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Q IWA Publishing 2010 Water Science & TechnologyWST | 61.1 | 2010

Advanced water recycling through electrochemical treatment of efuent from dissolved air otation unit of food processing industry
Sukjoon Yoo and Jeffery S. Hsieh

ABSTRACT
This study elucidates the feasibility of electrochemical treatment as a water recycling process in the dissolved air otation (DAF) unit in the food industry. Effects of operation parameters such as current density, electrolysis time, initial pH of efuent, and mixing process were investigated on the removal of COD, TSS, and TDS of the DAF pretreated efuent. An increase of current density enhances the removal rates and reduces the electrolysis time to reach the maximum performance. The initial pH less than 7 and the addition of mixing process were proven to increase the efciency of EC treatment. About 80% of COD, 100% of TSS, and 60% of TDS were successfully removed at 500 mA current for 1 hour of electrolysis. The nal treated efuent was found to meet the discharge standard from the US Environmental Protection Agency. It was concluded that EC process could be effective as an advanced water resourcing technology in the food industry.
Key words
Sukjoon Yoo Jeffery S. Hsieh (corresponding author) School of Chemical & Biomolecular Engineering, Georgia Institute of Technology, 311 Ferst Drive, Atlanta, GA 30332-0100, USA E-mail: jeff.hsieh@che.gatech.edu

| current density, dissolved air otation, electrochemical treatment, electrolysis time,

mixing process, pH

INTRODUCTION
The food industry is one of the most water-consuming industries along with the pulp and paper industry and the textile industry (Casani et al. 2005). A huge amount of wastewater is spent in food industry processes such as cleansing of raw materials and equipments, process operation, and cooling. Proper management of wastewater has always been an important task in the food industry for both economic and environmental concerns (Palumbo et al. 1997). A variety of wastewater treatment practices such as biological treatment, membrane separation and coagulation process were utilized throughout the food industry (Campos et al. 1986; Rusten et al. 1990; Blocher et al. 2002). The use and development of dissolved air otation (DAF) has particularly been expanding in the food industry for the pre-treatment of food and meat processing efuents because it operates based on a reasonably simple design and it is very efcient at removing suspended solids, fats, oils
doi: 10.2166/wst.2010.802

and greases, which are the main organic matters in wastewater from the food processing industry (Kiuru & Vahala 2001). In a DAF unit, air is dissolved into water under pressure to produce a saturated solution of air and water in a pressure vessel. The pressurized air/water feed is then injected into the otation tank and the sudden pressure drop in the tank causes the release of very ne air bubbles. These very ne bubbles play a crucial role in the high separation efciency of DAF process. Air microbubbles adhere to suspended particles in the wastewater, increasing the buoyancy of the particles, causing them to oat to the surface and to form a oating layer. The oated sludge is skimmed off from the top of reactor or collected through the screening in the down stream. Mittal (Mittal 2006) reported that DAF units can achieve about 35% reduction of total COD (TCOD) and soluble solids (SS) from the abattoirs wastewater. Johns (1995) reported that

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DAF units with chemical addition can reduce 30 90% of COD, 70 97% of TSS and 89 98% of fats, oil & grease (FOG) from the meat processing wastewater. However, the resulting stream after DAF process is unlikely to meet the increasingly stringent regulation on the discharge limits (Johns 1995). The combination of proper secondary treatment process after DAF process is required and the effective water recycling through waste water treatment can bring the economic advantage in the food industry by utilizing a huge quantity of drain water in DAF process. Electrochemical (EC) treatments such as electrocoagulation, electrootation and electrochemical oxidation have been studied extensively because of their several advantages over a typical wastewater treatment plant (Rajeshwar et al. 1994). The electrochemical based systems allow rapid and controlled reactions with robust and compact instrumentation, which provide ease of automation (Chen 2004). Instead of using chemicals and micro-organisms, the electrochemical systems only employ electrons to facilitate water treatment, which offer better environmental compatibility (Mollah et al. 2004). Electrochemical treatments generally have lower temperature requirements and require less space, and produce fewer by-products or sludge (Mollah et al. 2001). EC treatment is a complicated process involving many chemical and physical phenomena that use the in situ generation of coagulants by electrolytic oxidation of the sacricial electrode materials. Through the connection to the external DC source, the electrode materials such as Fe or Al are dissolved from the anode generating corresponding metal ions, which almost immediately hydrolyze to polymeric iron or aluminium hydroxides. These polymeric hydroxides are excellent coagulating agents which can combine with charged particles or colloidal contaminants in the wastewater. The coagulated contaminants are then removed by electrootation, sedimentation, or ltration to provide clean water in the end. The promising performance of electrochemical treatment has been proved in the diverse types of wastewater treatments including heavy metals (Thaveemaitree et al. 2003), foodstuff (Chen et al. 2000), textile dyes (Naumczyk et al. 1996), oil wastes (Gotsi et al. 2005), suspended particles (Bukhari 2008), uorine (Mameri et al. 1998), phenolic wastes (Korbahti & Tanyolac 2003), ultra-ne

particles (Matteson et al. 1995), mine wastes (Jenke & Diebold 1984) and water disinfection (Feng et al. 2004). Conventionally, electrochemical treatment or coagulation via chemicals have been applied prior to DAF process in order to improve the efciency of waste water treatment by increasing particle size or neutralizing the charge effect of efuent. In the recent work by Yoo et al. (Yoo et al. 2009), the DAF unit was utilized as a tool to recover the valuable products such as calcium carbonates from eggshell waste. In this paper, the electrochemical treatment was applied as the post treatment process after DAF process, which makes EC treatment work only for waste water treatment without contaminating the recovered products from DAF separation unit. The feasibility of the water recycling system through electrochemical treatment after the DAF process was investigated in a laboratory batch study. The performance of electrochemical treatment of DAF pretreated eggshell wastewater was explored by the measurement of several environmental parameters such as Chemical Oxygen Demand (COD), Total Suspended Solids (TSS), Total Dissolved Solids (TDS) and pH. Effects of various operating parameters such as current density, treatment time, initial pH, and mixing on the performance of EC treatment were further studied to optimize conditions for the electrochemical post-treatment of DAF pretreated eggshell wastewater.

MATERIALS AND METHODS

Dissolved air otation (DAF) process In this paper, we simulate the DAF efuent by using a lab scale DAF separation process with eggshell waste(Yoo et al. 2009). The DAF process for eggshell waste treatment is shown in Figure 1. The eggshell mixture was prepared by mixing 620 g of eggshell waste with 400 ml water and was ground using a homogenizer for 10 min to separate the eggshell membrane from the eggshell and to produce organic matters in solution. The ground eggshell was placed in the DAF separation vessel. Air and water ows were mixed and injected through a Mazzeiw injector (Bakerseld, CA, USA, Model#: 384X). The DAF separation unit was normally run with 0.85 standard cubic meters per hour

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Figure 2

Schematic of the lab-scale electrochemical treatment.

E-C Apparatus Corporation, St. Petersburg, FL) was used to

Figure 1

Dissolved air otation (DAF) process combined with the water recycling system.

supply a regulated electricity current to the EC reactor. The positive terminal of the DC power supply is connected to the aluminium rod while the negative terminal is connected to the stainless steel wall of the EC reactor. In a typical run, 2 L of DAF pretreated eggshell wastewater was batch loaded into the EC reactor and treated at three different constant current densities (100, 300 and 500 mA) within the specied time periods (0 to 4 h). In some runs, mixing was performed by a mechanical stirrer (Arrow 1750, Arrow Engineering Co., Hillside, NJ) to investigate the effect of mixing on the performance of the EC treatment. Sulfuric acid or sodium hydroxide solutions were added to adjust the initial pH of the wastewater to the desired level for experiments. Samples were taken from the EC reactor at predetermined electrochemical treatment times (15, 30, 60, 120, and 240 min) after skimming off the oated ocs. All samples were allowed to settle for about 30 min in a graduated glass vessel to complete the sedimentation. An undisturbed sample (50 mL) of the supernatant was collected for examination at the end of the sedimentation process.

(SCMH) air ow at 275 kPa and 189 liters per hour water ow. The air/water mixture ows from the bottom of the separation vessel and causes the lighter component of the eggshell to oat up and the heavier eggshell calcium carbonate particles to settle out at the bottom of the vessel. The oated stream passes through a screen ltering system to recover the suspended eggshell particles. The DAF efuent is collected after the screening system for further electrochemical treatment. Table 1 shows the characteristics of the DAF efuent that were relevant to the electrochemical post-treatment in this study.

Electrochemical treatment Electrochemical treatment has been carried out using a lab-scale electrochemical (EC) reactor in a batch mode. The experiment set-up is shown in Figure 2. The reactor used in this study was a cylindrical stainless steel reactor of 4 L capacity which has a diameter of 17.2 cm and a height of 20 cm. A circular aluminium electrode, which has a diameter of 0.7 cm and a length of 25 cm, was used as the anode. The aluminium rod was oriented vertically in the center of the cylindrical reactor and placed 1 cm apart from the bottom of the EC reactor. A DC power supply (EC135,
Table 1

Analysis methods The effects of electrochemical treatment were analyzed by determining physicochemical parameters such as Chemical Oxygen Demand (COD), Total Suspended Solids (TSS), Total Dissolved Solids (TDS) and pH. The pH was measured using a pH voltage meter (F350 pH/Temp/mV Meter, Beckman Coulter, USA). The COD values were measured by the following procedure: 2 ml of samples were digested using Digestion Solution for COD 0 1,500 ppm (CAT# 21259-15, HACH, USA), incubated in 1508C oven

Characteristics of the DAF pretreated eggshell wastewater

Parameter

Value

COD (mg/l) TDS (mg/l) TSS (mg/l) pH

465 ( ^ 128) 518 ( ^ 216) 373 ( ^ 188) 7.89 ( ^ 0.13)

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for two hours, cooled down for three hours, and analyzed using a UV-Visible spectrophotometer (Spectronic 610, Milton-Roy, USA) at 620 nm wavelength. TSS and TDS were measured according to the methodology described in the Standard Methods (Clesceri et al. 1998). All the experiments were performed in triplicate to ensure reproducibility.

the effect of treatment time on the removal efciencies of COD, TSS and TDS with various current density conditions such as 100, 300 and 500 mA. As the current density increased, the treatment time needed to achieve similar efciencies decreased. In removal of COD (Figure 3A), EC treatment with high current densities of more than 300 mA brings 70% of COD removal within 30 min while it takes 2 hours with low current density of 100 mA to get the same performance. The removal efciency of TSS also increases

RESULTS AND DISCUSSION

Effect of electrochemical treatment time and current density In the EC process, current density and treatment time are important condition parameters. We investigated the effect of electrolysis time and current density on the EC treatment of DAF pretreated eggshell wastewater. Figure 3 represents

as the applied current density increases (Figure 3B). After 1 hour of treatment, TSS decreases by 70, 90 and 100% with 100, 300 and 500 mA, respectively. But after 2 hours of treatment, the removal rate of TSS reaches up to 100% in all current densities. Figure 3C shows that the efciency of TDS removal is also improved when the wastewater is treated for a longer time and with high current densities. These positive effects of current density and electrolysis

Figure 3

Effects of current density and electrolysis time on changes of (A) COD, (B) TSS, (C) TDS and (D) pH of the treated efuent.

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time on the removal of COD, TSS, and TDS can be explained by Faradays law of electrolysis: m QM ItM zF zF 1

where m is the mass of the substance altered at an electrode (g cm22), Q is the total electric charge passed through the substance (C cm22), I is the current density (A cm22), t is the total time (sec) the constant current was applied, M is the relative molar mass of the substance, z is the valence number of ions of the substance, and F is Faradays constant (96,500 C mol21). Because M, F, and z are constants in this system, the amount of electrode materials dissolved from the anode was determined by the current density (I) and the electrolysis time (t). Higher current density and longer electrolysis time facilitates the dissolution of electrode materials by forming much more polymeric aluminium hydroxide coagulants in the solution, which results in the faster precipitation of contaminants from wastewater. The higher current density not only increases the coagulant generation rate but also enhances the production of small bubbles of oxygen at the anode and hydrogen at the cathode by parallel electrolysis of water. These bubbles attract and oat the occulated pollutants to the surface through natural buoyancy, which improves the efciency of electrootation in the EC treatment. The electro-oxidation of organic matters also can be improved at high current density. Therefore, the amount of dissolved and suspended solids in the wastewater can be reduced more effectively by the active EC treatment at high current density. This accelerated removal of organic or inorganic particulates effectively reduces COD values as well. The removal rates show a plateau after a certain electrolysis time, indicating that they reach their own maximum performance. With applying a current of 500 mA for 1 hour, the removal efciencies reached their own maximum values such as 80% and 100% for COD and TSS respectively and were not improved signicantly after that. As shown in Figure 4, the consumption of both electrical energy and the soluble electrode, which are main components of the operating cost, increases progressively as the applied current density is higher and the electrolysis time is longer. Taking into account both process cost and performance efciencies with 300 mA and 500 mA of current densities, the difference Effect of initial pH on the removal of COD, TSS and TDS The initial pH of wastewater is an important parameter in the electrochemical treatment. Through the dosage of acids (sulfuric acid) or alkaline (sodium hydroxide) solutions, the
Figure 4

Consumption of electrical energy (A) and sacricial electrodes (B) in the EC process.

of performance efciencies is negligible but the operating cost will be much higher with 500 mA of current density. Therefore, one hour of electrolysis time with 300 mA current density is considered to be optimal for a batch system to treat 2 L of DAF pretreated eggshell wastewater without adding additional electrolyte salts. The pH values (Figure 3D) have been maintained between 8.0 and 8.5 during 4 hours of treatment to prove that no additional treatment will not be required to correct the efuent pH to regulatory discharge values.

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pH was adjusted to different values such as 3, 7 and 11, which represent the acidic, neutral and alkaline conditions of efuents, respectively. The effect of the initial pH on the removal of COD, TSS and TDS was explored at the constant current density of 100 mA and the results were shown in Figure 5. For the COD removal (Figure 5A), acidic or neutral conditions show better removal efciencies than alkaline conditions. COD removal efciencies reached up to 75% at pH 3 and 7 while only 40% of COD removal was achieved at pH 11 after 2 hours of treatment. The TSS removal efciencies are more than 90% at pH 3 and 7 while only 65% of TSS removal was achieved at pH 11 after 1 hour of treatment. However, after 2 hours of treatment, more than 85% of TSS removal efciencies were obtained for all cases of initial pH conditions (Figure 5B). In the EC process, aluminium dissolution (Equation 2) and oxygen evolution (Equation 3) compete on the anode side and hydrogen evolution (Equation 4) is the main expected

reaction on the cathode side. The aluminium ions and hydroxyl ions generated by reactions (Equation 2) and (Equation 4) combine to synthesize insoluble polymeric aluminium hydroxides as coagulants in the EC process. At the anode: Al ! Al3 3e2 Aluminium electrode dissolution 2H2 O ! O2 4H 4e2 Oxygen evolution At the cathode: 2H2 O 2e2 ! H2 2OH2 Hydrogen evolution 4 2 3

The initial pH can affect these reactions and inuence the performance of EC treatment. At low pH, high concentration of protons facilitates the hydrogen evolution at the cathode to produce the more hydroxyl ions. At the same time, it reduces the oxygen evolution rate at the anode

Figure 5

Effects of initial pH on the removal efciencies of (A) COD, (B) TSS and (C) TDS.

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and consequently enhances the reaction between the potential hydroxyl ions and the dissolved aluminium ions near the anode to increase the generation of aluminium hydroxide coagulants. On the other hand, alkaline media brings the reverse effects. In addition, it is known that the solubility of aluminium hydroxide has its minimum at a lower pH close to 4 and that high pH conditions solubilize aluminium hydroxide to form AlO2 which is ineffective for water treatment (Picard et al. 2000; Canizares et al. 2005). It can be concluded that low pH conditions might be benecial to achieve high removal efciencies for COD and TSS. But it should be noted that similar performance could be achieved at the original pH of the DAF pretreated eggshell wastewater around pH 7 to 8. In a real application, the pH adjustment through chemical addition may be expensive, and the pH adjustment also increases TDS values signicantly (Figure 5C). Thus, a further pH adjustment may not be necessary for this case.

Effect of mixing on the removal efciency of COD, TSS and TDS The effect of mixing on the EC process was investigated and shown in Figure 6. Results indicated that when the mixing was applied to the EC process, the removal efciencies of COD and TDS were improved after 1 hour of treatment. But, TSS removal efciency does not show the difference with or without mixing process. The EC process is a diffusion controlled process. Adequate mixing can provide effective collisions between coagulant and pollutant particles to enhance coagulation. The mixing effect can increase the current efciency also. According to Bards work (Bard & Faulkner 1980), the operating current can be expressed the following equation: I nFAm0 C 0 5

where I is the current, n is number of electrons per molecule oxidized or reduced, F is Faradays constant, A is the

Figure 6

Effects of mixing on the removal efciencies of (A) COD, (B) TSS and (C) TDS.

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electrode surface area (cm2), m0 is the mass transfer coefcient (cm/s), and C0 is the molar solute concentration, which usually indicates the concentration of electrolytes in solution such as sodium chloride. The above equation indicated that the operating current is primarily dependent on the electrode surface area, mixing rate, and electrolyte concentration. As the mixing rate increases, the mass transfer inside the EC reactor is enhanced to bring high current density which was proven to play an important role in the EC treatment. It was also observed that if there is no mixing at all, ocs tend to build up on the anode. Besides oc formation, it is known that the absence of the proper convection in the EC reactor allows the accumulation of the oxygen and hydrogen gas bubble nucleates at the electrode surface to produce an insulating layer (Mollah et al. 2004). These passivation layers on the electrodes reduce the available electrode surface area to generate aluminium ions and hydroxyl ions and increase the overall electrical resistance of the cell to bring the more energy consumption and deteriorate the efciency of the EC process. Mixing increases the turbulence level inside the EC cell enough to sweep away these blocking layers and prevent the expected interference. Our results presented the positive effect of mixing to show the improvement of the removal efciencies of COD and TDS. However, it should be noted that the vigorous stirring or the strong agitation might hinder coagulation through breaking up the ocs (Matteson et al. 1995; Ilhan et al. 2008). Our results also present the possible adverse effect of mixing on coagulation process to show that TSS removal efciency was not improved with mixing process. Therefore, the optimum mixing rate needs to be found to ensure the performance of EC treatment. Further study is highly required to develop the advanced mixing technologies.
Figure 7

Sludge generation from electrochemical treatment of DAF pretreated eggshell wastewater.

which represents the amount of sludge, increases along with electrolysis time and applied current density. After 4 hours of treatment, TSS values without settling increase up to 200%, 300%, and 400% with 100 mA, 300 mA, and 500 mA of applied current densities, respectively. It demonstrates that strong electrochemical treatment enhances the formation of much more aluminium hydroxide and simultaneously increases the aggregation of pollutant particles, which consequently improves the treatment efciency but produces more sludge. TDS values decrease and reach a plateau after 1 hour of treatment, which also veries the coagulation of small particles in the EC treatment. It can be concluded that sludge is produced in large volumes as the EC process achieves better removal of pollutants through coagulation and sedimentation. Considering the mechanism of EC process, it can be easily deduced that EC sludge should contain a considerable amount of heavy metals whose toxicity is an important issue environmentally. It was

Sludge production in electrochemical treatment The EC process produces sludge as a by-product which needs to be handled and disposed of properly. The effect of EC treatment conditions on sludge formation was investigated through measuring values of TSS and TDS without settling after treatment. Figure 7 shows the change of TSS and TDS for different current densities and electrolysis times. Results show that the amount of suspended solids,

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reported that compared with other chemical precipitation processes, the EC process produces less sludge and the generated sludge is environmentally friendly in that metals in the EC sludge are stabilized in a non-hazardous form as oxides (Mollah et al. 2001). However, the proper disposal of EC sludge still needs to be suggested in order to verify the feasibility of EC treatment. EC sludge from commercial or industrial wastewater is usually disposed of in a landll or incinerated to provide heat as a low grade fuel. Besides simple disposal, several ways to utilize EC sludge have been investigated in recent years. Chu reported that recycled alum sludge can be utilized in wastewater treatment processes such as metal removal (Chu 1999) and dye removal (Chu 2001). Xu et al. (Xu et al. 2002) demonstrated that the sludge from EC treatment of food process efuent contains high digestible protein and fat values. But these methods have limitations in being applied universally due to diverse characteristics of EC sludge from different efuents. Consequently, reasonable reduction or destruction of EC sludge is required. The combination of other treatment processes such as advanced oxidation processes or electrochemical oxidation can be considered for this.

Agency (EPA). All presented values are obtained from the EC run of 2 hours with 500 mA current density and no pH adjustment. It is indicated that electrochemical treatment claried the DAF eggshell wastewater enough to match the EPA requirement in terms of TSS, BOD, and pH. Other environmental standard quantities such as COD and TDS also show a signicant decrease with EC treatment. Results clearly demonstrate that EC treatment is effective in treating efuent from the DAF process and recycling clean water.

CONCLUSION
In this research work, we explored the applicability of electrochemical treatment as a post-treatment process to purify DAF pretreated wastewater for advanced water resourcing technology. Effects of various operation parameters such as current density, electrolysis time, initial pH of efuent, and mixing in the EC system on the removal of COD, TSS, and TDS of the DAF pretreated eggshell wastewater were investigated and optimized. It was shown that application of higher current density and longer electrolysis time enhances removal efciencies of COD,

Comparison of EC treatment performance compared with the EPA regulation Table 2 shows the summary of EC treatment of DAF treated eggshell wastewater compared with the requirement for wastewater discharge from the Environmental Protection
Table 2

TSS and TDS. But it is also indicated that sludge generation, consumption of electrodes, and electrical energy also increment linearly along with current density and electrolysis time. Acidic or neutral pH conditions were found to be better than alkaline conditions to improve removal efciencies for COD and TSS in EC treatments. It was also recognized that the mixing process could improve the mass transfer rate in the EC cell and consequently bring high current density which is critical for EC treatment. Results showed that 80% of COD, 100% of TSS, and 60% of TDS were successfully removed from the DAF pretreated eggshell wastewater after 1 hr of electrolysis at the operating condition with a current density of 500 mA, and the natural pH condition of DAF efuent around 7 to 8 in the lab scale batch system. The quality of the nal discharge after EC treatment in terms of BOD, TSS, and pH was also proven to match EPA regulations. Consequently, EC treatment is conrmed to be technically feasible as a post-treatment step after the DAF process and an advanced water resourcing technology in the food industry.

Comparison of EC treatment performance with the EPA regulation EPA Requirementp

Before Treatment

After Treatment

COD (mg/l) TDS (mg/l) TSS (mg/l) BOD (mg/l) pH

p

436 (^ 80) 517 (^ 58) 433 (^ 104) 64 7.69 (^0.12)

104 (^37) 200 (^87) 0 (^ 0) 16 8.26 (^0.13)

N/A N/A Below 30 Below 45 Below 30 Below 45 6.0 , 9.0

EPA (Environmental Protection Agency), 40 CFR (Code of Federal Regulations) Parts 133 Secondary Treatment Regulation.

30-day average: the arithmetic mean of pollutant parameter values for samples collected in a period of 30 consecutive days. 7-day average: the arithmetic mean of pollutant parameter values for samples collected in a period of 7 consecutive days.

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ACKNOWLEDGEMENTS
The authors would like to thank Georgia Food Processing Advisory Council (FoodPAC) for funding this study.

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