings, which is ranked among the top

* Corresponding author.
E-mail address: surinder_sodhi@rediffmail.com (S. Singh).

https://doi.org/10.1016/j.optlastec.2022.108246
Received 15 November 2021; Received in revised form 21 April 2022; Accepted 27 April 2022
Available online 6 May 2022
0030-3992/© 2022 Elsevier Ltd. All rights reserved.
A. Kumar Shakya and S. Singh Optics and Laser Technology 153 (2022) 108246

ten deadly diseases for human beings by the world health organization Table 2
(WHO) [44]. Thus, detecting the HM concentration on time is essential Toxicity caused by the prominent heavy metals.
to protect the agriculture fields, underground water quality, and human S. Heavy Toxicity Ref.
civilization from untimely destruction [45 46]. No Metals
Several conventional HM detection technologies include spectro­ 1 Weakness, anemia, kidney problems, brain
Lead (Pb2+ )
photometry [47], seductively coupled plasma mass spectroscopy [32
damage
(ICPMS) [48], atomic absorption spectroscopy (AAS) [49], chem­ 33]
2 Mercury Nervous system disorders, memory loss, mental
iluminescence [50], electrochemical methods [51] and ion exchange coordination, kidney disorder and affect fetus
[34
(Hg2+ )
methodology [52]. Spectrophotometry has been described as a tech­ growth 35]
nique in which light is made to fall on a chemical substance, and the 3 Chromium Lung cancer, respiratory disorders, kidney
[36
intensity of the light absorbed by the chemical substance is measured. (Cr2+ ) diseases, gastrointestinal infections
37]
The main advantage of this methodology is that it follows a simple 4 Cadmium Respiratory system damage, nervous breakdown,
[38
detection process. The critical shortcoming of this process is that when (Cd2+ ) reproductive problems, urinary infections,
39]
two HM ions have exact dimensions. It becomes difficult to distinguish a cardiovascular problems
5 Nickel (Ni2+ ) Asthma, congenital malformations and cancer
particular HM between them. The sensitivity results obtained from this [40
methodology are nominal [53 54]. 41]
ICPMS is an advanced technique for HM detection. In this technique, 6 Arsenic Skin related disorders, lung cancers, liver cancers,
[42
inductively coupled plasma is used to ionize the sample. This method­ (As2+ ) bladder cancer, cardiovascular disorder
43]
ology is suitable for detecting HM presence even in a very small liquid
analyte. The liquid analyte can be chemical, biochemical, water sample,
etc. The problem with this methodology is that it requires expensive exchanging HM ions from the porous bead resin materials, resulting in
equipment support, a complicated detection methodology, and a long- water purification. This methodology possesses several advantages like a
running time [55 56]. simple setup, easy operation, little use of solvent, and low operational
AAS is a procedure for detecting chemical-based impurities or ele­ cost [63 64].
ments from the sample through the interaction of light by free atoms. Compared to these traditional methods for detecting HM from the
AAS is based on the adsorption of light by “free metallic ions.” This groundwater and analytes. Optical sensing-based methods have several
technique aims to obtain the concentration of a particular element in a advantages like integration, high resolution, small sample requirement,
sample. This is a well-known methodology for detecting more than 70 remote sensing application, transmission medium, high sensitivity, and
different elements in a solution [57 58]. miniaturization [65 66]. Thus, this work aims to present a study on
Chemiluminescence can be understood as the methodology in which various methods used in optical sensing for HM detection. This work also
the intensity of the light is produced when the chemical reaction occurs seeks to identify the potential antigens, antibodies, chemicals, material
between two analytes. This methodology shows the transition of an coatings, techniques, and procedures available in fiber optics for the
electron from the “ground” to the “excited state.” After a specific time earliest possible detection of HM ions.
interval when electrons from the excited state return to the electronic The article is organized into four sections. Section 2 provides
ground state, Chemiluminescence emission occurs, resulting in light exhaustive details about various optical methods, chemicals, and mo­
emission at several wavelengths. Thus light corresponding to different lecular structures of antigens for HM detection. Section 3 summarizes
wavelengths for distinct HM is acquired [59 60]. the works done by multiple researchers and scientists along with the
Electrochemical methods are used to determine the HM concentra­ advantages and disadvantages of different HM detection techniques.
tion in various analytes. This method can detect HM, but the technique Finally, section 4 provides the concluding remarks on the performed
requires some treatment of the sample before testing, due to which there study.
are chances that the sample gets infected with some other contamina­
tion. Thus there is always a possibility that accurate detection results are 2. Study of various optical methods for heavy metal detection
not obtained [61 62].
Ion-exchange methodology performs the exchange of water ions Several optical sensing methodologies have been developed to date,
through porous bead resin materials ions. These resin materials are solid among which some prominent procedures are the fiber grating tech­
in physical appearance, and water ions are in liquid form. Thus, ion nique [67], fiber modal interference [68], optical absorbance technique
exchange occurs in an aqueous solution. This methodology assists in [69], fluorescence technique [70], plasmonic sensing [71] and surface-

Table 1
Classification of the heavy metals.
S.No Heavy Metal Symbol Atomic Mass/Number Physical Appearance Source Ref.

1 Lithium Li 6.941u/3 Silver White Pegmatitic minerals [8]

2 Lead Pb 207.2 u/82 Metallic gray Natural Source [9]
3 Manganese Mn 54.938044 u/25 Silvery metallic Pyrolusite [10]
4 Silver Ag 107.8682 u/47 Lustrous white metal Ores of copper [11]
5 Boran B 10.811 u/5 black-brown Colemanite [12]
6 Zirconium Zr 91.224 u/40 Silvery white Zincon [13]
7 Titanium Ti 47.867 u/22 Silvery grey-white metallic Manaccanite [14]
8 Nickel Ni 58.6934u/28 Lustrous, metallic, and silver with a gold tinge Silicon burning [15]
9 Aluminum Al 26.981539u/13 Silvery gray metallic Bauxite [16]
10 Iron Fe 55.845u/26 Lustrous metallic with a grayish tinge Hematite and Magnetite [17]
11 Cobalt Co 58.933194u/27 Hard, lustrous bluish-gray metal Cobaltite and smaltite [18]
12 Cadmium Cd 112.411u/48 Silvery bluish-gray metallic Zinc by-products [19]
13 Copper Cu 63.546u/29 Red-orange metallic luster Sulfides of copper and iron [20]
14 Zinc Zn 65.38u/30 Silver-gray Sulfidic ore deposits [21]
15 Chromium Cr 51.996u/24 Silvery metallic Chromite [22]
16 Silica Si 28.0855u/14 Crystalline, reflective with bluish-tinged faces Composite of Silicon [23]

2
A. Kumar Shakya and S. Singh
enhanced Raman scattering (SERS) [72]. In the optical sensing tech­
nique, surface plasmon resonance biosensors are designed and devel­
oped based on internal metal deposition (IMD), D-shaped fiber, external
metal deposition (EMD) techniques. Antigens and antibodies are coated
on the fiber surface to enhance the analyte’s interaction with the sen­
sitive material. The prototype developed for HM detection through the
optical fiber is presented in Fig. 1. Here, the light source is connected
with the optical fiber, allowing light to flow within the fiber. The light
enters the fiber’s sensing region, which has a coating of the advanced
antigen and antibody (sensing material) to detect the HM. The HM
presence is detected by changing the volume, refractive index value, or
solution concentration. The presence of the HM results in a change in
polarization, wavelength spectrum, amplitude spectrum, and even
resolution.
After interacting with the sensing material, the light signal passes
toward the spectrometer, where the signal’s demodulation occurs. Thus
the HM concentration is detected by analyzing the change developed in
the output signal of the optical fiber. The sensing region plays a prom­
inent role in HM detection in this sensing setup. Different doping tech­
niques are explored with the optical fibers like Ge doped Si core fiber
with a high refractive index value than Si, which can be used for HM
detection in the HM ion sensor. This combination allows the proper light
confinement and can be used as sensitive material in the HM ion sensing
setup. Optical fibers themselves can detect some parameters for HM if
doping is done accurately. It is also true that optical fiber produces less
sensitive parameters and needs to merge with other methods and ele­
ments to deliver enhanced and sensitive results.
During the HM testing, it has been observed that coating of different
materials, blocking agents, antigens, and antibodies are applied to the
sensing region for the improved interaction between analyte and HM.
Antibody designation 2AS1G5 having a metal chelate complex “EDTA −
Cd(II), p − nitrobenzyl − EDTA − Cd(II), BSAthioureido − l − benzyl − EDTA
− Cd(II),” 2C12 having a metal chelate complex “DTPA − Pb(II), BSA −
thiourreido − L − benzyl − DTPA − Pb(II), CHXDTPA − Pb(II), BSAthioureido
− L − benzyl − CHXDTPA − Pb(II),” 15B4 having a metal chelate complex
“DTPA − Co(II), BSA − thioureido − L − benzyl − CHXDTPA − Pb(II),” and
8A11 having a metal chelate complex “DCP − U(VI), BSA −
thioureido − DCP” etc. are some chemicals which can be used in HM ion
sensor as antigens and antibodies for the HM detection [73]. Fig. 2
presents the molecular structure and chemical formula of the various
Fig. 1. (a) Optical fiber structure (b) prototype of conventional heavy metal ion sensing setup (c) SEM image of optical fiber (d-f) optical fiber core with different
light intensity.
3
Optics and Laser Technology 153 (2022) 108246
antibodies and chelate complexes used as sensitive material in the HM
ion sensor.
2.1. HM ion sensors based on “Fiber Bragg grating”
Fiber Bragg Grating (FBG) sensing system monitors the shift in
wavelength of the “Bragg signal,” which is returned after interacting
with the sample [74]. The resonance condition of the Bragg signal is
expressed by Equation (1), where n is the effective index of core and Ʌ is
the grating pitch [75].
λBg = 2n × Λ (1)
In this mechanism, spectrally broadband light is injected within the
fiber, and the sensing grating reflects a narrow band of light. The light
reflected is dependent on several factors but mainly on the length of the
grating. It is observed from several experimental results that this width
is typically in the range of 0.05nm to 0.30nm. The shift in the Bragg
wavelength is either detected in the transmitted or the reflected spec­
trum [75]. Fig. 3 represents the block diagram of the sensing method­
ology for the FBG sensor [76].
Grating fibers are classified into five different categories based on
grating period, i.e., FBG [77], long-period fiber grating (LPFG) [78],
chirped fiber grating (CFG) [79], tilted fiber grating (TFG) [80], and
sampled fiber grating (SFG) [81]. If the measuring conditions of the
grating period or effective refractive index changes. There is a possibility
that the “resonance wavelength” of the fiber can also get altered. By
investigating the reasons for the wavelength shift, one can get infor­
mation about the surrounding environment [82].
The FBG based HM ion sensor responds according to the sensitive
layer coating and the HM ions. This interaction results in a change in the
effective refractive index of the grating period. This shift is known as the
“Bragg shift.” When HM ions are absorbed by the sensitive layer coating
volume of the grating surface and the grating spacing changes. The shift
in the wavelength of the Bragg grating (λBg ) is expressed by Equation (2).
ΔλBg = λBg .{f (∊, C) + g(∊, C) }.c (2)
Where terms {f(∊, C) + g(∊, C) } represents the sensitivity coefficient
of the FBG, λBg is the wavelength corresponding to Bragg grating, and ˝c˝
is the constant. When the sensitivity coefficient is determined, the spe­
cific HM is detected accordingly.
A. Kumar Shakya and S. Singh Optics and Laser Technology 153 (2022) 108246

Fig. 2. Structural design of various chemicals (a) Assay of a metal ion based on microwell [73] (b) KinExA based assay of metal ion [73] (c) Molecular codes,
structures, metal chelate complex, and equilibrium disassociation constants of some prominent antigens [73].

Fig. 3. Sensing methodology of the fiber Bragg grating sensor [76].

Tan et al. [82] demonstrated a novel structure of the FBG refractive
index sensor based on “Fabry–Perot interference” to detect HM. They
have chosen a metal chelator known as EDTA, which is used as the
coating agent at the end of the fiber. This legend possesses a hexagonal
geometry that suggests that HM binding is possible from six directions.
This metal chelator consists of two amine groups and four carboxylates.
The HM detected from this setup are Pb2+ and Cd2+ .
Yang et al. [83] demonstrated an FBG based sensing probe to detect
the concentration of HM Nikel (Ni2+ ). In their sensing probe they
functioned the probe using two different materials known as chitosan/
polyacrylic acid. The chemical formula of chitosan/polyacrylic acid is
represented in Fig. 4 (a). Through their sensing probe, they have ob­
tained a sensitivity of 40.52dB/mM.
Tan et al. [84] developed an LPFG sensor using an electrical arc-
induced technique to detect the concentration of HM. They have
functioned their sensor using gold nanoparticles and a polyelectrolyte
(PE) layer illustrated by Fig. 4 (b). During their experiment, they have
varied the concentration of the Hg2+ between 0.5ppm to 10ppm. As the
result they concluded that there sensor has obtained a shift of 1.34nm,
transmission power has increased up to 1.74dBm over just 5 hr. These
results are far better than the results obtained from the LPFG sensor
without the gold nanoparticle coating.
Du et al. [85] proposed an FBG based sensor having a dual-layer of
antigens and antibodies. Tetrasulfide and titanium are used as the
sensing material in their developed FBG sensor. The interaction of the
selective chemical ligands with tetrasulfide results in the detection of
HM Pb2+ . The detection of Pb2+ results in the shift of the wavelength
corresponding to LPFG sensor. It is also important to note that antigens
and antibody coating should have an optimum thickness (< 1μm) for the
proper interaction of analytes and blocking agents. Fig. 4 (c) presents the

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A. Kumar Shakya and S. Singh Optics and Laser Technology 153 (2022) 108246

Fig. 4. Pictorial representation of the molecular structure of various chemicals used in the heavy metal sensing employing FBG (a) Structural arrangement of
chitosan and PAA [83] (b) (i) bilayer coating of PDDA and PSS for LPFG sensor [84] (ii) PE − AuNP coated LPFG[84] (c) coating of the Tetrasulfide- and Ti- mes­
oporous materials on LPG sensor PMO surface [85].

installation of the Tetrasulfide- and Ti- mesoporous materials on the
PMO film over the fiber cladding for HM detection.
2.2. HM ion sensors based on “Fiber modal interference”
The HM ion sensor based on fiber modal interference methodology
works on splitting and recombining coherent light. The fiber structure is
designed so that the light entering the fiber gets divided into numbers of
beams, and later they get recombined.
While splitting and recombining the light signals through different
transmission paths, constructive and destructive interferences are
generated due to the coupling of the light signals. Fig. 5 (a) represents
the splitting and recombining of the light signal. Fig. 5 (b) illustrates the
formation of constructive and destructive interferences, and Fig. 5 (c)
presents the evanescent wave generation within the optical fiber.
The interference spectrum of a light signal traveling within the
modal fiber is known as the “two-mode interference model” and is
expressed by Equation (3) [87].
Iout = Icore + Iclad. + 2(Icore × Iclad. )1/2 × cos(φ) (3)
Where Icore represents the light intensity around the core mode, Iclad.
represents the intensity of light along the cladding region, and φ

Fig. 5. (a) Light propagation from SMF to MMF [86] (b) formation of constructive and destructive interferences [86] (c) schematic diagram of the evanescent wave
generation [86].

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A. Kumar Shakya and S. Singh Optics and Laser Technology 153 (2022) 108246

represents the angle between the “core mode” and the “cladding mode.” 1. Offer low-cost perfusion splice.
The refractive index difference between the core and the cladding mode 2. Produce insertion loss < 0.1dB.
is expressed by Equation (4) [87]. 3. Provide clean and smooth recombining of the optical fiber core.
4. Best choice for single-mode operation.
(4)
RI RI
Δn0 = nRI eff RI eff eff
core − nclad. (ncore > nclad. )
eff
5. The lowest back reflection is produced.
RI RI
Where nclad.
eff
and ncore
eff
are the fundamental part of the effective
Disadvantages of the fusion splicing.
refractive index of the cladding and core modes, respectively. Thus the
phase difference between the cladding mode and the core mode is
1. The high cost of the fusion splicing device.
expressed by Equation (5) [87].
2. There are some situations in which fusion splicing is very difficult,
2π L and in those cases, it is better to switch toward mechanical splicing.
(5)
RI eff
φ= × (nRI
core − nclad. )
eff
λ
RI Generally, in an HM ion sensor based on “fiber modal interference,”
Where λ represents the wavelength of the light and nclad.
eff
is slightly
the coating of susceptible film for detecting the HM is applied over the
larger than the effective refractive index. Thus, the modified phase
surface of the modal interference sensor, due to which the change in the
difference φ is expressed by Equation (6) [87].
refractive index of the exposed film occurs. HM ion adsorption and
2π L phase difference are among the two transmission paths, resulting in a
φ= × (Δn0 − Δnslight change in RI eff ) (6)
λ change in wavelength and causing a wavelength shift. This shift in the
wavelength responds differently for the different HM.
To overcome the modal mismatch problem in the fiber, two fibers of
Gu et al. [88] developed an HM ion sensor based on the “thin-core
different cores can be spliced together using the splicing technique. The
fiber modal interferometer.” They have coated their fiber with the
procedure to splice an optical fiber is presented in Fig. 6.
combination of poly(4 − vinylpyridine)(PDDA), (P4VP) and
Splicing is performed over an optical fiber having a diameter of
poly(acrylicacid)(PAA) which is deposited on the side of the fiber
900microns. Fig. 6 (a) presents the real-time fusion splicing device and
through hydrogen bonding for HM detection. Fig. 7 (a) represents the
the essential equipment required for the splicing. Fig. 6 (b) illustrates
molecular structure of the PDDA, PAA and P4VP antigens and Fig. 7 (b)
adding a heat shrink protective sleeve to the fiber before splicing. This
represents the SEM images of the (PAA/P4VP)10 antigens used for HM
can be considered a defensive step to avoid any problem after splicing.
detection. The developed fiber has a core diameter of 3μm and a cut-off
Fig. 6 (c) shows the stripped optical fiber, which needs to be cleaned
wavelength of 450nm. The developed sensor has been designed to detect
with the IPA cleaning solution. Fig. 6 (d) represents optical fiber
placement inside the cleaver. Fig. 6 (e) presents closing the cleaver to HM Cu2+ , Zn2+ and Fe2+ ions. The developed sensor is tested under
obtain the appropriate dimension of the optical fiber. One thing that is stable room temperature. It has been observed from the proposed sensor
essential to note here is that the fiber core needs not to be touched after that transmission dips more towards a higher wavelength range when
this step. Fig. 6 (f) presents the top view of fiber to be cleaved in the the concentration of the HM ions is increased. Thus it can be understood
fusion splicer. Fig. 6 (g) represents the result of splicing the fiber, which that HM is quite sensitive toward coating material. They experimentally
represents 0.49dB optical loss. This step shows that the loss gets observed that with the increase in the ion concentration from 10nM to
generated during the splicing process, which needs to be minimal or zero 0.1M. The shift is wavelength of 3.2nm, 3.6nm and 3.8nm occurs cor­
for good splicing. Fig. 6 (h) represents the result of the successful responding to the HM ions Fe2+ , Cu2+ and Zn2+ respectively. Thus it is
splicing with 0dB loss. Fig. 6 (i) presents the final spliced fiber with a concluded that ion concentration is also related with shift in the
heat shrink protective sleeve. wavelength.
Fusion splicing possesses some advantages and disadvantages, which Yu et al. [89] presented a modified microfiber Ag2+ sensor based on
are listed as follows. nucleic acid probes. The DNA probes designed to catch HM Ag2+ is
Advantages of fusion splicing. represented by Fig. 7 (c). Fig. 7 (d) represents the prototype of their

Fig. 6. Demonstration of the practical splicing of 900micron optical fiber.

6
A. Kumar Shakya and S. Singh Optics and Laser Technology 153 (2022) 108246

Fig. 7. (a) Molecular structure of PDDA, PAA, and P4VP along with the deposition process [88] (b) SEM image of the (PAA/P4VP)10 nanocoating [88] (c) Func­
tionalization of the DNA probe [89] (d) Prototype of taper microfiber based interferometer sensor [89].

developed taper microfiber-based interferometer sensor. The interaction enters the fiber and causes “total internal reflection (TIR)” to occur,
of these sensing probes and nucleic acid results in a shift in the wave­ some light propagates in the fiber cladding and generates the evanescent
length. Their proposed sensor has improved concentration detection field. During the process of TIR intensity of the light beam hits the
capacity to 0.22nm/logM and resolution of the detection is 1.36 × interface between two mediums at an angle more significant than the
10− 9 M. Thus their proposed sensor has shown good selectivity in the critical angle (θc ) corresponding to the plane which is perpendicular to
presence of many other HM and demonstrated promising results for the surface. The critical angle determines whether the TIR will occur or
detecting different HM. not. The critical angle is expressed by Equation (7) [92].
Tou et al. [90] used the “Mach Zehnder fiber interferometer” for n2
detecting the HM Ni2+ . They used poly(vinylalcohol)(PVA) based θc = arcsin( ) (7)
n1
hydrogel as the sensitive material coating for their sensor. The chemical
Where refractive index of core (n1 ) is greater than the refractive
formula for PVA/PAA hydrogel formation is represented in Fig. 8 (a).
index of cladding (n2 ).
The PVA components interacting with Ni2+ reduce the cross-linking and
The wave equation corresponding to the incident field at the inter­
increases the refractive index value, which results in the shift in wave­
face between the medium is expressed by Equation (8) [93].
length. Thus in their sensor design, a new combination of PVA-based
hydrogel is explored, which can efficiently be used for the Ni2+ detec­ → →
∇2 × E + n2 × k02 × E = 0 (8)
tion. This combination can also be explored for the detection of HM
→ 2 2
other than Ni2+ . Ji et al. [91] used a fiber drawing machine (Vytran, Where E is the electric field and is expressed as ∇2 = ∂
∂x2 + ∂
∂y2 +
GPX − 3000) for developing their proposed fiber. Their proposed fiber ∂2
∂z2 ,k0
is the wavenumber in free space, and n represents the refractive
has a diameter of 3.9μm, a total length of 8mm, waist-length 4 ± 0.5mm, index of the propagating medium.
left transition 2.4 ± 0.5mm, and right transition length of 1.6 ± 0.5mm. An evanescent field is a near-standing wave that shows exponential
The final free spectral range is 20nm which is acceptable for the slight decay with the distance to the source. Therefore, when the electric field
detection of the microfiber surface. Fig. 8 (b) represents the function­ is parallel to two mediums. The evanescent field is obtained for the
alization of the microfiber surface using EDC/NHS coupling. They have second medium and is expressed by Equation (9) [93].
tested HM like Pb2+ , Cu2+ , Zn2+ , Cd2+ from their advanced sensor. They √̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅
have kept the concentration of the sample below 10ppb and investigated Ex2 = ET .e− (jk0 n1 xsinθi ) e(k0 n2 y) (n1 /n2 )2 sin2 θi − 1 (9)
2

the combination of various chelating agents for HM detection. In their

HM detection study, they have found the hierarchy of binding affinities Where Ex2 represents the optical intensity and ET represents the in­
2+ 2+ 2+ 2+ tensity at the interface. Thus the interface distance between the medium
with ETDA as Cu > Pb > Cd > Zn but in the proposed study
is decreased by 1/e and is expressed by Equation (10). This distance is
they have obtained binding affinities with ETDA as
known as penetration depth [94].
Pb2+ > Cu2+ > Cd2+ > Zn2+ .
λ0
dp = √̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅
̅ (10)
2π n21 sin2 θi − n22
2.3. HM ion sensors based on “Optical absorbance”
Penetration depth is dependent on the wavelength of the light in a
In optical absorbance, the light intensity varies with the concentra­ vacuum, θi represent the incident angle, n1 and n2 represents the
tion of the HM. This methodology analyzes the interaction of light with refractive index of core and cladding, respectively. It is important to
the HM through the evanescent field absorption sensor. When light note that “penetration depth” relates to the light direction. Equation

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A. Kumar Shakya and S. Singh
Fig. 8. (a) Molecular structure of PVA/PAA hydrogel formation [90] (b) Functionalization of the microfiber using EDC/NHS coupling [91].
(10) illustrates that the penetration depth can increase by increasing the
numerator term and decreasing the denominator term.
The HM sensing layer acts as an interfacing medium when a change
in its refractive index value is observed. This indicates variation in the
evanescent field and transmitted light intensity. Thus HM concentration
can be identified by analyzing the “intensity of the transmitted light
signal.” The detection ability of the HM ion sensor can be further
enhanced by making some modifications in the geometrical design of
the fiber, like increasing the core size, removing the cladding region, etc.
These modifications change the evanescent field partially or wholly,
resulting in improved HM interaction with the sensing medium.
Bhavsar et al. [95] developed a LED-based fiber optic sensor for
detecting the HM from the groundwater. The LED is used as the source of
light and is coupled with the assistance of a fiber coupler. They have
used multimode poly lead fiber of 200μm diameter in their developed
sensor. The proposed setup is exposed to a sample solution containing
HM ions. The optical signal of the sample solution is analyzed through
the “Stellarnet” spectrometer. They have investigated HM like copper
dithizonate, chromium dithizonate, mercury dithizonate, and dithizone
through their developed setup. The chemical formula of dithizone and
metal dithizonate is presented in Fig. 9 (a). They have also studied and
explored the combination of HM like Hg2+ and Cu2+ . They have
analyzed that their sensor is not responding accurately toward a low
concentration of HM but works efficiently for a higher HM
concentration.
8
Optics and Laser Technology 153 (2022) 108246
Chandra et al. [96] developed a U shaped copper sensor to detect HM
Cu2+ ion represented by Fig. 9 (b). Their advanced sensor can work in a
wide range of detection, varying from “femto” to “micro” molar con­
centration. The developed sensor design is coated with a combination of
immobilized polyaniline (PAni) and immunoglobulin (IgG), which act as
the sensitive material for the sensor. The interaction of the HM with
sensitive material results in a change in the evanescent field. The sensor
is more sensitive towards HM Cu2+ and shows less sensitivity towards
other HM. The sensor efficiency is tested in marine and lake water to
determine the concentration of Cu2+ ion. Finally, the sensor is embedded
in a portable handheld device for remote sensing applications. Zhong
et al. [97] presented a three-layered “fiber optics evanescent field
(FOEW)” sensor. The sensitive material used in their sensor design is
“diluteCanadabalsaminxylene.”. The sensing probe of their proposed
sensor is functionalized with cyclotriveratrylene(TPC),
phenylaminoethoxy, polycation (tris(2 − (4 − phenyldiazenyl))),
polydimethyl diallylammoniumchloride (PDDAC), and
polyanion(TPCpluspolyacrylicacid(PAA)). The sensing probe model, SEM
image of the HM Hg2+ and the deposition procedure on the thin films is
presented in Fig. 9 (c). Their proposed sensor has efficiently detected the
HM Hg2+ and glucose content with a lower detection limit of 0.1mg/L.
The sensitivity of their proposed sensor for different HM concentrations
is (− 0.037(mg/L)− 1 ) which is claimed to be 6.5 times higher than the
sensitivity reported by the conventional FOEW sensors. The sensor
A. Kumar Shakya and S. Singh Optics and Laser Technology 153 (2022) 108246

Fig. 9. (a) Chemical structure of dithizone and metal dithizonate [95] (b) U- bend shaped sensor probe fabrication for Cu2+ detection [96] (c) Sensor probe
fabrication procedure, SEM images of Hg 2+ sensitive films and deposition process of Hg2+ as selective process [97].

response time for the HM Hg2+ detection is 50 secs. hexagonal geometry (p6mm), biscontinuous cubic (Ia − 3d) and cage-
Urek et al. [98] used different mesoporous materials in their designed type cubic (Pm3n) respectively. These material have a highly porous
HM ion sensor presented in Fig. 10 (a-c). These materials consist of 2D − nature that becomes an excellent optochemical sensor combined with

Fig. 10. Structure of the mesoporous material (a) (p6mm) [98] (b) (Ia − 3d) [98] (c) (Pm3n) [98] (d) Molecular structure of the water-soluble TMPP [99].

9
A. Kumar Shakya and S. Singh
low adsorption and emits under visible spectra. Mesoporous materials
with pores have a diameter of 2nm to 50nm. The surface area of the core
varies from 1000m2 /g and the volumes of the large pores are 1 mL
g . These
materials are formed from the solution by cross-linking and co-
assembling the typical oxides in the presence of “structure-directing
agents (SDAs).” The structure of mesoporous material depends upon the
geometry, length, saturation of the sensing tail, molecular shape, and
charging of the group head. HM concentration is obtained in this sensing
methodology by changing the light properties excited by a definite
electromagnetic wavelength. The proposed sensor detects toxic HM like
Hg2+ and Cu2+ by sensing probes build with mesoporous material. Sal­
lam et al. [99] used the UV − Vis absorption, stopped-flow, cyclic vol­
tammetry, and time-resolved fluorescence scheme to detect HM
concentration in the aqueous solution of
Meso − tetra (N − methyl − 4 − pyridyl)porphyrintoluenesulfonate(TMPP)
and water. The molecular structure of water soluble TMPP is presented
in Fig. 10 (d). The optical studies for the TMPP show less significant
interaction with the HM Mn2+ , Co2+ and Ba2+ , but showed impressive
results for the detection of HM Hg2+ , Pb2+ , Cu2+ , and Ni2+ .
2.4. HM ion sensors based on “fluorescence”
Luminescence can be understood as the phenomenon in which light
is emitted by a material that is not even strongly heated. This emission of
light has no relation to thermal radiation. Based upon several factors like
the nature of the excited electrons and the lifetime of these excited
electrons. Luminescence is categorized in two terms, i.e., phosphores­
cence and fluorescence. The primary optical sensing mechanism used in
optical sensors is known as “fluorescence quenching.” One of the main
advantages of fluorescence sensors is that they possess incredibly high
sensitivity for combining HM ion and the sensing material [100]. The
optical fiber HM ion sensor uses the “functionalized molecules” of the
sensor to produce a “chemical change” in the detected HM ion, which
changes its fluorescent spectrum. Thus, when an HM ion interacts with
the sensor’s functionalized molecule, the HM ion’s fluorescence signal
occurs. Thus HM presence is detected [101]. Fig. 11 represents the
developed prototype of the fluorescence sensor for HM detection and
having sensitive material inserted in the analyte solution.
The molecular formula of the analyte solution
Dansyl +Met − NH2 +Hg2+ is presented in Fig. 12 (a). Aliberti et al. [102]
Fig. 11. (a) Prototype of the fluorescence sensor (b) sensing methodology of the proposed sensor [102] (c) fluorescence spectra corresponding to Hg2+ ion for
varying concentration [102].
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Optics and Laser Technology 153 (2022) 108246
developed a new optical sensor for Hg2+ detection from marine water.
They investigated the probability of dansyl − aminoacids for the HM Hg2+
detection. They performed a detailed study on the binding features of
various chemosensors for Hg2+ detection. They have concluded that the
N − dansylatedmethionine is the best chemosensors in terms of sensitivity
which produces a LOD value of 140nM. The LOD value is further
improved to about 5nM from the developed sensing setup. Ma et al.
[103] developed a nanofibrous membrane (FNFM) that is highly sensi­
tive and selective. The developed layer detects the amount of HM Hg2+
through electrospinning and subsequent immobilization. A fluorescent
chemosensordithioacetalmodifiedperylenediimide (DTPDI) is installed on
the surface of polyacrylonitrile(PAN)nanofibers by the electrostatic force.
The DTPDI layer can be separated from PAN following hydrolysis of
dithioacetals in the presence of Hg2+ . Thus it is observed that FNFM
permits great sensitivity towards Hg2+ . The molecule binding method­
ology of FNFM to Hg2+ is presented in the Fig. 12 (b). The high detection
limit of 1ppb is obtained from the proposed sensing methodology. Thus it
is observed that from FNFM, the concentration of Hg2+ can be easily
detected. Wang et al. [104] presented a “CsPbBr3 perovskite quantum
dots (CPBQDs)” which has optical properties and have the potential to
detect HM based on fluorescence resonance energy transfer (FRET). The
electrospinning method is used in their research to improve the con­
centration of CPBQDs for FRET detection. A 400nm thin membrane of
polymethylmethacrylate (PMMA) and CPBQDs(CPBQDs/PMMAFM) is
fabricated for HM detection. The combination of CPBQDs/PMMA FM
together possessed more optical properties, narrow peak width (14nm),
and high quantum yield (88%) when compared with the CPBQDs alone
represented by Fig. 12 (c). Thus the proposed sensor detects Cu2+ and
the detection limit is increased by 10− 15 M.
Wu et al. [105] developed a nanofiber to detect HM Cu2+ by elec­
trospinning the polymers poly[(Nisopropylacrylamide) − co − (N − hydro
xymethylacrylamide) − co − (4 − rhodamine hydrazonomethyl − 3 − hydro
xyphenylmethacrylate)] [poly(NIPAAm − co − NMA − co − RHPMA), PNNR]
represented by Fig. 13 (a). The random copolymers in the acidic back­
ground PNNR show excellent sensing and selectivity towards the HM
Cu2+ in both solid and liquid form. Thus PNNR can be considered suit­
able for the detection of HM Cu2+ . Long et al. [106] proposed an
evanescent DNA-based biosensor that can detect HM Hg2+ . The DNA
probe contains “oligonucleotide sequences” that have the feature to
A. Kumar Shakya and S. Singh Optics and Laser Technology 153 (2022) 108246

Fig. 12. (a) Structure of Dansyl Amino acid [102] (b) sensing of FNFM to Hg2+ [103] (c) illustration based on the CPBQDs/PMMAFM [104].

Fig. 13. (a) Chemical structure of RHPMA and PNNR [105] (b) DNA probe immobilization [106] (c) Detection principle of Hg2+ [107] (d) Fluorescence switching of
Hg 2+ [108].

hybridize fluorescent DNA. This DNA probe consists of a T − T sequence
with gets binded with Hg2+ to form a new sequence of T − Hg2+ − T. The
fabricated DNA sensing probe is presented in the Fig. 13 (b). A high
concentration of Hg2+ lead to the less fluorescence − labeledcDNA to the
surface of the sensor. Their sensor produces a detection limit of 2.1Nm,
pH value of 1.9 correspondings to HM Hg2+ , but the sensor has presented
its capability to detect other HM also. Han et al. [107] developed a
biosensor using functional nucleic acids to detect the HM Pb2+ and Hg2+
from the water samples. The binding of nucleic acids with T − T
mismatch results in the precise detection of Hg2+ . Similarly
8 − 17DNAzyme and interaction of the cleavage of a substrate resulting in
the detection of Pb2+ . Fig. 13 (c) presents the detection principle of HM
Hg2+ . The presented biosensor has provided a detection limit of 22pM
and 20Nm for HM Hg2+ and Pb2+ , respectively. Nguyen et al. [108]
developed a portable sensing system to detect HM Hg2+ based on fluo­
rescent quenching. A combination of two materials is performed for the
Hg2+ detection. These materials are “fluorescent polymeric material”
and “azathia crown,” both are some sought of Hg2+ ion receptor

11
A. Kumar Shakya and S. Singh
represented by Fig. 13 (d). When Hg2+ comes in contact with these
material combinations, a significant increase in the electron excitation is
observed, which symbolizes that this material is quite sensitive to the
HM Hg2+ . The proposed sensor is quite sensitive to Hg2+ . A washing
protocol is also explained through which the sensing probe can be
washed, and the sensor probe is again prepared for some other HM
detection. Prestel et al. [109] presented an HM ion sensor having sensi­
tive agents like Newport Green™, BTC-5 N, chromotropic acid, and
neocuproine acid. These acids allow the detection of the HM like Cu2+ ,
Ni2+ , and Cd2+ from the water samples of rivers and harbors. They found
that some ligands are sensitive to some specific HM like BTC-5 N is
sensitive towards Cd2+ , AnthBT is sensitive for Hg2+ , Newport Green™ is
sensitive for Ni2+ , DEPyT can detect Cu2+ , efficiently. Similarly chro­
motropic acid shown high sensitivity towards Be2+ . They also investi­
gated the effects of the HM on the environments. They also come up with
a study that excess HM content in the water is hazardous to the physical
structure of the dams and retention basins.
2.5. HM ion sensors based on “Surface plasmon resonance”
The surface plasmon resonance (SPR) phenomenon occurs at the
intersection of the dielectric surfaces and plasmonic material [110]. This
assists plasmonic sensors in detecting various chemicals, biochemicals,
liquids, HM fused water samples and analytes. Initially, the prism-based
configuration was popular in optics, but with the advancement in fiber
optics [111]. This configuration became outdated, and fiber optics-
based sensors evolved. Sensors based on optical fiber have attracted
the attention of many researchers due to their unique features like small
size, minute sample volume, high integration, remote sensing applica­
tions, online monitoring, etc. [111]. In optical fibers, several types of
reflection occur, among which one is TIR. In TIR light gets wholly re­
flected at the interface of the two mediums [112]. TIR can also be
considered as the principal behind the working of most optical fibers.
Equation (11) represents the wave equation of the electromagnetic wave
traveling in the air [113].
ω √̅̅̅̅̅
kx = εo sin(θ) (11)
c
Where ω is the incident light frequency, “c” is the speed of light in a
vacuum, εo represents the dielectric constant of the cladding, and θ is the
angle of the incident light. Thus the wave vector of the surface plasmon
wave corresponds to the dielectric and metal interface, which is
expressed by Equation (12) [113].
√̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅
( )
kspw = (
ω ε1 ε2
) (12)
c ε1 + ε2
Where ε1 is the dielectric constant of the plasmonic material, ε2 is the
dielectric constant of the medium. During the effective mode index
analysis, the value of the fundamental part of the core mode becomes
precisely equal to the fundamental part of the SPP mode, giving birth to
the plasmonic condition [114]. According to the plasmonic condition,
the surface plasmon modes are classified into two categories, i.e.,
SPR[115] and localized surface plasmon resonance (LSPR) [116]. In the
SPR phenomenon, incident light strikes the metal-dielectric interface at
a particular angle. Depending upon the thickness of the plasmonic ma­
terial, the SPR phenomenon is generated and resulting in reducing the
intensity of the reflected light. The operational phenomenon of the LSPR
is similar to the SPR. In other words, it can be considered that LSPR is a
particular type of SPR in which the electromagnetic field remains
localized in a nanoscale region around the nanoparticle-dielectric
interface.
Photonic crystal fiber (PCF) is a new revolution in fiber optics, which
has several advantages over conventional fiber-like design modification
freedom, plasmonic material selection, and sensing methodology se­
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Optics and Laser Technology 153 (2022) 108246
lection for specific use [117]. PCF based plasmonic sensors are physi­
cally designed and developed in three different categories based on the
internal metal deposition on the air holes [118], D-shaped plasmonic
fiber with a polished flat surface [119], and fiber-based on the external
plasmonic material deposition over the background material [114 115].
A single or multiple coating of the plasmonic material can also be per­
formed in these fibers, which can also be increased based on the appli­
cation. An analyte sensing layer is placed over the plasmonic material
for interaction with the plasmonic material with the analyte. Thus,
PCFSPR sensors detect HM content and provide a high sensitivity during
the detection process [120].
Kyaw et al. [121] developed an SPR based sensing system to detect
HM ions from the water. In their developed system, ions are pushed
towards the surface of the sensing system for enhanced adsorption. High
sensitivity is obtained by monitoring the schedule of the shifted signal.
The ion deposition principle follows the theoretical model for ion
mobility in water. The proposed sensing setup monitors the content of
Cd2+ ion in water. The developed sensing system can obtain the con­
centration of Cd2+ up to 250ppb and several parts of ppm. Fig. 14 (a)
represents the SPR based sensing system for detecting HM in the water
samples. This system is based on the Kretchman configuration. Boruah
et al. [122] presented a U-shaped PCF SPR biosensor for the detection of
HM Pb2+ . They have used oxalicacid − functionalizedAuNPs as the
detecting agent in their sensor setup to functionalized the sensing ma­
terial. Fig. 14 (b) illustrates the developed sensing probe functionalized
with AuNP for detecting the Hg2+ . Their presented sensor is based on the
LSPR phenomenon. Their sensing probe has reached the detection limit
of 1.2ppb and has a linear range of variation from 1ppb − 20ppb. The
proposed sensor is able to detect only the concentration of Pb2+ in water,
whereas the other HM sensor does not present effective detection
capability.
Fen et al. [123] introduced an SPR based optical sensor for the
detection of HM Pb2+ . They have used
p − tert − butylcalix[4]arene − tetrakis(BCAT) immobilized ions in chitosan
thin film as the sensitive layer to detect the HM. The concentration of the
HM ion was detected by measuring the SPR signal strength when the
BCAT layer is exposed in the aqueous solution. They performed the
sensing for Pb2+ concentration varying from 30ppb to 3ppm. It has been
observed that the sensitive layer used in their experiment is so sensitive
towards the Pb2+ concentration that it has detected the presence of Pb2+
among solution containing other HM like Hg2+ , Mn2+ , Zn2+ , and Cu2+ .
Fig. 14 (c) represents the angle scan SPR system for detecting the pres­
ence of the Hg2+ ions.
Lin et al. [124] developed a dedicated sensing probe based on the
LSPR to detect the HM Cd2+ . In their sensing probe development, they
have used the phytochelatins(PCs)(γGlc − Cys)8 − Gly fused with the Au
nanoparticles termed NMAuOF. The cystamine setup developed for
detecting Cd2+ is presented in the Fig. 14 (d). It has been observed in
their experiments that as the concentration of the Cd2+ changes from
1ppb to 8ppb, the sensitivity and the detection limit of 1.24ppb − 1 and
0.166ppb is obtained. The value of the disassociation constant (kd ) ob­
tained for the PCs with Cd2+ is about 6.77 × 10− 8 M. Thus it is concluded
from the research work that the developed PCs − functionalizedNMAuOF
can detect HM Cd2+ with high sensitivity. Kamaruddin et al. [125]
developed an SPR based biosensor system using a combination of
Au − Ag − Au as a multimetallic layer over
chitosan − grapheneoxide(CS − GO) for the HM Pb2+ detection. The
developed sensor is represented by Fig. 14 (e). The proposed sensor uses
SPR technology to determine the signal-to-noise ratio (SNR), sensitivity,
and repeatability. They have used “X-ray photoelectron spectroscopy
(XPS),” “atomic force microscopy (AFM),” “Raman spectroscopy”, “X-
ray diffraction (XRD),” and “field emission scanning electron micro­
scopy (FESEM)” to functionalize their nanostructure layer. They have
A. Kumar Shakya and S. Singh
Fig. 14. (a) Ion mobility in a flow channel [121] (b) Sensor tip functionalized with AuNPs attracting Pb2+ [122] (c) Sensing setup of angle scan SPR technique [123]
(d) Cystamine setup for detecting Cd2+ [124] (e) Tri metallic sensor system with N = 6 [125].
observed that the SPR angle has obtained a shift of 3.5 in the range of
◦
0.1 − 1ppm due to the development of enhanced evanescent field at the
interface of the sensing layer. The proposed sensor shows an SNR value
of 0.92 for the 5ppm Pb2+ concentration. Fen et al. [126] used Kretsch­
mann SPR technique to detect HM. A metallic covering of 50nm gold is
used as a thin film that is installed over the fiber using the sputter coater.
The transmitting medium of the proposed sensor is air which is changed
to the sample HM ion solution. It has been observed from the experiment
that as the concentration of the HM is changed, the value of the
refractive index of HM also gets changed. HM ion solutions containing
Hg2+ , Cu2+ , Pb2+ , and Zn2+ are examined from the developed sensing
setup. Finally, they have concluded that the SPR technology can be used
to detect HM from any solution. May et al. [127] developed a novel
PCF-based SPR biosensor for the detection of HM Cd2+ . Urea is quite
sensitive towards HM Cd2+ when urea gets binded with the Cd2+ . The
structural design of the enzyme gets changed, which can also be inter­
preted as urea’s ability to detect Cd2+ ion. This ability of urea is explored
in this research. The inventors have fabricated a monolayer of urea and
gold-coated sensing probe. The enzyme N − succinimidyl3 − (2 −
pyridyldithiol)propionate(SPDP) is used in their work for the detection of
Cd2+ . It has been observed in the experiment that interaction of the urea
and Cd2+ result in the change in the enzyme monolayer and concen­
tration of Cd2+ ion having range from 0 − 10mg. The developed sensor
also shows a change in the refractive index by 5 − 10%. Thus their
proposed sensor presents a high detection capability for the HM Pb2+ .
2.6. HM detection through surface-enhanced Raman scattering (SERS)
Surface-Enhanced Raman Spectroscopy or Surface-Enhanced Raman
Scattering (SERS) is an advanced technique of molecular sensing for
several applications like biological molecule detection, chemical moni­
toring in petroleum industries, pharmaceutical industries, and HM
detection from groundwater [101]. The most crucial advantage of SERS
is that it offers rich molecular data related to Raman scattering. This
improved information is obtained by amplifying the magnitude of the
signal to a higher order, thus increasing the detection limit to the
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Optics and Laser Technology 153 (2022) 108246
molecular signal level. Previously several researchers used single-use
films, colloidal solutions, etc., to create SERS effects. However, these
substrates may be robust, reusable, and portable during practical ap­
plications. Recently significant advancement has been achieved to
obtain SERS effect in fiber optics sensors. End tips fiber optics and op­
tical fibers sensors with tapered, angled, and flat tips are modified using
silver, roughened, and inland silver films over nanospheres to produce
the SERS substrate. The main advantage of these configurations is their
inexpensive nature, fabrication feasibility, and reproducibility. These
configurations also possess some shortcomings, such as the requirement
of long integration time between molecules, fewer numbers of SERS
particles in the fiber’s active region, and the high laser intensity to
successfully obtain attain reasonable SERS spectrum.
Zhang et al. [128] proposed a D-shaped Raman probe having the coat
of SERS substrate on the flat fiber surface. They have observed that the
developed fiber successfully coupled the 70% of the input light in the
SERS active region. The SERS fibers are created in their experiment by
mixing 5μL of 0.1mM rhodamine 6G(R6G) with 20μL Ag nanoparticles
later the solution is dried under ambient conditions. Their investigation
has concluded that the D − shaped fiber has more exposed SERS active
area of 1cm × 8μm = 8000μm2 as compared to the 50μm2 of the end
polished fiber of the same kind. Fig. 15 (a) represents the pictorial view
of the Raman probe employing D-shaped fiber coated with the SERS
substrate. Zhang et al. [129] used calcined ZnO submicron flower
(ZnOSFs) as a substrate to enhanced SERS activities for fabricating a
novel biosensor for the detection of Pb2+ . The presented combination of
ZnOSFs performs better than the ZnO submicron particle (ZnOSPs). The
advantage of using ZnOSFs over ZnOSPs are achieving the Raman effect
easily and the development of a narrow energy band for charge transfer
for easy generation of the exciton transition to achieve Raman
enhancement effect. Thus the capability of ZnOSFs to develop the SERS
effect result in the accurate detection of HM Pb2+ . The biosensor
developed in this approach also show a linear relationship ranging from
10pM to 100μM and can operate upto lower detection limit of 3.55pM.
Thus in this research work authors successfully achieved two objectives,
i.e., the development of an ultrasensitive biosensor for Pb2+ detection
and identification of a novel substrate for developing the SERS. Wu et al.
A. Kumar Shakya and S. Singh Optics and Laser Technology 153 (2022) 108246

Fig. 15. (a) D shaped Raman probe with SERS substrate coating [128] (b) Three SERS probes for indirect detection of HMs [131] (c) Inorganic ion detection through
SERS sensors [131].

[130] proposed a biosensor for the sensitive detection of HM Hg2+ for [131].
human health monitoring and environmental protection. Their pre­
sented biosensor is based on a radiometric SERS aptasensor. In their 1. Raman reporters molecules alone.
sensor the sensing probe is functionalized with Au, Ag core shell nano 2. Raman reporters conjugated with plasmonic nanomaterials.
particles (Au@AgNPs) for the detection of HM Hg2+ . Here firstly the 3. Raman reporters sandwiched in between metal nanoparticles and
thiolated 5 − Cy3 aptameter probe is immobolized with the SERS sub­
′ silica nanoparticles.
strate surface which is later hybridized with 5 − Rox labeled comple­
′

The direct/indirect SERS detection through SERS reporters is pre­

mentary DNA (cDNA) to form a rigid double standard DNA(dsDNA). The
Rox Raman label and Cy3 are used to produce the Raman signal. It has
been observed from their research that due to the presence of the HM
Hg2+ thymine T − Hg2+ − T changes into a hairpin like structure, that
leads to disassociation of dsDNA. Thus the Rox label get away from the
(Au@AgNPs) whereas Cy3 label lie close. Thus their proposed biosensor
is enable to detect HM Hg2+ in the range of 0.001 to 0.01nM with the
detection limit of 0.4pM. Tang et al. [131] presented an exhaustive re­
view of SERS sensor for food safety and HM Hg2+ , Pb2+ , Cd2+ and As3+
detection. In Raman scattering SERS substrate plays an important role
for enhancing the Raman signals. SERS substrate follow two different
mechanisms based on electromagnetic enhancement (EM) and chemical
enhancement (CE). The SERS signal intensity (PSERS ) under both EM and
CE are expressed by the Equation (13) and Equation (14) respectively
[132 133].
PSERS ∝EM × CE (13)
PSERS ∝N.σRabs .|(A(ve )|2 .|(A(vs )|2 .I(ve ) (14)
Where N is the number of absorbed molecules, A(ve ) and A(vs ) are the
enhancement factors of excitation light and Raman scattering light. I(ve )
represents excitation light intensity. The term σRabs mainly contribute to
the CE. In the case of EM the SERS enhancement factor is expressed by
Equation (15) [134].
EFEM =
PSERS
= |(A(ve )|2 .|(A(vs )|2 (15)
PoSERS
Where PoSERS represents the SERS intensity in the absence of EM.
They further present details about the SERS probes. There are three
types of SERS probes categorized as follows and illustrated in Fig. 15 (b)
sented in Fig. 15 (c). They have also observed that the presence of
different HM ions like Cu2+ , Cd2+ , Pb2+ , Hg2+ , arsenic (As3+ ) and
chromium (Cr6+ ) can cause several diseases in human beings and
sometimes even deaths as these HM do not degrade quickly.
They have further concluded that it is challenging to identify mon­
oatomic HM ions by SERS sensors as there are no chemical bonds to
generate Raman scattering. Thus only a few oxidations can be identified
by Raman vibrational bands [135]. Therefore, the HM detection re­
quires some specific chemical bond formation or the use of extrinsic
SERS probes for SERS detection. HM arsenate (As5+ ) and arsenite (As3+ )
can be directly detected using vibrational characteristics of As − O bond
[136].
Eshkeiti et al. [72] developed a novel SERS substrate based on silicon
wafer for detecting HM compounds like zinc oxide (ZnO), mercury sul­
fide (HgS) and calcium sulfide (CdS). They have used inkjet printing
techniques to fabricate the SERS substrate. Ag nanoparticles having a
particle size of 400nm are used in their experiment for developing a thin
film of AgNP based SERS substrate. They experimentally concluded that
AgNP aggregates due to the presence of hot spots. The hotspot’s location
on the fabricated SERS substate using inkjet printing technique
employing AgNP on silicon wafer is presented in Fig. 16 (a) and Fig. 16
(b), respectively. Fig. 16 (c) represents the schematic of the SERS based
experimental setup for detecting the HM. Tang et al. [137] presented a
highly sensitive SERS based HM ion sensor for detecting HM Cu2+ and
Hg2+ . They used spectroscopy technique in their experiment for HM
detection. They used Au nanorod (AuNR) and polycaprolactone (PCL)
based nanocomposite fibers functionalized with
2, 5 − dimercapto − 1, 3, 4 − thiadiazoledimer (di − DMT) and
trimercaptotriazine (TMT) which act as a metal ion binding ligands to

14
A. Kumar Shakya and S. Singh Optics and Laser Technology 153 (2022) 108246

Fig. 16. (a) SERS hotspots between AgNP [72] (b) SERS substrate fabricated through inkjet printing using AgNP on silicon wafer [72] (c) SERS based experimental
setup for HM detection [72] (d) Absorbance spectra, relative absorbance and HM based colloidal solutions [138].

Fig. 17. (a) Developed spectroscopy-based sensing setup (b) SEM image of optical fiber M93L01; analytes (c) propyl alcohol (d) oil (e) water (f) milk (g) red palm oil
(h) transmission (%) from analytes (i) absorbance (AU) from analytes (j) developed relationship between refractive index, transmission, and absorbance. (For
interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

15
A. Kumar Shakya and S. Singh Optics and Laser Technology 153 (2022) 108246

capture HM ions Cu2+ and Hg2+ . They further performed the quantita­
tive analysis of HM ions through an internal calibration curve and ob­
tained a peak intensity ratio 287/387 cm− 1 and 1234/973 cm− 1 for HM
Hg2+ and Cu2+ respectively. Chadha et al. [138] developed an innovative
sensor employing SERS and XPS based on
2 − thiazoline − 2 − thiolfunctionalizedgold(Au − TT) for detection of HM
Hg2+ and Pb2+ . In their experiment they have tested several HM like
Cu2+ , Cd2+ , Co2+ , Zn2+ , Ni2+ , Hg2+ , Mn2+ , Fe2+ , Ca2+ , Sn2+ and Pb2+ but
have observed that only Pb2+ and Hg2+ show distict SERS spectral
behaviour. Thus they concluded that their developed sensor is quanti­
fied to detect HM Pb2+ and Hg2+ . Their sensor have obtained LOD of
0.1ppm and enhanced Raman intensity of 1026cm− 1 . Fig. 16 (d) repre­
sents the adsorption spectra of Au − TT probe, relative absorbance plot
(A675/A520.5) with HM ions of 1mM concentration and different
colloidal solutions in presence of HM ions.
Therefore fiber optics-based SERS sensors have shown enough po­
tential to detect various HM ions through the development of substrate
and application of different antigens and antibodies. Recently
spectroscopy-based fiber optics biosensor have also demonstrated their
ability to detect HM through multiple factors [139]- [140]. Aloisi et al.
[141] present an exhaustive study on fiber optics sensors for HM
detection from water and milk using spectroscopy techniques. Lin et al.
[142] used the near-infrared (NIR) technique for the detection of HM
Pb2+ and Hg2+ . They have further used several optimization algorithms
to model the data obtained from the spectroscopy analysis. They have
observed that the ant colony optimization-PLS (ACO − PLS) have pro­
duced the optimum result in the linear range of 0.001100ppm with LOD
≤ 1ppb. They have further concluded that their proposed technique is
best for HM detection from household oils. Shakya et al. [143] developed
a low-cost spectroscopy setup based on Beer-Lambert law for analyzing
the transmission (%) and absorbance (AU) from various analytes like
milk, alcohols, oils and HM fused water samples. They investigated these
analytes based on their refractive index values and developed a novel
relationship between refractive index, transmission, and absorbance.
Fig. 17 presents the layout of the developed spectroscopy-based sensing
setup for analyzing multiple liquids.
Thus different techniques have shown their capacity to detect spe­
cific HM ions after applying various antigens, antibodies, and chemicals.
Therefore, fiber optics sensors are intelligent, sensitive, and portable
devices that identify and detect different HM.

Table 3
Summary of the prominent features of various optical fiber sensing methodologies.
S. SM Structure Sensitive Material HM ion Sensitivity/ Concentration Ref.
No detected LOD Range

1 Fiber Bragg grating SSFBG-Fiber cleaved end Ethylene-diamine-tetraacetic acid Cd2+ ——— ———
[82]
(FBG) sensor and Fabry–Perot cavity
2 Normal FBG Chitosan and PAA Hg 2+
Pb 2+
Ni 2+ 40.52dB/mM 1.0mM
[83]
3 LBPG PDDA and PSS Hg2+ ——— 0.5 ppm − 10 ppm
[84]
4 LPFG Tetrasulfide- and Ti-containing Pb2+ ——— ———
[85]
mesoporous materials
5 Fiber modal interference Thin-core fiber PDDA, PAA, P4VP Cu2+ ——— 10nM − 0.1M
[88]
sensor interferometer sensor
6 PCF splicing based on SMF PAA and PVA hydrogel Ni 2+ 0.214nm/μM up to 50 μM
[90]
7 125 μm thin core normal EDC/NHS coupling Pb2+ , Cu2+ ——— ———
[91]
fiber
8 Hair Pin structure C-rich ssDNA probes Ag + 0.22 nm/ log ———
[89]
M
6
9 Optical absorbance 2D-hexagonal mesoporous MCM-41 functionalized with quinoline Cu2+ Hg2+ ——— 0.01–30 × 10− M
[98]
based sensor materials
10 Polyamine-functionalized BPEI-CDs Fe2+ Cu2+ Mg2+ ——— 0–100 μM
[99]
carbon dots
11 6 cm commercial Optical Ddithizone and Metal Dithizonate Cu2+ Hg2+ ——— 78 μM
[95]
fiber
12 U shaped sensing probe Copper-HIgG coating Cu 2+ ——— 0–10 μM
[96]
13 Fluorescence-based MMF with sensing probe Dansyl-amino acids Hg2+ 140 nM 5–140 nM
[102]
sensors
14 MMF with sensing probe Immobilization of DNA Hg2+ 2.1 nM 10–20 nM
[106]
15 Tapered fiber with sensing Glycine, 3-aminopropyltriethoxysilane, Hg2+ 22 pM 0–10.0 nM
[107]
probe and glutaraldehyde
Pb 2+ 20 nM 0–10.0 nM
[108]
16 Surface plasmon U shaped fiber Gold Nanoparticles Pb 2+ 2.1 ppb ———
[122]
resonance sensor
17 Glass cover film with 50nm BCAT immobilized chitosan thin film Pb 2+ ——— 30 ppb − 5 ppm
[123]
Au coating
8
18 MMF Si fiber Au nanoparticle Cd 2+ 0.16 ppb 0–6.77 × 10− M
[124]
19 AuNP coated fiber Gold chloride hydrate HAuCl4⋅3H2O Pb2+ ——— 0.67 mM to 30
[144]
mM
20 Surface Enhanced Raman D shaped Raman probe ZnOSFs Pb2+ 3.55 ppm 10 ppM-100 µM
[129]
Scattering (SERS)
21 Radiometric SERS Au@AgNPs Hg2+ 0.4 pM 0.001–0.01 nM
[130]
aptasensor
22 SERS-based HM ion sensor AuNR-PCL based nanocomposite fibers Cu 2+
Hg 2+ ——— ———
[137]
23 SERS and XPS based HM ion Au − TT Hg2+ Pb2+ 0.001 ppm 1 mM
[138]
sensor

*SM = Sensing mechanism.

16
A. Kumar Shakya and S. Singh Optics and Laser Technology 153 (2022) 108246

3. Discussion materials, and ultra-thin coating of blocking agents. Several optical fiber
methodologies and processes possess advantages and shortcomings,
This study has analyzed the emergence of several fiber optics sensors both simultaneously. Thus, a particular technique depends entirely on
developed to detect HM ions from water and aqueous solutions. These the application, e.g., if a high sensitivity from a sensor is required, then
sensors are demonstrated both experimentally and theoretically by sci­ etching or tapering processes can be adopted. Still, at the same time, one
entists and researchers. These sensors possess coating and functionalized has to compromise the mechanical strength of the sensor as these pro­
layers of advanced antigen, antibodies, chemicals, etc., for HM detec­ cesses increase sensitivity and reduce stability. The temperature is also
tion. These sensors have been broadly categorized into six different an essential factor while calculating the sensor’s accuracy. Increasing or
categories. HM ion sensors are based on Bragg grating, fiber modal decreasing temperature may cause expansion or contraction in the fiber
interference, optical absorbance, fluorescence, surface plasmon reso­ grating, resulting in variation in the sensor’s accuracy. HM ions sensors
nance, and surface-enhanced Raman scattering. Beside through spec­ are targeted towards a specific HM for which sensitive material coating
troscopy analysis techniques also, HM can be detected from liquid or some antigen and antibody coating is applied over the fiber. There­
solutions based on transmission (%) and absorbance (AU). Table 3 fore, it is essential to have apparent specific adsorption of particular HM
summarizes the outcomes obtained from the various optical sensing ions by the membrane. Thus, optical fiber-based HM ion sensors have
methodologies. shown good stability, high sensitivity, and better stability. The future
Thus, different fiber optic sensors possess various properties, struc­ scope for developing advanced HM ions sensors based on the demand
tural designs, and physical parameters. These fibers can be transformed and recent growth are expressed as follows.
into U − shaped, D − shaped, inverted U − shaped using tapering,
etching, etc. The SMF can be spliced with different thin core fibers, 1. Most of the HM ion sensors proposed in the literature are only
MMF, PCF to form a modal interferometer. Fiber surfaces are function­ theoretical models. The emphasis should be on developing a real-
alized with other material films of Au, Ag, Cu, AuNP, etc., for generating time HM ion sensor by improving long-time usage and reversibility
exciting the SPR effect within the fiber. Functionalized DNA chains, stability. The detection of HM from fiber optics sensor depends upon
different adsorbents, etc., are used as HM ions sensitive membranes. the thin material coat applied over the fiber for HM detection. The
Thus, various fiber optics sensors for detecting HM ions can be compared coating of thin film needs to be done precisely so that uninterrupted
based on the following features. Various advantages and disadvantages interaction between sensing film and evanescent field occurs.
of the fiber optic sensor for HM detection are summarized in Table 4. Different coating techniques like electrostatic self-assembling [155],
Ultimately, it has been observed from the presented work that optical BLB self-assembling [156], and Langmuir Blodgett [157] are effec­
fiber sensors have shown exponential growth in their physical structures tively used and proposed in the literature. But it has been observed
and detection capabilities with advancement in time. Optical fibers have that these sensitive films easily fall off and are not reusable. Thus, the
substantially increased structure flexibility, withstands electromagnetic first future work is to develop a more prominent and rigid method­
interferences, miniaturization, strong bonding with sensitive materials ology for fixing sensitive films with optical fiber. The sensor life can
and coatings, multipurpose applications, etc. Thus, optical fibers are be further increased to some extent.
broadly used in liquid sensing applications due to all these advantages. 2. The identification of the HM ions is strongly dependent on the
However, most of the sensor discussed in this work consists of composite interaction between the sensitive material and the HM ion.
geometrical structures, molecular composite polymers, sensitive nano­ Currently, polyelectrolytes like PSS [158,159]PAA, and CS [160] are
some of the popular materials for HM detection. However, they show
sensitivity towards different HM ions, thus offering low selectivity.
Table 4
Combining DNA bases with HM ions results in stable and robust
Advantages and disadvantages of various fiber optics sensors.
complexes [161]. Several aptamers of nucleic acids are used to detect
S. Fiber optic sensor Advantage Disadvantage
HM Hg2+ , Pb2+ , Cd2+ , Ag+ etc [162]. Besides, some conducting
No
polymers like PAni [163], PTh [164], PPy [165], etc., have also
1 Fiber Bragg Controllable and flexible Possess inherent demonstrated their ability to detect HM ions. In the future, the
grating-based structural design, large sensitivity towards change
optical sensors operational bandwidth, in strain, less mechanical
introduction of carbon nanotubes [166], graphene [167], and carbon
ideal multiplexing strength in FBG, and nanomaterials [168] can be used to detect HM ions with improved
capability, compact size, difficulty in signal selectivity and enhanced sensitivity.
reduced insertion loss demodulation in LPFG 3. Identifying the feasibility between new optical fiber and technolo­
[145] [146]
gies for HM detection is a great challenge. Appropriate technology
2 Fiber modal Easy to construct, long Low sensitivity, difficulty
interference-based term operation, simple in signal demodulation can provide a broad measurement range, high precision, and
optical sensors structure, inexpensive, [148] improved sensitivity. Sensors based on whispering gallery mode
repeatability, robustness (WGM) present high accuracy and sensitivity toward measured ob­
[147] jects [169]. Sensors based on fiber direction couplers show high
3 Optical Simple structural design Less mechanical strength,
absorbance based [149] sensitive towards external
sensitivity toward the external refractive index [170]. Vernier effect
sensors environment interferences can also be introduced to the sensor to increase its sensitivity [171].
and excitation light [150] Thus selecting an optimum sensing methodology for an advanced
4 Fluorescence- High sensitivity, Susceptible to light optical fiber is an area of investigation from future perspectives.
based optical portability, easy excitation and
4. Finally, a fiber optics sensor with multiple parameters detection is
sensors fabrication, highly environment fluctuations
accurate [151] [152] the need of the future. Generally, the HM ion is present in the water
5 Surface plasmon Ultra-sensitive, wide Fabrication losses, sample, which is affected by several other components like pH,
resonance-based range of resolution, complicated temperature, and other HM components. Thus an optical fiber sensor
optical sensors multiple analyte manufacturing to detect all these features is highly required. The main application of
detection [121] procedures, and expensive
equipment [123]
these sensors will be a comprehensive analysis of the water sample
6 Surface-enhanced Rapid data collection, Relative complexity of the for catching all the components present in the water. An optical fiber
Raman scattering sensitive, simple output signal and the sensor for detecting two components is demonstrated in [172]. Thus,
(SERS) sampling, and non- difficulty in obtaining the work in the proposed direction is started. In the coming time, a
invasiveness [153] repeatable signal
enhancements [154]

17
A. Kumar Shakya and S. Singh
new sensor will be evolved that can simultaneously detect various
elements, including HM, from the investigating sample.
4. Conclusion
Fiber optics sensors have tremendous potential to detect heavy
metals ion. These sensors possess several properties like minute size,
remote sensing monitoring, real-time investigation, chemical inertness,
non-reactiveness, etc., which are considered ideal for heavy metal
detection. This work discusses optical methods, such as fiber grating,
modal interference, fluorescence sensing, optical absorbance, surface
plasmon resonance, and surface-enhanced Raman scattering to detect
different heavy metals. These methods are described based on their
physical structures, sensitive materials, molecular structures, and
sensing characteristics. The advantages and disadvantages of the
particular method present their suitability to be used for specific ap­
plications. The future scope of the optical sensor presents innovations
that need to be adopted in fiber optics sensors fabrication to tackle
current challenges. Thus fiber optics sensors can be considered an effi­
cient device through which various heavy metals can be detected easily.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgments
“The authors are thankful to all anonymous reviewers and Editor-in-
Chief for their comments, concerns, queries, and constructive sugges­
tions. This R&D work is performed under the All India Council of
Technical Education (AICTE), National Doctoral Fellowship (NDF) for
the AICTE NDF RPS project sanctioned order no: File No.8-2/RIFD/RPS-
NDF/Policy-1/2018-19 dated 13 March 2019”.
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