Bioresource Technology 100 (2009) 7478

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Bioresource Technology
journal homepage: www.elsevier.com/locate/biortech

Effect of mixing on spontaneous struvite precipitation

from semiconductor wastewater
Daekeun Kim, Jinhyeong Kim, Hong-Duck Ryu, Sang-Ill Lee *
Department of Environmental Engineering, Chungbuk National University, Cheongju, Chungbuk 361-763, Republic of Korea

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

Article history: The objective of this study was to investigate on the effect of mixing intensity (G) and mixing duration
Received 27 December 2007 (td) on struvite precipitation in the chemical mechanical polishing (CMP) wastewater generated from
Received in revised form 13 May 2008 the semiconductor manufacturing process. Batch-scale experiments revealed that struvite crystallization
Accepted 17 May 2008
was affected by both G and td. The mixing effect was to enhance the mass transfer of solute to the crystals
Available online 2 July 2008
in the process, resulting in the improvement of struvite crystallization and growth. By forming struvite,
removal efciencies of N and P increased logarithmic with the multiple values of G and td, i.e., Gtd. Insuf-
Keywords:
cient mixing energy with the Gtd value less than 105 caused an increase in the formation potential of
Struvite
Mixing
unexpected precipitate unlike to pure struvite, causing a decrease in removal efciencies of N and P in
Nitrogen the process. At the Gtd value over 106, struvite precipitation was not restricted by uoride, of which high
Phosphorus level inherently contained in the CMP wastewater. The study results can be taken into consideration in
Fluoride the design and operation of the struvite precipitation process for both nutrient (N and P) removal and
recovery.
2008 Elsevier Ltd. All rights reserved.

1. Introduction
The semiconductor manufacturing process generates a large
quantity of hazardous wastes, which include organic solvents,
acids, bases, salts, heavy metals, ne suspended oxide particles,
and other organic compounds (Huang and Liu, 1999; Lai and Lin,
2003). The management of these wastes has become an important
issue in the industry. Especially, since the high levels of ammonia,
phosphate, and uoride are presented in the wastewater generated
from the process of chemical mechanical polishing (CMP), the
treatment of the CMP wastewater is still a pending question in
the industry.
It is believed that the biological application is inadequate in the
CMP wastewater because it has various toxic substances which in-
hibit active nitrication by nitrifying bacteria (Lin and Kiang,
2003). As an alternative, the precipitation of nitrogen and phos-
phorus in a struvite crystal would be attractive in treating high le-
vel of ammonia and phosphate in the stream (Kabdasli et al., 2000;
Kim et al., 2007; Nelson et al., 2003). Struvite (Magnesium ammo-
nium phosphate, MgNH4PO4  6H2O) crystallized as a white ortho-
rhombic crystalline structure, which is composed of three
components, i.e., magnesium, ammonium, and phosphate, in equal
molar concentrations (Lee et al., 2003). The factors affecting the
struvite crystallization reaction include pH, temperature, supersat-
* Corresponding author. Tel.: +82 043 261 2469; fax: +82 043 272 2469.
E-mail address: gatorlee@cbnu.ac.kr (S.-I. Lee).
2+ 3
uration of solutes (NH 4 ; Mg ; PO4 ), the presence of crystalliza-
tion nucleus, the type of magnesium source, and impurity ions
(Bouropoulos and Koutsoukos, 2000; Kim et al., 2007). In terms
of nutrient (i.e., nitrogen and phosphorus) recovery, struvite gained
from the stream can be taken for its agricultural reuse.
In our previous study (Ryu et al., 2008), the eld-scale applica-
tion of struvite precipitation has been conducted in the CMP
wastewater treatment. The system performance was evaluated
with respect to the operational parameters, i.e., pH, solute concen-
2+
tration, and impurity ions (other ions except for NH 4 , Mg , and
PO3
4 ). It is worthwhile to note from our unpublished study that
the CMP wastewater showed possible toxicity because organic sol-
vents are unavoidably contained in the wastewater through the
polishing process, while any toxicity was not detected in the stru-
vite samples obtained through the precipitation process.
It was also observed from our previous study (Ryu et al., 2008)
that the reaction of struvite formation apparently varied at the dif-
ferent mixing strength applied in the system (Details have been
not reported). It is general in crystallization process that crystal
formation is primarily made by nucleation from crystal embryos
and nucleus growth in sequence (Doyle and Parsons, 2002; Jones,
2002). The generation of a nucleus depends on the intensity of ini-
tial mixing, and its growth relies on mixing duration (Jones, 2002).
Ohlinger et al. (1999) observed in their study of the struvite precip-
itation process that the mixing intensity had a signicant effect
on struvite crystal nuclei development. Wang et al. (2006)
demonstrated that both sturivite crystal size and settling were

0960-8524/$ - see front matter 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.biortech.2008.05.024
 D. Kim et al. / Bioresource Technology 100 (2009) 7478
signicantly affected by mixing strength. However, details about
the effect of mixing on struvite precipitation are still limited in
our best knowledge. Further investigation should be made to pro-
vide information to improve the practical application of struvite
precipitation in the CMP wastewater. It is also worthwhile to note
that since the CMP wastewater contains a high level of uoride, the
effect of uoride on the struvite formation should be considered in
the process.
For this purpose, batch-scale experiments were designed to
identify the mixing effect on struvite precipitation in the CMP
wastewater. The goal was to investigate (1) the effect of mixing
intensity (G) and duration (td) on struvite precipitation with re-
spect to the removals of ammonia and phosphate; (2) the effect
of initial concentration of nitrogen in the sample as a function of
the multiple value of G and td; (3) mass balance analysis and (4)
uoride removal as a function of the multiple value of G and td.
2. Methods
2.1. Characteristic of CMP wastewater
The CMP wastewater tested was obtained from the semiconduc-
tor manufacturing plant in Cheongju, Korea. It had pH of 2.9, NH4N
concentration of 100 mg/L (7.1 mM), and PO4P concentration of
286 mg/L (9.2 mM) on the average. High concentration of uoride
was found about 172 mg/L (9.1 mM) on the average. The character-
istics of the sample wastewater were summarized in Table 1.
2.2. Materials
For the struvite reaction, magnesium chloride (MgCl2  6H2O)
solution was used as an alternate source of magnesium ions. In
all experiments, magnesium was fed to reach at the molar ratio
of NH4:Mg of 1:1.2 because struvite precipitation occurs when
the combined concentrations of the three components, i.e., NH4,
Mg, and PO4, exceed the struvite solubility limit (Ohlinger et al.,
1998). 2.5 N NaOH was used to adjust pH to 9 in the solutions. In
the previous study (Ryu et al., 2008), the optimum pH for struvite
formation was found to range from 9 to 10. All chemicals used
were analytical grade.
2.3. Experimental setup
The standard jar tester with six paddles was used in all experi-
ments. Jars were made of acrylic plastic with dimensions of
11.5  11.5  21 cm and held 2.0 L of liquid. The paddles at the
end of each stirrer shaft, which were made of stainless steel, had
a diameter of 7.6 cm and a height of 2.5 cm. The stirring device in-
cluded a tachometer and a controller so as to adjust the revolution
rates ranging from 0 to 360 rev/min. All experiments were carried
out at ambient laboratory temperature.
In all experiments, struvite formation proceeded by simulta-
neous addition of excess magnesium sources and the sample solu-
tion, and the buffering reagent was nally fed. This experimental
procedure provided the optimum condition to reach the thermody-
Table 1
The characteristics of the wastewater samples used in this study
Cations Concentration range (mg/L) Anions Concentration range (mg/L)
+ 
Na 6.819.5 F 129.3199.72
NH Cl
4 N 74.9179 6.911.8
K+ 2.010.1 NO 3 8.311.7
Mg 2+
1.82.5 PO3
4 P 209.1360.4
2
Ca2+ 5.012.2 SO4 012.7
pH 2.9a
a
Dimensionless.
75
namic equilibrium of struvite precipitation (Kim et al., 2007). Mix-
ing intensity (G) values tested in this study varied from 49 s1 to
940 s1. The applied mixing duration (td) ranged from 2 min to
90 min. The applied G value was calculated based on the interac-
tion between the revolutions of paddle and the velocity gradient
based on the suggestion by Cornwell and Bishop (1983), in which
study the velocity gradient had the linear correlation to the impel-
ler speed.
2.4. Analytical method
The concentration of ammonia nitrogen was measured by using a
UV-Spectrophotometer (HACH DR-4000, Loveland, CO, USA). Ortho-
phosphate level was determined by the ascorbic acid method. The
analyses of ions including uoride were done by using an ion chro-
matograph (DX-80, Dionex, USA). For the separation of anion, an
IonPac AG4A-SC (50 mm  4 mm) guard column and an IonPac
AG4A-SC (250 mm  4 mm) analytical column were used. The elu-
ent was 1.8 mM Na2CO3/1.7 mM NaHCO3 at a ow rate of 2 mL/
min. For cationic separation, an IonPac CG412 (50 mm  4 mm)
guard column and an IonPac CS12 (250 mm  4 mm) analytical col-
umn were used. 20 mM Methane sulfonic acid was used as the elu-
ent at a ow rate of 1 mL/min. The precipitate crystal structure was
determined with an X-ray diffraction (XRD, Model DMS2000 sys-
tem, SCINTAG) and a scanning electron microscopy (SEM, Model
S-2500 C, Hitachi) equipped with an energy-dispersive X-ray ana-
lyzer (EDX, MS2, Sigma). All soluble parameters were determined
in samples ltered through 0.45 lm membrane lter.
3. Results and discussion
3.1. Effect of mixing intensity (G) and mixing duration (td)
Fig. 1 describes the effect of values of G and td on the removal of
nitrogen and phosphorus in the process of struvite precipitation.
Overall removal performances of nitrogen and phosphorus were
observed to be similar. At low values of G and td, removal efcien-
cies of nitrogen and phosphorus were unexpectedly low. In con-
trast, as those values were increased, removal efciencies of
nitrogen and phosphorus correspondingly increased. Interestingly,
the removal curves presented in Fig. 1 well corresponded to the
contour line of the multiple values of G and td (i.e., Gtd), indicating
that high value of Gtd was unavoidable to achieve sufcient removal
performance of nitrogen and phosphorus from the sample. How-
ever in Fig. 1, a little different observation was inquiringly found
at the 70% PO4P removal line as compared with that for NH4N.
It should be noted that phosphorus concentration was much higher
than that of nitrogen in the sample; struvite crystallizes in equal
molar concentrations of NH4, PO4, Mg; and mixing energy affects
struvite crystallization. These facts might have remarkable rela-
tions with the removal of nitrogen and phosphorus through struvite
formation. Detailed discussion is made in the following sections.
In Fig. 2, removal efciencies of nitrogen and phosphorus were
plotted as a function of the Gtd value. The data were obtained from
the sample with initial concentrations of 94 mg NH4N/L (6.7 mM
NH4N) and 293 mg PO4P/L (9.5 Mm PO4P). It is apparent in
Fig. 2 that both removal patterns of nitrogen and phosphorus were
a logarithmic increase with the Gtd value. Nitrogen removal ef-
ciencies increased to the 80% level, but remained at this level while
the G  td value was at least 106. For phosphorus, the removal ef-
ciency increased to the 70% level while the G  td value reached at
106. Overall, high mixing energy was effective in the removal of
nitrogen and phosphorus by forming struvite. Wang et al. (2006)
demonstrated that relatively high mixing energy could shorten
the time needed for the development of struvite crystal nuclei. It
76 D. Kim et al. / Bioresource Technology 100 (2009) 7478

Fig. 1. Effect of mean velocity gradient (G) and mixing duration (td) on NH4N removal (a) and PO4P removal (b) in the process of struvite precipitation: the dotted line
represents the contour line for the multiple value of G and td value (Gtd). Initial concentrations in the sample were 94 mg/L (6.7 mM) and 299 mg/L (9.7 mM) for nitrogen and
phosphorus, respectively.

tial concentrations of nitrogen, removal performance seems to

Fig. 2. NH4N and PO4P removal efciencies as a function of the multiple values of
G and td. Initial concentrations in the sample were 94 mg/L (6.7 mM) and 293 mg/L
(9.5 mM) for nitrogen and phosphorus, respectively. R2 values of both regression
curves were over 0.99.
have a similar pattern. For each case, nitrogen removal efciency
logarithmically increased with the Gtd value. The maximum re-
moval efciencies were 98%, 88% and 86% for initial nitrogen con-
centrations of 179 mg/L (12.8 mM), 110 mg/L (7.9 mM), and
94 mg/L (6.7 mM), respectively. It was also shown in Fig. 3 that
the removal efciency was observed to be relatively high when
much higher initial concentration of nitrogen was contained in
the sample. Further discussion is made that even at a low initial
concentration of nitrogen in the sample, the mixing energy en-
hanced the nitrogen removal.
It is worthwhile to note that the conict intensity among the
solute particles might become stronger as the solute concentration
increased. Hence at a low level of the Gtd value applied, the conict
intensity among the solute particles can be a driving force to gen-
erate the crystal nucleus. In other words, the particles in solution
can accelerate the speed of crystal nuclei generation while the sol-
ute concentration increased. Bouropoulos and Koutsoukos (2000)
observed that the induction time to reach the crystallization had
an inverse relation with the solution saturation, demonstrating
that spontaneous nucleation is possible at supersaturation level.

was also interestingly observed from Fig. 2 that below 2  105 of

Gtd, phosphorus removal efciencies were much better than those
of nitrogen. In contrast, this performance was in reverse at the Gtd
value above 2  105. This observation might be caused by the mix-
ing effect. Further discussed is made in Section 3.3 of mass balance
analysis.
Microscopic examination of the struvite crystals by using SEM
illustrates that the morphology of the crystals precipitated was dif-
ferent depending on the Gtd value applied, while at the same value of
Gtd it was alike regardless of the matrix of G and td (Detailed data
were not shown). The observation revealed that the morphology
of the struvite crystal can be affected by the Gtd applied, but it would
be apparently stable regardless of each value of mixing intensity (G)
and duration (td) only if the multiple values of G and td are the same.

3.2. Effect of initial concentration of nitrogen in sample

It should be noted that the sample targeted had a wide range of Fig. 3. Effect of initial concentration of nitrogen in the sample on nitrogen removal.
nitrogen concentration. Fig. 3 illustrates that at three different ini- R2 values of regression curves were over 0.98.
 D. Kim et al. / Bioresource Technology 100 (2009) 7478
Momberg and Oellermann (1992) found that at a low ammonia
nitrogen concentration, the growth of struvite precipitate was re-
stricted due to the limitation of the transport of ammonium ions
to the crystal surface. In terms of mass transfer coefcient as cor-
relations of dimensionless numbers, Sherwood number is roughly
proportional to mixing intensity (G) based on the observation by
Garcia-Ochoa and Gomez (1998). This demonstrates that by accel-
erating the mixing in the process, the potential of struvite precip-
itation can be enlarged due to an enhancement of mass transport
of ammonium ions in the system.
3.3. Mass balance analysis
In this analysis, it was assumed that chemical precipitation is
the only removal mechanisms in the present process, and the ideal
molar ratio of Mg:P:N is to be 1:1:1 (Lee et al., 2003) only if the
precipitate after the reaction is pure struvite. Hence the compari-
son of molar mass of three components removed from the sample
might give details about the resulting precipitate. The sample, in
which pure struvite was precipitated, had to provide a molar mass
of three components to be 1:1:1. Fig. 4a shows the comparison of
molar mass of three components removed from the sample at dif-
ferent Gtd values. The observed molar ratios of three components
were different, depending on the applied Gtd value. While the ap-
plied Gtd values were less than 105, molar mass of magnesium
was greater than or similar to those of phosphorus and ammo-
nium. In contrast, while the applied Gtd values were over 105, it
was smaller than others. Fig. 4b indicates the corresponding re-
moval efciency of nitrogen in the sample. Nitrogen removal ef-
ciency was relatively high while the applied Gtd values ranged
over 105. The precipitate obtained at Gtd of about 2  105 was char-
acterized by using an X-ray diffractrogram, revealing that the
peaks at this case exhibited several peaks indicative of the pres-
ence of struvite. However, the precipitates at other range of Gtd
were unlike to that of struvite.
Inconsistent mass balance presented in Fig. 4 might be resulted
by unexpected precipitates. Since the excess mass of external mag-
nesium sources was fed in the system in order to exceed the stur-
vite solubility limit, magnesium ions can predominately react
with OH ions in the solutions readily to produce amorphous prod-
ucts such as Mg(OH)2. The generation of this product correspond-
ingly attributed to relatively high molar ratio of magnesium to
ammonium removed from the solution. Further discussion is made
that in the condition of excess concentration of magnesium and
Fig. 4. Mass balance analysis of three components (N, P, and Mg) in the precipitation process: (a) Molar ratio of three components in precipitate; (b) NH4N removal as a
function of molar ratio of PO4P removed to NH4N removed.
77
phosphate, magnesium preferentially react with phosphate to
produce different magnesium phosphates such as hannayite
(Mg3(NH4)2H4(PO4)4  8H2O), shertelite (Mg(NH4)2H2(PO4)2 
4H2O), bobbierite (Mg3(PO4)2  8H2O), and newberyite (MgHPO4 
3H2O). Seckler et al. (1996) discussed in their study of the process
of calcium phosphate precipitation that the possibility of magne-
sium phosphate formation can increase up to 45% only if there is
no calcium ion. If calcium ion exists, calcium ion might preferen-
tially react with phosphate to produce hydroxyapatite, dicalcium
phosphate, and octacalcium phosphate. In the present study, cal-
cium concentration ranged from 5 mg/L to 12.2 mg/L in the CMP
wastewater as shown in Table 1. Golubev et al. (2001) demonstrated
that the unseeded precipitation kinetics of magnesium phosphate
might not only depend on the operational parameters such as the
pH, phosphate, and magnesium concentration in the system, but is
also affected by the stirring condition including induction period
and mixing intensity. Therefore, these unexpected cases were
mainly due to insufcient mixing energy applied in the process.
This also explains the observation in Fig. 2 that nitrogen re-
moval efciencies overwhelmed those of phosphorus over
2  105. Since nitrogen concentration was lower than that of phos-
phorus in this study, nitrogen concentration would be a limiting
factor in struvite precipitation with respect to struvite solubility
product. This is worthwhile only if sufcient mixing energy was
provided in the system. In other cases, pure struvite precipitation
may be limited because of poor crystallization and formation of
amorphous precipitate or different magnesium phosphates, which
was mainly caused by insufcient mixing energy applied.
3.4. Fluoride removal
Since the CMP wastewater had a high level of uoride, it is
important to investigate the effect of uoride on the struvite for-
mation. Fig. 5 shows the removal efciencies of uoride in the
sample by struvite precipitation at the applied different mixing en-
ergy, which was represented by the Gtd value. Fluoride removal
performance was different to those of nitrogen and phosphorus ob-
served in Fig. 2. At the Gtd value of 105, uoride removal was ob-
served to be about 20%. However, it decreased as an increase in
the Gtd value, and nally reached at the 1% level while applying
over 106 of the Gtd value. Based on the regression analysis as
shown in Fig. 5, the relation between the uoride removal and
the Gtd value applied can be explained by as following: log [percent
removal of uoride] = 0.61 log [Gtd] + 4.2, r2 = 0.84.
78 D. Kim et al. / Bioresource Technology 100 (2009) 7478
Fig. 5. Fluoride removal in the process of struvite precipitation: Initial concentra-
tions in the sample were 131 mg/L (6.9 mM), 78 mg/L (5.6 mM), and 191 mg/L
(6.2 mM) for uoride, nitrogen, and phosphorus, respectively.
At a relatively low value of Gtd, uoride would be involved in
the struvite crystallization reaction. Fluoride can be considered
as one of impurities in this reaction. It has been demonstrated by
other studies (Kabdasli et al., 2006; Le Corre et al., 2005) that some
foreign ions can be easily adsorbed on the surface of crystals, and
hence the crystal growth is likely to be retarded. It has been re-
ported by Ryu et al. (2008) that at high concentrations of uoride,
uoride inhibited struvite crystallization because uoride may re-
act with magnesium, forming magnesium uoride (MgF2). How-
ever, while the process was made at a relatively high Gtd value,
uoride would not work for an impurity in struvite crystallization
because sufcient mixing energy amplies the potential of struvite
crystallization as well as its growth. In terms of solubility product,
struvite (Ksp = 1013.12 at 25 C) tended to form easily as compared
with magnesium uoride (Ksp = 108.1 at 25 C) because solutions
were supersaturated with three compounds, i.e., Mg2+, NH4+, and
PO3
4 . This can explain why the uoride removal trends was oppo-
site of nitrogen and phosphorus removal.
The other explanation can be made by analyzing the precipitate
crystallized. It is also important to note that uoride was not de-
tected in the precipitates by using EDX. This demonstrates that
the only removal mechanism of uoride in the system would be
the weak adsorption on the surface of the precipitate, hence the
potential of the adsorption of uoride on the precipitate became
weak as an increase in the mixing energy, probably due to an up-
ward tendency of its desorption.
4. Conclusions
This study elucidated the effects of the mixing energy, i.e., mix-
ing intensity (G) and duration (td) in the struvite precipitation pro-
cess in order to enhance the removal of N and P from the CMP
wastewater. Both G and td were the physical variables in the pro-
cess. The obtained results provide information to improve the
practical application of struvite precipitation in the industry. Con-
sidering the agricultural use of struvite, the present study gave fea-
sible information of the mixing effect on struvite precipitation in
order to obtain pure struvite from the stream. The detailed ndings
had been drawn as following
The Gtd value, the multiplying value of mixing intensity (G) and
mixing duration (td), was a useful parameter to explain the mixing
effect in the struvite precipitation process. In the process, the re-
moval patterns of nitrogen and phosphorus was a logarithmic in-
crease with the Gtd value.
The mixing effect was to enhance the mass transfer of ammo-
nium ions in the solution, which induced the potential of struvite
crystallization and growth to increase. The resulting removal of
nitrogen and phosphorus was effectively enhanced in this process.
At the Gtd value over 105, the precipitates were close to pure
struvite. Insufcient mixing energy provided the formation of the
unexpected precipitate unlike to struvite.
High level of uoride in the CMP wastewater was not an oper-
ational problem in the application of the struvite precipitation pro-
cess in case high mixing energy was applied.
Acknowledgements
This research was supported both by the Brain Korea (BK) 21
Project which is administrated by the Korean Ministry of Education
and the Eco-Technopia 21 Project which is administrated by the
Ministry of Environment, Republic of Korea.
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