Synthesis and application of mixed manganese-Iron oxide nanoparticles for adsorption of As(V) from aqueous solutions
KỶ YẾU HỘI NGHỊ KHOA HỌC THƯỜNG NIÊN TRƯỜNG ĐẠI HỌC ĐÀ LẠT NĂM 2018
SYNTHESIS AND APPLICATION OF MIXED MANGANESE-IRON
OXIDE NANOPARTICLES FOR ADSORPTION OF As(V)
FROM AQUEOUS SOLUTIONS
Synthesis of adsorbent and its adsorption
Le Ngoc Chunga*, Le Thanh Quoca
aThe Faculty of Chemistry, Dalat University, Lamdong, Vietnam
Correspoding author: Email: chungln@dlu.edu.vn
Abstract
A simple method has been used to synthesize nanoparticles of mixed manganese-iron oxide
for the adsorption of As(V) metal ions from aqueous solutions. Transmission Electron
Microscopy (TEM), X-Ray diffraction (XRD), Scanning Electron Microscopy (SEM), Fourier
transform infrared spectroscopy (FTIR), BET analysis were used to determine particle size
and characterization of produced nanoparticles. The x-ray diffraction pattern indicated that
the as-synthesized adsorbent is amorphous with 288.268 m2/g surface area; the amorphous
synthesized products were aggregated with many nanosized particles. The crystallinity of the
Mn2O3/Fe2O3 were obtained at 400°C and 600°C calcination temperature. The FTIR spectra
confirmed the presence of -OH group and H-O-H group localized at 3200 - 3400 cm–1 and
1618-1653 cm−1; theses intense bands is weak (fade) at the high calcination temperature of
the mixed manganese-iron oxide nanoparticles. In addition, when the calcination
temperature of the mixed manganese-iron oxide nanoparticles was 400OC, the weak
absorption bands at 630 cm−1 due to the vibrations of (Fe-O). The results showed that the
mixed manganese-iron oxide nanoparticles has high selectivity for As(V).
Keywords: Mixed manganese-iron oxide nanoparticles; Amorphous; As(V).
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KỶ YẾU HỘI NGHỊ KHOA HỌC THƯỜNG NIÊN TRƯỜNG ĐẠI HỌC ĐÀ LẠT NĂM 2018
TỔNG HỢP VÀ ỨNG DỤNG HỖN HỢP NANO OXID MANGAN-
SẮT ĐỂ HẤP PHỤ As(V) TỪ DUNG DỊCH NƯỚC
Tổng hợp chất hấp phụ và tính chất hấp phụ
Lê Ngọc Chunga*, Lê Thành Quốca
aKhoa Hóa học, Trường Đại học Đà Lạt, Lâm Đồng, Việt Nam
*Tác giả liên hệ: Email: chungln@dlu.edu.vn
Tóm tắt
Một phương pháp đơn giản cho sự tổng hợp chất hấp phụ hỗn hợp nano oxid mangan-sắt để
hấp phụ ion kim loại As(V) từ dung dịch nước. Phương pháp kính hiển vi điện tử truyền qua
(TEM), nhiễu xạ tia X (XRD), kính hiển vi điện tử quét (SEM), phổ hồng ngoại (FTIR), phân
tích BET được sử dụng để xác định kích thước hạt và đặc trưng của hỗn hợp nano oxid
mangan-sắt. Nhiễu xạ tia X cho thấy chất hấp phụ tổng hợp là hỗn hợp nano oxid mangan-
sắt có cấu trúc vô định định hình có diện tích bề mặt 288.268 m2/g và bị hiện tượng
aggregation. Khi nung hỗn hợp nano oxid mangan-sắt ở nhiệt độ 400OC và 600OC sẽ xuất
hiện cấu trúc của tinh thể Mn2O3/Fe2O3. Phổ hồng ngoại FTIR cũng xác nhận hỗn hợp nano
oxid mangan-sắt được tổng hợp có sự hiện diện của nhóm –OH và nhóm H-O-H tại dải hấp
thụ 3200 - 3400 cm–1 và 1618-1653 cm−1; cường độ của dải hấp thụ này sẽ yếu đi khi hỗn
hợp nano oxid mangan-sắt nung ở nhiệt độ cao. Hơn nữa, khi hỗn hợp nano oxid mangan-
sắt nung đến nhiệt độ 400OC thì xuất hiện peak hấp thụ yếu tại 630 cm−1 gây nên do nhóm
Fe-O. Kết quả cũng chỉ rằng hỗn hợp nano oxid mangan-sắt có tính chọn lọc cao đối với
As(V).
Keywords: Mixed manganese-iron oxide nanoparticles, Amorphous , As(V).
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KỶ YẾU HỘI NGHỊ KHOA HỌC THƯỜNG NIÊN TRƯỜNG ĐẠI HỌC ĐÀ LẠT NĂM 2018
INTRODUCTION
1.
Water plays important roles in the natural environment, human activities, and
social development. However, the presence of arsenic in natural waters has become a
worldwide problem in the past decades [1,2]. Arsenic pollution has been reported recently
in USA, China, Chile, Bangladesh, Taiwan, Mexico, Romania, United Kingdom,
Argentina, Poland, Canada, Hungary, New Zealand, Vietnam, Cambodia, Japan and India
[1-7]
.
3−
Arsenic commonly exists as two inorganic forms of arsenite (AsO3 ) and arsenate
3−
(AsO4 ) which are the popular forms in water and referred to as As(III) and As(V). In
general, As(V) is stable in aerobic environment and As(III) often exists in anaerobic
environment. The toxicity of arsenic species is different, generally the toxicity of
inorganic arsenic compounds is about 100 times higher than organic arsenic compounds,
and the toxicity of inorganic As(III) compounds are approximately 60–80 times higher to
humans than As(V) compounds [4-10]. They causes skin, lung, bladder and kidney cancer
as well as pigmentation changes, skin thickening (hyperkeratosis), neurological disorders,
muscular weakness, loss of appetite and nausea [5-12]. Therefore, it is really necessary to
remove arsenic from water to make sure that our environment is safe.
Adsorption has been recognized as a promising technique for removing arsenic
from drinking water due to its high removal capacity and ease of operation. However,
As(III) is less efficiently removed than As(V) from aqueous solutions by almost all of the
[4-17]
arsenic removal technologies and pre-oxidation of As(III) to As(V) is required
.
Recently, increasing attention has been focused on metal oxide sorbents such as
iron, aluminum, titanium, manganese, and zirconium. Among these iron oxides were the
mostly studied because of their high affinity to arsenic species, low cost and
environmental friendliness [8-21]
.
Most recently, many researchers used metal composite materials (containing two
or more metals) as adsorbents to remove As from contaminated water. The results showed
that the composite metal oxides can not only inherit the advantages of parent oxides but
also show a synergistic effect of higher adsorption capacity than that of individual metal
oxides (Lata and Samadder 2016). For instances, Zhang et al. (2005) developed an Fe-Ce
bimetal oxide sorbent, which has a much higher As(V) adsorption capacity than the
individual Ce and Fe oxide. Zhang et al. (2007) prepared an Fe-Mn binary oxide sorbent,
[20-26]
exhibiting a greater enhancement in both As(V) and As(III) removal
.
Previously, we have synthesized the MnO2 nanoparticles via the reduction–
oxidation between KMnO4 and C2H5OH at room temperature [27-29], in this paper we
report a simple method to synthesize the mixed manganese-iron oxide nanoparticles and
used it as selective adsorbent for adsorption of As(V) from aqueous solutions.
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EXPERIMENTS
2.
2.1.
Chemicals and Instruments
2.1.1. Chemicals
Chemicals used included potassium permanganate (KMnO4), FeCl2.4H2O, ethyl
alcohol (C2H5OH), HNO3 and NaOH. All chemical reagents used as starting materials are
of analytical grade and purchased without any further purification.
2.1.2. Preparation of Adsorbate Solutions
The solutions of As(V), Cd(II), Co(II), Cu(II), Zn(II) were used as adsorbates, the
As(V), Cd(II), Co(II), Cu(II), Zn(II) solutions were prepared by the standard solutions
(1000 ppm) of Merck production for AAS. Studied solutions have been diluted to
concentration about 20, 50, 100, 150, 200, 250, 300,…ppm (~mg/L), and used for a short
period of time that not exceeding three days.
2.1.3. Instruments
Atomic Absorption Spectrophotometer (Spectrometer Atomic Absorption AA –
7000 made in Japan by Shimadzu.). The pH measurements were done with a pH-meter
(MARTINI Instruments Mi-150 Romania); the pH-meter was standardized using
HANNA instruments buffer solutions with pH values of 4.01±0.01, 7.01±0.01, and
10.01±0.01. Temperature-controlled shaker (Model IKA R5) was used for equilibrium
studies.
2.2.
Synthesis of mixed manganese-iron oxide nanoparticles
In our previous work, gamma-MnO2 nanostructure was synthesized via the
reduction–oxidation between KMnO4 and C2H5OH by adding gradually KMnO4
saturated solution to the mixture of C2H5OH and H2O at room temperature. In the present
work, the mixed manganese-iron oxide nanoparticles was prepared by adding gradually
KMnO4 and FeCl2.4H2O solutions to the mixture of C2H5OH and H2O under stirring at
the room temperature. Stirring continued for four hours.
The effect of reaction time as well as the molar ratio between KMnO4 and
FeCl2.4H2O also H2O and C2H5OH was studied. After the reaction was completed, the
solid precipitate was washed with distilled water, and then dried at 1000C for 4h to get
the product. The synthesized products are amorphous nanoparticles. The amorphous
nanoparticles were crystallized using an annealing process at different temperatures
(fig.1-2).
2.3.
Batch adsorption study of metal ions
Place 0.1 g mixed manganese-iron oxide nanoparticles to 50 mL metal ion solution
in a 100 mL conical flask. Effect of pH (26), contact time (20240 minutes) and initial
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KỶ YẾU HỘI NGHỊ KHOA HỌC THƯỜNG NIÊN TRƯỜNG ĐẠI HỌC ĐÀ LẠT NĂM 2018
metal ion concentration (Co) (20500 mg/L) were examined. The obtained mixture was
centrifugal at 5000 rpm within 10 minutes, then was purified by PTFE Syring Filters with
0.22 µm of pore size to get the filtrate. Atomic Absorption Spectrophotometer
(Spectrometer Atomic Absorption AA – 7000) was used to analyze the concentrations of
the different metal ions in the filtrate before and after adsorption process.
Adsorption capacity was calculated by using the mass balance equation for the
adsorbent[1-14]
.
C C .V
e
o
q
(1)
m
Here, q is the adsorption capacity (mg/g) at equilibrium, Co and Ce are the initial
concentration and the equilibrium concentration (mg/L), respectively. V is the volume
(L) of solution and m is the mass (g) of adsorbent used.
3.
RESULTS AND DISCUSSION
3.1.
Characterization of the mixed manganese-iron oxide nanoparticles.
The crystal structure of mixed manganese-iron oxide nanoparticles was identified
with X-ray powder diffraction analysis, as shown in Figure 1-2. The diffraction patterns
were obtained in the 2θ range from 15-70O.
VatLieuNano_Mn_Fe_1_2
100
90
80
70
60
50
40
30
20
10
0
15
20
30
40
50
60
70
80
2-Theta - Scale
VatLieuNano_Mn_Fe_1_2
-
File: VatLieuNano_Mn_Fe_1_2.raw
-
Type: 2Th/Th locked
-
Start: 15.000
°
-
End: 84.990
°
-
Step: 0.030
°
-
Step time: 1.
s
-
Temp.: 25 °C (Room)
-
Time Started:
8
s
-
2-Theta: 15.000 ° - T
Figure 1. X-ray powder diffraction of the Mn-Fe mixed sorbent
Figure 1 reveal that the mixed manganese-iron oxide nanoparticle is amorphous.
Absence of sharp peaks confirms the absence of ordered crystalline structure in the
prepared sorbent nanoparticles.
Figure 2(a,b,c) shows the XRD pattern of the mixed manganese-iron oxide
nanoparticles (the synthesized products) after calcination at 200,400 and 600OC. Based
on the XRD pattern, whereas the synthesized products calcined at 200°C proved to be
amorphous (Fig. 2a).
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KỶ YẾU HỘI NGHỊ KHOA HỌC THƯỜNG NIÊN TRƯỜNG ĐẠI HỌC ĐÀ LẠT NĂM 2018
Nano_Mn_Fe_1_2_L2_200C
200
190
180
170
160
150
140
130
120
110
100
90
80
70
60
50
40
30
20
10
0
15
20
30
40
50
60
70
80
2-Theta - Scale
Nano_Mn_Fe_1_2_L2_200C - File: Nano_Mn_Fe_1_2_L2_200C.raw - Type: 2Th/Th locked
-
Start: 15.000
°
-
End: 84.990
°
- Step: 0.030
°
-
Step time: 1.
s
-
Temp.: 25 °C (Room)
-
Time Started: 15
s
-
2-Theta: 15.0
Figure 2a. X-ray powder diffraction of the Mn-Fe mixed sorbent after calcination
at 200°C
Nano_Mn_Fe_1_2_L2_400C
200
190
180
170
160
150
140
130
120
110
100
90
80
70
60
50
40
30
20
10
0
15
20
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40
50
60
70
80
2-Theta - Scale
Nano_Mn_Fe_1_2_L2_400C
-
File: Nano_Mn_Fe_1_2_L2_400C.raw
-
Type: 2Th/Th locked
-
Start: 15.000
°
-
End: 84.990
°
-
Step: 0.030
°
-
Step time: 1.
s
-
Temp.: 25 °C (Room)
-
Time Started: 14
s
-
2-Theta: 15.0
00-033-0664 (*)
-
Hematite, syn
-
Fe2O3
-
WL: 1.5406
-
Rhombo.H.axes
-
a
5.03560
-
b
5.03560
-
c
13.74890
-
alpha 90.000
-
beta 90.000
-
gamma 120.000
-
Primitive
-
R-3c (167)
-
6
-
301.926 - I/Ic PDF 2.4 - F30=
Figure 2b. X-ray powder diffraction of the Mn-Fe mixed sorbent after calcination at 400°C
Nano_Mn_Fe_1_2_L2_600C
200
190
180
170
160
150
140
130
120
110
100
90
80
70
60
50
40
30
20
10
0
15
20
30
40
50
60
70
80
2-Theta - Scale
Nano_Mn_Fe_1_2_L2_600C
-
File: Nano_Mn_Fe_1_2_L2_600C.raw
-
Type: 2Th/Th locked
-
Start: 15.000
13.74890
alpha 90.000
°
-
End: 84.990
°
-
-
Step: 0.030
beta 90.000
°
-
-
Step time: 1.
gamma 120.000
Body-centered
s
-
Temp.: 25 °C (Room)
-
Time Started: 14
301.926
832.998 I/Ic PDF 4.5 -
s
-
2-Theta: 15.0
00-033-0664 (*)
00-041-1442 (*)
-
-
Hematite, syn
-
Fe2O3
-
WL: 1.5406
-
Rhombo.H.axes
-
a
5.03560
-
b
5.03560
-
c
-
alpha 90.000
-
Primitive
-
R-3c (167)
16
-
6
-
-
I/Ic PDF 2.4 - S-Q 7
S-Q 24.3
Bixbyite-C, syn
-
Mn2O3
-
WL: 1.5406
-
Cubic 9.40910
-
a
-
b
9.40910
-
c
9.40910
-
-
beta 90.000
-
gamma 90.000
-
-
Ia-3 (206)
-
-
-
Figure 2c. X-ray powder diffraction of the Mn-Fe mixed sorbent after calcination
at 600°C
Figures 2b, the synthesized products calcined at 400°C, clearly revealed that the
diffraction peaks presented in synthesized samples at 2θ values of 24.06O, 33.15O, 35.7O,
40.98O, 49.41O, 54.21O, 62.52O and 64.11O were due to Fe2O3, and these correlated with
the reported data of hematite. However, the XRD data did not show any presence of Mn
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KỶ YẾU HỘI NGHỊ KHOA HỌC THƯỜNG NIÊN TRƯỜNG ĐẠI HỌC ĐÀ LẠT NĂM 2018
oxide particles in the Mn-Fe mixed oxide system which confirmed that Mn (III) enter into
the Fe2O3 lattice substitution. In fact, ionic radius of Mn (III) of 58pm is similar to that of
ionic radius (55pm) of Fe (III) thus the substitution in the matrix of Fe2O3 is a favorable
process [30]
.
Nevertheless, when the calcination temperature of the synthesized products was
600OC, the peaks observed at 23.1O, 33.12O, 38.19O, 55.11O, 62.46O, 64.05O indicate the
formation of Mn2O3 crystalline and the peaks at 24.21O, 33.12O, 35.64O, 40.89O, 49.5O,
54.12O, 62.46O and 64.05O are the characteristic peaks of Fe2O3. It was observed that after
calcination at 600OC for 2h, the manganese iron mixed oxides change from amorphous
structure to both Fe2O3 and Mn2O3 crystal structures (fig. 2c).
Formation of the mixed manganese-iron oxide nanoparticle was further supported
by FTIR analysis.
Fig. 3. FTIR spectrum of the manganese-iron oxide nanocomposite particles
Fig. 3 shows the FTIR spectrum of the mixed manganese-iron oxide nanoparticles
before and after calcination at 200, 400 and 600OC. The intense band around 3200 - 3400
cm–1 may be due to the stretching modes of -OH group from adsorbed water in the sample.
The bending vibration of H-O-H group also localized at 1618-1653 cm−1; theses intense
bands is weak (fade) at the high calcination temperature of the mixed manganese-iron
oxide nanoparticles. In addition, when the calcination temperature of the mixed
manganese-iron oxide nanoparticles was 400OC, the weak absorption bands at 630 cm−1
may be the vibrations of (Fe-O), which are indicative of formation of mixed metal oxides.
SEM and TEM Analysis
The SEM images of the mixed manganese-iron oxide nanoparticles (the
synthesized products) were obtained to observe the particle size and morphology (fig.4)
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KỶ YẾU HỘI NGHỊ KHOA HỌC THƯỜNG NIÊN TRƯỜNG ĐẠI HỌC ĐÀ LẠT NĂM 2018
Fig. 4. The SEM images of the manganese-iron oxide nanocomposite particles (the
synthesized products) with different magnification
From the SEM photographs, it was understood that the grains are connected with
each other. (It was found that the grains present jointly with each other). In few places,
bigger grains are also seen. It is seen that the synthesized products consists of
nanoparticles aggregated together to form large clusters. It is a common phenomenon
when amorphous nanoparticles are annealed [31]
.
Fig. 5. The TEM image of the manganese-iron oxide nanocomposite
The TEM analysis shows the particles size of the mixed manganese-iron oxide
nanoparticles are in the range of 20-30nm (fig.5). The surface area of the mixed
manganese-iron oxide nanoparticles were measured by a BET analyzer, and the surface
area of the samples was calculated to be 288.268 m²/g.
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3.2.
Adsorption of As (V) onto mixed manganese-iron oxide nanoparticles
3.2.1. Affecting Factors
Effect of pH
Determination of optimum pH is very important since the pH value affects not
only the surface charge of adsorbent, but also the degree of ionization and speciation of
adsorbate during reaction. Adsorption experiments were carried out in the pH range of 2-
6 for the synthesized products by keeping all other parameters constant (As(V)
concentration = mg/l; stirring speed = 240 rpm; contact time = 120 min, adsorbent dose
= 0.1g, room temperature = 25°C).
The result showed that more adsorption at acidic pH indicates that the lower pH
results in an increase in H+ ions on the adsorbent surface that results is significantly strong
electrostatic attraction between positively charged adsorbent surface and As(V) arsenate
-
ions (divalent HAsO42- or monovalent H2AsO4 ). Lesser adsorption of As(V) at pH values
greater than 6.0 may be due the dual competition of both the anions (HAsO42- and OH-)
to be adsorbed on the surface of the adsorbent of which OH- predominates.
Figure 6. Effect of pH on the As(V) adsorption
Effect of contact time
The effect of contact time was studied at optimum condition of dose, pH, and
agitation speed. From Fig. 7, it is observed that the adsorption of As(V) increased as
contact time increased. The adsorption percentage of metal ions approached equilibrium
within 120 min. After this equilibrium period, the amount of adsorbed metal ions did not
significantly change with time.
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KỶ YẾU HỘI NGHỊ KHOA HỌC THƯỜNG NIÊN TRƯỜNG ĐẠI HỌC ĐÀ LẠT NĂM 2018
Figure 7. Effect of contact time on the As(V) adsorption
Effect of initial As(V) concentration
The adsorption of As(V) with synthesized products was studied by varying As(V)
concentration (100ppm - 1000ppm) keeping other parameters (adsorbent dose, stirring
speed, solution pH, temperature and contact time) constant. As illustrated in Fig. 8, As(V)
uptake reduced from 99.89% to ~ 30%, as the As(V) concentration increased from
100ppm to 1000ppm.
Figure 8. Effect of initial As(V) concentrations on the As(V) adsorption
3.2.2. Comparation of Bivalent Cationic Metals Adsorption Cd(II), Co(II),
Cu(II), Zn(II) and As(V) on mixed manganese-iron oxide nanoparticles
The results of Table 1 showed that the mixed manganese-iron oxide nanoparticles
have not successfully used for the adsorption of Cd(II) , Cu(II), Co(II), Zn(II) ions from
aqueous solution on concentration of 20ppm for each (or more), inversely strongly
adsorption of As(V) on mixed manganese-iron oxide nanoparticles. This remarkable
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KỶ YẾU HỘI NGHỊ KHOA HỌC THƯỜNG NIÊN TRƯỜNG ĐẠI HỌC ĐÀ LẠT NĂM 2018
difference is probably due to the difference ionic radius (table 2) and the greater the valence.
Danny et al. (2004) and Lee and Moon (2001) explained that the smaller the ionic radius
[32-34]
and the greater the valence, the more closely and strongly is the ion adsorbed
.
Therefore, the mixed manganese-iron oxide nanoparticles have successfully used for the
adsorption of As(V) from aqueous solution.
Table 1. Adsorption percentage of metal ions on to mixed manganese-iron oxide
nanoparticles
pH
Adsorption of metal ions on to mixed manganese-iron oxide nanoparticles, (%)
As(V)
Cd(II)
Co(II)
Cu(II)
Zn(II)
(150ppm)
(20ppm)
(20ppm)
(20ppm)
(20ppm)
Adsorption
SD*
percentage, %
2
3
4
5
6
99.89
98.45
95.28
96.46
96.51
0.01
0.09
0.05
0.06
0.01
non-ads.
non-ads.
non-ads.
non-ads.
non-ads.
non-ads.
non-ads.
non-ads.
non-ads.
non-ads.
-
-
-
-
non-ads.
non-ads.
-
-
-
-
Note: (*) Standard deviation (SD)
Table 2. Effective ionic radii in pm of elements
Ion
As(V)
46
Cd(II)
95
Co(II)
65
Cu(II)
73
Zn(II)
74
Effective ionic radii (pm)
CONCLUSION
4.
A simple method has been used to synthesize nanoparticles of mixed manganese-
iron oxide for the adsorption of As(V) metal ions from aqueous solutions under batch
conditions. Transmission Electron Microscopy (TEM), X-Ray diffraction (XRD),
Scanning Electron Microscopy (SEM), Fourier transform infrared spectroscopy (FTIR),
BET analysis were used to determine particle size and characterization of produced
nanoparticles. Moreover, the effects of pH, contact time and adsorbent weight on
adsorption process were investigated. The high uptake of As(V) by the mixed manganese-
iron oxide nanoparticles may be due to its relatively high surface area.
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