International Journal of Civil & Environmental Engineering IJCEE-IJENS Vol: 12 No: 03
Metal Ions Removal From Synthetic Solutions
and Produced Water Using Activated Zeolite.
Maria do Rosrio T. de Abreu1, Francisco Cludio de F. Barros1, Giselle S. C. Raulino2, Ccero P.
Moura1, Ronaldo F. do Nascimento1
Abstract In this study synthetic zeolite 4A was used for metal
ions removal from synthetic aqueous solutions and produced
water samples of oil platforms in Cear state-Brazil. The pH
effect on the metal ions removal using zeolite 4A was investigated
for 1.0, 5.0 and 7.0 values. Experimental data obtained with
synthetic solutions showed that at a pH 1.0 value strontium and
potassium ions are removed almost 100% and 90% respectively,
while for other metal ions the removal was around 60%. In
contrast, the metal ions removal from producer water on the
zeolite was lower due to presence of several matrix effect.
Index Terms Produced Water, Wastewater treatment;
Adsorption; Zeolites
I. INTRODUCTION
P RODUCED water is the largest waste stream generated in
oil and gas industries. In oil exploration, it can exist in oil
reservoirs since its formation and as being injected into the
secondary recovery processes [1] [4]. The produced water in
general is more saline than seawater, and contains inorganic
compounds dissolved, such as anions (Cl-, SO42-, CO32-, HCO3-
), cations (Na+, K+, Ca2+, Mg2+, Ba2+, Fe2+) and traces of toxic
metal ions, and has been subject of several studies [1], [3], [5]
[9].
The discharging of produced water or pollution by
petroleum has become a significant issue of environmental
concern due to importance of this natural resource in the
energetic matrix. In most cases, petroleum-related pollution is
a chronic problem, due to port activities and the outflow of
urban and industrial wastewater contaminated with petroleum
and its derivatives [1], [8], [10].
The behavior of metals ions in aqueous systems can be
predicted from chemical equilibrium data. The Eh - pH
diagrams using different metal ions concentrations
M. R. T de Abreu is with the Federal University of Cear, Cear, Brazil
(e-mail: rosario_teofilo@hotmail.com).
F. C. F. Barros is with the Federal University of Cear, Cear, Brazil
(e-mail: fcoclaudio@hotmail.com).
G. S. C. Raulino is with the Federal University of Cear, Cear, Brazil
(e-mail: gisellescr@yahoo.com.br).
C. P. Moura is with the Federal Institute of Cear, Cear, Brazil
(e-mail: teonemoura@yahoo.com.br).
R. F. Nascimento is with the Federal University of Cear, Cear, Brazil
(Corresponding author, phone: +55 85 33669042; e-mail: ronaldo@ufc.br).
129003-4848 IJCEE-IJENS June 2012 IJENS
20
corresponding to the metal ions concentrations in produced
water are shown in Fig. 1. Fig. 1 shows the diagram for all
species studied which indicate the predominance species under
various potential (E, volts) and pH values. It can be observed
that the Na+ species is predominant at about -2.8 volts, and
below the specie metallic Na is the predominant. This same
observation can be applied to the vertical lines at pH values of
0 to 14 for the K species. The diagram for Mg species shows
that the Mg2+ ions is predominant at potential higher -2.0 volts,
which converts to Mg(OH)2 at a pH 8. The diagram shows
Ca2+ species soluble for -3.1 to 1.3 volts, which converts to
Ca(OH)2 at a pH value of about 11. Similar analysis can be
applied for E-pH diagram of Sr species which converts to
Sr(OH)2 at a pH value of 14 [11].
Thus, the methods usually used to remove metal ions in
water, such as chemical precipitation, ion exchange and
adsorption need to have accounted the species distribution
dependence with pH.
Zeolites are hydrated aluminosilicates with a precise
geometry of crystal structure and pores of uniform size, which
form channels of molecular dimensions with high capacity of
exchange cations from their structure. They are widely studied
as low-cost ion exchangers for the treatment of wastewater
containing inorganic solutes. The synthetic zeolites have
replaced the natural ones because of their higher thermal
stability and selectivity in catalytic reactions. In this context,
metal ion exchange, using zeolites, has been used for metal
ions removal from aqueous solution due to the relatively low
cost [12] [21].
The aim of this study was verify the efficiency of a synthetic
zeolite 4A on the removal of Ca2+, Mg2+, Na+, K+ and Sr2+
from multielement synthetic solutions and produced water of
oil industry
II. MATERIALS AND METHODS
A. Chemical and Reagents
To prepare the synthetic solutions the following salts of
metal ions were used (VETEC, So Paulo, Brazil):
MgCl2.6H2O (98% purity), KCl (99.95% purity), NaCl (99.5%
purity), Sr(NO3)2.6H2O (99% purity) and CaCl2.6H2O (99%
purity).
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 International Journal of Civil & Environmental Engineering IJCEE-IJENS Vol: 12 No: 03 21

Multielement synthetic solutions were prepared from their Na+ (10738.83 mg L-1), K+ (1066.42 mg L-1), Sr2+ (586.39 mg
respective salts in distilled water, in the following L-1), and final pH adjusted with NH4OH and HNO3 solutions
concentrations: Ca2+ (1471.67 mg L-1), Mg2+ (89.52 mg L-1), (analytical grade).

Fig. 1. E-pH diagrams for soluble species concentration: Na (10 moL L-1), K (3.50 moL.L-1), Mg ( 20.0 moL L-1), Ca ( 27.50 moL.L-1) and Sr (2.50 moL L-1 ) for
aqueous solutions at ionic strength constant ( for calculate, I = 10.0 moL.L-1) and temperature (25oC). The Eh -pH diagrams were constructed by the Medusa software.

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 International Journal of Civil & Environmental Engineering IJCEE-IJENS Vol: 12 No: 03 22

containing 0.4 g of zeolite 4A. Aliquots of 5.0 mL of the eluate

A. Adsorbent
A zeolite type 4A as synthetic adsorbent was used for
removal of dissolved cations in synthetic solutions and
produced water. Zeolite 4A was synthesized according to
previous report [22]. Kaolin material was used as Si and Al
source. Controlled conditions and SiO2/Al2O3, Na2O/SiO2 and
H2O/Na2O appropriate stoichiometric ratios were used [23].
Then, a mass of 1.0 g of zeolite 4A was activated with 10.0 ml
of ammonium acetate 1.0 mol.L-1 and then calcined at 400 C
for 30 minutes in a muffle oven. The activation aimed to
provide a greater ion exchange capacity of zeolite 4A.
B. Column Adsorption
Adsorption studies using a fixed bed column (7.5 cm x 1.4
i.d cm) packed with 0.4 g of zeolite 4A (bed height of 1.2 cm )
were conducted at room temperature (272C) to verify the
removal efficiency of the metal ions by the column.
A peristaltic pump (model miniplus 3 - Gilson) was used to
percolate the multielement ions synthetic solutions (50 mL) at
pH 1.0, 5.0 and 7.0 and for a sample of produced water (at pH
1.0) through the column with down flow rate of 1.0 mL min-1.
Aliquots of 5.0 mL of eluate were collected for analysis and
construction of breakthrough curves.
were collected for determination of the ion concentration.
The produced water samples used in this study were
collected from oil platforms located in city of Paracuru, Cear
State -Brazil. The pH samples were between 5 to 7. Before the
column adsorption study the pH value of the produced water
was adjust to 1, as a consequence of previous studies with
synthetic solutions as described in item 2.5. An aliquot of 10.0
mL of produced water sample was diluted to 50.0 mL (at pH
1.0) in a volumetric flask for reduce the high concentrations of
metal ions. After dilution, the metal ions concentration were:
Mg2+ (495.90 mg L-1); K+ (126.60 mg L-1); Na+ (8853.33 mg
L-1); Sr2+ (216.38 mg L-1); Ca2+ (1098.62 mg L-1). This
solution was percolated through the column in same conditions
as described previously.
E. Metal Ions Determination
The metal ions concentrations in the aqueous solutions were
performed using atomic absorption spectrophotometer
VARIAN model AA240FS. The analytical curves were
obtained by external standard method of five points from the
standard solutions 1000 mg L-1 of each metal for the analytical
conditions in according to Table I.
TABLE I

C. Adsorption Capacity OPERATING CONDITIONS OF ATOMIC ABSORPTION SPECTROPHOTOMETER IN

FLAME.
The amount of metal ions adsorbed was calculated in
according to equation 1: Ion Wavelength (nm) Linear Range (mgL-1) Type of flame
+
Na 330.3 5 - 200 air / acetylene
(1) K+ 404.4 15 - 75 air / acetylene
Ca2+ 239.9 5 - 200 air / acetylene
Mg2+ 202.6 1 - 20 air / acetylene
Where C0 and C are the initial and final concentration (mg Sr2+ 460.7 0.5 - 4 air / acetylene
L-1) of the metal ions solutions in contact with the mass of
zeolite
The adsorption capacity (Q) of zeolite 4A was determinate F. Characterization of Zeolite
by equation 2: Infrared
Each sample of zeolite (2 mg) was combined with Kbr (98
(2) mg) making the pellet applying a pressure of 2 tons. The
pellets were dried at 130 C under vacuum. Each spectrum was
recorded only once by accumulation of 20 scans at 4 cm-1 with
Where: Q is the adsorption capacity on each experiment
resolution between 400 to 4000 cm-1 using Fourier transform
(mg g-1), C0 is the initial concentration of metal ions (mg /L-1),
infrared spectrophotometer (Shimadzu, Japan).
Ci is the final concentration of metal ions on each collected
point i (mg L-1), Vi is the volume percolated on the column
X-ray
between two collected points (L) and mads is the mass of
XRD experiments were performed in Rigaku (DMAXB) x-
zeolite used for each experiment (g).
ray powder diffractometer by using a Bragg-Brentano
geometry. The powder patterns were collected in the
D. Study of pH Effect continuous mode with scan speed of 0.5.min-1 (2). Cu K
The pH of multielement solutions synthetic of Na+, K+, radiation was used with the tube operated at 40 kV and 25 mA.
Mg2+, Ca2+ and Sr2+ was adjusted at 1.0, 5.0 and 7.0 with nitric The sample with the particle size below 74 m (400 mesh) was
acid and ammonium hydroxide. Thus, each solution was selected for the diffraction measurement.
percolated with a flow rate of 1.0 mL min-1 through columns

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 International Journal of Civil & Environmental Engineering IJCEE-IJENS Vol: 12 No: 03
III. RESULTS AND DISCUSSION
A. Adsorbent characterization
The zeolite was activated with the ammonium ion in order
to replace the sodium ions present in its composition and allow
the formation of acid sites by the introduction of H+ in the
zeolite primary structure, which consists basically of Al-O-Al,
Al-O-Si, and Si-O-Si groups, converting them into groups.
Protons are binding to oxygen atoms, and enabling them to
promote ion exchange with other ionic species. Fig. 2 shows
the infrared absorption spectra of the activated zeolite.
Absorbance
3700 3190
2360 1650
3850 3500 3150 2800 2450 2100 1750
-1
Wavenumber, cm
Fig. 2. IR Spectra of (A) Zeolite 4A, (B) Zeolite Ammoniacal, and (C)
Activated Zeolite.
Fig. 3. a) XRD pattern of synthesized zeolite A and b) reference XRD
zeolite A pattern.
As can be observed in spectra (Fig. 2), sodium ion was
replaced by ammonium ion, and after their thermal
decomposition obtained the activated material. There was no
change in the basic structure of the zeolite, because the signals
at 1020 cm-1, 1650 cm-1 and broad band near 3000 cm-1, which
refer to structural groups Si-O (deformation and stretching)
and O-H (stretching), show no change. On the other hand, the
presence of ammonium ion was evidenced by bands at 1400
cm-1 and broadband with doublet between 3190 cm-1 and 3700
cm-1, concerning the deformation and stretching N-H,
respectively. After calcination the protons are trapped in the
23
structure. These events can be noted with the emergence of
two new bands at 680 cm-1 and 810 cm-1, which are attributed
to groups OH+ linked to aluminum or silicon atoms.
The zeolite XRD measured pattern is shown in Fig. 3. As
expected, only one crystalline phase of zeolite 4A was
achieved. It can be observed by comparing the zeolite A
pattern (Fig. 3a) with the reference pattern [24] (Fig 3b), as the
relative intensities and peaks locations are satisfactorily
similar.
B. Study of pH Effect
The efficiency of the ion exchange processes for different
metal ions depends on the size and charge of cations as well as
the zeolite structure [13] However, the pH value is a
A significant parameter for metal ions removal by zeolite as well
B as it can influence the characteristic of the exchangeable ions
and of the zeolite [25].
The metal ions removal from synthetic solution at pH 1; 5
C
680
and 7 value is shown in Fig. 4. It was observed that the amount
1400 of metal ions adsorbed by zeolite studied is dependent of pH,
810
and which it increases with decrease of pH solution.
The results shown in Fig. 4 indicate that strontium and
1020
potassium ions are removed almost 100% and 90%
1400 1050 700
respectively, while for other ions such as magnesium, calcium
and sodium was around 60% at value of pH 1. This result
suggests that there is no competition between protons and
strontium ions for zeolite sites. In contrast, the lowest removal
for potassium, magnesium, calcium and sodium ions was
obtained at pH 5 and 7, probably due to the effect of
competition with H+.
Fig. 4. Metal ions removal from synthetic solutions at pH values.
The removal of mono and divalent metal ions follows the
tendency, Na+ < K+ and Sr2+ < Mg2+ < Ca2+ , respectively. It is
known that the ion exchange capacity increases with increasing
ion charge, but decreases with its hydration [26], [27]. These
results are consistent with the ones found in the literature [26]:
H+ > Cs+ >Rb+ > NH4+> K+> Na+> Li+
Ba2+ > Sr2+> Ca2+>Mg2+
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The results at values of pH 5 and 7 also are shown in Fig. 4.

It was observed that the metal ion removal decreases TABLE III
ADSORPTION CAPACITIES OF ZEOLITES FOR 50 ML OF MULTIELEMENT METAL
significantly at values of pH 5. The strontium ion removal IONS SYNTHETIC SOLUTION AND PRODUCED WATER.
from synthetic solution at pH 7 (Fig. 4) was greater than other
ions metal. On the other hand, magnesium was strongly Q (mg g-1)
affected by increasing of pH. Ca 2+
Mg 2+
Na+ K+ Sr2+
It can be noted, in general, that increasing of pH tend to a pH 1.0 92.3 71 637.3 88.7 73.2
decrease of metal ions removal in zeolite 4A. This effect was pH 5.0 74.4 - 276.9 96.6 47.4
pH 7.0 119.1 - 353.1 13.9 58.7
greater for magnesium and sodium ions. Strontium ions produced water
showed greater removal than the other metal ions studied. The (pH 1.0) 135.1 15.4 180.4 - 19.2
calcium ions removal was between 40 and 65%.

TABLE IV
C. Produced Water Sample METAL IONS REMOVAL FROM PRODUCED WATER BY VARIOUS METHODS.

The results obtained for produced water and synthetic Removal Reference
Ions Material (%)
solution at pH 1 are shown in Tables II and III for a Ca2+, Mg2+, Na+, Zeolite 4A 60 - 99 Present
comparison. It can be seen that the metal ions removal was K+, Sr2+ study
greater for calcium and strontium ions. The removal of sodium Zn , Cd2+, Cr3+,
2+
Sponges-like Luffa 66 - 92 [3]
Pb2+ cylindrica
and magnesium ions is about 20%, and 30% for potassium.
Ca2+, Mg2+, K+, Electrodialysis 50 [29]
Investigations with the produced water at pH 5 or 7 were not N+
carried out, because data experimental obtained from synthetic Na+, K+, Ca2+, Carbon aerogel-based 8 -22 [30]
solutions showed a better metal ions removal at pH 1. Mg2+
Ni2+, Cd2+, Cr3+ Waste stabilization 95 - 99 [31]
The comparative results between synthetic solution and ponds
produced water are shown in Table IV. It can be observed that
zeolite has a greater efficiency for the metal ions removal from
synthetic solution, except for calcium ions. This can be IV. CONCLUSION
attributed to the matrix effect from produced water, due to
presence of several dissolved solutes, which increase the ionic The pH affects the ion-exchange capacity of zeolite 4A. The
strength from solution as well the ions competition by the metal ions removal was higher at pH 1.0. In this pH the
zeolite adsorption sites. removal of strontium and potassium ions was more efficient.
It is well known that increasing pH, metal complexes can be The removal of metal ions in produced water was affected
formed due to reactions with the inorganic ligands present in by matrix effect.
produced water, such as CO32-, SO42-, OH-, PO43-and CH3COO- Even if the results are satisfactory, further studies are
which are more or less soluble and can influence in the process needed like: breakthrough curves, ionic effect, flow rate and
of ion exchange [28]. column length.
Zeolite 4A has a satisfactory capacity adsorption to remove
TABLE II certain metal ions presents in solutions, and has therefore
COMPARISON OF METAL IONS REMOVAL OF THE SYNTHETIC SOLUTION AND potential to be used as an adsorbent in the treatment of
PRODUCED WATER SAMPLE AT pH 1.0.
produced water.

Removal (%)
Ca2+ Mg2+ Na+ K+ Sr2+
synthetic solution 55.75 63.58 52.76 83.43 99.91 V. ACKNOWLEDGMENT
produced water 98.35 24.83 19.38 33.2 88.7 The authors would like to thank the organizations
FUNCAP, CAPES and CNPq (Process No. 486059/2007-3)
D. Produced Water Sample for financial assistance and the LANGUA and LAT
Table III shows the zeolite adsorption capacity. It can be laboratories (Federal University of Cear) for its technical
seen, except for calcium and magnesium, that the zeolite support.
adsorption capacity is lower for production water than
synthetic solution. However, more studies are needed to
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