Desalination 210 (2007) 225235

Ammonia, iron and manganese removal from potable water using trickling filters
A.G. Tekerlekopoulou, D.V. Vayenas*
Department of Environmental and Natural Resources Management, University of Ioannina, Seferi 2, 30100 Agrinio, Greece Tel.+30 26410 74117; Fax++30 26410 39576; email : dvagenas@cc.uoi.gr

Received 10 November 2005; revised 9 March 2006; accepted 11 May 2006

Abstract Pilot scale trickling filters were constructed and tested in order to study biological removal of ammonia, iron and manganese from potable water. The effect of the size of the support material on nitrification performance was studied extensively. The mean size of the gravel and hence, the specific surface area was found to be critical for optimal nitrification operation. A steady-state model developed in previous work was used to predict filters performance. The model was very accurate only for the gravel size for which maximum nitrification rates were observed. The effect of the operational conditions on the physico-chemical and combined physico-chemical and biological iron oxidation was also studied. It was found that the contribution of biological oxidation is significant, increasing filters efficiency by about 6% and reducing the required filter depth by about 40%. Manganese biological removal was studied using gravel with small mean diameter, thus providing high specific surface area. Feed concentrations up to 4.0 mg/l were treated sufficiently. Finally, experiments were performed to investigate the simultaneous removal of ammonia, iron and manganese. Experimental results showed that the combined, as well as the simultaneous removal of the aforementioned pollutants, can be achieved by single-step filtration. Keywords: Ammonium removal; Iron removal; Manganese removal; Potable water; Trickling filter

*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

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1. Introduction Ammonia, in the form of ammonium, is an important pollutant of surface and subsurface potable water deposits. The increasing and very often uncontrollable use of fertilizers has led to increased amounts of ammonia in potable water, which often exceed the upper permitted limit of + 0.5 mg NH4 -N/l [1]. The impact of ammonia presence in water systems reflects on oxygen depletion, eutrophication of surface water and toxicity for fish [2]. When iron and manganese are present in a water supply at concentrations exceeding the permitted limits of 0.2 and 0.05 mg/l [1], respectively, they are objectionable for the following reasons: (a) their precipitation gives water a reddish and brown-black color, respectively, when exposed to air, (b) iron and manganese give water an unpleasant metallic taste, (c) home softeners become clogged by iron and manganese precipitates and thus their softening efficiency is reduced and (d) deposits of iron and manganese precipitate in the distribution system, reduce the pipe diameter and eventually clog the pipe. In addition, manganese has been found to affect the central nervous system [3]. Ammonia, iron and manganese are often encountered in water deposits at concentration levels above the upper permitted limits for human consumption. Redox is the key parameter which determines the sequence of the oxidation of these pollutants. Iron is oxidized at low redox values (< 200 mV), ammonia at higher values (200 400 mV) while manganese needs even higher redox values (> 400 mV) for neutral pH [4]. Thus the simultaneous removal of these pollutants, when present in a water deposit, requires several step processes or spatial redox variation. The above pollutants may be removed chemically or biologically from a water supply. Biological removal is preferable, since there is no need for the addition of extra chemicals and the volume of the regenerated sludge is appreciably

smaller and hence easier to handle. Trickling filters, in contrast with activated sludge processes, provide a support medium for biofilm growth. Bacteria remain in the filter for long periods of time, thus making high hydraulic and pollutant loadings possible. The filter medium is of great importance for the function of biofilters and several experiments have been carried out both to study and compare different filter media types [5,6]. The support materials used in trickling filters are either granulated or fixed media. Among the selection criteria for filter media in trickling filters are: void ratio, specific surface area, homogeneous water flow and economics. An adequate flow of air is of fundamental importance to the successful operation of a trickling filter. The principal factors responsible for air flow in an open top filter is the natural draft. The driving force for airflow is the temperature difference between the ambient air and the air inside the pores. Thus, the use of a trickling filter has the advantage of not requiring an external air supply or an aeration system. If, in addition, the mean diameter of the filter media is sufficiently small (up to 5 mm), then complete aeration and very good filtration may be affected at the same time [7]. The aim of the present work was to study ammonia, iron and manganese removal from potable water using pilot-scale trickling filters. The influence of the specific surface area on nitrification of potable water was examined, and the validity of the steady-state model of Vayenas and Lyberatos [8] for various gravel sizes used was tested. Experiments were also performed in order to investigate the contribution of biological and physicochemical oxidation on total iron oxidation, using a pilot-scale trickling filter under various operating conditions. Manganese oxidation is a much more difficult and slow process than iron and ammonia oxidation for natural pH values. Therefore, in order to increase significantly manganese oxidation rates or the specific surface area of the support material, a pilot scale trickling fil-

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ter with gravel of small diameter was used to study manganese removal from potable water. Finally, experiments were performed to investigate the single stage biological removal of ammonia-iron and ammonia-iron-manganese from potable water. 2. Materials and methods All pilot-scale trickling filters consisted of Plexiglas tubes, 160 cm high and 9 cm internal diameter. The water feeding was downwards (gravity flow) and the beds were always wet but not flooded. There were 10 sampling ports, along the filters depth, for ammonia-, nitrite-nitrogen, nitrate-nitrogen, iron and manganese concentration measurements in the bulk liquid. The feed solution resulted from mixing concentrated solutions of ammonia (in the form of NH4Cl), iron (in the form of FeSO47H2O) and manganese (in the form of MnSO4H2O), also containing phosphorous, with water from the water supply network in mixing chambers located at the top of the filters. The concentrated solutions were always kept in a refrigerator located close to the filters, in order to avoid undesirable bacterial growth in the feed medium. For the start-up of the filters inoculums were used from the wastewater treatment plant of the city of Agrinio. An underdrain system collected the treated water and any biological solids that would detach from the media. Aeration was taking place through natural draft and no external mechanical aeration source was used in the filters while pH, temperature and total ammonia, iron and manganese concentrations were measured on a daily basis according to the Standard Methods for the Examination of Water and Wastewater [9]. The pH and dissolved oxygen measurements were made using the Hanna pH211 pH meter, and the Hanna HI9143 dissolved oxygen meter, respectively. 2.1. Ammonia removal Three pilot-scale trickling filters with differ-

ent calcitic gravel sizes were used for the experiments. The mean diameters of the gravels were 2.4 (small-sized), 3.9 (medium-sized) and 5.5 mm (large-sized), with specific surface areas of 2124, 1372 and 1059 m2/m3 respectively. The depth of the support media was 143 cm in all cases and filters porosity was 0.36, 0.38, 0.4, respectively. The dissolved oxygen concentration in the bulk liquid at the effluent and the interior of the trickling filters was always between 7.0 and 8.0 mg/l, thus suggesting no oxygen limitation [10]. Also throughout the experiments the temperature and the pH were fairly constant at about 20C and 7.0 respectively. Experiments lasted for several months, ensuring that long term processes were taking place, that filters had enough time to adjust to the feed ammonia concentration and that biofilm thickness had reached a steady state. Before sampling, the filters were operated in a continuous mode and influent conditions were kept constant for at least six hours to ensure pseudosteady-state conditions with respect to ammonium-, nitrite- and nitrate-nitrogen concentrations. 2.2. Iron removal A pilot-scale trickling filter was used for iron removal (Fig. 1). The support material was silicic gravel with a mean diameter of 3.9 mm, and specific surface area of 1372 m2/m3, while the depth of the support media was 143 cm and the filter porosity 0.38. The pilot-scale filter was kept in continuous operation for four months to ensure that a steady state was achieved. Throughout all experiments, water temperature was fairly constant at about 141C, while ambient temperature was constant at about 20C (room temperature). The pH in the liquid phase throughout the filter depth ranged from 7.0 to 7.5. In this range of pH ferrous iron was the only form of dissolved iron in the liquid phase. The precipitated form of iron was detained on the support material of the filter. The concentration of the dissolved oxygen in the liquid phase throughout the filter depth was always between 7 and 8 mg/l. Under these oper-

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Distributor

Dosometric pump

Sampling valve

D=3.9 mm

Fe
Drainage system Refrigerator with feed tank Effluent

Water supply network

Fig. 1. Schematic drawing of the pilot-scale trickling filters arrangement.

ating conditions, and since the redox potential ranged from 0.3 to 0.4 V (as measured with a redox potential electrode), according to Hem [11], both physico-chemical and biological iron oxidation were taking place simultaneously. In order to assess the extent of physico-chemical iron oxidation, the filter was disinfected using commercial chlorine bleach (NaOCl 5%) every 2 days, for 2 h, and then passing network water through the filter before starting to feed with the iron concentrated solution. Under these conditions, only physico-chemical iron oxidation was possible. 2.3. Manganese removal A pilot-scale trickling filter was also used for manganese removal. The support material was silicic gravel with a mean diameter of 1.9 mm, and specific surface area of 3105 m2/m3, while the depth of the support media was 143 cm and the filter porosity 0.39. The pilot-scale filter plant was kept in continuous operation for more than ten months before the experimental series took

place, in order to ensure that a steady state was achieved. Throughout all experiments, water temperature was fairly constant at about 25C. The pH in the liquid phase ranged from 7.07.3 at the inlet of the filter to, 8.08.3 at the outlet of the filter. In this range of pH, homogenous manganese oxidation by oxygen is very slow. The precipitated form of manganese was detained on the support material of the filter. The concentration of the dissolved oxygen in the liquid phase throughout the filters depth was always between 7.0 and 8.0 mg/l. The redox potential throughout the filter depth ranged from 0.3 to 0.5 V (as measured with a redox potential electrode). 2.4. Simultaneous removal of iron-ammonia and iron-ammonia-manganese Two pilot-scale trickling filters were constructed and tested for combined and simultaneous removal of ammonia-iron and ammonia-ironmanganese, respectively. The support material for combined NH3 and Fe removal was silicic gravel

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with a mean diameter of 3.9 mm. The lower part of the filter (72 cm) was filled with gravel with immobilized ammonia oxidizing bacteria, while the upper part was filled with the same gravel with iron oxidizing bacteria. The pilot plant was kept in continuous operation for eight months to ensure that steady state was achieved. The feed solution was the result of mixing a concentrated iron and ammonia solution with water from the water supply network (that contained no measurable iron and ammonia amounts). The temperature of water in the filter was maintained at 22C, while the pH was at the range of 7.58.0. The dissolved oxygen in the liquid phase throughout the filter depth was always between 7.0 and 8.0 mg/l. For simultaneous ammonia, iron and manganese removal the filter consisted of two different support materials. The upper part of the filter (70 cm) was filled with silicic gravel of mean diameter 3.9 mm, specific surface area (As) of 1385 m2/m3 and porosity 0.38. This support material came from an already established filter which was responsible for ammonia and iron removal from potable water, so immobilized ammonia and iron oxidizing bacteria were on the surface of the gravel. The lower part of the filter (73 cm) was loaded with gravel of mean diameter 1.9 mm, with immobilized manganese bacteria. The use of gravels with immobilized acclimated bacteria led directly to continuous operation, thus avoiding a start-up period. The pilot-scale filter was kept under continuous operation for seven months to ensure steady-state conditions. The feed solution was the result of mixing a concentrated solution of ammonia, iron and manganese (with small quantities of nitrogen and phosphorous) and water from the water supply network (containing negligible ammonia, iron and manganese amounts). The temperature of the water in the filter was at 22oC, while the pH throughout the filter depth was at the range of 6.87.8. The dissolved oxygen in the liquid phase throughout the filters depth was always between 7.0 and 8.0 mg/l.

3. Results and discussion 3.1. Ammonia removal In order to design reliable trickling filters and assess nitrification performance, appropriate mathematical models that adequately describe the key physicochemical and biological processes are necessary. This work is based on the steady-state model of Vayenas and Lyberatos [8]. This model considers nitrification as a one-step process, thus resulting in analytical recursive equations. The model also predicts the steady state profiles of ammonia and oxygen concentration as well as the biofilm thickness along the filter depth. Based on this model, Tekerlekopoulou and Vayenas [12] constructed the operating diagram of a nitrifying trickling filter, which defines the operating conditions for complete and safe nitrification. In an attached growth process, the support material plays a key role on the biodegradation of the pollutants that takes place on its surface, and may affect biodegradation in several ways. The choice of the size of the support material is of great importance. Since nitrifying bacteria are autotrophic microorganisms, their growth rate is at least one order of magnitude less than the growth rate of heterotrophic ones. Thus, adequate surface per volume unit of the reactor should be provided in order to achieve satisfactory nitrification rates. Small-sized gravel provides a high specific surface area while at the same time the void space becomes smaller and pore clogging, high local flow velocities, shear stress, and mass transfer limitations become substantial. In order to study the effect of support material three different calcitic gravel sizes were used, namely small-sized, medium-sized and large-sized. Fig. 2 shows experimental (symbols) ammonia concentration profiles along the filter depth and the corresponding steady-state model (lines) predictions for the three different gravels. This Figure shows clearly the negative effect of the extreme increase of specific surface area on biological nitrification in a fixed bed filter in comparison with

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2.0

Ammonia concentration (mgN/l)

Large-sized gravel Medium-sized gravel Small-sized gravel

Q=1000 ml/min

1.5

1.0

0.5

0.0 0 20 40 60 80 100 120 140

Filter depth (cm)

Fig. 2. Effect of gravel size in nitrification comparison of experimental data (symbols) and model prediction (lines) for feed ammonia concentration 2.0 mg N/l and volumetric flow rate 1000 ml/min for the three different support materials.

time void space becomes smaller, resulting in easier pore clogging. The results of the experiments performed revealed that the mathematical model of Vayenas and Lyberatos [8] could predict filter performance very well for medium-sized gravel, and in some cases (low flow rates and ammonia load) for largesized gravel, while for the small-sized gravel model predictions were inaccurate. In the case of large-sized gravel and high ammonia load the model seems to underestimate the filter performance. The development of the above model was based on the implicit hypothesis that flow conditions do not affect biofilm growth and that there are no limitations by mass transport and shear stress. Fig. 3 presents experimental and predicted ammonia concentration profiles along the filters

2.0
model

medium-sized gravel. On the other hand, the use of large-sized gravel may lead to easier substrate and oxygen transfer and avoiding pore clogging but it reduces the specific surface area and hence the filters efficiency. Thus, there is an appropriate support material size (medium sized gravel) to achieve optimal nitrification performance. For example, Fig. 2 shows that for medium sized gravel about 70 cm are needed in order to reduce ammonia concentration below the maximum permitted limit of 0.5 mg/l, while for the large sized gravel the required filter depth increases from 75 to 110 cm. This was expected because as the specific surface area is reduced so does the filter efficiency. It would have been expected that the use of small-sized gravel would have reduced the required filter depth. Nevertheless, experimental data did not demonstrate the expected behavior. Small-sized gravel may provide a higher specific surface area but at the same

Ammonia concentration (mgN/l)

1.5

experimental

1.0

1000 ml/min 2000 ml/min

0.5

0.0 0 20 40 60 80 100 120 140

Filter depth (cm)

Fig. 3. Comparison between experimental (symbols) ammonia concentration profiles along the filter depth and the corresponding steady-state model predictions (lines) for volumetric flow rates Q = 1000 (circles and dotted lines) and 2000 (triangles and solid lines) ml/min, feed ammonia concentration 1.0 and 2.0 mg N/l, and support material: medium-sized calcitic gravel.

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Iron concentration (mg/l)

depth (with the medium-sized gravel) for various ammonia feed concentrations and volumetric flow rates. Very good agreement between experimental data and model prediction was observed. Fig. 3 shows that an increase of the volumetric flow rate reduces filter efficiency. Particularly, for ammonia feed concentration of 1.0 and 2.0 mg/l an increase of the volumetric flow from 1000 ml/min (226 m3/m2d) to 2000 ml/min (453 m3/m2d) reduces filter efficiency from 100% to 81% and 77.3% respectively. 3.2. Iron removal Two series of experiments were performed in order to investigate the effect of feed iron concentration and the volumetric flow rate on filters performance for physicochemical and combined physicochemical and biological oxidation. Fig. 4 shows iron concentration profiles along the filter depth for volumetric flow rate 1000 ml/min and iron feed concentration 1.0 and 3.0 mg/l under physicochemical and combined physicochemical and biological oxidation. The combined iron oxidation leads to better filter performance and increases iron removal efficiency. Fig. 5 shows a similar diagram for a higher volumetric flow rate of 2000 ml/min and iron feed concentration 1.0 and 2.0 mg/l. We observe that, as in the previous case, the contribution of biological oxidation results in increased iron oxidation rates. Outlet iron concentration remains below the upper permitted limit of 0.2 mg/l (dotted line) for both cases. According to experimental data, the effect of bio-oxidation improves filter efficiency by about 5 to 6% for the particular experimental conditions (nutrients, pH, and temperature). Although biological oxidation increases filter efficiency only about 5%, the corresponding filter depth to achieve outlet iron concentration below the upper permitted limit decreases drastically. For example, Fig. 5 shows that for inlet iron concentration 1.0 mg/l, the effect of biological oxidation

3.5 Physicochemical and Biological oxidation Physicochemical oxidation

3.0

2.5

2.0

1.5

1.0

0.5

0.0 0 20 40 60 80 100 120 140

Filter Depth (cm)

Fig. 4. Effect of physico-chemical and combined physicochemical and biological oxidation on total iron oxidation for volumetric flow 1000 ml/min and feed iron concentrations 1.0 and 3.0 mg/l.

2.2 2.0 1.8 Physicochemical and Biological oxidation Physicochemical oxidation

Iron concentration (mg/l)

1.6 1.4 1.2 1.0 0.8 0.6 0.4 0.2 0.0 0 20 40 60 80 100 120 140

Filter Depth (cm)

Fig. 5. Effect of physico-chemical and combined physicochemical and biological oxidation on total iron oxidation for volumetric flow 2000 ml/min and feed iron concentrations 1.0 and 2.0 mg/l.

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increases filter efficiency by about 5% while reduces the required depth by about 40%.

3.3. Manganese removal The oxidation of Mn (II) to Mn (IV) by aeration alone is a slow process unless the pH is raised above neutrality [1315]. Therefore, manganese cannot be removed by simple aeration and precipitation in neutral waters. It is well established that microorganisms are responsible for manganese oxidation in neutral environment [16,17]. The start up period of biological filters for the removal of manganese generally takes 36 months [18]. Since biological manganese removal rate is lower than ammonia and iron, gravel with small mean diameter (1.9 mm) was used as support material in order to increase the specific surface area. Fig. 6 shows typical manganese concentration profiles along the filters depth for volumetric flow rate
5.5 5.0 4.5

500 ml/min (113 m3/m2d) and various feed concentration (1.05.0 mg/l). It is obvious that manganese concentration at the outlet of the filter is under the maximum permitted limit of 0.05 mg/l (dotted line), even for high feed concentrations (up to 4.0 mg/l). 3.4. Simultaneous removal of iron, ammonia and manganese The simultaneous biological removal of the three elements is very complicated issue mainly due to the different redox potential values needed for their oxidation [4]. According to the literature [4,18,19] when raw water contains ammonia, biological manganese removal can only take place after complete nitrification because of the necessary evolution of the redox potential. However there are few references which prove the applicability of a single stage, simultaneous biological removal process of ammonia, iron and manganese,

Manganese concentration (mg/l)

4.0 3.5 3.0 2.5 2.0 1.5 1.0 0.5 0.0 0 13 26 39 52 65 78 91 104

1.0 mg/l 2.1 mg/l 3.2 mg/l 4.2 mg/l 5.2 mg/l

117 130

143

Filter depht (cm)

Fig. 6. Manganese concentrations profiles along the filter depth for volumetric flow rate 500 ml/min and feed manganese concentrations of about 1.0, 2.0, 3.0, 4.0 and 5.0 mg/l.

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by using pilot plants, from different ground waters [2022]. A pilot-scale trickling filter was used to study the simultaneous iron and ammonia removal using medium sized diameter gravel as support material, while another one was used to study the removal of the three pollutants (iron, ammonia and manganese). Fig. 7 presents iron and ammonia concentration profiles along the filters depth, for a flow rate of 1000 ml/min. Both pollutants are reduced below the upper permitted limits at the upper compartments of the filter while redox increases from 140 to about 400 mV. The addition of manganese (Fig. 8) under the same volumetric flow rate reduced filter efficiency concerning ammonia and iron removal, while redox increased to 550 mV at the outlet of the filter. Therefore, lower feed concentrations of ammonia and iron can be treated under the presence of manganese. However, Fig. 8 shows that the simultaneous removal of ammonia, iron and manganese is posORP Fe NH3

sible in one stage processes. Since manganese is the rate-limiting pollutant, it determines the appropriate hydraulic and pollutant loading for the simultaneous removal of ammonia, iron and manganese. The feed concentrations used in Fig. 8 are typical for groundwater in Greece. 4. Conclusions Biological ammonia, iron and manganese removal using trickling filters, offers an alternative method to conventional water treatment plants. The main conclusions of this work are: The high retention time of biomass in the filters enables high hydraulic and pollutant loadings. The natural aeration of the filters minimizes the operational cost while achieving at the same time high removal efficiencies. The size of the support material plays a key role for optimal ammonia removal rates.

2.0 1.8 1.6

440

400

Fe, NH3 concentration (mg/l)

360

ORP (mV)

1.4 320 1.2 1.0 0.8 0.6 200 0.4 0.2 0.0 0 20 40 60 80 100 120 140 160 280

240

120

Filter Depth (cm)

Fig. 7. Concentrations profiles of iron and ammonia in the filter for volumetric flow rate 1000 ml/min and feed concentrations 1.1 and 1.9 mg/l, respectively.

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1.0 ORP

550 500 450 400 ORP (mV) 350

Fe, NH3, Mn concentration (mg/l)

Fe NH3
0.8

Mn

0.6

0.4

300 250

0.2

200 150

0.0 0 20 40 60 80 100 120

Filter Depth (cm)

Fig. 8. Concentrations profiles of iron, ammonia and manganese in the filter for volumetric flow rate 1000 ml/min and feed concentrations 0.97, 0.61 and 0.45 mg/l, respectively.

Biological oxidation of iron enhances total iron oxidation while drastically reduces the required filter depth. Simultaneous ammonia and iron removal is feasible in one stage process even for high hydraulic and pollutants loadings. Even if manganese is the rate limiting pollutant and different redox values are needed, simultaneous ammonia, iron and manganese removal is also feasible in one stage process under satisfactory hydraulic and pollutant loadings. Acknowlegments This research was funded by the program Heraklitos of the Operational Program for Education and Initial Vocational Training of the Hellenic Ministry of Education under the 3rd Community Support Framework and the European Social Fund.

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