Journal of Luminescence 161 (2015) 117–122

Contents lists available at ScienceDirect

Journal of Luminescence
journal homepage: www.elsevier.com/locate/jlumin

Synthesis of carbon nanoparticles using one step green approach

and their application as mercuric ion sensor
V. Roshni, Divya Ottoor n
Department of Chemistry, Savitribai Phule Pune University, Ganeshkhind Road, Pune 411007, India

art ic l e i nf o a b s t r a c t

Article history: Carbon nanoparticles (CNPs) have been evolved as a promising candidate for the metal sensing
Received 26 September 2014 applications due to their synthesis from naturally occurring and easily available non-toxic molecular
Received in revised form precursors by green chemistry. A simple and one step procedure is reported here for the synthesis of
19 December 2014
CNPs from coconut milk by thermal pyrolysis at a temperature of 120–150 1C for 2–5 min without using
Accepted 23 December 2014
Available online 2 January 2015
any carbonizing or passivating agent. On pyrolysis the coconut oil is separated from the carbon rich
residue and the residue when dissolved in water showed blue fluorescence under UV light. The CNPs
Keywords: produced are found to show an emission maximum at 440 nm when excited at 360 nm. Synthesis by
Carbon nanoparticles (CNPs) green approach makes CNPs a promising substitute for the metal sensing applications. Series of metal
Fluorescence
ions which have a hazardous impact on the ecological system have been taken for the analysis and it is
Coconut milk
observed that the fluorescence of CNPs gets remarkably quenched by mercuric ions. Fluorescence
Metal ions
Quenching quenching was studied using standard Stern–Volmer quenching model. Limit of detection was found to
Limit of detection (LOD) be 16.5 nM Hg2 þ concentration.
& 2014 Elsevier B.V. All rights reserved.

1. Introduction
The scope of optical sensing has been broadened with the
invention of highly fluorescent non-toxic carbon nanoparticles
(CNPs) or carbon nanodots as the sensing probes [1–3]. Historically,
starting from the natural organic dye to the recent semiconductor
nanoparticles, the researchers have experimented with various
advances in this area. The latest one among them was the use of
semiconductor nanoparticles which shows some remarkable prop-
erties like high emission quantum yields, size-tuneable emission,
chemical and physical stability, narrow spectral bands, possibility of
surface modification for a specific sensing application, etc. [4]. But
they suffer from the serious limitation of major health problems
caused by the toxic effect of the heavy metal elements from which
they are produced [5]. In this scenario, the non-toxic CNPs are
benign alternative to semiconductor nanoparticles. Apart from the
high photo-stability and lack of any cytotoxicity, the size and the
excitation dependent photoluminescence are the versatile charac-
teristics of these carbon nanoparticles. Sun and co-workers had
synthesised carbon nitride dots from organic amines, N,N-dimethyl-
formamide, CCl4, etc. and these were successfully used for specia-
lised catalytic applications [6–11]. Yu and co-workers had reported
a lasing emission from carbon nanodots in organic solvents [12].
n
Corresponding author. Tel.: þ 91 20 25601395; fax: þ 91 20 25601728.
E-mail address: divya@chem.unipune.ac.in (D. Ottoor).
Hu and co-workers had prepared cabon nanodots from single chain
polymeric nanoparticles and investigated their photoluminescence
mechanism in organic solvents [13]. Various efforts were carried
out to synthesise carbon nanoparticles from natural precursors.
Peng and coworkers had used naturally occurring carbohydrates
like glucose [14], Yang and co-workers used sucrose, and citric acid
[15], and Sun and co-workers used pomelo peel [16], willow bark
[17], etc. for the synthesis of carbon dots. It is reported that the
optical, physical and chemical properties of produced CNPs are
influenced by the molecular precursors used, methodology and the
pre-treatment performed. Apart from optical sensing CNPs have
found widespread applications in the areas of bioimaging [18,19],
photocatalysis [20], optoelectronics [21], etc.
Synthesis of CNPs from naturally occurring and economically
viable molecular precursors and their promising application towards
various fields are important areas worth looking at. Application of
fluorescent nanomaterials as a luminescent probe is the current
trend. There are various reports on the use of the above mentioned
CNPs for the metal sensing application [22]. Still the application of
CNPs for the selective detection of metal ions is in the developing
stage. The environmental and health hazards caused by the presence
of toxic chemical waste containing heavy metals are of great concern
for the modern industrial world. Presence of even traces of mercuric
ions is a threat to the ecosystem due to their toxic nature [23].
Various sensitive and selective methods like atomic absorption
spectroscopy, liquid chromatography, adsorptive stripping voltam-
metry, electrochemical, spectrophotometry and spectrofluorimetry

http://dx.doi.org/10.1016/j.jlumin.2014.12.048
0022-2313/& 2014 Elsevier B.V. All rights reserved.
118 V. Roshni, D. Ottoor / Journal of Luminescence 161 (2015) 117–122
are used for the qualitative and quantitative estimation of mercuric
ions [24,25]. Among them, fluorescence spectroscopy has some
added advantages such as low cost, facile sample preparation, high
selectivity and easy detection [26]. So far many fluorescent probes
especially based on carbon dots are employed for the detection of
mercuric ions using various types of molecular precursors [27–31].
It has been reported that unmodified CDs can be used as a selective
and sensitive fluorescence probe for rapid detection of Hg2 þ . A good
linear correlation was observed over the concentration range of
0–3 mM, with a detection limit of 4.2 nM based on a 3δ/slope [32].
However, many of the methodologies used for the synthesis of CNPs
have the drawbacks of unfavourable reaction conditions like high
temperature, prolonged reaction duration, usage of oxidising agents,
the lack of aqueous solubility, etc.
Coconut milk which contains a high percentage of saturated fat
(lauric acid) is a rich source of coconut oil. Coconut oil is extracted
from coconut milk by thermal pyrolysis which is a traditional
method to synthesise the virgin coconut oil. In the food industry
normally the black residue obtained after the separation of coco-
nut oil is discarded. Herein, we report a novel approach for the
synthesis of CNPs from the waste by-product obtained by the
thermal pyrolysis of coconut milk. This pyrolysis procedure does
not involve any acid treatment or any surface passivating reagents.
The obtained residue is found to be water soluble and the solution
contains carbon nanoparticles of fluorescent characteristics. These
CNPs are highly fluorescent and photostable, dissolves readily in
water and other organic polar solvents and show excitation tune-
able emission spectra. The efficiency of CNPs for metal ions
sensing was tested using fluorescence quenching approach and
the analytical characteristics are discussed.
2. Experimental
2.1. Materials
Coconut milk was extracted from grated coconut. This was used
for the study without any preservatives. A.R. Grade Cupric nitrate
(Cu(NO3)2), cobalt nitrate (Co(NO3)2), cadmium nitrate Cd(NO3)2,
mercuric chloride (HgCl2), nickel nitrate (Ni(NO3)2, lead nitrate Pb
(NO3)2, manganese sulphate (MnSO4) and iron sulphate (FeSO4)
were purchased from SDFCL and used as received without any
further purification. Triply distilled water was used as a solvent
throughout the experiment.
2.2. Instrumentation
The absorbance and fluorescence measurements were recorded
using a UV–vis spectrophotometer (Shimdzu spectrophotometer) and
spectrofluorimeter (JascoFP-8300), respectively. The absorbance of
the sample was monitored between 200 nm and 600 nm. Excitation
Fig. 1. (A, B) Digital images of the coconut milk and crude CNPs produced by the thermal pyrolysis of coconut milk, respectively. (C) Photographs of CNPs excited under
daylight at 360 nm. (For interpretation of the references to colour in this figure, the reader is referred to the web version of this article.)
wavelength was kept at 360 nm and emission was recorded from
365 nm to 600 nm. The slit width for excitation and emission was
kept at 2.5 nm for all the measurements. An Infrared spectrometer,
FTIR-8400 (Shimadzu) was used to characterise the functional groups
on the CNPs. A transmission electron microscope (TEM, Model
TECNAI G2-20 U-Twin) with an operating voltage of 200 kV was
used for the physical characterisation of the synthesised CNPs. The
fluorescence life time measurements were carried out using a FL-
TCSPC fluorescence spectrometer (Horiba Jobin Yvon Inc., France).
2.3. Synthesis
Fig. 1 shows the facile and one step synthesis of carbon nanopar-
ticles from coconut milk in a cost effective and greener method. This
involves the thermal pyrolysis of coconut milk under a mild tempera-
ture range of 120–150 1C for 2–5 min. On heating the sample, coconut
oil was separated leaving behind a black residue. This residue obtained
after the separation of coconut oil was air dried.
The dried sample was easily dispersed in water and an appreci-
able amount of the substance get dissolved in water and shows a
yellowish brown colour as shown in Fig. 1C. The undissolved particles
are removed by filtration and the centrifuged solution showed
an appreciable blue fluorescence when exposed to UV light. These
lyophilised CNPs were diluted with water till the appropriate
concentration was reached and used for further analysis and sensing
applications.
3. Results and discussion
3.1. Morphology and fluorescence characteristics
A few drops of CNPs aqueous solution is placed on a copper
grid and dried and viewed under TEM. Fig. 2 shows the TEM and
HRTEM images of the sample which contains spherical shaped
carbon nanoparticles with an average size distribution ranging
from 20 nm to 50 nm. This large size range could be the result of
inhomogeneous pyrolysis process adopted in the synthetic step.
Fourier Transform Infrared spectroscopy was used to determine
the functional groups present in carbon nanoparticles. FTIR spectrum
of carbon nanoparticles produced from coconut milk is shown in
Supporting information (Fig. S1). A characteristic absorption peak is
observed at 3354 cm  1 which is due to –OH in the alcohol or phenol
group. The stretching vibration bands at 2929 cm  1, 1647 cm  1 and
1284 cm  1 are due to alkyl C–H bond, C–O bond in the amide groups
and C–O bond in carboxylic acid, respectively. The bending vibration
band of aromatic C–H bond was found at 887 cm  1, suggesting the
presence of alcohol or phenol, alkyl, carboxylic acid, amide and
aromatic groups.
Fig. 3 shows the UV–vis absorbance spectrum of CNPs when
dispersed in water. The absorption spectrum shows an edge at
 V. Roshni, D. Ottoor / Journal of Luminescence 161 (2015) 117–122
Fig. 2. The TEM image of the CNPs produced by the thermal pyrolysis of coconut milk at 120–150 1C for 2–5 min.
Fig. 3. UV/vis absorption spectra of the produced CNPs.
276 nm which can be attributed to the π–π* transitions of the
functional groups. The emission spectra (Fig. 4A and B) of CNPs are
broad, ranging from 423 nm to 484 nm depending on the excitation
wavelength which varied from 320 nm to 420 nm. As the excitation
wavelength is increased the emission peak position get shifted to
longer wavelength. The maximum emission intensity is obtained at
440 nm when exited at 360 nm. Then intensity of fluorescence
spectrum decreases and shows a red-shift when excitation wave-
length changes from 360 nm onwards. The red-shift in fluorescence
emission spectra may be due to different sized carbon nanoparticles
in the sample. These excitation tunable emission spectra are
considered to be the versatile characteristic of CNPs and this
property may be due to quantum confinement, size distribution
or the presence of emissive traps on the surface [33].
The effect of pH on the fluorescent property of CNPs was also
studied. The fluorescence characteristic of the CNPs strongly depends
upon the pH value as shown in Fig. 5. Appreciable quenching is
evident in the acidic and basic pHs with maximum emission
intensity at the neutral medium. This pH effect enables the CNPs to
be used as an efficient sensing probe in the neutral pH especially in
biological systems. Fig. 5 shows the fluorescence response of the
CNPs when irradiated continuously for 1 h with an excitation
wavelength of 360 nm. The CNPs were able to retain about almost
100% of fluorescence after 1 h proving its good photo-stability.
119
3.2. As a metal sensing probe
Although there are a large number of reports of Hg2 þ sensors,
simple and effective detection of the ion still remains a challenge.
Considering its remarkable fluorescent property the thought of
utilising CNPs as a metal sensing probe came into the picture. This
study was encouraged by the reports which suggested that
irrespective of the sources and method of preparation, the CNPs
could be used as potential sensing probes [34–39]. In view of this, a
detailed procedure was carried out to find the interaction of CNPs
with various metals. The metal ions were selected by keeping
in mind their presence in the industrial areas as well as their
hazardous impact on the environment. The metal ions selected
were Pb (II), Ni (II), Co (II), Cd (II), Hg (II), Zn (II), Mn (II) and Fe (II).
The metal ion concentration in the solution was maintained at
100 mM. From Fig. 6, it is evident that the fluorescence of CNPs has
been quenched in the presence of metal ions. Out of these, Hg (II)
shows appreciable quenching of fluorescence. This observation is
very interesting because the presence of Hg (II) is considered to be
the major culprit for industrial pollution. The fluorescence quench-
ing of CNPs with Hg (II) ions could be due to the facilitation of non
radiative electron/hole recombination through an effective charge
transfer process [32]. Recombination of excited electrons in the
conduction band with the holes in the valence band could be a
possible reason for this metal mediated fluorescence quenching.
This charge transfer process may be a strong binding interaction
between Hg (II) and the functional groups mainly hydroxyl and
carboxyl or carbonyl groups present on CNPs surface. The fact that
without doing any surface modification these CNPs are selective
towards Hg (II) makes this study interesting.
3.3. Analytical characteristics of fluorescence quenching
For analysing the fluorescence quenching characteristics of
CNPs by metal ions, three series of solutions were prepared. The
metal ions concentrations in these three sets vary from 1 mM to
10 mM, 10 mM to 100 mM and 10 nM to 100 nM. Fluorescence
intensity of CNPs in the absence and in the presence of metal ions
was recorded. Fluorescence spectrum of CNPs with various metal
ions concentrations is shown in Fig. 7. From this figure, it is
evident that the quenching is very less in nanomolar concentra-
tions and becomes appreciable in micromolar concentrations.
Standard Stern–Volmer relationship explains the phenomenon
of bimolecular fluorescence quenching. A linear relationship was
observed showing an increased quenching with concentration. From
the Stern–Volmer plots the analytical characteristic of quenching is
120 V. Roshni, D. Ottoor / Journal of Luminescence 161 (2015) 117–122

Fig. 4. (A) Excitation and emission spectra of CNPs. (B) Normalised emission spectra of CNPs when excited at wavelengths ranging from 320 nm to 420 nm in 10 nm
increment. Inset: emission spectra of CNPs without normalisation.

700 600

pH 2
600
pH 4 500
pH 7
500 pH 9
pH 12 400
Intensity(a.u)

Intensity(a.u)

400
300
300

200
200

100
100

0 0
400 450 500 550 0 10 20 30 40 50 60
Wavelength(nm) Time(min)

Fig. 5. (A) Fluorescence spectra of CNPs in different pH conditions. (B) Fluorescence intensity of CNPs with respect to time on continuous irradiation for 1 h.

determined. The Stern–Volmer equation is represented as follows:
F0
¼ 1 þ K SV ½C 
F
where F0 and F are fluorescence intensities of the CNPs before and
after addition of metal ions, respectively. [C] is the concentration of
metal ions and KSV is the Stern–Volmer quenching constant. The
Stern–Volmer quenching plot based on the fluorescence data is
generated to evaluate KSV, which is the Stern–Volmer quenching
constant (Fig. 8).
A linear relation is obtained when concentration of metal ion is
plotted against F0/F value. Correlation coefficient (R2) and slope of
the line (KSV value) were obtained on fitting the data and were
found to be 0.98 and 3.1  105 M  1 respectively. The equation used
to find out limit of detection (LOD) is 3σ/s where σ denote the
standard deviation of CNPs corrected blank signals and s denote
the slope of the linear curve derived from Stern–Volmer equation.
In accordance to the linear relationship obtained by adding the
different concentration of Hg (II) ions to the CNPs, the limit of
ð1Þ detection (LOD) of the synthesised CNPs towards Hg (II) was
calculated. LOD was found to be 16.5 nM. This value is slightly
greater than the acceptable value mandated by the U.S. EPA for the
concentration of mercury in the drinking water (10 nM, 2 ppb);
however, the sensor can be useful in detecting inorganic mercury
in samples of biological products, rivers, lakes and also in samples
where regulations for mercury are less stringent.
The bimolecular quenching constant, kq has to be evaluated
using the average lifetime value of carbon nanoparticles and KSV
value. The relation between bimolecular quenching constant and
Stern–Volmer constant is given in the following equation:
K SV ¼ kq τ 0 ð2Þ
where KSV is the Stern–Volmer quenching constant and τ0 is the
fluorescence lifetime in the absence of metal ion. τ0 value was
 V. Roshni, D. Ottoor / Journal of Luminescence 161 (2015) 117–122 121

obtained using fluorescence lifetime measurements. The decay The kq value is calculated using the above expression and was
profile of CNPs shows tri-exponential decay with an average found out to be 1.7  1014 M  1 s  1 indicating the presence of both
lifetime of 1.81 ns. (Fig. S2, Supporting information). diffusion as well as static quenching in the system. The kq value
obtained is considerably larger than those possible for a diffusion-
controlled quenching in solution (about 1010 M  1 s  1) hence it is
2000

1.040

1500
1.035
Intensity(a.u)

1.030

1000

F/F0
1.025
2
R = 0.98287
1.020 -1
k SV =310626M
500
LOD =16.5nM
1.015

1.010
0
Blank Cd(II) Mn(II) Ni(II) Zn(II) Pb(II) Co(II) Fe(II) Hg(II) 0.0 2.0x10
-8
4.0x10-8 6.0x10-8 8.0x10-8 1.0x10-7
Metal Ions Concentration (moles/litre)

Fig. 6. The effect of different metal ions (concentration of 100 mM) on the emission Fig. 8. Stern–Volmer plot of fluorescence quenching of CNPs with mercuric ions
intensity of the CNPs (excitation wavelength at 360 nm). (10–100 nm).

1400
2000
Blank 0μΜ
1200 1800
1μΜ 10μΜ
2μΜ 20μΜ
1600
1000 3μΜ 30μΜ
4μΜ 1400
40μΜ
Intensity(a.u)

5μΜ 50μΜ
Intensity(a.u)

800 6μΜ 1200 60μΜ

7μΜ 70μΜ
8μΜ 1000 80μΜ
600 9μΜ 90μΜ
800 100μΜ
10μΜ

400 600

400

200
400 450 500 550 350 400 450 500 550 600
Wavelength(nm) Wavelength(nm)

2500 Blank
10nM
20nM
2000 30nM
40nM
50nM
60nM
Intensity(a.u)

1500
70nM
80nM
90nM
1000
100nM

500

0
400 450 500 550 600
Wavelength(nm)

Fig. 7. Fluorescence quenching of CNPs in the presence of mercuric ions of concentration (A) 1–10 mM, (B) 10–100 mM and (C) 10–100 nM.
122 V. Roshni, D. Ottoor / Journal of Luminescence 161 (2015) 117–122
Table 1
Comparison of different fluorescent probes for Hg (II) detection.
Sr. no Fluorescence probe
1 Carbon dots
2 Carbon dots
3 CPs
4 Histidine based C dots
5 Carbon dots
6 Carbon dots
7 Carbon dots
8 Carbon dots
9 N-CQDs
10 CNPs
evident that some types of binding interaction is existing between
fluorophore and quencher.
The response of CNPs as a sensor for mercuric ions is compared
with the other recently reported mercuric sensor based on carbon
dots/nanoparticles. The details regarding the fluorescent probe
employed, detection limit, linear range and reference are provided
in Table 1.
The feasibility of CNPs for detecting Hg (II) in real water
samples was explored by taking tap water sample spiked with
standard solutions containing different concentrations of Hg (II).
Fluorescence intensity decreases with increased concentration of
Hg (II) from 10 to 100 nM. Calibration plot is developed with F0/F
along y axis and metal ion concentration along x axis. The solution
which is spiked with 50 nM Hg (II) is predicted using the calibra-
tion graph and a concentration of 57 nM Hg (II) is achieved with a
percentage error of 14.6%. The experiment was performed thrice
and a standard deviation of 7.4 was obtained. These results show
that the fluorescent probe obtained is capable of detecting
mercuric ion and can be effectively used for further research.
4. Conclusion
We have adopted a general strategy for preparing the CNPs
from a bio-precursor which is economically cheap and naturally
abundant. The conversion method involved was simple thermal
pyrolysis without any passivating or stabilizing agents. The CNPs
produced were highly fluorescent and show a blue fluorescence
when excited at 360 nm with λem at 440 nm. Due to their excellent
photoluminescent property the synthesised CNPs were utilised for
the metal sensing application where the intensity of fluorescence
of CNPs was effectively quenched by Hg (II) ions.
Acknowledgements
This work is financially supported by the Science and Engineer-
ing Research Board (SERB), Department of Science and Technology
(DST), New Delhi, India (SB/FT/CS-109/2012) and the authors are
thankful to IISER Pune and Physics Dept., SPPU for TCSPC and TEM
facilities, respectively.
Appendix A. Supporting information
Supplementary data associated with this article can be found in
the online version at http://dx.doi.org/10.1016/j.jlumin.2014.12.048.
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