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2.1 Coconut

The coconut palm, Coco Nucifera L., is a member of the family Arecaceae. The term coconut can refer to the entire coconut palm, the seed, or the fruit, which botanically not a nut but a drupe. The fruit is harvested for its white flesh, husk, and coconut water (Lerner, 2007). It is cultivated for its various benefits, namely nutritional, medicinal advancement against diseases and for the development of industrial products (Mandal, 2011).

The coconut takes between 11 and 12 months to reach full maturity. At five months, the kernel begins to form a thin layer of jelly around the inside of the endocarp or shell. The shell encloses the tender water, a clear sweet liquid (Prades, et al., 2011). Coconut is a fruit in which an outer skin (exocarp) and fibrous husk (mesocarp) surrounds a hard husk (endocarp) with a coconut meat (endosperm) inside (Armstrong, 2008). Coconut fruit is shown in Fig.2.1.

Figure2.1 Coconut Fruit

The production of coconut shows a significant role in the economy of the Philippines. Being the worlds largest producer of coconuts, an average of 2.712 million metric tons of said products were harvested in medium-sized farms in year 2009 up to 2012 as shown in Table 2.1 (FAO, 2011).

Table 2.1 Production of Coconut in year 2008-2012

(Source: Philippine Coconut Authority)

2.1.1 Coconut water

Coconut is unique among other fruits because it contains a large quantity of liquid. When it has not yet reach full maturity they are called tender coconut

water which can be harvested for drinking. Coconut water in its natural form is recognized as a refreshing drink. Popularity of this drink is increasing due to its good nutritional value, low calorie and free from added ingredients (Paniappan, 2012).

Tender coconuts after removing from the tree can be kept for 15 days without spoilage in ambient conditions (Chandy, 2009). Once opened the

coconut water becomes off-flavored in taste and turns sour due to intense enzymatic activity (USDA, 2009).

Coconut water became a popular drink in the tropics, especially in India, Africa, Caribbean and here in the Philippines. It is presented in the market fresh, canned, and bottled. It has a shelf life of 24 months when placed in bottles (Belargo, 2010). Benefits and Composition

Coconut water contains antioxidants, vitamins and minerals, sugar, proteins, dietary fibre and provides an isotonic electrolyte balance. The biologically pure, coconut water helps to replace fluids, electrolytes and sugars lost from the body during heavy physical activities (Fife, 2008). This natural drink is believed to be useful in preventing and relieving many health problems including dehydration, constipation, digestive disturbances, malnutrition, fatigue, heatstroke, boils, diarrhea,

kidney stones, osteoporosis, urinary tract infections, and sterility (Fife, 2008).

Table 2.2 below shows that coconut water is also rich in many essential amino acids including lysine, cystine, phenylalanine, histidine, and tryptophan (Gopikrishna, 2008).

Table 2.2 Composition of tender coconut water

(Source: Journal on Quantitative Analysis of Coconut water) Nutritional Contents

This Table 2.3 shows nutrition value per 100 grams (g) of tender coconut water. It reflects available nutrition facts, vitamins, electrolytes, minerals and its nutrient value and percentage recommended dietary allowances.

Table 2.3 Nutrition Value per 100g of Coconut Water


Nutrient Value 19 Kcal 3.71 g 0.72 g 0.20 g 1.1 g

Percentage of RDA 1% 3% 1.5% 1% 3%

Energy Carbohydrates Protein Total Fat Dietary Fiber Vitamins Folates Niacin Pantothenic acid Pyridoxine Riboflavin Thiamin Vitamin C Electrolytes Sodium Potassium

3 g 0.080 mg 0.043 mg 0.032 mg 0.057 mg 0.030 mg 2.4 mg

0.75% 0.5% <1% 2.5% 4% 2.5% 4%

105 mg 250 mg

7% 5%

Minerals Calcium Copper Iron Magnesium Manganese Zinc 24 mg 40 mcg 0.29 mg 25 mg 0.142 mg 0.10 mg 2.4% 4.5% 3.5% 6% % 1%

(Source: USDA National Nutrient data base)

2.2 Membrane Technology

Membrane technology is used in the beverage industry especially in clarification of fruit juice. Membranes range from finely porous structures to nonporous and can remove contaminants such as bacteria and protozoa down to ions (Wang 2013). In last two decades, there has been a significant growth and increase in its application. Membrane technology has full scale global applications in municipal and industrial wastewater, ultra-pure water, speciality chemicals, recovery/reuse, agriculture,

pharmaceutical, power generation, drinking water and beverages (AMTA, 2007).

There are four levels of membrane filtration. These levels are from largest to smallest pore size namely microfiltration, ultrafiltration, nanofiltration, and reverse osmosis. This table also enumerates particular target contaminants from 1 m to 0.001 m that are being removed in different filtration level (Dave, 2013).

Table 2.4 Comparison of Membrane Filtration Levels

(Source: Virginias Community College)

2.2.1 Microfiltration

Microfiltration (MF) is a type of physical filtration process where a contaminated fluid is passed through a special pore-sized membrane to separate microorganisms and suspended particles from process liquid (Baker, 2012).

Microfiltration can be an alternative to fruit juice preservation and conservation, because it does not involve the use of heat treatment since thermal processes largely affect the characteristics of fruit juices. The advantages of microfiltration are the use of mild temperature and pressure conditions, which maintain the nutritional quality and the sensorial attributes of the products (Carvalho, 2010). Dead-End Filtration

In dead-end filtration, the feed flow perpendicular to the membrane. The particulates will accumulate and form a cake at the membrane surface. The cake increases in height throughout the filtration period resulting in a decrease in permeate flux (Fumatech, 2010). Therefore the membranes in dead-end operations have to be cleaned at regular intervals either by backwashing or other physical cleaning methods (Lenntech, 2009).

2.2.2 Ceramic Filter Cartridge

In 1846, Henry Doulton has invented the modern form of ceramic that was widely recognized as a premier manufacturer of an effective prevention device for treating infective water. Doulton's original organization for water filters remains in existence, although it has been sold and renamed several times (Berks, 2008). As with most filtration methods, fluid stream is carefully introduced to one side of the filter, which acts to block the passage of anything larger than the pore size.

Ceramic filters are inexpensive and effective type of filter that rely on the small pore size of ceramic material to remove dirt, debris, bacteria, protozoa, and microbial cysts but are not effective against viruses since they are small enough to pass through. The major risks to the success of all forms of ceramic filtration are hairline cracks and cross-contamination (Brown et.al, 2011). In comparison to

polymeric membranes, ceramic membranes are slower to foul and can be regenerated using more extreme membrane performance recovery methods, which polymeric membranes are unable to handle due to thermal limitations of polymeric materials (Panglisch, 2009).

2.2.3 Permeate Flux

Permeate flux is usually analyzed by the decline in flux and the decrease of transmission over time resulting to the reversible accumulation of particles on the membrane surface, which eventually progresses to the irreversible cake build-up (Hwang, & Liao, 2011).

Permeate flux may change with filtration time according to the fouling behaviour of the feed solution. High initial permeate flux followed by a rapid flux decrease is characteristic of constant TMP operations. The initial high increase of pressure cause rapid particle deposition which results in a fast build-up of a boundary layer at the membrane surface (Buetehorn et al., 2012). Permeate flux during a microfiltration process of pineapple juice is illustrated in Fig.2.2.

Figure 2.2 Permeate flux during a microfiltration process of pineapple juice

This graph showing filtration of pineapple juice is a typical example of permeate flux during a microfiltration process. There is a decline of the permeate flux attributed to fouling due to pore blocking and cake built up (Yasan et al., 2007).

2.2.4 Membrane Fouling

Membrane fouling is accumulation of non-dissolved material that is either deposited on the pore mouths or walls of the membrane. Fouling leads to an increase in resistance giving less flux for a given vacuum pressure difference. For example, using a metering pump to maintain a fixed permeate flow rate. Understanding the other resistances is important and it is imperative to distinguish a reduction in driving force across the membrane from an increase in resistance because of fouling of the membrane (Field, 2010).

Membrane fouling can be classified as physically reversible or irreversible fouling. Physically reversible fouling can be eliminated totally by physical cleaning or certain pretreatment while physically irreversible fouling can be overcome by chemical cleaning limited to a minimum frequency since repeated chemical cleaning may affect membrane life (Hiroshi et al., 2007).

2.2.5 Transport Phenomena in Membrane Processes

In membrane processing, the external pressure that must be applied for significant permeate flux must be higher than the osmotic pressure of the solution. The basic relationship between applied pressure (by a pump), osmotic pressure, and flow of solvent through a membrane is expressed in terms of the flux and the driving force and resistances. Eqn1. is for an ideal semipermeable membrane:


Where J is the flux, A is a membrane permeability coefficient, PT is the transmembrane pressure, and is the osmotic pressure of the feed solution.

For an ideal membrane and feed solution the Eqn.1 is rewritten given by Eqn.2


Where A is a membrane permeability coefficient, and

is the viscosity of

permeate. For a particular feed solution at a given temperature, viscosity is usually included with the A value and can written as in Eqn.3 where water as the feed. which is rewritten below

is the intrinsic membrane resistance determined using pure

Eqn.3 In actual operation with a real feed, the membrane resistance may be only a small part of the total resistance.

Eqn.4 If significant membrane fouling occurs because of specific membranesolute interactions, the intrinsic membrane resistance may change based on the Eqn.4. It is accounted for by adding another resistance term, RF because of fouling to the model (Cheryan, 1989).

2.2.6 Cleaning Process

The cleaning process is just as important as the actual filtration process. It is fundamental in determining the technical and economic viability of the processes on an industrial scale where efficiency and repeatability are essential (Coutinho, 2009). Membrane cleaning methods can be divided into physical, chemical and physio-chemical. In practice, physical cleaning methods followed

by chemical cleaning methods are widely used in membrane applications (Arnal et al., 2011).

In general, acids namely nitric, phosphoric, hydrochloric and sulphuric are often used to remove precipitated salts or scalants, while alkaline cleaning is suitable for organic fouling removal. Other categories of chemical cleaning agents are metal chelating agents, surfactants and enzymes (Mohammadi et al., 2007).

2.2.7 Backwashing

Backwashing is a type of cleaning method that uses reverse mechanism of filtration process wherein the suction pressure is applied on the retentate side. The accumulated cake flushed out from the membrane pores. The pressure on the permeate side of the membrane is higher than the pressure within the membranes, causing the pores to be cleaned. Many techniques have been developed to overcome fouling. Backwashing is typically used to clean membranes, while more persistent foulants are removed by the use of chemical reagents. However, these chemicals sometimes damage the membrane materials reducing the lifetime and efficiency of the membrane and even cause a secondary pollution over cleaned membrane (Arnal, 2011). Fig.2.3 shows the cleaning flow direction in backwashing.

Figure 2.3 Backwash Mechanism


3.1 Materials and equipment

Coconuts with maturity of 6-7 months, shown in Figure 3.1, were harvested from the province of Famy, Laguna.

Figure 3.1 Raw material used in the study: Coconut fruit

Laboratory instruments used in the preparation of the solutions needed for the tests were hot plate model design by company Corning, analytical balance model, pump set up fabricated by Schuco Inc. Model 5711 130 including the vacuum receiving container and basic instruments like beaker, flasks, cylinder and stirrer. The

microfiltration apparatus was supplied by the company Osmosis. The ceramic filter cartridge, with a 0.3-0.9m pore diameter, was manufactured by MegaFresh Company.

3.2 Preparation of the Reagents

3.2.1 Dilute bleach solution

The dilute bleach solution was prepared by dissolving 300ppm or one (1) tablespoon of bleach into 4.5 liters of water. The solution was used for the sanitization of the coconuts (Rolle, 2007).

3.2.2 Preparation and Standardization of 0.1M NaOH

A 0.1 molar sodium hydroxide (NaOH) solution was prepared by weighing 4.00 grams of NaOH pellets supplied by Lab-Scan Analytical Sciences Asia Co. Ltd. Using a 250 mL beaker, the pellets were dissolved in a 200 mL of warm freshly boiled deionized water. The deionized water was supplied by Pharmacology Laboratory, Room 307, Thomas Aquinas Research Center (TARC). The beaker was covered with a plastic film and was cooled to room temperature. Using a volumetric flask, the same freshly boiled distilled water was added to the solution until a volume of one (1) L was achieved. Four (4) liters of 0.1M NaOH solution was prepared during the experiment.

3.2.3 Preparation of 0.1M H2SO4

Sulfuric acid is corrosive and obtaining 10 mL needed for the preparation was done under the fume hood. The 10 mL sulfuric acid was obtained using graduated cylinder. The acid was then poured into a 1 L of deionized water and was stirred. The acid prepared was 1% v/v sulfuric acid. Four (4) liters of 0.1M H2SO4 solution was prepared during the experiment.

3.3 Extraction of Coconut Water

3.3.1 Good hygienic practices

The persons involved in the sanitation and extraction of the coconut water observed good hygienic practices. The washing of hands before and after every process was strictly observed. All laboratory glass wares were properly cleaned and dried. Laboratory gowns, masks and gloves were used at all times during the experimental proper (Rolle, 2007).

3.3.2 Sanitization of the coconut

The coconuts were washed and brushed using potable running water to thoroughly remove dirt and debris of any form on the surface of the coconut husk. Damaged coconut and those with visible cracks were discarded. The water-washed coconuts were then soaked into the dilute bleach solution for 15

minutes to reduce the number of microorganisms on the surface of the nut. Then, the clean nuts were allowed to air dry in a clean surface (Ohler, 1999).

3.3.3 Sanitization of chopping board and bolo knife

The chopping board was thoroughly scrubbed using antibacterial dishwashing liquid. Dirt and sand traces were also removed using a scrubber. The chopping board was soaked in the bleach solution for 15 minutes. The bolo knife was newly bought and cleansed thoroughly using scrubber to remove traces of rust and dirt. Then it was soaked in the bleach solution for 15 minutes. The tools were rinsed with running water for five (5) minutes and then air-dried.

3.3.4 Coconut water extraction and pre-filtration

All tools were properly sanitized and air-dried in order to reduce microbial contamination. Sanitation of the tools and glass wares were done by soaking them into boiling water for 15 minutes and were dried at ambient air condition. Small hole was pierced at the surface of the coconut using the bolo knife. The coconut water was coarse filtered using sanitized filter cloth (cheese cloth) to remove solid particles and coconut kernels and stored in sanitized containers. According to the Philippine Coconut Authority (PCA), the average volume of fresh coconut water per nut is 300 mL. Sixty (60) coconuts were extracte during this experiment having an approximate of 18 liters of fresh coconut water.

Figure 3.2 Microfilter Equipment

3.4 Cleaning of Microfilter equipment

Contaminants were removed with proper cleaning. Three steps were done to avoid the contamination of the coconut water during filtration. This includes the running of deionized water, caustic solution followed by the acid. The alkali used has a molarity of 0.1 NaOH solution and the acid cleaning by 1% v/v sulfuric acid solution of pH 4. The acid and alkali solutions were circulated in the equipment for 20 minutes then rinsed again with deionized water to remove the residues. The whole process was roughly done within 1 hour and 30 minutes.

3.5 Microfiltration

3.5.1 Membrane Material The feed was microfiltered at constant vacuum pressure of 21 inHg on each trial using 0.3-0.9 m pore ceramic membrane manufactured by MegaFresh Co., Ltd. The membrane used has a property of being unreactive to chemicals because it consists of titania, zirconia and alumina. It was compatible with all solvents, acids and alkaline solutions (Csem, 2010). The dimension of the ceramic membrane is 9.093 inches (23.0962 cm) length and has a diameter of 2 inches (5.08 cm). The effective surface area of the filter is 57.1330 in2 (0.03686 m2). Clean membrane was used for every run in the experiments. After each run, the membrane was cleaned and kept in a sealed container soaked in bleach solution to avoid bacterial contamination.

3.5.2 Microfiltration Set-up The experiment was done using Lab-scale water filtration apparatus, which was fabricated by the company Osmosis. A centrifugal pump with a constant suction pressure of 21 inHg was observed in the experiment. The vacuum pressure was maintained constant and measured by a pressure gauge directly attached to the pump. Permeate was collected by a receiving container under vacuum condition. The time of permeate collection was expected to be non-linear and may vary in each trial.

3.5.3 Procedures in Assembling the Microfiltration Set-up All materials and equipment should be sanitized by the prescribed procedures. It will be followed by air-drying at ambient conditions to avoid microbial contamination. The sanitized ceramic filter will be inserted intact in the ceramic filter casing. Any small holes and misfittings will affect the efficiency of the membrane. To be able to put the membrane intact, rubber fittings should be used wrapped in Teflon tape to avoid any pressure that may interfere with the performance of the pump. The filter casing should be tightly closed after placing the ceramic filter inside. Connect the suction pump to the receiving flask using clean rubber tubes. The flask is at vacuum condition. Teflon tape should be wrapped on the mouth of the container to avoid any pressure interference. By using clean rubber tubes, connect the different equipments by following the set-up shown below in Figure 3.3. To assure that there will be no pressure interference in every tube connections, wrap every end-point of the tubes using Teflon tape. The set-up is dead-end filtration. The efficiency of the filter will be affected by any pressure interference.

Figure 3.3 Schematic diagram of the dead-end microfiltration set-up

3.5.4 Water Flux Determination The deionized water flux was measured after conditioning the clean membrane to establish the baseline of operation. The water flux was determined by measuring the volume of permeate obtained for 20 minutes. All the experiments were performed under ambient temperature and the volume of the deionized water in the feed container was kept constant to a steady state flow. The resistance to permeation was

obtained based on the measured clean flux, and from this membrane resistance will be calculated. 3.5.5 Coconut water microfiltration The feed was microfiltered under a constant suction pressure of 21 inHg on each trial using 0.3-0.9 m pore size ceramic membrane. Discharge flow rates were gathered every 250 mL permeate collected using a receiving flask under vacuum condition. Time was also noted in every 250 mL increment of discharge permeate. Time was expected to vary in every trial because of membrane fouling.

3.6 Flux Analysis

For this experiment, time was expected to vary in every trial of filtration because of membrane fouling. Determination of time when the membrane will be fouled will be predicted. If the fouling time will be determined, another parameter will be considered, the back-pulsing or the back wash time. The performance of the ceramic membrane will also be evaluated if it is applicable for beverage specifically the coconut water.

3.7 Cleaning Contaminants such as those that foul the membranes can be removed with proper cleaning of the equipment. To avoid contamination it is required to clean the system after conducting the experiment. It was carried out in three steps, which typically include the running of water, caustic solution and then acid. Fouling on the membrane

surface needs to be removed as effectively as possible after the run. Membrane cleaning is necessary to keep the membranes in a good condition. Membrane cleaning is most effective when proper cleaning solution will be applied. High temperature cleaning solutions will shorten the efficiency and life of the membrane (Global Membranes, 2012). The alkali cleaning has a molarity of 0.1 NaOH solution and the acid cleaning by 1% (v/v) sulfuric acid solution. Both solutions used for cleaning were run in the filtration apparatus for 20 minutes at ambient condition and then rinsed with deionized water.