Microchemical Journal 166 (2021) 106265

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Microchemical Journal
journal homepage: www.elsevier.com/locate/microc

Electrophoretic assembly of Sn-Bi film for the voltammetric determination

of Cd(II) and Pb(II)
Daixiong Zhang a, *, Qing Xiang b, *
a
College of Environment and Resources, Chongqing Key Laboratory of Catalysis and New Environmental Materials, Chongqing Technology and Business University,
Chongqing 400067, PR China
b
School of Materials and Architectural Engineering, Guizhou Normal University, Guiyang 550001, PR China

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

Keywords: In this work, a Sn-Bi film was successfully fabricated via the electrophoretic deposition (EPD) of nano-Sn powders
Electrophoretic deposition and nano-Bi powders in an ethanol dispersion medium. Study on film composition showed that a coefficient of
Bi proportionality between the mass ratio in the deposited film and that in the suspension was observed for the EPD
Sn
of Sn-Bi, which controlled the composition of the Sn-Bi film. Therefore, Sn-Bi films with different mass ratios
Electroanalysis
Film
were designed with this linear relationship for the codetection of Cd(II) and Pb(II). Square-wave anodic stripping
voltammetry (SWASV) measurements using an in-situ plating strategy were performed after the electrochemical
oxidation of Sn and Bi at 0.3 V for 120 s, and the results indicated that the Sn-Bi film with a mass ratio of 0.75
had the best determination ability.

1. Introduction when an electrode composed of Bi nanoparticles is employed [12].

Due to a very lower toxicity in comparison with traditional mercury
electrodes, bismuth-film electrodes (BiFEs) have been recently sug­
gested as an alternative for the determination of trace metal ions such as
Cd and Pb by stripping voltammetry [1–5]. During the detection of
metal ions, BiFEs exhibit high sensitivity and excellent peak resolution,
while being insensitive to the dissolved oxygen in aqueous solutions,
which make these electodes competitive for practical applications [6,7].
BiFEs can be prepared on the surface of the substrate in advance, or be
plated in situ onto the substrate during the preconcentration. Clearly,
substrate materials with large specific surface areas are more attractive
because they can provide more electrochemically active sites, which
helps to improve the electrochemical response signal. The other desir­
able attributes for ideal BEFs are a low background current (high signal-
to-noise ratio), and reproducible response [8,9]. Therefore, the method
of modifying the substrate with bismuth is critical for the satisfactory
performance of BiFEs.
The in-situ plating method is known as the most widely used strategy
for forming bismuth films by directly adding Bi(III) ions into the sample
solution [10,11]. As a special in situ plating strategy, a means of
generating a bismuth film in-situ without using Bi(III) salts can be
realized through a pre-electrochemical oxidation from Bi to Bi(III) ions
The chemical composition of BiFEs also has a significant impact on
the determination ability. Generally speaking, the determination ability
of BiFEs can be further improved by doping suitable substances, and
these substances can be divided into two types: (1) carbon materials,
include graphene [13,14], carbon nanotubes [15], carbon paste[16,17],
etc. These carbon materials can enhance the conductivity and specific
surface area of BiFEs, which is beneficial to improve the electrochemical
response signal. (2) other doped metals, and gold is the most reported
one [11,18]. The improvement in determination ability of BiFEs may be
attributed to the synergic effect, the large surface and good electrical
conductivity caused by the doped gold. Moreover, doping Sn into the Bi
film can also significantly enhance its detection ability [4]. As a non-
precious metal, Sn-Bi film electrode has a more attractive prospect
than Au-Bi film electrode. Therefore, assembling a film electrode con­
taining both Bi and Sn nanoparticles may be a new route for enhancing
the detection ability.
Electrophoretic deposition (EPD) is an attractive method that can
assemble nanoparticles into a film architecture. EPD has many advan­
tages such as its simplicity, low cost, easy controllability of film thick­
ness, and wide adaptability to complex shapes [19–24]. In this work, we
present the first attempt at fabricating Sn-Bi films with EPD by
employing Bi and Sn nanoparticles. With an EPD kinetics study for Sn

* Corresponding authors.
E-mail addresses: 224178187@qq.com (D. Zhang), 373519326@qq.com (Q. Xiang).

https://doi.org/10.1016/j.microc.2021.106265
Received 17 December 2020; Received in revised form 4 April 2021; Accepted 5 April 2021
Available online 20 April 2021
0026-265X/© 2021 Elsevier B.V. All rights reserved.
D. Zhang and Q. Xiang
and Bi, a suitable dispersion system for both nano-Sn and nano-Bi was
introduced. An efficient route to control the composition of the Sn-Bi
film was also explored, and the influence of the film composition on
the detection ability was investigated.
2. Experimental section
2.1. EPD of nano Sn and nano Bi film
Nano-tin (nano-Sn, 40 nm, 99.9%), nano-bismuth (nano-Bi, 100 nm,
99.9%) were purchased from Beijing DK Nano Technology Co., Ltd.
(Beijing, China), Polyethyleneimine (PEI) with an average molecular
weight of 10,000, was purchased from Aladdin Chemical Co., Nitric acid
(HNO3, 69%), iron(III) nitrate nonahydrate (Fe(NO3)3⋅9H2O, 98.5%),
cobaltous nitrate (Co(NO3)2⋅6H2O, 98.5%), nickel(II) nitrate hexahy­
drate (Ni(NO3)2⋅6H2O, 98.5%), and anhydrous ethanol (C2H5OH,
99.5%) were obtained from Chengdu Chemical Reagents (Chengdu,
China). All the chemicals were used without further purification.
Ethanol was employed as the solvent for the suspension mixture, and
PEI (1 wt% dissolved deionized water) and nitric acid (0.1 M) were used
as additives to improve the deposition behavior of nano Sn and nano Bi.
For all EPD processes, the solid loading amounts of nano-Sn and nano-Bi
were 1 g⋅L-1. The suspensions were dispersed under ultrasonication for
30 min to break up agglomerated particles. For the codeposition process,
the mass ratio of nano-Sn to nano-Bi in the suspension (Rs) was adjusted
in the weighted samples.
EPD was performed in the suspension with a constant voltage of 50 V
for 10 min. Graphite sheet and titanium (Ti) sheets were used as the
anode and cathode, respectively. After deposition, the cathode was
removed from the suspension. The as-deposited films were dried in an
oven at 60 ℃ for 1 h, and the deposit was weighed by an electric balance
with precision of ± 0.10 mg.
2.2. Characterization
The phase composition of the films was measured with X-ray
diffraction (XRD, 6000, Shimadzu, Japan). The morphology and
elemental distribution of the film were analyzed using field emission
scanning electron microscopy (FESEM, JSM-7800F, JEOL), and the mass
ratio of nano-Sn to nano-Bi in the deposited film (Rd) was measured by
atomic absorption spectroscopy (AAS, 180–80, Exter Analytical, USA).
2.3. Square-wave anodic stripping voltammetry (SWASV) measurements
for the determination of heavy metals
For the SWASV test, a glassy carbon electrode (GCE, with diameter of
3 mm, Gaossunion, Wuhan) was used instead of the Ti sheet as the
cathode substrate for preparing the nano-Bi film. All stock solutions of
Cd(II) and Pb(II) were prepared at 0.01 mol⋅L-1 concentration from
analytical grade chemicals in 18 MΩ⋅cm− 1 deionized water. Square-
wave anodic stripping voltammetry (SWASV) was performed with a
CHI 660 electrochemical workstation (Shanghai Chenhua, China) in
combination with a magnetic stirrer. SWASV was used in the measure­
ment of the stripping voltammograms. A three-electrode arrangement
was used in all experiments. A Ag/AgCl (3 mol⋅L-1 KCl) electrode and a
platinum sheet were used as the reference electrode and counter elec­
trode, respectively. A deaerated acetate buffer solution with a concen­
tration of 0.1 mol⋅L-1 (pH = 4.5) was used for all electrochemical
measurements. The predissolution of the Sn-Bi film was performed via
electrochemical oxidation at 0.3 V (vs. SCE) for 1 min in a 0.1 M acetate
buffer solution (pH 4.5). The potential and time for the preconcentration
of Cd and Pb was − 1 V and 5 min, respectively. The equilibration time
was 15 s, after which the voltammogram in differential pulse mode was
recorded with an anodic scan (pulse height of 25 mV). The scan was
terminated at − 0.3 V. After each measurement the electrode surface was
renewed with a constant potential at − 0.3 V. For the analysis of real
2
Microchemical Journal 166 (2021) 106265
samples, the deaerated acetate buffer solution with a concentration of
0.1 mol⋅L-1 (pH = 4.5) was made of the waste water obtained in our
laboratory, and the precise concentration of Cd(II) and Pb(II) for the
waste water samples were measured by flame atomic absorption spec­
trometry (FAAS).
3. Results and discussion
3.1. EPD for both nano-Sn and nano-Bi
It is well known that a successful EPD of multicomponent film mainly
depends on a suitable additive scheme that can charge each kind of
particle surface with the same sign. In this work, the influence of PEI and
nitric acid on the deposition rate of nano-Sn and nano-Bi was investi­
gated. Moreover, as reported by Tang [25], the simultaneous addition of
acid and PEI might have a positive synergistic effect on the deposition
rate in certain cases. Therefore, three additive schemes were selected in
this work: 1) PEI, 2) nitric acid, and 3) PEI + nitric acid.
The effect of the additive on the deposition rate of nano-Sn is shown
in Fig. 1a. It can be clearly seen that the deposition rate increases first
and then decreases with the increasing addition of both PEI and nitric
acid. However, the absolute value of deposition weight per area
(mg⋅cm− 2) with the PEI addition (1.51 mg⋅cm− 2 for 10.00 mg⋅L-1 PEI) is
much higher than that with the nitric acid addition (0.11 mg⋅cm− 2 for
0.10 mM nitric acid). These results show PEI is a suitable additive for the
EPD of nano-Sn. Unexpectedly, for the bi-additive of PEI + nitric acid, no
positive synergistic effect on the deposition rate for nano-Sn was
observed (Fig. 1b), and the deposition rate even slightly decreased with
the increasing addition of nitric acid. However, the attenuation of the
deposition rate was not substantial (1.31 mg⋅cm− 2 for 0.50 mM nitric
acid + 10.00 mg⋅L-1 PEI vs 1.51 mg⋅cm− 2 for 10.00 mg⋅L-1 PEI). In other
words, both PEI and PEI + nitric acid could be used for the successful
EPD of nano-Sn films.
For nano-Bi, as shown in Fig. 1c, when the added PEI and nitric acid
are in the same concentration range as the EPD of nano-Sn, the depo­
sition rate also increases first and then decreases. The optimum con­
centrations of PEI and nitric acid are 10.00 mg⋅L-1 and 0.50 mM
respectively, and the corresponding deposition weights per area are 0.81
and 0.91 mg⋅cm− 2 respectively. Moreover, a positive synergistic effect of
the bi-additive of PEI + nitric acid also occurs with to the deposition rate
of nano-Bi (Fig. 1d). With the addition of 0.50 mM nitric acid + 10.00
mg⋅L-1 PEI, the deposition rate of nano-Bi significantly increases (2.78
mg⋅cm− 2).
Thus, for designing the Sn-Bi film, we suggest that a bi-additive of
PEI + nitric acid is more suitable. With this type of additive, although a
small compromise has been made on the deposition rate of nano-Sn, the
feasibility of the simultaneous deposition of nano-Sn and nano-Bi can be
ensured.
3.2. Characterization of the nano-Sn and nano-Bi film
Fig. 1e-f shows both the nano-Sn and nano-Bi films fabricated by
EPD. Regions of large-scale component separations are not observed
optically in the smooth films, which exhibit good film characteristics
and uniformity. Furthermore, the XRD patterns of the film obtained
from EPD at 50 V for 10 min are shown in Fig. S1a-b. The XRD patterns
are mainly indexed to Sn (JCPDS card no. 65–0296) and Bi (JCPDS card
no. 44–1246). These results indicate that both the nano-Sn and nano-Bi
films are successfully prepared.
The SEM images of both the nano-Sn and nano-Bi films prepared by
EPD are shown in Fig. S2a-b. From the top-view images, both the nano-
Sn and nano-Bi films exhibit a homogeneous and uniform morphology,
which is in line with the expectation of preparing smooth and flat
microscale films by the EPD method.
D. Zhang and Q. Xiang Microchemical Journal 166 (2021) 106265

Fig.1. (a) The deposition weight of Sn film as a function of addition of nitric acid and PEI, (b) deposition weight of Sn film versus addition of nitric acid with 10 mg⋅L-
1
PEI. (c) The deposition weight of Bi film as a function of addition of nitric acid and PEI, (d) deposition weight of Bi film versus addition of nitric acid with 10.00
mg⋅L-1 PEI. Images of electrophoretic (e) nano-Sn film and (f) nano-Bi film fabricated by EPD.

3.3. Design for controlling the Sn-Bi film composition

The composition of the Sn-Bi film plays an important role in its

ability to detection metal ions [4]. Therefore, it is crucial to design a
simple and effective method for controlling the composition of electro­
phoretic films. Due to the difference in the deposition rates between the
Sn (1.31 mg⋅cm− 2) and Bi nanoparticles (2.78 mg⋅cm− 2) with the
employment of the bi-additive of 0.50 mM nitric acid + 10.00 mg⋅L-1
PEI, the mass ratio of Sn to Bi in the deposited Sn-Bi film (Rd) is different
from the mass ratio of Sn to Bi in the Sn-Bi suspension (Rs). In previous
work, we have reported that a linear relationship between Rd and Rs is
feasible for the EPD of bicomponent films [26,27]. Thus, the validity of
the linear relationship for designing the Sn-Bi film was verified here.
Five samples were prepared by EPD with Rs values of 0.50, 1.00, 1.50,
2.00 and 2.50. The Rd of the five samples measured by the AAS method is
plotted as a function of Rs in Fig. 2. As expected [26,27], there is a linear
translation between Rd and Rs, which is shown in equations below. This
linear relationship between Rs and Rd can facilitate further research on
the optimum equivalence ratio in the Sn-Bi film for the purpose of
improving detection ability. Fig.2. Mass ratio in the deposited Sn-Bi film (Rd) as a function of mass ratio in
Rd = 0.47*Rs 2
R = 0.9998 the Sn-Bi suspension (Rs).

Using this equation, five samples with Rd values of 0.25, 0.50, 0.75,
1.00 and 1.50 were prepared for the detection of metal ions.
3.4. Determination of Cd and Pb by the electrophoretic Sn-Bi film
The stripping responses of the five samples are shown in Fig. S3a. The
concentrations of both Pb(II) and Cd(II) were 7.00 × 10-8 mol⋅L-1. In the
anodic stripping voltammetry performed under the same conditions, the
stripping oxidation peaks of Cd and Pb appear at potentials of approx­
imately − 0.75 and − 0.55 V, respectively. For both Pb(II) and Cd(II), the
Sn-Bi film with an Rd of 0.75 exhibits the highest current response.
Therefore, the Sn-Bi film with an Rd of 0.75 was employed in the
following work. The comparison of the detection ability between the Sn-
Bi film with an Rd of 0.75 and the pure Bi film is shown in Fig. S3b. The
stripping oxidation peaks of Cd and Pb on the Sn-Bi film with an Rd of
0.75 are much higher than those of the pure Bi film, which is a strong
evidence that the detection ability for the Bi-based film electrode can be
significantly improved by doping with Sn.
The influence of the preconcentration time on the sensitivity of the
stripping oxidation peak currents of 7.00 × 10-8 mol⋅L-1 for Cd(II) and Pb
(II) from 1 to 10 min is shown in Fig. S4. The stripping oxidation peak
currents of the Cd(II) and Pb(II) at the Sn-Bi film electrodes increase

3
D. Zhang and Q. Xiang
rapidly with the preconcentration time and then decrease slightly. Thus,
an accumulated time of 5 min was chosen, because it provides an
adequate sensitivity to determine Cd(II) and Pb(II).
The measured curves of the Sn-Bi film at different concentrations of
both Cd(II) and Pb(II), along with calibration plots inside, are shown in
Fig. 3. The stripping oxidation peaks of Cd and Pb appear at potentials of
− 0.77 and − 0.53 V, respectively. All of the peaks are well resolved and
increase linearly with the metal concentration from 7.00 × 10-8 to 7.00
× 10-7 mol⋅L-1. Calibration curves for the electrophoretic nano Bi film
can be represented by equations:
ICd = 8.48 + 0.70CCd , R2 = 0.9965
IPb = 0.52 + 1.40CPb , R2 = 0.9946
where I is the stripping oxidation peak current in μA and C is the
concentration of Cd or Pb in 10-8 mol⋅L-1. The correlation coefficients
(R2) of the calibration curve are 0.9965 (for Cd) and 0.9946 (for Pb). The
high linear correlation coefficient between the current and metal-ion
concentration indicates the potential of the electrophoretic Bi film in
the design of electrochemical sensors.
Repeatability is an important evaluation index of the detection
reliability for electrochemical sensors. The repeatability test of the Sn-Bi
film electrodes with am Rd of 0.75 was conducted with 3 consecutive
measurements in a 0.10 mol⋅L-1 acetate buffer solution containing target
metals at a concentration of 2.00 × 10-7 mol⋅L-1. As shown in Fig. 4a, the
Sn-Bi film electrode shows good repeatability of the stripping oxidation
peak currents: the relative standard deviations (RSD) for Cd(II) and Pb
(II) are 1.36 and 1.50%, respectively.
Moreover, we also investigated the reproducibility between the Sn-Bi
film electrodes. Three GCEs were connected in parallel as anodic sub­
strates to prepare Sn-Bi film electrodes with an Rd of 0.75, and the ob­
tained samples were denoted as Sn-Bi-1, Sn-Bi-2, and Sn-Bi-3. The
stripping oxidation peak currents of Cd(II) and Pb(II) at the three Sn-Bi
film electrodes are shown in Fig. 4b. The RSDs for Cd(II) and Pb(II) are
2.27 and 1.91%, respectively. This result indicates that the electrodes
prepared under the same EPD conditions have reliable detection
Fig.3. Square-wave stripping voltammograms (Estep = 10 mV, Epulse = 50 mV and frequency 50 Hz). Dependence of stripping oxidation peak currents of the
electrophoretic Sn-Bi film on the concentration of target metals in 0.10 mol⋅L-1 acetate buffer (pH 4.5); preconcentrated at − 1 V for 5 min, calibration plots inside.
4
Microchemical Journal 166 (2021) 106265
performance.
Usually, the sample solution of heavy metal ions also contains other
metal ions, so the stripping oxidation peak currents of ideal electro­
chemical sensors for Cd(II) and Pb(II) should not show interference by
other metal ions. In this work, an interference study for the Sn-Bi film
electrode was also performed by adding Fe(III), Co(II), and Ni(II) solu­
tion into the sample solution containing 2.00 × 10-7 mol⋅L-1Cd(II) and
Pb(II). The concentrations of Fe(III), Co(II), and Ni(II) solutions were all
fixed at 2.00 × 10-6 mol⋅L-1. The electrochemical oxidation peak cur­
rents of Cd(II) and Pb(II) with and without the addition of interfering
ions are shown in Table 1, and the relative signal change is also calcu­
lated. The absolute values of relative signal changes vary from 4.05 to
7.98%, which suggests a satisfactory selectivity for the simultaneous
determination of Cd(II) and Pb(II) ions.
The electrophoretic Sn-Bi film electrode with an Rd of 0.75 was also
selected for the real sample analysis. Firstly, the solution samples were
measured by Sn-Bi film electrode and FAAS method, respectively. Then,
the solutions added 1.00 × 10-7 mol⋅L-1Cd(II) and Pb(II) were measured
by Sn-Bi film electrode again. The measured result is shown in Table. 2,
the results showed that the electrophoretic Sn-Bi film electrode has a
high degree of accuracy (in all cases the recovery values were within
90.0–110.0%) [28], which exhibiting great potential in designing novel
electrochemical sensors.
4. Conclusion
In summary, the fabrication of a Sn-Bi film via EPD method was
successfully realized by employing an additive. The composition of the
Sn-Bi film could be easily tuned by changing the mass ratio of Sn to Bi in
suspension via a simple linear transformation, which resulted improving
the sensitivity of metal-ion detection. These findings exhibit an exciting
improvement in the potential applications of designing Sn-Bi films as
electrochemical determination sensors for heavy metal ions.
D. Zhang and Q. Xiang Microchemical Journal 166 (2021) 106265

Fig.4. (a) Repeatability of stripping oxidation peak currents of the Sn-Bi film electrodes with 2.00 × 10-7 mol⋅L-1 Pb(II) and Cd(II), preconcentration time: 5 min. (b)
Reproducibility of stripping oxidation peak currents of Sn-Bi-1, Sn-Bi-2, and Sn-Bi-3 film electrodes with 2.00 × 10-7 mol⋅L-1 Pb(II) and Cd(II), preconcentration time:
5 min.

org/10.1016/j.microc.2021.106265.
Table 1
Effect of interference ions on the detection of 2.00 × 10-7 mol⋅L-1Cd(II) and Pb
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