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Optimization of alum-coagulation/flocculation
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 Desalination 211 (2007) 113127

Optimization of alum-coagulation/flocculation for COD and

TSS removal from five municipal wastewater

Marco Guidaa, Marialuisa Matteia, Clauido Della Roccab, Giovanni Mellusoc,

Sreyya Merib*
a
Federico II Naples University, Department of Biological Sciences, Section of Fis. and Hygiene, I-80134 Naples, Italy
b
Department of Civil Engineering, University of Salerno, 84084 Fisciano (SA), Italy
Tel. +39 (089) 96-4016; Fax +39 (089) 96-4100; email: smeric@tin.it; msureyya@unisa.it
c
Federico II Naples University, Department of Structural and Functional Biology, I-80134, Naples, Italy

Received 17 November 2005; revised 16 December 2005; accepted 16 February 2006

Abstract
In this study, the coagulation process is evaluated in treatment of municipal wastewater on the basis of organic
material (e.g. chemical oxygen demand, COD) and suspended solids (TSS) removal efficiency. Alum-coagulation
was optimized on the samples (24 sampling campaigns) taken from 4 wastewater treatment plants and a pilot plant
at the University laboratory (Naples, Italy) to meet the Italian water quality discharge limits. A series of jar test
experiments was run at 100 rpm for 1 min, 30 rpm for 20 min and 30 min for settling. 150 mg/l and 450 mg/l doses
of alum were applied at pH ranging from 4 to 10 and room temperature. An anionic polyelectrolyte was used for
flocculation. Raw and coagulated wastewater samples were analyzed for their COD, TSS and aluminium (RA)
concentrations. The jar test experiments provided evidence that coagulation process could not provide sufficient
COD removal efficiency in the Cuma and the University pilot plant wastewater even at an alum dose of 450 mg/l
whereas the treatment with coagulation process using 150 mg/l alum in Nola and S. Giovanni plants was sufficient
to meet COD (<160 mg/l) and TSS (80 mg/l) limits. The highest COD removal (80%) was obtained at the range of
6.08.0 pH values in the Nola plant, whereas COD removal was lesser in the Marcianese wastewater although its
initial COD value was in the same order with the Nola plant. COD removal of the university plant improved from
55 to 7585% in parallel to TSS removal by pH increase (up to 8.0). The statistical analyses showed different
correlation values/behaviour between COD and TSS removals in each plant due to wastewater origin, pH and
applied alum dose. RA was found significantly related to pH of coagulation process. RA concentration increased at
pH value <5.0. These obtained results should contribute to, in particular, further RA studies dealing with the RA

*Corresponding author.

Presented at the 9th Environmental Science and Technology Symposium, September 13, 2005, Rhodes, Greece.
Organized by the Global NEST organization and prepared with the editorial help of the University of Aegean,
Mytilene, Greece and the University of Salerno, Fisciano (SA), Italy.

0011-9164/07/$ See front matter 2007 Elsevier B.V. All rights reserved
114 M. Mattei et al. / Desalination 211 (2007) 113127
risk in the coagulated effluents. Moreover, this study evidenced once again that coagulation process can assure the
limits of COD, TSS and RA for municipal wastewater treatment plants if the process is well optimized and operated.
Keywords: Municipal wastewater; Coagulationflocculation process; Aluminium sulphate; Residual aluminium;
Wastewater treatment; COD and TSS removal
1. Introduction
The coagulation process proves a high removal
efficiency of different parameters, mainly chemi-
cal oxygen demand (COD) and suspended solids
(SS). The process is based on the use of Al(III) or
Fe(III) salts alone or in combination with calcium
salts and the use of polymers as flocculants. Co-
agulant doses vary in a wide range like 150
600 mg/l and 2502000 mg/l of Al2(SO4)318 H2O
(alum) used for treatment of domestic [13] and
industrial wastewaters [4,5], respectively while
2060 mg/l of alum was applied as the proper in-
terval for drinking water production [6,7]. Alum
results the following equation in water decreas-
ing the alkalinity:
Al2 (SO4 )3 + 6HCO3 2Al(OH)3 + 6CO 2 (1)
Aluminium in coagulated drinking water and
in wastewater effluent has been regarded as a sub-
ject of human and environmental health concern
[8]. Maximum contamination level (MCL) of
Al(III) was established between 0.2 and 1 mg/l
for drinking water [9]. Aluminium concentration
in natural waters is usually lower than 100 g/l,
however, its concentration and speciation between
toxic (free Al3+ and Al-OH) and complex (Al-F
and Al-Org complexes) forms varied much due
to seasonal changes and pH of water body [10].
Alum speciation in water has been well docu-
mented [11]; however, the fate of alum treated
wastewater has been evaluated limited. Driscoll
et al. [12] reported that the use of alum increased
the total Al(III) concentration from 0.370.33
mol/l in raw water to 1.80.33 mol/l in filtered
water. The evidence on Al(III)- and Fe(III)-asso-
ciated toxicity, either as complex mixtures or as
Al(III) or Fe(III) salts on sea urchins embryos was
observed at 105 M concentrations [13,14]. A re-
cent study also evaluated the toxicity of alum and
its mixture with an anionic polymer on Daphnia
magna and Selenastrum capricornutum [15]. The
Italian Official Journal set 1 and 2 mg/l of Al(III)
as the limits in the case of sewer and receiving
water discharge endpoints, respectively [16].
Alternative aluminium based coagulants, such
as polyaluminium chloride [3], polyaluminium
silica-chloride and polyaluminium ferric chloride
[1719] and polymer addition [20] were studied
to improve coagulation efficiency as well as ob-
taining of minimum residual aluminium (RA) in
the water. Furthermore, the coagulation process
was optimized for minimum residual aluminium
and turbidity by statistical methods [21] or sim-
plex method [22].
The present study was carried out on four
municipal wastewater (MW) and a pilot plant
(southern Italy) installed at a university labora-
tory to evaluate the efficacy of alum coagulation
for complying with the Italian discharge standards
[16]. The effect of wastewater origin, coagulation
pH, applied alum dose and influent COD and TSS
concentrations on coagulation efficiency and RA
concentration was elaborated statistically.
2. Materials and methods
2.1. Sampling
The samples were collected from the inflow
(after coarse screen) of the existing municipal
wastewater treatment plants of Cuma (C1C6),
Marcianese (M1...M3), Nola (N1...N3), San
Giovanni a Teduccio (SG1..SG6) and the univer-
sity pilot plant (U1..U6). The main characteris-
 M. Mattei et al. / Desalination 211 (2007) 113127 115

tics of the MWs are shown in Table 1. The samples
were kept cold in ice boxes and were delivered
into the laboratory in 1 h and were refrigerated at
4C for subsequent experiments.
2.2. Jar test
A series of jar tests was carried on the grab
samples taken from the influent of the MWs, they
were coagulated at 100 rpm for 1 min, 30 rpm for
20 min sequentially stirring and then were settled
for 30 min. 150 mg/l and 450 mg/l doses of
Al2(SO4)318H2O were used at pH ranging from
4.0 to 10.0 [1]. Prodefloc anionic polymer
(2 mg/l), which is currently used in San Giovanni
MW plant, was added [1].
2.3. Analysis
Raw and coagulated samples were analyzed
for their COD, TSS and RA contents according
to Standard Methods [23]. Samples were filtered
through 0.45 m GF/C Whatman filter papers.
Al(III) was measured by flame atomic absorption
spectrophotometry (Varian spectraAA 10 Plus,
USA).
2.4. Statistical analysis
The effect of in-put parameter on coagulation
results was tested by multiparametric ANOVA test
to evaluate the significance level, followed by test
of Tukey using Statistica Software [24]. In par-
ticular, the effect of wastewater origin, coagula-
tion pH, alum dose and influent COD and SST on
COD and SST removal were tested. Moreover,
the data related to wastewater origin, coagulation
pH, alum dose and influent aluminium were elabo-
rated to see their effect on released aluminium (the
difference between final and initial concentration).
Furthermore, Student t-test for dependent vari-
ables was conducted between COD and TSS re-
moval efficiency. Statistical figures were obtained
on the base of effective hypothesis method [25].
Significance level of statistical analyses was set
at = 0.05.
3. Results and discussion
3.1. Jar test results
As reported in Table 2, influent COD and TSS
concentrations were different from one plant to
another one, e.g. the mean values of COD varied
from 330 mg/l (S. Giovanni) to 560 mg/l (Cuma).
COD removal efficiency in Cuma plant was high
(77%) at pH 5.0 and it decreased to 40% at pH
10.0 when 150 mg/l alum was used. That decrease
was lesser (7260%) for 450 mg/l alum (Fig 1a).
TSS removal efficiency was almost stable (more
than 90%) at all values of pH (Fig. 1b). Increase
in TSS at higher pH was due to destabilization of
the flocks influenced the removal differing from
COD removal.

Table 1
Characteristics of the MWs

Sampling points Inflow rate (m3/d) Existing treatment plant Operational problems
Cuma (C) 200000 Activated sludge Foaming-bulking, effluent toxicity*
Nola (N) 60000 Activated sludge Foaming-bulking, effluent toxicity*
S. Giovanni (SG) 30000 Coagulation (200 mg/l FeSO4 + 60 mg/l Low efficiency, Effluent toxicity*
Ca(OH)2
Marcianese (M) 100000 Activated sludge Low efficiency
University (U) Pilot aerobic disk
*measured using 24 h new born Daphnia magna for 24 h acute toxicity end point (unpublished)
116 M. Mattei et al. / Desalination 211 (2007) 113127

Table 2 (63%) to 8.0 (77%) whereas it decreased to 68%

Influent characteristics of the municipal wastewater at pH 10 using 150 mg/l alum. A 10% COD re-
samples moval efficiency could be recorded when 450 mg/l
alum was used at pH 8.0 (Fig. 3a). However, COD
Sampling points Sample COD TSS
removal efficiency in the samples taken from the
(mg/l) (mg/l)
M plant was low which was attributed to the
Cuma (C) C1 560 1160 chemical composition of the wastewater, e.g. sur-
C2 1000 85
C3 330
face active materials of wastewater also because
C4 500 330 TSS was removed effectively (Figs. 4a and b).
C5 270 205 The highest COD removal was obtained at pH
C6 800 360 8.0 for the samples from U plant, similar to N and
Nola (N) N1 450 165 SG samples (Figs. 5a and b).
N2 360 265
As seen in Table 3, RA was measured to in-
N3 420 180
S.Giovanni (SG) SG1 460 100 crease due to coagulation process which was re-
SG2 165 125 ported in drinking water previously [12]. This in-
SG3 540 265 crease, somewhat decrease, varied due to coagu-
SG4 210 135 lation pH, alum dose and wastewater composi-
SG5 290 115 tion as well as influent aluminium concentration
SG6 330 70
[26].
Marcianese (M) M1 350
M2 450 90 This study evidenced once again that coagu-
M3 240 85 lation process can assure the limits of COD, TSS
University pilot plant U1 2100 455 and RA for municipal wastewater treatment plants
(U) providing high removal efficiency using relatively
U2 350 125 low level of aluminium sulphate [1,37] if the
U3 530 125
U4 340 140
process is well optimized and operated. Here, the
U5 290 85 process efficiency was greatly affected by pH and
U6 310 65 wastewater origin, however, using alternative co-
agulants as well as operational details (mixing
velocity) [4], or using different polymers [15,20]
are also to be further investigated in detail.
These obtained results should contribute to, in
COD removal efficiency showed a different particular, RA studies dealing with the aluminium
pattern in the Nola plant (Fig. 2a). COD was re- speciation in wastewater, in its complex mixture
moved by 45% at pH 4.0 while at pH 6.0 it was [11] in the effluents to avoid to increase its envi-
79% for 150 mg/l alum use. COD removal con- ronmental levels [19] and toxicity [8,1315].
tinued to increase at pH 8.0 (81%) but it decreased
drastically to 59% at pH 10. TSS removal effi-
3.2. Statistical evaluation
ciency was relatively lower compared to the Cuma
plant (Fig. 2b). Higher COD and TSS removal ef- As can be seen from Table 4 that all param-
ficiencies were obtained by increasing alum con- eters (wastewater origin, pH, alum dose, influent
centration to 450 mg/l, e.g. COD removal in- COD) were found significantly affecting the COD
creased from 81% to 87% at pH 8.0. removal while only wastewater origin did not af-
In the S. Giovanni plant COD removal effi- fect TSS removal by coagulation (Table 5). COD
ciency increased due to pH increase from 4.0 removal dependent on the wastewater character-
 M. Mattei et al. / Desalination 211 (2007) 113127 117

100

90 A
B
80
COD removal (%)

70

60

50

40

30

20
4 5 6 7 8 9 10
pH

100

90
TSS removal (%)

80

70

60
A
B
50
4 5 6 7 8 9 10
pH

Fig. 1. COD and TSS removal by jar test using 150 (A) and 450 mg/l (B) of alum in the Cuma (C) samples.

istics, in particular, the wastewater samples from
U and M presented very low COD removal (Fig.
6a) whereas TSS removal was higher (Fig. 6b).
This phenomenon can be attributed to the pres-
ence of high surfactant levels in the samples taken
from U and M points (data not shown).
pH significantly affected COD and TSS re-
moval (Figs. 7 a and b). The optimum pH was
recorded 8.0 resulting in the highest both COD
and TSS removal.
Fig. 8 illustrates the effect of alum dose on
both COD and TSS removal. Increasing alum dose
from 150 to 450 mg/l provided higher COD (Fig.
8a) and TSS (Fig. 8b) removal.
ANOVA analysis on effluent TSS and COD
of jar test showed an analogy to the results ob-
118 M. Mattei et al. / Desalination 211 (2007) 113127

100

90

80
COD removal (%)

70

60

50

40
A
30
B

20
4 5 6 7 8 9 10
pH

90

80
TSS removal (%)

70

60
A
B

50
4 5 6 7 8 9 10
pH

Fig. 2. COD and TSS removal by jar test using 150 (A) and 450 mg/l (B) of alum in the Nola (N) samples.

tained for COD and TSS removal (data not
shown). Furthermore, the removal of TSS and
COD was correlated according to Student t test
for dependent variables as shown in Table 6. COD
removal was dependent on different factors of that
TSS removal was affected.
Released aluminium was dependent on waste-
water origin, pH of coagulation process and ini-
tial aluminium concentration (Fig. 9). In particu-
lar low pH increased significantly the released alu-
minium, while no statistical difference was ob-
served at pH ranging from 5 to 10 (Fig. 9a). It
was remarkable that released aluminium for the
samples of M was significantly high (Fig. 9b),
probable due to low COD removal efficiency.
4. Conclusions
The jar test experiments were performed on
five municipal wastewater (Cuma, C; Nola, N;
 M. Mattei et al. / Desalination 211 (2007) 113127 119

100

90

80
COD removal (%)

70

60

50

40
A
30 B

20
4 5 6 7 8 9 10
pH

100

90
TSS removal (%)

80

70

60 A
B

50
4 5 6 7 8 9 10
pH

Fig. 3. COD and TSS removal by jar test using 150 (A) and 450 mg/l (B) of alum in the San Giovanni (SG) samples.

San Giovanni, SG; Marcianese, M: University
pilot plant, U) collected in Naples district (Italy).
The coagulation experiments indicated that co-
agulation process affectively removed COD
(>65%) and TSS (>75%) on the average values
of COD using 150 mg/l of aluminium sulphate at
a pH range of 58. However, the case for the
wastewater of C was different, because its influ-
ent varied exceptionally displaying a medium
character municipal wastewater. COD removal ef-
ficiency was not sufficient to meet discharge lim-
its even at alum dose of 450 mg/l. COD removal
decreased vs. pH varying from 5 to 10. Differing
from C, the optimum pH for COD (7585%) re-
moval was 8.0 for N, SG and U wastewater. How-
ever, COD removal efficiency in the samples taken
from M was low which was attributed to the
chemical composition of the wastewater, e.g. sur-
120 M. Mattei et al. / Desalination 211 (2007) 113127

100

90 A
B
80
COD removal (%)

70

60

50

40

30

20
4 5 6 7 8 9 10
pH

100

90
TSS removal (%)

80

70

60 A
B

50
4 5 6 7 8 9 10
pH

Fig. 4. COD and TSS removal by jar test using 150 (A) and 450 mg/l (B) of alum in the Marcianese (M) samples.

face active materials of wastewater while TSS was
removed effectively.
ANOVA statistical evaluation test showed that
all factors examined including water origin, pH,
alum dose and influent COD and TSS affected
COD removal while only pH, alum dose and in-
fluent TSS factors were found effective on TSS
removal. Student t-test confirmed these results.
Therefore, both COD and TSS parameters must
be considered on the design and operation phase
of a coagulation process instead optimising only
turbidity removal. Aluminium release due to co-
agulation process was relevant only at low pH
value; in particular, it was significant when a low
COD removal efficiency was recorded.
 M. Mattei et al. / Desalination 211 (2007) 113127 121

100

90

80
COD removal (%)

70

60

50

40
A

30 B

20
4 5 6 7 8 9 10
pH

100
A
B
90
TSS removal (%)

80

70

60

50
4 5 6 7 8 9 10
pH

Fig. 5. COD and TSS removal by jar test using 150 (A) and 450 mg/l (B) of alum in the university pilot plant (U) samples.

Acknowledgements References
The authors would like to thank treatment plant [1] S. Meri, M. Guida, M. Mattei, A. Anselmo and G.
authorities and Dr. Giusy Sirico for their kind Melluso, Evaluation of coagulation flocculation pro-
collaboration. cess for S. Giovanni a Teduccio municipal waste-
water treatment plant. Fresenius Envir. Bull., 11
(2002) 906909.
122 M. Mattei et al. / Desalination 211 (2007) 113127

Table 3
Residual aluminium concentrations in the samples

A B
Sample Raw pH = 4.0 pH = 6.0 pH = 8.0 pH = 10.0 pH = 4.0 pH = 6.0 pH = 8.0 pH = 10.0
wastewater
C2 3.04 3.72 1 3.08 2.11 2 3.19 3
C2* 3.04 3.43 1 3.70 3.36 2 3.09 3
C5 1.90 4.45 1 1.30 3.76 2 1.88 3 1.58 1 1.3 1.56 2 1.92 3
C5* 1.90 4.73 1 3.20 2.51 2 4.76 3 2.11 1 1.69 2.40 2 1.65 3
C6 0.42 0.88 1 0.58 0.52 2 2.55 1 0.68 0.54 2 0.45 3
M2 2.23 6.95 1.60 1.12 3.95 15.15 1.71 2.92 1.55
M3 0.26 9.32 6.05 8.46 1.03 17.02 0.25 3.60 13.60
N1 3.78 10.19 3.39 4.42 8.34 13.91 0.15 3.85 5.88
N2 0.61 2.06 1.80 2.05 3.08 5.75 1.91 2.75 3.27
N3 2.45 3.78 2.85 2.87 5.02 4.25 3.28 3.43 5.67
U2 0.75 7.65 2.98 1.65 2.58 10.10 8.01 4.30 8.87
U3 0.43 3.45 0.94 0.33 2.10 2.15 0.27 0.45 0.67
U4 1.45 5.87 2.39 4.68 5.84 3.55 1.23 3.12 4.34
U5 0.66 1.12 0.45 0.24 0.69 1.78 0.23 0.45 0.92
U6 0.58 1.45 2 0.14 1.34 4 1.29 2 0.13 0.56 4
1
at pH = 5.0; 2 at pH = 7.0; 3 at pH = 8.0; 4 at pH = 9.0

Table 4
ANOVA test results for COD removal

Parameter Degree of freedom Variance F value of Fisher test Probability* (p)

Wastewater origin 3 4562.823 34.55277 0.000000
COD in 18 995.137 7.53585 0.000000
pH 3 1730.466 13.10426 0.000000
Alum dose 1 2693.815 20.39938 0.000015
Error 118 132.054

*p indicates the significance of the correlation to F value

Table 5
ANOVA test results for TSS removal

Parameter Degree of freedom Variance F value of Fisher test Probability* (p)

Wastewater origin 1 264.0625 2.278815 0.133993
TSS in 16 544.0212 4.694811 0.000000
pH 3 995.2192 8.588574 0.000035
Alum dose 1 694.1066 5.990022 0.015954
Error 111 115.8771
 M. Mattei et al. / Desalination 211 (2007) 113127 123

Table 6
Student t test results

Mean St. dev. N Diff St. dev. T df P

COD removal 66.23308 20.4713
TSS removal 79.52632 14.6652 133 13.2932 21.184 7.23677 132 0.000

100

80
COD rem

60

40

20

0
M U C N S
plant

100

80
TSS rem

60

40

20

0
M U C N S
plant

Fig. 6. COD (a) and TSS (b) removal vs. wastewater type (vertical bar denotes 0.95 confidence interval, pCOD = 0.00000,
pTSS = 0.13399).
124 M. Mattei et al. / Desalination 211 (2007) 113127

100

90

80
CODrem

70

60

50

40
pH 4 pH 6 pH 8 pH 10
pH

100

90

80
TSS rem

70

60

50

40
pH 4 pH 6 pH 8 pH 10
pH

Fig. 7. COD (a) and TSS (b) removal vs. pH (vertical bar denotes 0.95 confidence interval, pCOD = 0.00000, pTSS =
0.00004).

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COD rem

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70

65

60

55
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Aldose

100

95

90

85
TSS rem

80

75

70

65

60

55
150 450
Aldose

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6
5
Al release (mg/l)

4
3
2
1
0
-1
-2
-3
-4
4 5 6 7 8 9 10
pH

5
Al release (mg/l)

-1

-2
M U C N
plant

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