DESALINATION

ELSEVIER Desalination 130 (2000) 255-264 www.elsevier.com/locate/desal

Removal of iron and manganese from groundwater by oxidation

and microfiltration
• ° a*
Donald Ellis a, Christian Bouchard , Gaetan Lantagne b
aCivil Engineering Department, LarvalUniversity, Sainte-Foy (Quebec), Canada G1K 7P4
Tel. +1 (418) 656-2868; Fax +1 (418) 656-2928; email: cbouchar@,gci.ulaval.ca
bLTEE, Hydro-Quebec, 600, avenue de la Montagne, Shawinigan (Quebec), Canada G9N 7N5

Received 18 April 2000; accepted2 August 2000

Abstract
Iron and manganese can be removed from groundwater by a process which combines oxidation and microfiltration
(MF), especially when the concentrations of these metals are high and variable. The present experimental work focused
on the MF of iron and manganese oxide suspensions in order to study the effects of the operating variables (tangential
flow rate, pressure, metal feed concentrations) on permeate quality and permeation flux decline, i.e., membrane fouling.
Artificial and natural groundwaters in which iron and manganese were previously oxidized were used to perform
laboratory-scale MF experiments. The results show that the oxide particles, with sizes ranging from 1.5 to 5~m, were
efficiently microfiltered even at high concentrations. Within the experimental limits, the effect of operating pressure
appeared to be much more significant than the those of tangential flow rate and feed concentration. A relatively high and
constant permeation rate of 0.5 m/h was obtained at a pressure below 10 kPa, whereas rapid permeation flux declines
were observed at higher pressure. Both artificial and natural groundwaters always exhibited very similar behavior.

Keywords: Microfiltration; Oxidation; Iron; Manganese; Groundwater; Membrane fouling

1. Introduction domestic needs. Generally speaking, groundwater

Groundwater is an important source of
drinking water. In Canada, for example, 26% of
the population, mostly living in small rural
communities, depend on groundwater for their
*Corresponding author.
is characterized by a low temperature (7-10°C),
a low redox potential (absence of oxygen), a high
carbon dioxide concentration, a high mineral
content (high alkalinity and hardness) and a very
low suspended solid content. Iron and manga-
nese, which are usually present in groundwater as
divalent ions (Fe 2+ and Mn2+), are considered as

0011-9164/00/$- See front matter © 2000 Elsevier Science B.V. All rights reserved
PII: S0011-9164(00)00090-4
256 D. Ellis et al. / Desalination 130 (2000,) 255-264
contaminants mainly because of their organo-
leptic properties. In Canada the maximum
recommended levels of Fe and Mn in drinking
water are 0.3 mg/L and 0.05 mg/L, respectively
[I], whereas the international standards are
0.3 mg/L for Fe and 0.1 mg/L for Mn [2].
Conventional treatment for iron and manga-
nese removal from groundwater consists of
oxidation and depth filtration. Oxygen or stronger
oxidants, such as chlorine and potassium
permanganate (KMnO4), are generally used for
Fe 2÷ and Mn 2+ oxidation. The solid products of
oxidation (FeOOH.H20 and MnO2) are then
filtered through a granular bed, commonly green
sand [3]. An aeration step may precede oxidation
for oxygenation and removal of carbon dioxide
(pH increase), sulfurs and other volatile sub-
stances. The conventional process works fairly
well for a total concentration of Fe and Mn below
5 mg/L and in the absence of dissolved organic
matter. For higher concentrations, excessive
amounts of solids tend to shorten filtration cycles
and render the overall process unprofitable.
Moreover, the filterability of manganese oxides
is poor and process control may become difficult
with raw water variations.
Alternative processes have been proposed in
order to facilitate the operation and to allow the
removal of high amounts of iron and manganese
in the presence, or absence, of dissolved organic
matter. These alternatives are enhanced conven-
tional treatment [4], biological treatment [5] and
membrane treatment. Two approaches are
possible for the latter option: direct membrane
separation or combination of oxidation and
membrane separation. Lapointe and Barrette [6]
reported results for reverse osmosis of a
groundwater whereas Middleton and Hendershaw
[7] presented full-scale results for nanofiltration
of a colored groundwater. In both cases, a pH
adjustment was necessary to maintain iron in the
dissolved state to avoid membrane fouling.
Mourato and Smith [8] and later C6t6 et al. [9]
presented a case study on the removal of iron and
manganese from groundwater by oxidation and
microfiltration (MF). This treatment is similar to
the conventional one except that depth filtration
is replaced by MF. The expected advantage of
this treatment is to have a compact separation
unit which produces high quality water from a
wide range of raw water quality.
In the present study the MF of iron and
manganese oxide suspensions is examined. More
specifically, the effects of the operating variables
(tangential flow rate, pressure, feed concen-
tration) on permeate quality and permeation flux
decline, i.e., membrane fouling, are studied using
artificial and natural groundwaters.
2. Materials and methods
2.1. Natural and artificial groundwaters
A natural groundwater containing high
amounts of iron and manganese was chosen as
the model water for the study (see Table 1). This
water has been supplying the municipality of
Sainte-Marie (Quebec, Canada) for years. It
contains 7-15 mg/L of Fe and 1.8-2 mg/L of Mn.
No iron or manganese solids were found in this
raw groundwater because there was no signifi-
cant difference between the metal concentrations
of filtered (0.45 lam) and unfiltered raw waters. A
container, which prevents contact between air
and water (no air gap), was used to transport the
groundwater samples from field to laboratory.
The analytical method are referenced in
Table 1. All the iron and manganese analyses
were performed using an atomic absorption
spectrophotometer (Perkin Elmer, model 3110).
All the samples were quickly acidified (pH<2)
with nitric acid prior to atomic absorption
spectrophotometry. Prelim inary tests showed that
in our case high temperature digestion did not
bring any significant difference in metal concen-
tration measurement, and so it was decided to
avoid it. The organic carbon content was
measured with a TOC-5000 apparatus from
 D. Ellis et al. /Desalination 130 (2000) 255-264 257

Table 1
Groundwater qualities

Parameter Natural groundwater Artificialgroundwater Analytical method"

pH 6.9-7.2 7.0 4500-H÷B

.Alkalinity, mg (CaCOJL) 190-230 210 2340B
Hardness, mg (CaCOJL) 190-230 180 From Caz+and Mg2+
Temperature, °C 7.0-7.2 7.0 2550B
Turbidity, NTU <0.2 <0.2 2130 B D
Dissolved 02, mg/L <0.2 <0.2 4500-0 G
Fe, mg/L 7-15 5 or 10 31lIB
Mn, mg/L 1.8-2.0 1.0 or 2.0 3111B
Ca, mg/L 69-75 72 3111B
Organic carbon, mg (C/L) <2 0 5310B
Na, mg/L 38-42 60 3111B
SO~z, mg/L 23-27 10-21 4110B
Sulfurs, mg (S/L) <0.1 0 2340B
Silicates, mg (SiO2/L) 23-25 0 4500-Si D

"AmericanPublic Health Association et al. [17].

Shimadzu. Prior to TOC measurement, the
samples were acidified and bubbled with air,
which does not contain any CO2, in order to
remove the inorganic carbon. But as the ground-
water contains a large amount of inorganic
carbon (see Table 1), it was difficult to measure
accurately the organic carbon content of the
water with this method. Other analysis reveals
that the UV254 nm absorbance of the ground-
water is close to 0.03 and that this groundwater is
totally colorless. This indicates that this
groundwater does not contains any significant
amount o f humic substances which can form
complexes with iron and manganese.
In order to simulate the behavior of the natural
water and to run experiments with a lesser
amount of iron and manganese, an artificial
groundwater was prepared (see Table 1) as per
the work ofKnocke et al. [4]. The preparation of
this artificial water is described in detail
elsewhere [10]. Deionized water and the
following salts were used: iron sulfate
(FeSO4o7H20), manganese sulfate (MnSO4 °
H20), sodium bicarbonate (NaHCO3), calcium
chloride (CaCI2) and sodium sulfate (Na~SO4).
Also a gas mixture of carbon dioxide (1.75%
CO2) and nitrogen (98.25% N2) was bubbled
through the artificial water prior to iron and
manganese additions. This gas composition
allowed reaching the conditions prevailing in the
natural aquifer. As shown in Table 1, the
artificial water properties were very similar to
those of the natural water. All the following
experiments were conducted both with the
artificial and natural groundwaters.
2.2. Oxidation procedure
A two-step oxidation procedure was chosen.
The first step was the oxidation o f ferrous iron
with oxygen. The water samples were oxyge-
nated by air bubbling and the pH was then
adjusted to 8.14- 0.1 with NaOH in order to fasten
the oxidation of iron for which 15 rain were
allowed to ensure complete iron oxidation. The
second step was the oxidation of manganous ion
258 D. Ellis et al. / Desalination 130 (2000) 255-264
with K M n O 4 for which 15 min were also allowed
to ensure complete manganese oxidation. This
procedure was chosen because the oxidation of
the manganous ion with oxygen is far too slow
and because, from a practical point of view, prior
treatment with oxygen reduces the consumption
of KMnO4,which is a fairly expensive oxidant.
All the MF experiments were conducted with
water containing totally oxidized iron and
manganese.
The particles formed after oxidation were
characterized with a particle size analyzer which
measures laser beam diffraction by particles
ranging from 0.05 to 500~tm (Mastersizer
Microplus ®, Malvern Instrument Ltd.). The
particle size measurements were conducted under
a strong agitation (2000 rpm) to prevent floccu-
lation and to simulate the conditions prevailing in
a MF system where the feed water is recirculated.
2.3. Microfiltration
The MF set-up, shown in Fig. 1, is a usual
membrane laboratory set-up. The feed iron and
manganese suspension is stored in a tank and
maintained at 8°C with a cooling bath to simulate
the actual temperature of the natural ground-
water. The suspension is circulated through a MF
cell by a positive displacement pump with
controlled flow rate. The suspension is circulated
tangentially to the membrane surface to minimize
Paw waterumpling
Pump PermlllllI Op
Pemlete urn~l~
Fig. ]. Microfiltration set-up.
the membrane fouling. The pressure inside the
MF cell is controlled by a needle valve located
downstream to the cell. Inlet and outlet cell
pressures are measured in order to determine the
average pressure difference across the membrane
(APM). The tangential flow channel is a rec-
tangular slit (5.3 cm × 0.2 cm) and the membrane
surface in contact with water is 78 cmL In order
to maintain the feed concentration as constant as
possible, the permeate and the concentrate are
circulated back to the feed tank.
A polymeric polyethersulfone MF membrane
was used (SUPOR200 ® from Gelman Sciences).
This membrane was chosen for its resistance to
strong acidic conditions (nitric acid 10% w/w), to
alkaline conditions (sodium hydroxide 10% w/w)
and oxidizing conditions (sodium hypochlorite
5.25% w/w). Its given absolute porosity is 0.2 pm
and its given pure water permeability is 15.7 m 3
m-2h-~bar-I at 20°C. Based on 153 measure-
ments, the average pure water membrane
permeability appeared to be 15.9 m 3m -~h-1bar-
with a standard deviation of 1.9m3m-2h -I bar-L
A new membrane coupon was used for each
experiment.
The tangential flow was always laminar since
the tangential Reynolds number (Re) ranged from
100 to 400. The pressure difference across the
membrane ranged from extremely low pressure
(6kPa) to low pressure (100kPa), and the
temperature was maintained close to 8°C. As
previously mentioned, two iron feed concen-
trations (5 and 10 mg/L) were tested in the case
of the artificial groundwater, in combination with
two manganese concentrations (1 and 2 mg/L).
Each MF experiment started with a membrane
rinsing and pure water permeability measure-
ments performed with deionized water. During a
pure water permeability test, the pressure
difference across the membrane was increased
from 6 to 100 kPa and then back-decreased from
100 to 6 kPa. After this initial permeability test,
...J the iron and manganese suspension, which was
obtained after oxidation of the natural or artificial
 D. Ellis et al. / Desalination 130 (2000) 255-264 259

groundwater (the procedure is described above),
was microfiltered for 1 to 2.5 h depending on the
membrane fouling rate. At the end of each run,
the membrane was rinsed and cleaned with a
10% nitric acid solution for 9 min. Finally, the
membrane was rinsed and its pure water
permeability was measured again. The permeate
iron and manganese concentrations and the
permeation flow rate were measured during the
MF of the suspension.
3. Results and discussion
3.1. Oxidation
As expected from the work of Stumm and Lee
[11], and as indicated by the absence of any
significant amount of dissolved iron (-<0.45 ~tm),
the oxidation of iron with oxygen, at pH 8 and at
8°C, was achieved within a few minutes both
with natural and artificial groundwater.
Surprisingly, 20% of the dissolved manganese
(_<0.45 ~tm) disappeared in the same conditions,
both with natural and artificial groundwater.
Experiments with artificial solutions containing
only manganese reveal that such phenomena do
not occur in the absence of iron, as shown by
Stumm and Morgan [12]. The adsorption of
manganous ions on iron oxides or the copreci-
pitation of iron and manganese may explain this
phenomenon. As indicated by the absence of any
significant amount of dissolved manganese, the
KMnO4 oxidation of manganese was very
quickly completed after K M n O 4 was added to the
water, in agreement with Knocke et al. [4] who
studied manganese oxidation kinetics with
different oxidants. The pH after iron and manga-
nese oxidation completions was approximately
8.5.
The evolution of the particle size distribution
after oxidation is shown in Fig. 2 for both natural
and artificial water samples. There are many
fewer manganese particles than iron particles in
the oxidized natural water sample since its iron
concentration is much greater than its manganese
concentration. The sizes of manganese oxides are
then much easier to appreciate in the curve
corresponding to the artificial manganese
solution oxidized with K M n O 4. For the purpose
of comparison, the results of an artificial iron
solution oxidation are also shown in Fig. 2. From
this figure, and from all other measurements, it

100 ' 1 +;
(

ii .
z
I

10 .2 10 "I 1 10 10 2 10 3
Particle dlameter (pro)

Fig. 2. Particle size distributions of oxidized natural and artificial groundwater samples.
260 D. Ellis et al. / DesaBnation 130 (2000) 255-264
appears that, from oxide particle sizes, there is no
significant difference between the natural
groundwater and the artificial groundwater.
Actually, all the particle size analyses reveal that
both iron and manganese oxide particle sizes
range from 1.5 (see the zoom in Fig. 2) to a
maximum of 50 ~tm both for natural and artificial
groundwater. This means that MF with
membranes with an absolute porosity lower than
1 ~tm should be an appropriate separation process
for removal of iron and manganese oxide
particles.
3.2. MF: permeate quality
In all the experiments conducted with both
artificial and natural groundwater, the iron
concentration of the MF permeate stayed below
0.1 mg/L, which is the detection limit. The vast
majority of the manganese permeate concen-
trations stayed below 0.03 mg/L, which is the
detection limit. A number of permeates were
slightly above 0.03 mg/L, but these concentration
values can probably be explained as sampling
errors since they were randomly dispersed
throughout the analyses. These results are
coherent with those of C6t6 et al. [9] who
reported total retention of iron and manganese
oxides in a full scale plant with a 0.1 ~tm MF
membrane. This confirms that MF is a very
efficient separation process for iron and
manganese oxide particles, even for groundwater
with high level of these metals.
3.3. MF: effects o f operating variables on
membrane fouling rate with natural groundwater
During MF of the iron and manganese oxide
particles, a permeation flux decline was
observed, the extent of which was strongly
dependent on the operating conditions. A MF
blank test with deionized water was run to
establish which part of this permeate flux decline
should be attributed to membrane compaction.
2O
|i,2
8
0 30 60 90 120 150 180
Time (mln)
Fig. 3. Microfiltrationblanktest (deionizedwater; APM=
95 kPa; Re = 260; pH = 6; T=21°C).
No significant flux decline was observed during
this blank test (see Fig. 3) which means that the
lost of permeability during the MF of iron and
manganese oxide particles is truly coming from
membrane fouling. Since the permeate quality
analysis reveals that neither iron nor manganese
passes through the membrane, it is also
concluded that membrane fouling is due to oxide
particle deposit at the membrane surface.
The effect of tangential flow velocity on
permeation flux decline is shown in Fig. 4 for a
natural groundwater sample. From these results
it appears that an increase in tangential flow does
not lead to a significant increase in the
permeation flux even at higher pressure. It should
be noted that the Reynolds number range is quite
low. A much higher tangential flow rate will
increase energy consumption but may also lead
to a decrease in the membrane fouling rate since
a high tangential flow rate promotes the back-
transport of particles from membrane surface to
bulk flow. For example, Bourdon et al. [13]
showed that, for the MF of karstic groundwater,
a two-fold change in tangential flow Reynolds
number (from 8,000 to 16,000) approximately
doubled the permeation flux.
The effect of pressure can also be seen in
Fig. 4. It is clearly shown that at higher
transmembrane pressure, the permeation flux
decreases much more rapidly than at lower
pressure. Another experiment was performed at
 D. Ellis et al. / Desalination 130 (2000) 255-264 261

5 (a)
i i i I
4
z NetundJ I I I
• P s 10,7 kPIK Re.,d141

i~3 i
•
B
•
o
o
P-. 12.1 kPs; R e - 95
PmSlS.I kPs; R e . 6 4 6
p s 102,?ldPll:/:b~ 111
I j°
| • Pa 10.TkPa; RRm441
[ ] P.95.1kPll; RO=646
O p . 0.4 kPII; Re m2~S
[]
| m

1 |* m
mI

Ill
I i
1 ""
e I
•e
0 15 30 4S 60 7S g0 106 120 135 150
r o 8 A o o o

~ 30 e0 90 120 1S0 ~80 210 240

Time (rain) T~* (m~)

Fig. 4. Effect of tangential flow velocity and pressure on (b)

membrane fouling rate (natural water samples: 9 < Fe <

11 mg/L, 1.6 < Mn < 1.8 mg/L, pH 8.5-8.7, T = 8°C).

'"
very low pressure (APM = 8.4 kPa) and at medium
tangential flow rate (Re = 270). In this case the
membrane was cleaned after 2 h o f filtration, and
i
then the filtration continued for another 2 h. The
results of this experiment are shown in Fig. 5a
,,
o o
.,.,,
~ ~ go 120 ~r~ ~8o zlo
I
2,o
rime (m~)
and 5b. Under these conditions, the permeation
flux, or filtration rate, stays close to 0.5 m/h over Fig. 5. Effect of pressure on membrane fouling rate
(natural water samples: 9 < Fe < 11 mg/L, 1.6 < Mn <
two consecutive periods of 2 h. It shows that, at
1.8 mg/L, pH 8.5-8.7, T = 8°C.)
least for 2 h, MF can be performed at very low
pressure without any significant permeation flux
decline. Also, Fig. 5a shows that a slight increase induced transport of particles from the membrane
in the pressure difference across the membrane surface back to the bulk flow is stronger than the
(8.4-10.7 kPa) makes a significant difference advective flux of particles toward the membrane
since at 10.7 kPa the permeation flux decreases [16]. According to Altmann and Ripperger [18],
with time, which is not the case at 8.4 kPa. This this may indicate that, for a permeation velocity
result is in agreement with those of Field et al. of 0.5 m/h, the iron and manganese particle sizes
[14] and Howell [15] who worked on the MF are higher than the critical size below which
separation of yeast and who proposed the concept particles should deposit onto the membrane
o f a critical permeation flux under which the surface.
permeation flux should stay almost constant. It is also very interesting to note that the MF
Field et al. [14] used a membrane with pure filtration rate, which is obtained at very low
water permeability of 0.78 m 3m -2 h-] bar-~ which pressure, ranges between those of conventional
yielded a constant permeation flux of 0.025 m/h rapid and slow sand filtration (see Fig. 5a) where
at a pressure of 9 kPa, a Reynolds number of 50 similar or higher pressures are used and for
and for a 5% dry weight yeast suspension. The which the filter medium thickness is much higher
absence o f permeation flux decline at very low than for MF. This indicates that a MF system
pressure indicates a lesser deposit of particles on operated at very low pressure could be much
the membrane surface. This may indicate that, more compact than a conventional slow sand
below a specific permeation flux, the shear- filter.
262 D. Ellis et al. / Desalination 130 (2000) 255-264

1.0 iO | eNatural: P=8.4kPa; Re = 266; Fe= 10.0 mg/L; Mn = 1.68 mg/I.

0'51I I I T
O Artlficiel; P = 8.7 kPa; Re = 284;
T Y
Fe = 8.3 rag/1.; Mn = 1.73 mg/L
g° 1.5,
I

!
I

! a
I ,, I

i
I

i
I

~. 1.0 ~ ' " ' • N,quml; P = 10.710¢ Re=441; F e - 11,0mprl.; Mn= 1.80 mg/l.
i :-. II ii Ii i •
& ArUflckll; P-11.1 kPa; Re=443; Fe= 8.4 mg/L; Mn= 1.76 mg/t.
0
4.0 D Natural; P= 95.1 kPa; Re= 646; Fe = 8.7 mg/t.; Mn= 1.71 mg/L
~lm_ /1 Artificial; P = 95.1 kPe; Re = 644; Ice= 8.3 mg/L; Mn,, 1.71 mg/L

0
0 30 60 90 120 150 180 210 240
Time (rain)

Fig. 6. Effect o f tangential flow velocity and pressure on membrane fouling rate: comparison o f artificial and natural
groundwater behaviors (pH $.5-8.7, T = 8°C).

[ e P = 8 . 7 lope; Re=28~ Fe= 8.3 mg/l.; Mn.

l o,0Q 2 - o 1.73
2 mg/L
o ¢~

0.5 I T T - T "- 1" "- I

0 P = 8.5 kPa; Re ,, 288; Fe ,, 4.8 rag/L; Mn = 0.90 mg/L /
g° 1.5
I I I I I

7. " P=11~1kPr' R~'443; ~'8"4m~L; Mn= I'78mg/L

1.0 i m ~ " I J| • • • J

i 0.5
0
o. 4.0
• P = 11.2 kPa; Re = 443; Fe = 4.6 rnl~t.; Mn ,, 0.91 mg/L

2.0

0
0 30 60 90 120 150 180 210 240
Time (rain)

Fig. 7. Effect o f iron and manganese concentrations on membrane fouling rate for artificial groundwater (pH 8.5-8.7,
T = 8°C).

The effect of pressure on fouling rate is shown pressure, indicating that it may be more
in Fig. 5b in terms of membrane permeability profitable to operate at low pressure.
variation during MF. The permeability corre-
sponds to the permeation flux divided by the
3.3. MF: comparison of natural and artificial
pressure difference across the membrane. This
behaviors
shows how much permeate can be produced per
unit of membrane surface and pressure, and so it Similar MF experiments were repeated with
is an indication of energy efficiency of the both natural and artificial groundwaters. A
process. Results presented in Fig. 5b show that comparison of such experiments is shown in
the energy efficiency is higher at very low Fig. 6 where three different operating condition
 D. Ellis et al. / Desalination 130 (2000) 255-264
sets were used. This figure shows clearly that
natural and artificial groundwaters have similar
behaviors. Therefore, it was concluded that
artificial groundwater simulates natural ground-
water behavior satisfactorily. Further experi-
ments were conducted with artificial groundwater
samples which contained less iron and
manganese than natural water in order to study
the effect of iron and manganese concentrations
on permeation flux. Results shown in Fig. 7
indicate that a two-fold reduction in concentra-
tion leads to a slightly slower decrease in
permeation flux. When the particle concentration
is reduced, fewer particles are brought close to
the membrane surface and so fewer particles may
be deposited on the membrane surface, resulting
in less fouling. In our case this phenomenon does
not greatly affect the membrane fouling rate.
Further experiments should be conducted on a
broader concentration range with artificial
groundwaters in order to better understand the
effect of concentration on fouling kinetics.
4. Conclusions
For both natural and artificial groundwaters,
ferrous ion oxidation with oxygen and
manganous ion oxidation with potassium
permanganate result in the formation of particles
ranging in size from 1.5 to 50 p.m. These oxide
particles were filtered continuously at the
laboratory scale on a MF polymeric membrane
with an absolute porosity of 0.2 lam. The MF
permeate analysis do not reveal any significant
presence of metal, indicating that the particles are
very efficiently filtered even at relatively high
concentrations of iron and manganese (10 and
2mg/L, respectively). The permeation flux
decline is strongly affected by transmembrane
pressure. A significant permeation flux decline
occurs at higher operating pressures whereas a
constant permeation flux of 0.5 m/h is obtained at
lower pressures, i.e., below 10 kPa. Under low
263
pressures MF permeation flux is comparable to
slow sand filtration rate at a similar pressure
difference but with a much thinner filtering
medium. The effect of tangential flow and iron
and manganese concentrations is much weaker
than the pressure effect within the experimental
limits of the present study. Behaviors of the
artificial and natural groundwaters are always
very similar, indicating that artificial waters can
be used to conduct more basic studies.
Acknowledgment
This study was funded by the National
Sciences and Engineering Research Council of
Canada (NSERC) and by Hydro-Quebec's LTEE
(Laboratoire des Technologies l~lectrochimiques
et des ]~lectrotechnologies).
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[3] C. Lessard, D. Ellis, J. S&odes and C. Bouchard,
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