Desalination 311 (2013) 227–233

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Desalination
journal homepage: www.elsevier.com/locate/desal

Evaluation of sodium hexametaphosphate as scale and corrosion inhibitor in cooling

water using electrochemical techniques
D.E. Abd-El-Khalek a,⁎, B.A. Abd-El-Nabey b
a
Marine chemistry Department, National institute of oceanography and fisheries, Elanfoshy, Alexandria, Egypt
b
Chemistry Department, Faculty of Science, Alexandria University, Ibrahimia, P.O. Box 426, Alexandria 21321, Egypt

H I G H L I G H T S

► Antiscalant properties of SHMP were investigated using electrochemical techniques.

► SHMP prolong nucleation period and consequently retard scale formation.
► SHMP is more efficient as antiscalant than PAA.
► Corrosion inhibitive characteristics of SHMP in cooling water were investigated.
► SHMP has acceptable efficiency as a corrosion inhibitor for steel in test solution.

a r t i c l e i n f o a b s t r a c t

Article history: The antiscale properties of sodium hexametaphosphate (SHMP) were studied using electrochemical
Received 14 March 2012 impedance spectroscopy (EIS), and chronoamperometry techniques in conjunction with a microscopic
Received in revised form 12 November 2012 examination. The corrosion inhibitive characteristics were investigated using EIS and potentiodynamic
Accepted 17 November 2012
polarization measurements. Mineral scales were deposited from the brine solution by cathodic polariza-
Available online 8 January 2013
tion of the steel surface at − 0.9 V (vs. SCE). Comparative study was carried out between antiscalant
Keywords:
efficiencies of SHMP and polyacrylic acid (PAA). Potentiodynamic polarization curves indicated that
Antiscalant SHMP inhibits the corrosion of steel by controlling the cathodic oxygen reduction process. The results
Corrosion showed that SHMP can inhibit corrosion of steel and scale build-up under the conditions tested.
Polyphosphate © 2012 Elsevier B.V. All rights reserved.
Electrochemical methods

1. Introduction Precipitation of calcium carbonate from hard waters has been

Two of the main problems of cooling systems are corrosion and
scaling phenomena. These phenomena have a great economic
impact. Nearly all problems associated with the use of water for
cooling purposes can be attributed to one or more of impurities
such as hardness causing salts (like Ca and Mg that deposit as
scale in pipes and particularly on heating surfaces), silica, iron,
microbiological species, oil and dissolved gases [1,2]. The problems
of scaling and corrosion associated with the use of natural hard
water in cooling towers during recirculation pose great problems
from both economical and technical points of view, such as
decreased system efficiency and increased frequency of chemical
cleaning. The nature and rate of scaling is decided by physical,
chemical and bacteriological effects [2].
⁎ Corresponding author. Tel.: +20 1003859412(mobile); fax: +20 34801499.
E-mail address: dalia1282002@yahoo.com (D.E. Abd-El-Khalek).
studied for a long time because, in addition of its fundamental inter-
est, it is at the origin of the majority of scale deposition, which is a
very important problem from a practical point of view [3,4].
A number of antiscalants are commercially available and new
formulations are continuously being developed and tested for
calcium carbonate scaling such as gelatin, carboxymethyl cellulose
and keratin [5]. Abdel-Gaber et al. investigated fig [6] and olive [7]
leaves extracts as novel environmentally friendly antiscalants. Nu-
merous polymers are commercially available, the most common
being polyacrylic acid [CH2CHCOOH]n [2,8,9]. Per Kjellin [10] inves-
tigated a water soluble copolymer that consists of a poly(ethylene
glycol) chain containing phosphate groups attached to a methyl
terminated poly (propylene) glycol as scale inhibitor. This copoly-
mer was found to adsorb strongly onto the metal surface and
prevent crystallization by a surface competitive effect. The first
scale inhibitor to be used within the membrane industry was
sodium hexametaphosphate, SHMP, [(NaPO3)6]. It was reported
that threshold treatment using SHMP in range of 1 to 5 mg/L was
found to be very useful in preventing the formation of calcium
carbonate scale in many industrial applications [11]. Several

0011-9164/$ – see front matter © 2012 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.desal.2012.11.017
228 D.E. Abd-El-Khalek, B.A. Abd-El-Nabey / Desalination 311 (2013) 227–233

0.35
2. Materials and methods
0.30
[1] 0 ppm 2.1. Solution preparation
current density,mA/cm 2

[2] 2 ppm
0.25 [3] 4 ppm
[4] 6 ppm
The CaCl2 brine solution was prepared to a concentration of
0.20
0.7 M NaCl, 0.0025 M NaHCO3, 0.028 M Na2SO4 and 0.01 M CaCl2
[6,24]. The 0.7 M NaCl solution was chosen to produce the total
0.15 ionic strength of natural seawater at 35 ppm salinity. All chemicals
were reagent grade obtained from El-Gomhouria Co., Egypt, and
0.10 [4] solutions were prepared using double distilled water.
[3]
[2]
0.05 2.2. Electrochemical techniques
[1]

0.00 The electrochemical measurements were carried out in a cell with

0 5 10 15 20
Time, hours
Fig. 1. Chronoamperometry curves for polarized steel electrode in the CaCl2 brine
solution in the absence and the presence of different concentrations of SHMP at 40 °C.
researchers studied SHMP as antiscalant using chemical methods [12,13]
in addition to SEM-EDS and XRD [14]. Moreover, SHMP has been studied
as corrosion inhibitor in tap water [15]. Also, various combinations of
antiscalants 1 hydroxyethane-1,1-diphosphonic acid (HEDP), sodium
hexametaphosphate (SHMP), sodium tripolyphosphate (STPP), and
trisodium phosphate(TSP), were investigated as corrosion inhibitors for
carbon steel [16]. It was observed that a 50/50 ppm combination of
HEDP and SHMP gave 98% corrosion inhibition efficiency and maximum
synergistic effect.
Electrochemical techniques have proven very useful in the study
of corrosion or scale processes in a range of media [7,17,18].
However, in many industrial applications, such as cooling systems,
these phenomena occur simultaneously and hence a study of their
development and inhibition under real conditions is an issue of
great interest [19]. Gabrielli and co-workers investigated electro-
chemical calcium carbonate scaling using electrochemical imped-
ance spectroscopy [20–22] and Quartz Crystal Microbalance [3,23].
This work aims to evaluate the efficiency of sodium hexameta-
phosphate (SHMP) as antiscalant using electrochemical techniques
and compare between its antiscalant efficiency and that of (polyacrylic
acid)PAA. Also the study aims to investigate the corrosion inhibition of
SHMP in CaCl2 brine solution.
three-electrode mode; platinum sheet and saturated calomel elec-
trode (SCE) were used as counter and reference electrodes. The mate-
rial used for constructing the working electrode was steel that had
the following chemical composition (wt.%): C, 0.21; S, 0.04; Mn, 2.5;
P, 0.04; Si, 0.35; balance Fe. The steel was encapsulated in epoxy
resin in such a way that only one surface was left uncovered. The
exposed area (1 cm 2) was mechanically abraded with a series of
emery papers of variable grades, starting with a coarse one and
proceeding in steps to the finest (800) grade. The samples were
then washed thoroughly with double distilled water, followed with
analar grade (A.R.) ethanol and finally with distilled water, just before
insertion in the cell. Chronoamperometry, electrochemical imped-
ance and polarization curves measurements were performed using
Gill AC instrument. Chronoamperometry curves were carried out by
polarizing the steel electrode to − 0.9 V (vs. SCE) in test solution for
20 h. Thus, the current passing through the steel electrode, during
calcareous deposits, is recorded with respect to time. Polarization
curves measurements were obtained at a scan rate of 20 mV/min
starting from highly cathodic potential going to anodic direction. EIS
measurements were done at − 0.9 V (vs SCE) during scale deposition
processes and at rest potential for inhibition studies. The frequency
range for EIS measurements was 0.1 to 1 × 104 Hz with applied
potential signal amplitude of 10 mV. All the measurements were
done at 40.0 ± 0.1 °C in solutions open to the atmosphere under
unstirred conditions. To test the reliability and reproducibility of the
measurements, triplicate experiments were performed in each case
at the same conditions.
2.3. Optical microscopic examination
Optical micrographs were taken by using Euromex Optical
Microscope with color video camera that is connected to a personal
computer.

3. Results and discussion

0.30
3.1. Antiscalant behavior of SHMP
[1]: 00 ppm
current density,mA/cm 2

0.25
[2]: PPA
[3]: SHMP For proper evaluation of the antiscalants, the tests must be con-
0.20 ducted as closely as possible to the actual system operating condi-
tions. An approach using electrochemical techniques to accelerate
0.15 the formation of scale on an electrode working as a cathode has
been developed. Even if the scale generated by applying a potential
0.10 is known to be of a different nature to that formed by immersing in
[3]
a supersaturated solution, this method is valid and allows a faster
0.05 [2] evaluation of the scaling power of various industrial, natural and
[1] chemically or physically treated waters [25].
0.00
0 5 10 15 20
3.1.1. Chronoamperometry measurements
Time, hours
Fig. 1 shows the chronoamperometry curves for polarized steel
Fig. 2. Chronoamperometry curves for polarized steel electrode in the CaCl2 brine electrode in CaCl2 brine solution in the absence and presence of
solution in the absence and the presence of 2 ppm of SHMP and PAA at 40 °C. different SHMP concentrations at 40 °C. The curve obtained in the
 D.E. Abd-El-Khalek, B.A. Abd-El-Nabey / Desalination 311 (2013) 227–233 229

blank 2 ppm

4 ppm 6 ppm

Fig. 3. Optical micrograph photo (40×) for cathodically polarized steel in the CaCl2 brine solution in the presence of different concentrations of SHMP after 20 h.

absence of SHMP could be separated into three regions: nucleation,
growth, and total coverage of the electrode surface. During the
nucleation period, up to 3 h, the scaling process is initialized by
increasing the local pH near the electrode surface by the reduction
of the dissolved oxygen in brine solution. The resulting hydroxide
ions force few nuclei of CaCO3 to be born on the electrode. In the
growth period, 3–10 h in the scaling environment, the current
decreased linearly indicating that the nuclei already born were
growing and occupied the surface leaving some parts free. In the
total coverage period, more than 10 h, the current reached a
limiting value, signifying the scaling time at which total coverage
of the electrode surface was obtained. The curve obtained in the
presence of 2 ppm of SHMP shows that the growth rate that is
described by the slope of the line representing the growth step
was decreased and the total coverage of the electrode surface
within the test period was prevented. Increasing the concentration
to 4 ppm prevents both scale growth and total surface coverage
stages. Further increase in SHMP concentrations causes slight in-
crease in current density. It can be concluded that the function of
SHMP is to increase the nucleation time and consequently, retard

Fig. 4. Nyquist plots for polarized steel for 20 h in the CaCl2 brine solution in absence and presence of different concentrations of SHMP.
230 D.E. Abd-El-Khalek, B.A. Abd-El-Nabey / Desalination 311 (2013) 227–233
CPEf
Rs
CPEdl
Rf
Rct
Fig. 5. Schematic for the equivalent circuit model. Reproduced from Abdel-Gaber et al. [7].
the scale formation. Threshold inhibition can describe the mec-
hanism of SHMP as scale inhibitor [11]. This threshold effect is
explained by an adsorption of the inhibitor onto the crystal growth
sites of sub-microscopic crystallites which are initially produced in
the supersaturated solution, interfering with crystal growth and
altering the morphology of those that grow. This process can
prevent crystal growth or at least delay it for prolonged periods
of time [26].
Fig. 2 shows the chronoamperometry curves for polarized steel
electrode in the CaCl2 brine solution in the absence and the pres-
ence of 2 ppm of each of SHMP and PAA. It displays that in presence
of PAA, the curve is characterized by appearance of the three
regions and the slope of SHMP curve, which characterize the
growth stage, decreases than that of PAA. In addition, in presence
of PAA, the total coverage stage is observed at 12 h, while in pres-
ence of SHMP, this stage is not observed within experiment period
indicating that the efficiency of SHMP to inhibit the scale formation
is higher than that of PAA.
3.1.2. Optical micrographic photo
Fig. 3 shows the optical micrographic photo for the steel surface
that was cathodically polarized at − 0.9 V (vs SCE) for 20 h in brine
solution in the absence and presence of different concentrations of
SHMP. These micrographs display that, in the absence of SHMP, a
complete surface coverage by extremely dense scale crystals takes
place that is mainly due to the fast growth rate and reduction of
nucleation time. The presence of SHMP increases the nucleation
time and decreases the growth rate which lead to a decrease in the
amount of the scale deposited over the entire area compared to the
uninhibited brine solution. The surface area occupied by the scale
particles decreases with increasing SHMP concentrations. The critical
concentration of SHMP required to inhibit the scale formation
completely is found to be 4 ppm.
3.1.3. Impedance measurements
In accordance with our previous work [6,7], the impedance
spectra could be used to characterize different scaling regions. The
shape of the obtained spectra was correlated to scale built up
stages over the electrode surface. A capacitive semi-circle at higher
frequency region followed by an inductive loop is a characteristic
Table 1
Computer fit results of the impedance spectra of steel electrode that was cathodically polarized for 20 h in the brine solution in absence and presence of SHMP or PAA.
Conc., ppm Rs, ohm.cm2 Qf, μF n1
SHMP 00 5.0 19.9 0.65
2 2.5 205.7 0.60
4 3.8 – –
6 5.5 – –
PAA 2 4.0 9.13 0.95
feature of nucleation region. On the other hand, a typical feature
of a depressed semi-circle followed by low frequency diffusion
tail corresponds to crystal growth and total coverage regions.
Fig. 4 shows Nyquist plots for steel that was cathodically polarized
at − 0.9 V for 20 h in brine solution in the presence of different
concentrations of SHMP. As seen, the figure shows different types
of a distorted semicircle whose size decrease with increasing the
inhibitor. In the absence of SHMP, the impedance spectrum was
related to complete surface coverage stage. Whereas, in the pres-
ence of 2 ppm of SHMP the spectra was correlated to the stage of
scale growth. On the other hand, on adding 4 or 6 ppm, the spectra
were connected to nucleation stage. Fig. 5 shows the equivalent
circuit that was earlier proposed by Beaunier et al. [27] to fit the
experimental data of impedance plots for the scale formation
processes. In the circuit Rs represents the solution resistance, Rf is
the resistance associated with the layer of products formed during
immersion, and Rct corresponds to the charge transfer resistance.
CPEf and CPEdl are the constant phase element corresponds to
film and double layer capacitance. The CPE is used in this model
to compensate for nonhomogeneity in the system and is defined
by two values, Q and n. If n equals one, the impedance of CPE is
identical to that of a capacitor and in this case Q gives a pure capac-
itance (C). For non-homogeneous system, n values range 0.9–1. On
the other hand, for the nucleation region where no film formation
could be expected, the impedance plots were fitted to the simple
Randle's equivalent circuit. However, the analysis of diagrams
was restricted to the high and mid frequency domains (10 kHz–
0.5 Hz), removing the low frequency data. The change in the film
resistance, charge transfer resistance, the non ideal film and double
layer capacitances in the absence and presence of SHMP or PAA
obtained after 20 h of polarizing steel electrode at − 0.9 V (vs.
SCE) are given in Table 1. The data clarify that increasing SHMP
concentrations decreases the charge transfer resistance and film
resistance while increases the non-ideal film capacitance. These
results confirm the inhibitive effect of SHMP towards scale forma-
tion process.
The percentage of scale inhibition could be determined from the
following equation [6,7]:
 
% scale inhibition ¼ ðRct Þ0 −ðRct Þi =ðRct Þ0   100
where (Rct)0 and (Rct)i are the obtained charge transfer resistances
after polarizing the steel electrode at − 0.9 V (vs. SCE) in scaling
environment for 20 h in the absence or the presence of the SHMP or
PAA. A critical concentration of 4 ppm of SHMP is required to obtain
81% of scale inhibition; further increase in the concentration of
SHMP causes slight increase in scale inhibition efficiency (Table 1).
These results agree with data of chronoamperometry measurements
and photographic results.
Fig. 6 shows Nyquist plots for polarized steel in brine solution in
absence and presence of 2 ppm of SHMP or PAA. As shown the size
of the semicircle in presence of PAA is larger than that of SHMP
with scale inhibition efficiency equal 30.1% for PAA and 55.9% for
SHMP (Table 1), which supports the data of chronoamperometry
measurements.
Rf, ohm.cm2 Qdl, μF n2 Rct, ohm.cm % Inhibition
9.35 10.1 0.85 2256 –
8.1 35.2 0.84 994 55.9
– 301.7 0.73 421 81.3
– 311.6 0.77 401 82.2
20 47.0 0.75 1576 30.1
 D.E. Abd-El-Khalek, B.A. Abd-El-Nabey / Desalination 311 (2013) 227–233 231

Fig. 6. Nyquist plots for polarized steel for 20 h in the CaCl2 brine solution in absence and presence of 2 ppm of SHMP or PAA.

Fig. 7. Potentiodynamic polarization curves for steel in the brine solution in the absence and presence of different concentrations of SHMP.

3.2. Corrosion inhibitive action of SHMP

3.2.1. Potentiodynamic polarization measurements

Fig. 8. Cyclic structure of SHMP (Sodium hexametaphosphate).
Fig. 7 shows the potentiodynamic polarization curves for steel in
the brine solution in the absence and presence of different concentra-
tions of SHMP. As seen, the cathodic polarization curves is character-
ized by a limiting current at moderate potentials indicating that the
cathodic process is controlled by diffusion of oxygen from the bulk
of solution to the electrode surface. The displayed curves show that
addition of SHMP shifts the corrosion potential (Ecorr) to less negative
values and decrease the corrosion current density (icorr) indicating
that SHMP behaves as an anodic type inhibitor. Harish and Chaudhary
[28] suggested that according to the cyclic structure of SHMP (Fig. 8)
[18], it forms cage-complex with Fe 2+ ions from any two adjacent
negatively charged phosphoryl anions.
232 D.E. Abd-El-Khalek, B.A. Abd-El-Nabey / Desalination 311 (2013) 227–233

Fig. 9. Nyquist plots for steel in the brine solution in absence and presence of different concentrations of SHMP.

3.2.2. Electrochemical impedance spectroscopy results 4. Conclusions

Fig. 9 shows Nyquist plots for steel in brine solution in the
absence and presence of different SHMP concentrations. The im-
1. Addition of SHMP to the brine solution even at low concentration
pedance response consisted of a distorted loop of a capacitive
(2 ppm) prevents the total coverage stage of the electrode surface
type whose size increases with increasing SHMP concentrations
in scaling process. In addition, SHMP prolong nucleation period
indicative of increasing inhibitive efficiency of the inhibitor with
and consequently retard scale formation
increasing concentration.
2. SHMP is more efficient as antiscalant than PAA, under the exper-
The impedance spectra of different Nyquist plots were analyzed
imental conditions described.
by fitting the experimental data to the equivalent circuit shown in
3. The impedance spectra and potentiodynamic polarization mea-
Fig. 5. Computer fit results of the impedance spectra obtained in
surements indicate acceptable efficiency of SHMP as a corrosion
absence and presence of different SHMP concentrations are given
inhibitor for steel in test solution.
in Table 2. The data show that the charge transfer resistance
increases by increasing the concentration of SHMP indicating that
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