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Fast adsorption of methyl blue on zeolitic

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imidazolate framework-8 and its adsorption

Cite this: RSC Adv., 2016, 6, 109608
mechanism†
Yi Feng,a Yu Li,a Minying Xu,a Shichang Liua and Jianfeng Yao*ab

Received 26th September 2016
Accepted 7th November 2016
DOI: 10.1039/c6ra23870j
www.rsc.org/advances
Zeolitic imidazolate framework-8 (ZIF-8) is synthesized and the adsorption behavior and mechanism of
methyl blue (MB) are studied in detail. Results show that ZIF-8 has a higher MB adsorption capacity than
most of adsorbents reported so far (the maximum adsorption capacity of ZIF-8 is 2500 mg g
1) and a fast
adsorption rate (sorption saturation can be achieved within 30 min). The adsorption kinetics and isotherms
were studied in detail. The mechanism study shows that the existence of Zn2+ exposed on the surface of
ZIF-8 nanoparticles plays an important role in the high adsorption of MB and the ionic bonding between
Zn2+ in ZIF and –SO3
in MB is formed. ZIF-8 nanoparticles also show high adsorption selectivity with
negligible adsorption for other dyes such as rhodamine B, methylene blue and methyl orange.

three-dimensional structures constructed from tetrahedral zinc

1. Introduction
Industrial dye effluents, such as paper, plastics, leather, phar-
maceutical, food, textiles and cosmetics, have always been
a serious environmental problem.1–4 Most of the dyes are toxic
and may cause direct destruction to aquatic communities.
Therefore, before discharging wastewaters to aquatic ecosystems,
it is necessary to reduce dye concentration and remove them
from water. Compared to other methods, an adsorption process
is known to be a promising technique due to the ease of opera-
tion, high adsorption capacity and comparable low cost of
application and operation.5–7 Highly functional porous materials
with high surface area are generally used as suitable adsorbents
to enhance adsorption efficiency for removing of dyes.
Metal–organic frameworks (MOFs) are crystalline porous
materials that are well known for their various application.8–10
The particular interest in MOF materials is due to the easy
tunability of their pore size and their high surface area.
Therefore, MOFs are widely used in the eld of adsorption,
separation and storage of gases and vapors. Recently, several
MOF materials such as UiO-66, MIL-101 and MIL-53 have been
tried as adsorbents to remove dyes from water and moderate
adsorbing capacity was achieved.11,12
Zeolitic imidazolate frameworks (ZIFs) is a subclass of
MOFs.13 In particular, ZIF-8 is one of the most studied proto-
typical ZIF compounds, which are porous crystals with extended
a
College of Chemical Engineering, Nanjing Forestry University, Nanjing, Jiangsu
210037, China. E-mail: jfyao@njfu.edu.cn
b
Jiangsu Key Lab of Biomass-based Green Fuels and Chemicals, Nanjing, 210037,
China
† Electronic supplementary information (ESI) available. See DOI:
10.1039/c6ra23870j
ions bridged by imidazolate. Based on previous studies, zinc
oxide (ZnO) show high and fast adsorption for several kinds
of dyes such as methyl blue and red 23, because of the bonding
formed between ZnO and dyes.14 Therefore, ZIF-8 is very
promising to be used as high-efficient adsorbents to remove
certain kind of dyes from water considering the well-dispersed
zinc ions inside the pores and the high surface area (>1000
m3 g
1). In this study, the adsorption behavior of MB adsorbing
on ZIF-8 was studied via adsorption kinetics and isotherms and
the mechanism of why ZIF-8 show high adsorption selectivity
for MB over other dyes is discussed in details. Through this
study, we expanded the application of ZIF-8 as promising
adsorbents for MB and offered some valuable design knowledge
to the synthesis of high-efficient adsorbents for dye removal.
2. Materials and methods
2.1 Chemicals
Chemicals were used as received without a further purication
process. They include zinc nitrate hexahydrate ($99%, Tianjin
Kemiou Chemical Reagent, China), 2-methylimidazole (Sino-
pharm chemical reagent Co. Ltd., China), ammonium
hydroxide solution (NH3, 25–28%, Nanjing Chemical Reagent
Co. Ltd., China), anhydrous ethanol ($99.7%, Sinopharm
chemical reagent Co. Ltd., China), 4A zeolites (Tianjin Nanhua
Catalysis Co. Ltd., China) and ZSM-5 (Tianjin Nanhua Catalysis
Co. Ltd., China).
2.2 Sample preparation
ZIF-8 was synthesized according to previously reported
studies.15–18 In a typical synthesis, 2.97 g of zinc nitrate

109608 | RSC Adv., 2016, 6, 109608–109612 This journal is © The Royal Society of Chemistry 2016

Paper
hexahydrate (Zn(NO3)2$6H2O) was dissolved in 3 g of deionized
water; 1.64 g of Hmim was added in 20.75 mL ammonium
hydroxide solution; aer that zinc nitrate and Hmim solutions
were mixed together. The solution immediately turned into
milk-like suspension, and stirred for 10 min at room tempera-
ture to complete the crystallization. The sample was collected by
centrifugation and washed with deionized water three times
until the nal product had pH value of 7, then dried at 60  C
overnight.
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In order to study the effect of surface area on adsorption
capacity, ZIF-8 derived ZnO and ZnO@C were synthesized. ZIF-
derived ZnO and ZnO@C were obtained via calcination or
carbonization of as-synthesized ZIF-8 at 550  C for 2 h with
a heating rate of 5  C min−1.
2.3 Characterization
X-ray diffraction (XRD) patterns of the samples were obtained on
an Ultima IV diffractometer with Cu Ka radiation at a scan rate of
2 min
1 with a step size of 0.02 . Nitrogen adsorption–desorp-
tion isotherms were measured at liquid-nitrogen temperature
(77 K) using a volumetric adsorption analyzer (Micromeritics
ASAP 2020). Surface areas were determined by the Brunauer–
Emmett–Teller (BET) method. The surface chemistry of ZIF-8
aer MB adsorption was characterized using an X-ray photo-
electron spectroscopy (XPS, AXIS UltraDLD, Japan).
2.4 Adsorption kinetics and isotherms of methyl blue (MB)
The adsorption capacity of MB on the adsorbent is calculated
as:
Qt ¼ V(C0
Ct)/m
where V is the solution volume, C0 is the initial MB concentra-
tion, Ct is the MB concentration in the solution at a given time
(t), and m is the adsorbent mass. In a typical adsorption test,
20 mg adsorbent was added in 40 mL MB solution with the
initial concentration of 100, 300, 400, 500, 800, 1000 ppm at
room temperature (20  C). The concentration of MB was
determined with an UV-Vis spectrometer (TU-1900, Persee Co.
Ltd., China) at l ¼ 600 nm and then calculated using the
analytical calibration curve. For MB solution with high
concentration, the solution was diluted for several times before
test. The adsorption kinetics was investigated using pseudo-
second-order models, as described below:19,20
t 1 t
¼  þ
Qt k2 Q e 2 Q e
h ¼ k2Qe2
where k2 is the pseudo-second order rate constant (mg g
1
min
1), Qe is the sorption capacity at equilibrium, Qt is the
sorption at the time of t and h is the initial adsorption rate
(mg g
1 min
1). The h and k2 can be obtained by linear plot of
t/Qt versus t.
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For adsorption isotherms, Langmuir isotherm and Freund-
lich isotherm equation are used. A plot of Qe vs. Ce, the residual
concentration in the solution, was then performed to validate
the applicability of Langmuir isotherm and Freundlich
isotherm. The Langmuir isotherm equation is shown below:21,22
1 1 1
¼ þ
Qe Qm ðKL Ce Qm Þ
where Qm is the maximum amount of adsorption (mg g
1) and
KL is the Langmuir constant related to the energy of adsorption.
If the plot of 1/Qe vs. 1/Ce is linear, the adsorption is Langmuir
isotherm.
For Freundlich isotherm, the equation is calculated below:
log Ce
log Qe ¼ log KF þ
n
where KF and n are Freundlich constants. If the plot of log Qe vs.
log Ce is linear, the adsorption is Freundlich isotherm.
2.5 Desorption of MB and recyclability of adsorbents
Aer adsorption, the adsorbents were collected by centrifuga-
tion. The desorption was performed using ethanol to desorb the
MB from adsorbent for several times and dried at 60  C before
next cycle of adsorption.
3. Results and discussion
3.1 Characterization of ZIF-8
XRD pattern of the as-synthesized sample is shown in Fig. 1a.
According to the XRD pattern, the samples can be assigned to
ZIF-8 and no other phase was observed in such samples.18
Fig. 1b shows the morphology of as-synthesized ZIF-8. From
Fig. 1b, it can be seen that ZIF-8 is a cubic-like structure with
average particle size of approximately 0.5 mm. Fig. 1c shows
FTIR spectra of ZIF-8. The intense and convoluted bands at
1350–1500 cm
1 are associated with the entire ring stretching,
the bands in the spectral region of 900–1350 cm
1 are for the in-
Fig. 1 (a) XRD patterns of the as-synthesized ZIF-8; (b) SEM image of
as-synthesized ZIF-8; (c) FTIR spectra of as-synthesized ZIF-8 and (d)
N2 sorption isotherm of ZIF-8.
RSC Adv., 2016, 6, 109608–109612 | 109609
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plane bending of the ring, and the band at 421 cm
1 is ascribed
to Zn–N stretch.23 Fig. 1d shows the nitrogen adsorption–
desorption isotherm of ZIF-8. It can be seen that there is no
mesoporous structure and only microporous in ZIF-8. The BET
surface area and Langmuir surface area of ZIF-8 are 1007.4 and
1322.9 m3 g
1, respectively.

3.2 Adsorption kinetics

Fig. 3 (a) Langmuir adsorption and (b) Freundlich adsorption isotherm
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A series of experiments was conducted to study the adsorption of MB adsorbing on ZIF-8.

kinetics of MB on ZIF-8. The plots of Qt versus time (t) for various
initial concentrations of MB on such adsorbents are shown in
Fig. 2. The adsorption capacity of such adsorbents increases
that the surface of ZIF-8 has a uniform adsorption energy
dramatically within the rst 5 min, and then increases slowly
and the adsorption is mainly monolayer instead of multilayer.
until equilibrium within 30 min. The adsorption capacities at
Based on the Langmuir isotherm equations, the maximum
equilibrium for ZIF-8 are 199.0, 597.4, 794.6, 990.9, 1544.8,
adsorption capacity of ZIF-8 is 2500 mg g
1 with the Langmuir
1917.5 mg gadsorbent
1 with the initial MB content of 200, 600,
constant of 0.0889 L mg
1 (KL).
800, 1000, 1600 and 2000 mg gadsorbent
1 (Table 1).

3.3 Adsorption isotherms 3.4 Adsorption mechanism

The Langmuir model and Freundlich model are used to
describe the adsorption process. From Fig. 3, it can be seen that
Langmuir model is more applicable compared to Freundlich
model because of the higher correlation of coefficient obtained
in Langmuir model (the correlation of coefficient of Langmuir
and Freundlich model is 0.982 and 0.888 respectively). The
Langmuir model assumes that the adsorption is monolayer and
is dependent on the assumption that the adsorbent surfaces
consist of active sites having a uniform energy and the
adsorption energy is constant.24,25 Therefore, it can be indicated
Fig. 2 Adsorption kinetics at different concentrations (from bottom to
up: 100, 300, 400, 500, 800, 1000 ppm) of methyl blue on ZIF-8.
It has been reported that ionic bonding between the negatively
charged functional groups of MB (–SO3
) and positively charged
center of ZnO (Zn(OH)+) can be formed. Similarly, in this study,
the formation of ionic bonding between Zn2+ in ZIF-8 and –SO3

might be the main contribution to the fast and high
MB adsorption on ZIF-8.
In order to verify the occurrence of such interaction between
MB and ZIF-8, the surface chemical information at an atomic
scale was investigated by detailed XPS analysis. The XPS of ZIF-8
before and aer adsorption of MB is shown in Fig. 4. The
binding energy of Zn 2p at 1023 and 1046 eV shis to higher
energy and new peaks show aer adsorption of MB. The new
peaks are mainly attributed to the ionic bonding between Zn2+
and O2
ions in the sulfonic groups of MB. Similarly, the
binding energy of O 1s in MB also shis to higher energy, which
further proves the above-mentioned reaction.
It should be noted that the pore diameter of ZIF-8 is about
3.4 Å whereas the theoretical size of methyl blue is too big to
enter the pores. The dye molecules might be encapsulated
in interparticular pores and/or pores of the outer surface of the
particles. The intrinsic micropores might have a function for
solvent transport away from the adsorbed dye molecules.
In order to determine the role of zinc ions and the pores on the
adsorption capacities, ZIF-8 derived ZnO and ZnO@C, ZSM-5 and
4A zeolites were used to adsorb MB (20 mg adsorbent added into

Table 1 The equilibrium capacities, pseudo-second order rate

constant and initial adsorption rate of ZIF-8 adsorbing MBa

Sample C0 (ppm) Qe (mg g
1) K2 mg (g min)
1

ZIF-8 100 199.0  1.33 0.00676

300 597.4  2.13 0.00251
400 794.6  4.03 0.00282
500 990.9  5.17 0.00167
800 1544.8  13.64 0.00038
1000 1917.5  5.86 0.00042
a Fig. 4 XPS spectra of (a) Zn 2p and (b) O 1s for ZIF-8, MB and ZIF-8
Note: 20 mg adsorbent was added into 40 mL MB solution.
after MB adsorption.

109610 | RSC Adv., 2016, 6, 109608–109612 This journal is © The Royal Society of Chemistry 2016
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500 ppm 40 mL MB solution at room temperature). Aer calci- Table 2 Adsorption capacity of different adsorbents
nation in air, ZIF-8 was converted to ZnO whereas porous carbon/
Adsorption Contact
ZnO was obtained when ZIF-8 was carbonized in inert gas (e.g.
Materials capacity time Reference
N2).26,27 From Fig. 5a, it can be seen that the adsorption capacity of
ZnO@C derived from ZIF-8 is similar to that of ZIF-8 and the ZIF-8 3.126 mmol g
1 30 min This work
adsorption capacity of ZnO is slightly lower compared to ZIF-8. (2500 mg g
1)
Moreover, if other porous materials, such as ZSM-5 and 4A Barium phosphate 1.88 mmol g
1 60 min 29
nano-ake
zeolites, were used, only less than 200 mg g
1 MB was adsorbed Ni-MCM-41 100 mg g
1 60 min 30
on such adsorbents. Therefore, from the above-mentioned 4.0–4.5 mmol g
1
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Graphene oxide (GO) 120 min 31

discussion, high surface area itself cannot guarantee high MB
adsorption whereas the high exposure of Zn2+ onto the surface is
the key factor for the high adsorption of MB onto ZIF-8.
Besides methyl blue (MB), we compared the adsorption
capacity of rhodamine B (RhB), methylene blue and methyl
orange using ZIF-8. The adsorption effect for RhB, methylene
blue and methyl orange solution are all negligible with the
adsorption capacity of 40, 20, 18 mg g
1 respectively as shown
in Fig. 5b (20 mg ZIF-8 added into 500 ppm, 40 mL dye solu-
tion), which indicates that the adsorption of MB by ZIF-8 is
highly selective.28
From the XPS results, it can be seen that the interaction
between –SO3
and Zn2+ is the major contribution to the high
adsorption of ZIF-8 for methyl blue but negligible adsorption
for other dyes, which has no –SO3
group. Though there is
–SO3
group in MO, it should be noted that the –SO3
groups in
MO usually exist as –SO3Na, and the –SO3
group in methyl blue
exist as –SO3Na and –SO3H(–SO3
) as shown in Fig. S1.† As
a result, ZIF-8 shows high adsorption for MB but negligible
adsorption for MO. Schematic illustration of mechanism of
MB adsorbed onto ZIF-8 particles is shown in Fig. S2.†
To further demonstrate the selective adsorption capacity of
ZIF-8, mixtures of MB–MO and MB–RhB were used and the
Fig. 5 (a) MB adsorption capacity of different adsorbents and (b)
adsorption capacity for different dyes on ZIF-8.
Fig. 6 Cycling ability of ZIF-8 for MB adsorption: (a) 500 ppm MB and
(b) 1000 ppm MB. Inserted photos: ZIF-8 after MB adsorption (left) and
desorbed ZIF-8 after three cycles of adsorption (right).
rGO 2.6–2.9 mmol g
1 120 min 31
Chitosan/GO 95.16 mg g
1 90 min 32
Ni0.5Zn0.5Fe2O4 60 mg g
1 100 min 21
Co-Based ternary 1200 mg g
1 10 min 33
nanocomposites
Activated charcoal 25.25 mg g
1 30 min 34
selective adsorption results were shown in Fig. S4.† For different
dye mixture, ZIF-8 still shows high adsorption of MB, and much
less adsorption of other dyes. It should be noted that compared
to the adsorption when only MO was used, ZIF-8 adsorbed more
MO when MB–MO mixture was used probably due to the fact
that MB is cationic whereas MO is anionic; therefore, when
MB was adsorbed onto ZIF-8, more MO was further adsorbed
due to the charge effect.
Fig. 6 shows the recycling ability of ZIF-8 (the adsorbent
loading is 0.5 mg mL
1 and the initial MB concentration is
500 and 1000 ppm respectively). The adsorption ability does
not lose much aer three cycles of adsorption (the adsorption
capacity decrease aer three cycles of adsorption is only 30 mg
g
1) and most of MB can be desorbed from ZIF-8, as shown in
the inserted photos in Fig. 6b. XRD and SEM were performed
to test the crystal structure aer ZIF-8 adsorbing MB, as
shown in Fig. S4.† It can be seen that ZIF-8 still maintains their
crystal structure, indicating the good stability of ZIF-8 as
dye adsorbents.
Table 2 shows the MB adsorption capacity of several typical
adsorbents reported in other studies. From Table 2, ZIF-8 shows
a higher adsorption capacity and faster absorption rate for
MB than most of adsorbents reported so far. The high adsorp-
tion capacity and fast absorption rate for MB are mainly due to
the ionic interaction between Zn2+ and sulfonic groups of MB.
4. Conclusions
In this study, ZIF-8 was synthesized and used as high-efficient
adsorbents for MB. ZIF-8 show very high adsorption capacity
(maximum adsorption capacity is 2500 mg g
1) and fast
adsorption rate (adsorption equilibrium can be achieved within
1 h). The adsorption rate is pseudo-second order and the
adsorption type is Langmuir adsorption. The exposure of Zn2+
onto the porous surface is the key factor for the high adsorption
of MB onto ZIF-8; yet only high BET surface area itself cannot
guarantee high adsorption capacity. Due to the ionic bonding
between Zn2+ in ZIF-8 and –SO3
in MB, the adsorption is highly
selective with high adsorption for MB, which has many –SO3

groups but negligible adsorption for other dyes.

This journal is © The Royal Society of Chemistry 2016 RSC Adv., 2016, 6, 109608–109612 | 109611

RSC Advances
Acknowledgements
The authors are grateful for the nancial support of Jiangsu
Specially-Appointed Professor Program, Natural Science Key
Project of the Jiangsu Higher Education Institutions
(15KJA220001) and Priority Academic Program Development of
Jiangsu Higher Education Institutions (PAPD).
Notes and references
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