Asia-Pacific Journal of Chemical Engineering
Removal of Pb2+, Cd2+and Cu2+ from phosphoric acid
solution using chitosan-modified natural zeolite
Journal:
Asia-Pacific Journal of Chemical Engineering
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Manuscript ID:
Wiley - Manuscript type:
Date Submitted by the Author:
Research Article
03-Mar-2015
Zhanbolatovna, Marzhan; Kazakh-British Technical University, Chemical
Engineering; Chemical Sciences Institution named after A.B.Bekturov»,
Laboratory of chemistry of fertilizers and salts
Pasa, Salih; University of Dicle, Department of Chemistry, Faculty of
Education
Chernyakovа, Raisa; Sciences Institution named after A.B.Bekturov»,
Laboratory of chemistry of fertilizers and salts
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Complete List of Authors:
APJ-15-0087
: Sorption , natural zeolite, modified zeolite, chitosan, heavy metals,
phosphoric acid
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Keywords:
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Removal of Pb2+, Cd2+and Cu2+ from phosphoric acid solution using chitosan-modified natural
zeolite
M.Zh. Kussainova1, R.M.Chernyakovа, U.Z. Jussipbekov2, Salih Pasa3, Hamdi Temel 4*,
1*
Kazakh-British Technical University, Almaty, Kazakhstan
2
JSC «Chemical Sciences Institution named after A.B.Bekturov», Laboratory of chemistry of fertilizers and
salts, 106 Ualikhanov Street, 050010, Almaty, Kazakhstan
3
Department of Chemistry, Faculty of Education, University of Dicle, Diyarbakir, Turkey
4
Faculty of Pharmacy, Pharmaceutical Chemistry, Dicle University, Diyarbakir, Turkey
Abstract
"H3PO4 - Pb - Cd -Cu natural-modified zeolite" model system and comparative analysis results
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revealed that preferred sorption capacity of the sorbent for Cd2+ cations has meaningful retention in
concentrated phosphoric acid in time interval. The highest degree of purification of acid was obtained
within 5 minutes of the process, then in the range 10-40 minutes decreases and then it increases again.
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Physico-chemical methods of analysis (FT-IR, SEM, X-ray, BET) have shown that in lead-containing
phosphoric acid natural zeolite is activated without destroying the structure and adsorbs lead, as well as in
conjunction with the cadmium, cupper cations.
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Keywords: Sorption, natural zeolite, modified zeolite, chitosan, heavy metals, phosphoric acid;
FT-IR, SEM, X-ray, BET.
1. Introduction
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Phosphoric acid produced by wet-process contains a variety of impurities. Among the most
typical impurities is toxic lead, cadmium and copper . Purification of H3PO4 is very major problem [1-5].
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Currently, a huge amount of pollutants, including heavy metals is discharged in biosphere as a result of
human activity. Heavy metals are among the most common and toxic pollutant. Presence of heavy metals
in biosphere leads to their accumulation in the soil in amounts many times greater than background levels,
which leads to soil productivity reduction, negative impact on flora and fauna and ultimately in humans
[6-10]. Natural zeolites are a relatively new class of mineral raw materials used in the purification process
and tertiary sewage treatment. Zeolite from the Shankanay deposits of Kazakhstan is used as a sorbent,
due to its high sorption characteristics, and its acid in recent years is the subject of extensive study. This
zeolite is described as a highly siliceous mineral having good sorption properties for cations lead,
cadmium, copper, in concentrated phosphoric acid [11].
*
Corresponding Author. e-mail: [email protected], Phone: +77072236184, Kazakh-British
Technical University, Almaty, Kazakhstan.
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Asia-Pacific Journal of Chemical Engineering
Promising sorbents in regard to heavy metal cations are acid-resistant natural zeolites with a
crystalline structure which allow removing heavy metals not only from aqueous solutions but also from
acid media. It is known that natural zeolite has a high sorption ability in regard to Pb2+ cations, and to a
less extent - to Cd2+ and Cu2+ cations. There are different ways to activate natural aluminosilicates:
mechanical and thermal activation, chemical modification, which includes acid and alkaline activation,
modification, inorganic and organic compounds, combined activation methods [12].
To increase the efficiency of using natural zeolites as adsorbents, it is necessary to increase their
exchange ability and create on their basis new and more effective sorbents in regard to heavy metals. One
of the promising ways of creating new types of sorbents is modification of the surface of natural zeolites
that allows widening the range of impurities being removed from different contaminated media and
increasing their selectivity. Promising modifiers of the sorbent surface is chitosan and its derivatives
possessing a number of valuable properties-the ability to fiber and film formation, ion exchange and
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complex formation. Chitosan is characterized by chemical stability, high reactivity, selectivity to heavy
metal ions [13]. Thus, we may suppose that the sorbent obtained by modification of zeolite by chitosan
will combine positive properties of zeolite and the modifier.
In this work sorption ability of Shankanay zeolite modified by chitosan in regard to bivalent
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cations Pb2+, Cd2+, Cu2+ in their joint presence in the concentrated phosphoric acid is studied.
Removal of heavy metals (Pb2+, Cd2+, Cu2+) from acidic medium with natural and modified
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zeolite with acetic acid solution of chitosan was investigated in this paper.
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2. Experimental
2.1. Adsorbent
Natural zeolite from Shankanay deposit (Kazakhstan) of the following composition (w.%): K2O:
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1.38; Na2O: 0.95; Fe2O3: 0.16; Al2O3: 10.81; CaO: 2.32; MgO: 0.93; SiO2: 65.28; losses on ignition: 18.5
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is used [13]. Preparation of a composite sorbent conducted by mixing natural zeolite and chitosan from
Turkey.
2.2. Adsorbate
Stock solution of heavy metals was prepared by dissolving analytical grade Pb(NO3)2,
Cd(NO3)24H2O , Cu(NO3)2 salts (from Sigma Aldrich and Fluka Chemical Corporations). The
concentration range of heavy metals prepared from stock solution varied between 50 to 80 mg ⁄ l. All
chemicals employed of analytical grade.
2.3. Methods
Concentrations of the investigated metals were determined atomic absorption spectrophotometer
AAS - 400 model PerkinElmer, USA. FTIR spectra of the Zeolites were recorded on a Perkin Elmer
Spectrum 100 with ATR apparatus, USA. Shapes and size of the Zeolites were examined by scanning
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electron microscope (SEM, model QUANTA 250 FEG). X-ray powder diffraction patterns were carried
out by X-ray powder diffractometer D8 Discovery of Bruker, using Cu Kα radiation at 40 kV and 40 mA.
The N2-adsorption and desorption of the samples were measured by Quadrasorb SI-KR/MP specific
surface area analytical instrument. Specific surface area was calculated from N2 desorption isotherms
according to Brunauer-Emmett-Teller (BET) equation, Quantachrome Instruments, USA. Thermo grams
were recorded using a thermo gravimetric analyzer by the Shimadzu DTG-60.
3. Results and Discussion
3.1. Removal Efficiency (R, %) and time Effect
Study of the sorption capacity of natural and modified zeolite with respect to cations of heavy
metals in the presence of their phosphoric acid medium was performed
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H3PO4:zeolite (S:L) and 25 °C = 10:100.
in the range of 5-60 minutes
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Pb2+
Pb2+
Cd
2+
50 ppm
50 ppm
(a)
Cu2+
Cd 2+
80 ppm
(b)
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Cu
Pb2+
50 ppm
50 ppm
2+
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Asia-Pacific Journal of Chemical Engineering
50 ppm
50 ppm
Cu
Cd2+
2+
80 ppm
50 ppm
(c)
Figure 1. Preparation of solutions containing heavy metals
Every metals the concentration in system "H3PO4-Pb2+-Cd2+-Cu2+ - zeolite" is
50-80 mg L-1. The
experiments were conducted in 250 ml flasks. The flasks were shaken for a desired period time in a water
bath shaker. Fig.1. (a) СРb=СCd<СCu (b) СРb =СCu<СCd (c) СРb=СCd=СCu. The contact time was varied
from 5-60 minutes. The samples were analyzed by AAC-400. The removal percentage adsorption (R%)
was calculated as
0
0
R=
Co − Ce
⋅ 100
Co
where C0 is the initial concentration of metal ions in solution, mg/L;
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(1)
Asia-Pacific Journal of Chemical Engineering
Сe is the concentration of metal ions in solution after their interaction with the sorbent, (mg/L)
3.2. Production of modified zeolite with chitosan
natural zeolite and 1M
NaCl
Na-zeolite
mixed for 24 h
suspension stirred
1 M NaCl washing 3 once
Separation of preciptate
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washing diss. water 3 once
drying
Na-zeolite
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chitosan in 5% acetic acid stirring 24 h
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20 ml H20
acetic acid solution of chitosan
Modified
zeolite
Modified zeolite
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Scheme 1. The preparation steps of modified zeolite
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The highest degree of purification of acid was obtained within 5 minutes of the process, then in
the range 10-40 minutes decreases and then increases again.
As for lead and cadmium optimum time is 5 minutes adsorption process. The appearance of the
maximum on the curves of sorption of lead and cadmium caused by the process of desorption from the
zeolite in phosphoric acid, which occurs upon prolonged contact of the sorbent with sorbate.
Comparison of the degree of sorption of lead and cadmium revealed that in the investigated
conditions more sorbed cations Pb2+, cations than Cd2+.
Comparison of the degree of sorption of lead, cadmium and copper revealed that under the
conditions (Pb<Cu Cd=0,0505; Cu=0,0802) most sorbed Cu, than cations Pb, Cd. For example, if a 5
minute process RPb=51.68%, RCd=37.12%, and RCu=74.93%. Sorption of copper 10-30 minutes decreases,
and then increases gradually (Table 1).
The character of sorption
curves under the conditions of equality of
Pb2+ and Cd2+
concentrations but greater content of Cu2+ cations is the same for all cations. The greatest adsorption of
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heavy metal cations from phosphoric acid occurs in the first 5-10 min of the process. Modified zeolite
manifests the greatest sorption ability towards Cd2+ cations which remains the same up to 60 min of the
process. The degree of cadmium sorption varies from 97.55 to 88.29%.
Table 1 The removal percentage of heavy metals from phosphoric acid by natural and activated zeolite
Cd< Cu Cd= 0,0505; Cu= 0,0802;
Removal
time, min.
zeolite
modified zeolite
5
Pb2+
51.68
Cd2+
37.12
Cu2+
74.93
Pb2++
91.54
Cd2+
95.48
Cu2+
92.69
10
49.23
31.93
69.48
92.90
97.55
95.42
26.76
37.02
52.49
86.26
92.69
84.42
67.85
54.61
41.69
82.16
89.32
76.27
16.67
54.61
44.88
86.73
92.02
82.27
38.38
18.51
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78.18
88.29
72.68
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Copper and lead are sorbed in a less amount, the degree of their sorption within 10 min makes up
95.42 and 92.90%.
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Under the conditions, when concentrations of lead and copper in phosphoric acid are equal and
that of cadmium cations is higher, their residual content decreases with the increase of the process time to
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10 min and increases in the period of time more than 10 min cations (Table 1).
Sorption curves for all the adsorbed cations as in the previous the case are of the same type of
character. However, unlike the above discussed experiments in case of high degree of purification cations
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cadmium from phosphoric acid copper is increased to 10 minutes, and lead and cadmium, as in the
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Asia-Pacific Journal of Chemical Engineering
previous case. From 10 to 40 minutes time range, the sorption curves show little tendency to reduce the
degree sorption. A 60 minute increases again. The degree of sorption of copper (80.32-70.68%), the
degree of sorption of cadmium (30.07-10.56%) and lead (50.76-28.69%) (Table 2).
Analysis of obtained data on condition equal to cation content of lead, cadmium and copper
showed that regardless of the nature of the cation at 10 and 40 min process phosphoric acid is
characterized by the smallest of their content. The minimum content of heavy metals in acid observed at
10 min of the process.
Sorption curves for all cations being sorbed, as in the previous case, have a one-type character.
However, unlike the above considered experiments, in case of high content of cadmium cations the
purification degree of phosphoric acid from heavy metals increases in the range within 10 min. In the
range 10-30 min the sorption curves show in significant tendency to the decrease in the sorption degree
of cations.
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Asia-Pacific Journal of Chemical Engineering
Table 2 The removal percentage of adsorptions of Pb (II), Cd (II) and Cu(II) with natural and
modified zeolite from of H3PO4 (Cd >Cu Cd= 0,0802; Cu=0, 0505)
Removal
time, min.
zeolite
modified zeolite
Pb2+
Cd2+
Cu2+
Pb2+
Cd2+
Cu2+
5
50.76
30.07
80.32
91.35
92.13
92.09
10
48.39
27.99
81.61
94.45
95.37
96.93
20
46.86
25.21
80.65
93.56
94.49
96.25
30
29.20
10.56
71.50
93.75
94.31
95.91
40
28.69
10.28
70.68
86.58
86.93
85.08
60
52.63
26.04
80.86
73.61
79.28
64.99
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As in the case of equal concentrations of all cations (Cd >Cu Cd= 0,0802; Cu= 0, 0505), the sorption degree
of copper is equal to (92,09-95,91%), and that of cadmium cations – (92,13-94,31%) and lead - (91,3593,75%) (Table 2 ).
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Sorption curves at 10 and 40 min are the maxima probably due to desorption from the sorbent
cations in acid. The degree of sorption of copper (81.99-67.35%), the degree of sorption of cadmium
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(21.45-48.17%) and lead (59.12-37.86%) (Table 3).
Table 3 The removal percentage of adsorptions heavy metals with natural-modified zeolite from
phosphoric acid Cd= Cu Cu, Cd=0,0505
zeolite
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Removal
time, min.
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Pb2+
Cd2+
Cu2+
5
37.86
21.45
67.35
10
59.12
48.17
77.97
20
51.45
34.46
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30
44.40
30.66
40
56.30
60
47.04
modified zeolite
Pb2+
Cd2+
Cu2+
90.77
93.55
96.78
93.47
95.15
96.11
94.81
96.55
97.53
72.23
92.18
93.96
94.31
46.60
81.99
95.09
97.50
98.14
30.24
73.10
80.84
97.32
81.61
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Sorption curves at 20 and 40 min there are maximums probably due to desorption of cations from
the sorbent into the acid. Judging by the obtained results, in the whole interval of time modified zeolite
least of all sorbs lead cations. The sorption degree of lead is within 80.84-95.09%, while that of cadmium
-93.55-97,50%, and copper-81,61-98,14% (Table 3).
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Solution of chitosan was chosen as a modifier because it increases the amount the most active
sorption centers. Modified chitosan zeolite has higher sorption capacity than natural zeolite, due to the
appearance of additional and active in sorption processes NH2 and OH¯ groups.
3. 3. FT-IR Study
FT-IR analysis of natural and modified zeolite and samples after sorption presented in Figure 2.
A analysis of the IR spectra of zeolite and isolated from the acid after sorption Pb2+ and Cd2+ was
conducted. As it can be seen from Figure 3(a,b,c,d), the IR spectrum of zeolite (a), intense frequency
987 cm-1 characterizing stretching vibrations Al, (Si)-O communication framework zeolite, and 761 cm-1
frequency - 571 cm-1 relating to the deformational fluctuations of its frame is shifted to higher
frequencies: 987 cm-1 → 993 cm-1, 761 cm-1 → 762 cm-1, 514 cm -1→ 520 cm-1 [14].
IR zeolite selected from the acid sorption after Pb2+, Cu2+ and Cd2+ (b) differ from the spectrum of
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natural zeolite (a). Simplified region stretching, deformation vibrations of water and the region of
oscillations for external relations of the tetrahedral geometry are prescribed in a single frequency at 3565,
1958, 1635 cm-1, respectively. [15].
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Figure 2 FT-IR spectra of the samples: (a) –natural zeolite, (b)- natural zeolite after sorption, (c)chitosan modified zeolite, (d) modified zeolite after sorption.
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Asia-Pacific Journal of Chemical Engineering
IR – spectroscopic analysis of zeolite modified by chitosan after sorption of cations showed the
decrease in intensity and shift of frequency maximum 3405 cm-1→3332 cm-1, 2170 → 2104 cm-1,
1635 cm-1→1628 cm-1 that is characteristic of vibrations of secondary amine and tertiary amines (Fig. 3
c,d). From the spectrum of the sorbent separated after sorption frequencies 1146.85 and 1203 cm-1
conditioned by vibrations of primary amine disappear. Appearance of frequency at 416.23 cm-1 indicates
strengthening of Me-O bond [16].
3.4. SEM and XRD patterns Analysis of Natural-Modified Zeolite
Electron microscopic analysis of natural zeolite, zeolite after sorption of heavy cations, modified
zeolite, modified zeolite after sorption of heavy cations was analyzed and their surface properties were
compared. As it can be seen from (Fig. 4 a) and (b), the porosity varies considerably under the influence
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of phosphoric acid. The micrograph indicated that the presence of natural zeolite has small bright spots
corresponding to the cavities and voids in the. The light spots become significantly larger in zeolite after
sorption of Pb2+, Cd2+, Cu2+ cations (Fig. 4 b) in comparison with a photomicrograph of natural zeolite
(Fig. 4 a). Thus, the study of the sorption properties of the natural zeolite and the physical-chemical study
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of natural zeolites and after sorption, revealed that the phosphoric acid is retained in the structure of the
natural zeolite and sorption properties of the zeolite exhibit their combined presence with respect to
cations Pb, Сd and Cu.
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Electron micro pictures of natural and chitosan modified zeolite are presented in Fig.5. The
obtained images indicate that zeolite surface is covered by chitosan. As is seen, the surface of chitosan
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modified zeolite is represented by a better arrangement of particles (Fig. 5a), and there is no intercalation
of chitosan into the internal pores of zeolite, i.e its pores are not clogged that agrees with the
investigations in.
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Figure 3 Part of the XRD patterns and SEM micrographs for: (a) natural zeolite and
(b) natural zeolite after sorption of Pb, Cd, Cu cations.
Electron micro pictures of chitosan modified zeolite before (a) and after sorption (b) differ. After
purification of acid on the surface of modified natural zeolite one can observe swelling of particles,
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formation of larger aggregates and their chaotic location, there takes place sticking of particles together,
probably due to sorption processes.
XRD analysis of the natural zeolite (Fig.4,5) selected from phosphoric acid before and after
adsorption of Pb, Cd, Cu showed that number of diffraction maximums with deviations occurred and
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Figure 4. Part of the XRD patterns and SEM micrographs for: (a) the modified zeolite and
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(b) modified zeolite after sorption of Pb2+, Cd2+, Cu2+ cations.
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after adsorption of Pb, Cd, Cu showed that number of diffraction maximums with deviations occurred
and the values of intensities and the theta positions can be summarized such: 4,65400 Ао (30)→4.53694
Ао (73), 43.83500 Ао (10)→3.75809 Ао (43), 3.38300 Ао (25)→3.34129 Ао (99,9), 3.16500 Ао (40)Ао
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→3.24040 А о (97), 3.07400 А о (20)→3.06198 Ао (72),2.97600 А о (65)→2.99379 Ао (10.4), 2.73300 Ао
(25)→2.57161 А о (73). In the X-ray spectra of the zeolite after sorption are new diffraction maxima
15.28560 Ао (37.8), 3.97100 А о (100), 3.91000 Ао (70) and intense line in (2.51198…..1.37208) Ао.
Specified changes in
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X-ray spectrum claim the presence new elements binding to the atoms in the
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natural zeolite structure [17].
Table 4 Specific surface area natural zeolite, Brunauer-Emmett-Teller (BET)
Sample Code
BET Specific
surface area (m2/g)
Total Pore
volume, cm3/g
natural zeolite
4,113
1,621*10
acidtread zeolite
4,504
1,466*10
after sorption natural zeolite
3.166
1.527*10
Pb, Cd, Cu
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Average
pore rādiuss (Å)
-2
78,80
-2
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-2
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Table 5 Specific surface area modified zeolite, Brunauer-Emmett-Teller (BET)
Sample Code
BET Specific surface
area (m2/g)
Total Pore volume,
Average pore
cm3/g
rādiuss (Å)
modified zeolite
4.382
1,662*10
acidtread modified
zeolite
5.425
1.714*10
after sorption modified
zeolite Pb-Cd-Cu
4,066
4.208*10
-2
75,85
-2
63,21
-2
30,42
Specific surface area of all zeolite samples was measured utilizing adsorption of N2 gas (purity
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99.99%) at - 196°C (Quadrasorb SI-KR/MP, Quantachrome Instruments, USA). For this purpose, 0.02 –
0.30 g of the zeolite samples were outgassed for 3 h at 300°C.
4. Conclusions
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Sorption of natural zeolite cations occurs in the following order: Cu> Pb> Cd. Modified chitosan
zeolite has higher sorption capacity than natural zeolite, due to the appearance of additional active and
sorption processes in the NH2 and OH- groups. Sorption capacity of modified zeolite ions Pb, Cd and Cu
er
is almost the same in terms of equality, their concentrations and high cadmium content, and in a high
copper content sorption occurs at the following number: Cd> Pb>Cu. Using physico-chemical analysis
Re
methods (IR, electronic microscopy, X-ray, BET) shows that natural zeolite activates without breaking
the structure and adsorbs cadmium alone or together with lead cations.
Acknowledgements
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The authors are grateful to thank to Professor Hamdi Temel, Director of the Dicle University
Science and Technology Research and Application Center (DUBTAM), for providing laboratory facilities
for this work.
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