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cn

Desalination 196 (2006) 237247

Inhibition of calcium and magnesium-containing scale by a new

antiscalant polymer in laboratory tests and a field trial
Hai-Yan Li, Wei Ma*, Lu Wang, Ru Liu, Lin-Sen Wei, Qiang Wang
Research Centre of Seawater Desalination and Multipurpose Utilization, School of Chemical Engineering,
Dalian University of Technology, Dalian, 116023, PR China
Tel. +86 (411) 8470-6303; email:mawei@dlut.edu.cn

Received 25 July 2005; accepted 18 November 2005

Abstract
Membrane scaling is caused by the deposition of unsoluble salts as feedwater converted to brine, affectting the
operation of seawater RO plants. Membrane scaling at the Dalian RO desalination plant was analyzed using Dalian
seawater. Based on the characteristics of Dalian seawater, a new environmentally friendly, biodegradable antiscalant
PAP-1 was synthesized in the laboratory. The performance of PAP-1 to inhibit calcium and magnesium-containing
scale was studied both in the laboratory and at the Dalian seawater RO desalination plant. It was found that PAP-1 is
effective in inhibiting scale formation. The experimental results in the laboratory indicate that the proper dose is
35 ppm when the concentration of calcium is 1000 mg/L and of magnesium is 2800 mg/L. The pH of the feed water
was in the range of 39. The efficiency of calcium scale inhibition of PAP-1 is higher than 97.24% and magnesium
scale inhibition is higher than 98.63% with 9 ppm PAP-1. The test performed at the Dalian seawater RO plant
confirmed the scale inhibition ability of PAP-1 compared with the Nalco PermaTreat 191 scale inhibitor. The results
from both antiscalants were similar. The average scale formation rates of calcium and magnesium of 14 samples was
2.822 g/h and 5.562 g/h separately with the addition of PAP-1 in each membrane unit; PAP-1 was more effective than
Nalco PermaTreat 191. At the same time, the algae growth inhibition test showed that the addition of PAP-1 does not
affect the growth of algae, which is an indication that PAP-1 has no toxicity and is a suitable and environmentally
friendly antiscalant.

Keywords: Membrane scaling; Antisclant; RO; Desalination

1. Introduction Desalination of seawater by RO to produce fresh

water has also been widely used in China. Several
The application of reverse osmosis (RO) for
seawater reverse osmosis (SWRO) plants of
desalination of seawater has increased rapidly
30005000 t/d have been constructed in Dalian,
with the construction of large RO plants [1,2].
China.
*Corresponding author.

0011-9164/06/$ See front matter 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.desal.2005.11.024


238 H.-Y. Li et al. / Desalination 196 (2006) 237247
The RO system has become an integral part to
the production of potable water and ultrapure
water in industry. It is planned that more than
200,000 t of fresh water will be produced from
seawater every day before 2010 in Dalian.
However, problems that affect the performance of
membranes and the application of RO still exist.
High cost is a major one; another critical problem
that affects the operation of SWRO plants is
membrane scaling. The third problem is the effect
of brine seawater to the sea environment because
several chemicals are added to the pretreatment
process.
Membrane scaling is caused by the precipi-
tation of unsoluble salts as feedwater is converted
to brine [36]. The concentration effect generated
by the separation of a pure water stream from
seawater leads to a supersaturation state for
sparingly soluble species such as CaCO3, CaSO4,
Ca2(PO4)3, Mg(OH)2, MgCO3, Mg2(PO4)3, BaSO4,
SrSO4 and so on. This leads to precipitation of
scale deposits on the membrane surface, which
greatly impairs the performance of RO desali-
nation systems [7]. Scale on the membrane sur-
face results in a progressive decline in perfor-
mance such as reduction in the permeate flux [8],
a decrease in salt rejection, increase in energy
consumption and a high cleaning frequency. If
allowed to develop sufficiently, membrane scal-
ing can lead to destruction of the membrane
(membranes represent 2030% of the capital of
the plant) [9].
Membrane scaling can be prevented by four
methods [1012]. The first is acidification. The
acid consumes part of the bicarbonate in the feed
and converts it to carbon dioxide. The second is
the scale inhibitor method where scale-inhibiting
chemicals are used to alter the physical or chemi-
cal nature or the growth mechanisms of precipi-
tation and prevent scaling until the brine stream
leaves the RO system. The third method depends
on operating the RO system at low recovery
where the solubility problems are not encoun-
tered. The last method is softening which consists
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of treating the water in tanks to which lime and
soda ash are added. The added lime reacts with
bicarbonate to produce CaCO3 sludge.
One of the most common methods used to
prevent or control the scaling of different salts in
seawater feed is the addition of scale inhibitors.
Antiscalants have been widely applied for many
years in RO membranes to prevent scaling and
improve RO plant performance and have proven
to be an efficient measure. At present, there are
various antiscalants on the market, but most of
them have problems such as high cost and serious
environmental influence, which have been the
focus of attention. It is calculated that the cost of
chemicals accounts for about 10% in the pro-
duction of fresh water in Dalian. Therefore, it is
important to reduce the cost of antiscalants and
reduce their harm to environment. The decrease
of chemical costs can reduce the cost of product
water and promote the development of seawater
desalination.
The seawater in China is different from that of
Middle East [1]. The TDS of Dalian seawater is
lower. Analysis indicates that the concentration of
calcium, magnesium, barium, strontium and sili-
con in Dalian seawater is all lower than that of
the Arabian Sea region. The scaling sample
analysis of the Dalian RO desalination plant also
shows that the content of calcium and magnesium
scale makes up almost all the inorganic scale;
none of the other sparingly soluble species are
found in the scale. Calcium and magnesium scale
becomes an important factor that affects the
operation of RO in Dalian, China.
A new antiscalant was developed by using
laboratory tests and field trials in the Dalian sea-
water RO desalination plant. Test results indicate
that the new antiscalant, PAP-1, is environmen-
tally friendly, biodegradable and efficient.
2. Experimental
The experimental work was carried out in four
successive stages. In the first stage, membrane

H.-Y. Li et al. / Desalination 196 (2006) 237247
scaling was analyzed by SEMEDS and XRD;
then the feedwater chemistry composition of
Dalian seawater was examined. In the second
stage the new PAP-1 antiscalant was synthesized
and tested by IR and viscometry in the laboratory.
In the third stage, a performance test of PAP-1
and its influence on the growth of algae was done
in the laboratory and the biodegradability of
PAP-1 was evaluated. Lastly, the performance of
PAP-1 compared to Nalco Permatreat 191 was
studied at the Dalian SWRO desalination plant.
2.1. Membrane scale analysis
Fig. 1 shows the membrane scale analysis of
the Dalian RO desalination plant by SEMEDS.
Cl and Na elements are especially high in the
scale, perhaps caused by adsorption of Cl and Na
ions on the scale. The content of calcium and
magnesium scale is relatively high among the
sparingly soluble species. Further examination
using the X-ray diffraction (XRD) spectrum has
demonstrated (data not shown) that there were no
peaks to indicate the crystallization structure,
suggesting that the scale is amorphous. From the
figure, the main unsolved salts such as CaCO3,
CaSO4, Ca2(PO4)3, MgCO3, Mg2(PO4)3 and
Mg(OH)2 probably exist in the membrane scale.
The element aluminum also exists in the scale,
Fig. 1. SEMEDS analysis for membrane scaling.
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239
but aluminum in the seawater is low, which may
have been introduced by the flocculation process.
In this study, the concentration of calcium and
magnesium was selected as indicators to inves-
tigate the effect of scale inhibition on this kind of
calcium and magnesium-containing scale.
2.2. Feedwater chemistry composition
Table 1 shows the typical chemistry compo-
sition of RO feedwater in the Dalian RO plant by
laboratory analysis. Calcium, magnesium, chlo-
ride, sulfate, total hardness, and total alkalinity
were measured with titration; iron, silicon dioxide
and orthophosphate with spectrophotometry; bar-
ium, strontium, sodium and potassium with ato-
mic absorption spectrometry. Total dissolved
solids were measured by a TDS instrument.
2.3. Synthesis of PAP-1
PAP-1 was synthesized in our laboratory
according to the following approach. First 50.00
doses maleic anhydride was dissolved in 25 doses
water, then 100 doses 30wt% aqueous ammonia
hydroxide was added slowly, the reaction last for
6h at 80-85 , then the temperature was increased
to 220 and held at that temperature for about 7 h,
a dark, yellow brittle product was obtained.
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240 H.-Y. Li et al. / Desalination 196 (2006) 237247

Table 1
Typical seawater analysis in Dalian, China

Ion Concentration (mg/L)

Calcium 377.75
Magnesium 1274.50
Barium 0.01
Strontium 0.45
Iron 0.38
Sodium 9854
Potassium 474.30
Silicon dioxide 0.51
Fig. 2. IR spectrum of PAP-1.
Chloride 18072
Sulfate 2270.25
Orthophosphate 0.14 Table 3
Total hardness (CaCO3) 6254.79 Composition of the simulated concentrated seawater
Total alkalinity 122.37
Total dissolved solid 39012.27 Calcium, mg/L as Ca 1000
pH 7.65 Magnesium, mg/L as Mg 2800
Chloride, mg/L as Cl 36950
Sodium, mg/L as Na 20000
Table 2 Bicarbonate, mg/L as CO32- 350
Analysis of characteristic peaks in IR spectrum Sulphate, mg/L as SO42- 5800
Potassium, mg/L as K 950
Wave numbers (cm!1) IR spectrum analysis pH 7.76
3387.96 O-H stretching vibration
1712.11 C=O stretching vibration
1642.43 C=O stretching vibration acids compound was added to the PASP, and the
1551.60 N-H bending vibration mixture reaction continued for 6 h at 50EC. When
1183.54 C-N stretching vibration it was transparent, the synthesis process of PAP-1
1042.22 C-O stretching vibration was completed. Its comparative molecular weight
is between 3000 and 6000 tested by viscometry.
The IR spectrum of the PAP-1 is shown in Fig. 2.
Then the product (about 30 doses) was slurried in An analysis of characteristic peaks in the IR
40 doses of water and the slurry stirred. Sodium spectrum is shown in Table 2.
hydroxide (about 25 doses of 50% wt/wt solu-
tion) was added to the stirred slurry at a rate so
2.4. Performance test in the laboratory
that the slurry temperature did not exceed about
80EC, and the pH value of the slurry did not The scale-inhibiting performance for calcium
exceed about 9.5. After the sodium hydroxide and magnesium-containing scale was evaluated in
solution addition was complete, sufficient water static experiments, also known as beaker experi-
was added to provide a solid concentration of ments. This method used simulated concentrated
about 42 wt%, constituted substantially by the seawater as shown in Table 3. The evaluation was
hydrolyzed product. Polyaspartic acid (PASP) also conducted in parallel tests under carefully
was produced. At last, a kind of polycarboxylic controlled conditions.

H.-Y. Li et al. / Desalination 196 (2006) 237247
2.4.1. Calcium scale inhibition test
This test was designed to measure the anti-
scalants ability to inhibit scale formation. The
soluble calcium was determined by titration with
EDTA.
Tests were made with 1.00, 2.00, 3.00, 4.00,
5.00, 7.00, and 9.00 ppm PAP-1. A blank solu-
tion was also prepared containing no PAP-1.
Simulated concentrated seawater (200 mL) was
poured into the beaker, the PAP-1 was added and
pH was adjusted using NaOH and HCl solutions.
Then the beakers were put into a water bath for
8 h at 80EC. When titrating the concentration of
calcium in the solution, it was first filtrated and
then diluted to 200 mL. The calcium scale
inhibition test was done at different pHs: 3.00,
4.00, 5.00, 6.00, 7.00, 8.00, 9.00. This test was
repeated three times, and the final result was the
average. To calculate the percentage inhibition of
PAP-1, the following equation was used [6]:
Ca 2+ Ca 2+
% inhibition = antiscalant
Ca 2+ Ca 2+
original
2+
where [Ca ]antiscalant is the concentration of soluble
Ca2+ in an antiscalant-containing solution (mg/L),
[Ca2+]original is the concentration of soluble Ca2+ in
the original solution (mg/L), and [Ca2+]blank is the
concentration of soluble Ca2+ in a blank solution
(mg/L). The higher the percentage inhibition, the
better the scale inhibition ability of the calcium
scale.
2.4.2. Magnesium scale inhibition test
The experiment method was the same for the
calcium scale inhibition test. The concentration of
total hardness and calcium were determined by
titration with EDTA. The soluble magnesium was
calculated. To calculate the percentage inhibition
of PAP-1, its equation was:
% inhibition =
Mg 2+
antiscalant
Mg 2 +
blank
Mg 2+ Mg 2+
original
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241
2.5. Algal growth inhibition test
This test was used to assess the toxic effects of
PAP-1 towards aquatic algae. The algal growth
inhibition test was performed using the Chlorella
autotrophica. The algal cells were cultured in test
tubes using the culture medium at 25EC under
continuous illumination. This test was carried out
with 0.00, 1.00, 2.00, 3.00, 4.00, 5.00, 7.00, and
9.00 ppm PAP-1 in eight culture flasks with
almost the same algae present and the culture
medium under the same conditions; the total
solution volume was 100 mL in the flasks. Inhi-
bition of the algal growth relative to the blank
sample was determined by measurements of opti-
cal density in a spectrophotometer at a wave-
length of 670 nm and the content of chlorophyll-a
(ch-a). Both of the two methods were widely used
to indicate the growth of algae [13]. All details of
the test protocol of ch-a were described in
GB17378.7-1998, China. The 24 h, 48 h, 72 h
(1) and 168 h values of optical density and ch-a were
blank
100 measured to calculate the growth of algae.
blank
2.6. Percentage biodegradability test
Percentage biodegradability of PAP-1 was
evaluated by the shaking-bottle incubating test
[14]. Test mixtures included activated sludge,
inorganic salts inoculum and the test compound
PAP-1. At the same time, blank solutions with
only inoculum were prepared. The test mixture
was mixed by shaking at 120 rev/min and
incubated at a constant temperature of 30EC. The
test lasted for 28 days. Both the potassium
permanganate index (CODMn) of test mixtures
and blank solutions at day 1, 4, 8, 12, 16, 20 and
28 were measured to calculate percentage biode-
gradability. The following equation was used:
(%) = 1
(
COD nMn ) 100% (3)
(2)
100
(
COD1Mn )
blank where n is the number of incubating days; n is
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242 H.-Y. Li et al. / Desalination 196 (2006) 237247

Fig. 3. Process scheme for the RO installation of the field trial.

the percentage biodegradability; (CODMnn) is the Table 4

(CODMnn) of the test mixture minus (CODMnn) Operational parameters of RO installation (units 1 and 2)
of the blank solution; (CODMn1) is the original
Recovery, % 40%
(CODMn1) of test mixture minus (CODMn1) of the
Feedwater conductivity after 45,80047,500
blank solution at the start of the test. filtering, s/cm
Feed flow, m3/h 5657
2.7. Performance test in the RO desalination Product flow, m3/h 2223
Reject flow, m3/h 3435
plant
Pressure of high-pressure pump, bar 51
Based on the satisfactory results in the Salt rejection, % 99.5
laboratory, in the subsequent stage the test was Number of membrane units 96
performed in a seawater RO desalination plant in Feed pressure of RO membrane, bar 51
Dalian for 6 months. The plant consists of two
parallel RO units, both single-stage RO systems.
Each unit was fitted with an antiscalant injection carried out. The random samples of feed, reject
system. Fig. 3 gives the schematic diagram of the and product were analyzed, and simultaneously
RO unit. Operational parameters are listed in scale formation rates of calcium and magnesium
Table 4. were calculated.
The Nalco PermaTreat 191 antiscalant, which
had already been widely applied in scale inhi-
2.8. Calculation of scale formation rates of
bition, was used in Unit 1, while PAP-1 was used
calcium and magnesium
in Unit 2. And the effectiveness of PAP-1 in
controlling scale formation was compared with The method to monitor the performance of
Nalco PermaTreat 191 under the same operating two different antiscalants was the calculation of
conditions. A direct comparison of the perfor- scale formation rates of calcium and magnesium
mance characteristics of the two antiscalants in in the RO system. The lower the scale formation
inhibiting calcium and magnesium scale was rates of calcium and magnesium, the better the

H.-Y. Li et al. / Desalination 196 (2006) 237247
antiscalants performance. To calculate the total
scale formation rate of the entire RO system, the
following equation was defined:
M C0V0 C1V1 C2V2
= =
t 1000 t
When recovery is Y, V1 is equal to (1!Y) times
of V0, and V2 is equal to Y times of V0. Thus, we
can deduce the following equation:
V0 C0 (1 Y ) C1 YC2
= rate values (g/L).
1000 t
Q t C0 (1 Y ) C1 YC2 (5)
t
= Q C0 (1 Y ) C1 YC2
where is the total scale forming rate of calcium
or magnesium in the RO system (g/h); C0, C1 and
C2 are the concentrations of feed, reject and
product of calcium or magnesium (mg/L); V0, V1
and V2 are the volume of feed, reject and product
(L); and Q is the feed flux of the RO system
(m3/h), and t is the running time of the RO
system (h).
Generally, the RO system is composed of
many identical membrane units. If the number of
membrane units is N, for each membrane unit in
the RO system, the scale formation rate can be
calculated as follows:
Q C0 (1 Y ) C1 YC2
0 = = (6)
N N
2.9. Calculation error in test
The experimental standard deviation was
calculated to evaluate errors in the real test. It
followed the Bessel formula:
1 n
( xi x )
2
S2 =
n 1 i =1
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243
To calculate the experimental standard deviation
in the scale formation rates of calcium and
magnesium, the Bessel formula can be deduced
as:
(4) 1 n
( 0 i 0 )
2
S2 =
n 1 i =1
where S is the experimental standard deviation, n
is the total number of scale formation rate value,
0i is each scale formation rate value separately
(g/L), and 0 is the average of all scale formation
3. Results and discussion
The SEMEDS analytical results of membrane
scaling and composition of Dalian seawater are
listed in Fig. 1 and Table 1. It was found that the
content of barium, strontium and silicon dioxide
is low in Dalian seawater. From the analysis of
membrane scaling at the Dalian RO desalination
plant, it was also found that inorganic scaling is
mainly composed of magnesium and calcium-
containing scale; other soluble species such as
barium, strontium and silicon were not present. It
can be predicted that magnesium and calcium
scale is the crucial factor affecting the perfor-
mance of RO membranes at the Dalian RO plant.
The amount of magnesium scale was larger than
calcium scale. The proportion between magne-
sium and calcium was nearly 2 to 1.
Figs. 4 and 5 show calcium and magnesium
scale inhibition percentages with different doses
of PAP-1 at different pHs. The results reveal that
when pH is low, the possibility of forming
calcium and magnesium scale is smaller, so the
low dose of PAP-1 displays excellent efficacy.
With the increase of pH, the inhibition percentage
declines somewhat when the dose of PAP-1 is the
same. The proper dose of PAP-1 varies with the
change of pH. When pH is 3, the efficiency to
(7)
inhibit scale formation reached 100% with 3 ppm

244 H.-Y. Li et al. / Desalination 196 (2006) 237247
Fig. 4. Calcium scale inhibition percentage of different
doses of PAP-1 at different pHs.
Fig. 5. Magnesium scale inhibition percentage of dif-
ferent doses of PAP-1 at different pHs.
PAP-1. When the pH is 9, the calcium scale
inhibition percentage of PAP-1 was 97.24% with
9 ppm PAP-1 and magnesium scale inhibition
percentage was 98.63%.
Using the optical density and the concen-
tration of Ch-a as indicators of the growth of
algae, Figs. 6 and 7 show the effect of PAP-1 on
the growth of algae. Eight different concentra-
tions under a concentration of 9 mg/L of PAP-1
were applied and the effect was tested after 0, 24,
48, 72 and 168 h. The results indicate that the
growth of algae is not limited by PAP-1.
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Fig. 6. Optical density with different concentrations of
PAP-1.
Fig. 7. ch-a with different concentrations of PAP-1.
Fig. 8 shows that percentage biodegradability
of PAP-1 reached 38.25% at day 8 and 58.3% at
day 20. PAP-1 was easily biodegraded under the
test conditions. PAP-1 degraded quickly between
day 1 and 12; then the degradation rate began to
slow, and lastly was turned into a plateau phase
on day 20 to the end of the test at day 28.
According to the results from this study,
PAP-1 is an environmentally friendly antiscalant.
Figs. 9 and 10 show the different scale forma-
tion rates of calcium and magnesium in each
membrane unit separately compared with two
kinds of scale inhibitors used in the same RO

H.-Y. Li et al. / Desalination 196 (2006) 237247
Fig. 8. Percentage biodegradability of PAP-1 vs. days.
Fig. 9. Comparison of calcium scale formation rate
between #1 and #2 RO units.
Fig. 10. Comparison of magnesium scale formation rate
between #1 and #2 RO units.
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245
Table 5
Experimental standard deviations in the calculation of the
real test
RO system (S2) #1 unit #2 unit
Calcium scale formation rate 0.048 0.142
in each membrane unit
Magnesium scale formation rate 0.488 0.239
in each membrane unit
desalination plant. The results from the plant
performance show that the scale formation rate of
calcium of Unit 2 in each membrane unit is lower,
which indicates that PAP-1 has a better calcium
scale inhibition capacity. The average scale
formation rate of calcium for 14 samples in
Unit 2 was 2.822 g/h, lower than Unit 1 whose
average scale formation rate was 3.585 g/h.
The results in Fig. 8 demonstrate that magne-
sium scale formation rates in each membrane unit
of both antiscalants are higher owing to the larger
concentration of magnesium in seawater than
calcium. Thus, the content of magnesium scale in
the membrane scaling was more than calcium
scale. The average scale formation rate of mag-
nesium from 14 samples in Unit 2 was 5.562 g/h,
a little lower than Unit 1 whose average scale
formation rate was 5.849 g/h.
The experiment in the RO plant confirmed the
scale inhibition ability of PAP-1. Therefore, it
can be established that PAP-1 is successful in
controlling scale formation at the tested condi-
tions and performance is quite good. The cal-
culation error is given in Table 5.
Fig. 11 shows the variation in product con-
ductivity and feed pressure of RO membranes
monitored in the plant for both RO units. The
results show almost a constant and stable value of
product conductivity for both inhibitors without
a large change from the initial operation con-
ditions. The value of product conductivity varied
between 187 s/cm and 206 s/cm. The feed-
water conductivity after filtering was 45,800

246 H.-Y. Li et al. / Desalination 196 (2006) 237247
47,500 s/cm. Salt rejection is above 99.5%. The
stability of PAP-1 is proven. The test performed
at the SWRO desalination plant in Dalian was
conducted continuously for 6 months, during
which the operation was smooth and steady. Feed
pressure of the RO membranes is also shown in
Fig. 9. The feed pressure of RO membranes was
maintained at 51 bar at all times in the two RO
units. Product flow did not vary greatly, and the
values varied from 22 to 23 m3/h. This also
proved the capability of PAP-1.
4. Conclusions
Through the scale inhibition experiments in
the laboratory, PAP-1 proved to be effective in
inhibiting scale formation. The proper dose is
35 ppm when the concentration of calcium is
1000 mg/L and concentration of magnesium is
2800 mg/L according to the different pHs. When
pH was 3.00, scale-inhibiting efficiency reached
100% with 3 ppm PAP-1. While pH was 9.00, the
calcium scale inhibition percentage of PAP-1 was
97.24% and magnesium scale inhibition was
98.63% with 9 ppm PAP-1.
The addition of PAP-1 did not affect the
normal growth of algae. Percentage biode-
gradability of PAP-1 reached 38.25% at day 8
and 58.3% at day 20.
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Fig. 11. Product conductivity and RO membrane mean
pressure vs. day.
The tests performed at the Dalian SWRO
desalination plant confirmed the scale inhibition
ability of PAP-1 compared to other scale inhi-
bitors. The average scale formation rates of
calcium and magnesium from 14 samples were
2.822 g/h and 5.562 g/h separately with the
addition of PAP-1 in each membrane unit.
The value of product conductivity varied
between 187 s/cm and 206 s/cm. Feedwater
conductivity after filtering was 45,800
47,500 s/cm. Salt rejection was above 99.5%.
PAP-1 is a suitable and environmentally friendly
antiscalant.
Acknowledgement
The authors would like to acknowledge the
support of the seawater RO desalination plant in
Dalian and Dr. Hou for the test.
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