Chapter 3 RESEARCH METHODOLOGY

This section of the report presents the materials and experimental procedures used, as well as the data analysis employed, during the course of the study.

Research Settings The experiments for the determination of the characteristics of CHF as an ion exchange media and the experiments for the determination of the design variables for the CHF ion exchanger unit in this study were conducted in the Chemical Engineering Unit Operations (ChE-UO) Laboratory of Xavier University- Ateneo de Cagayan from June of 2007 to February of 2008.

Sampling Procedure The coconut husks fibers used of this study were obtained from a furniture stall located in Gusa, Cagayan de Oro City. The purchased husks have already been crushed supposedly for furniture use. Coconut husk fibers employed in the experiments were prepared using the following steps: (1) Manual separation of the CHF from the coconut shell, (2) Prewashing with tap water, (3) Washing with brine, (4) Post-washing with distilled/deionized water, (5) Oven drying, and (6) Size reduction. The study used two kinds of water, deionized and distilled water. The deionized water was prepared using Barnstead/ Thermolyne deionizer and the distilled water was purchased outside of Xavier University.

15 Methods of Data Collection The objectives of this study are (1) to determine the characteristics of CHF and its ability to remove water hardness, (2) to describe the kinetic behavior of coconut husk fiber in the softening process, and (3) to describe the comparability of the designed CHFIE to commercial ion exchangers. Thus, the entire procedure has consisted of three phases.

I.

Properties and Characteristics of CHF as Cation Exchanger A. Solids Content: ASTM Standard Test D4456-99 Coconut husk fibers contain some amount of water in them. However, CHF will be sold, used, and its capacity be expressed on a dry-weight basis. Thus, it is important that the actual solids content of the resin be determined. This test method covered the determination of the moisture content in CHF through the determination of the loss of mass at 104.62 oC for 18 hours. Important to note is that CHF is subject is thermal degradation under the conditions of this test. Therefore, volatile degradation products are released along with moisture, resulting in a negative error (Full text of this standard test is provided in the Appendix). B. Isotherm Tests The single-solute isotherm tests are based on batch processes; CHF and solution are mixed in a batch container, the exchange of ions is allowed to come to equilibrium, then CHF is separated from the solution. The degree to which the exchange takes place is limited by the preference the CHF exhibits for the ion in the solution.

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Figure 1. Isotherm Test Experimental Set-up

The tests consisted of exposing 1 g of CHF to 50 mL of increasingly higher concentrations of the single metal hardness (Ca2+ concentration range: 0 – 200 mg/L) and allowing the contact to continue for at least 3 days such that equilibrium was reached between the CHF and the solution. The results of these tests were used to calculate the adsorption isotherms, including the solid phase concentration, for each media and to predict the CHF’s ion exchange capacity for Ca2+, assuming that equilibrium occurred.

II.

Kinetic Behavior of Coconut Husk Fiber A. Sorption- Kinetics Tests Sorption-kinetics test had been performed using a soda-lime glass batch reactor. This is to determine the required contact time between the CHF cation exchanger and the raw water. Results from this experiment will also be used to predict the breakthrough time of coconut husk fiber beds, which

17 value will be verified in the Breakthrough Test. The single-solute kinetics experiments consisted of exposing 10 g of CHF to 1 L of 100 mg/L calcium carbonate solution for different increments of time (0 minutes to 30 minutes). The data from these tests were also used to determine rate constants for the rate of the exchange of ions.

B. Breakthrough Test The test has consisted of filtering prepared solutions of hard water through CHF and testing of the effluent for calcium and magnesium. The filtration column used in this experiment was a 500-mL, graduated buret with inner diameter approximately equal to 38 mm. The CHF-filtration column was constructed first by cutting a piece of medical gauze, purchased at a local pharmacy, into a 5 cm x 5 cm square. This gauze was folded two times and placed in the bottom of the buret. Approximately fifteen centimeters of 2-mm diameter sand was poured on top of the gauze and the column was then rinsed with one hundred milliliters of deionized water. After the sand layer had drained, approximately thirty centimeters of CHF were added to the column on top of the sand underlayer. After the CHF had been added, the filter was then rinsed with brine and then with deionized water. The effluent water was then collected at the bottom and its hardness was determined. If the effluent is found to contain hardness, the column is rinsed again with brine and then with distilled water. The process continued until the effluent water contained little or no hardness. The column was now then ready for the breakthrough test.

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Figure 2. Breakthrough Test Experimental Set-up

III.

Comparability of CHF to Commercial Ion Exchangers

Performance Performance comparison tests between CHF and a commercial zeolite consisted of testing the effluent water from both media. The test was done by batch and employed equivalent masses and equivalent column-height masses of both media in the conduct of the experiment. One (1) gram of CHF, and 1 gram and 14.9 grams of commercial resin (Purolite® Softening Resin C100EFM) were placed in different Erlenmeyer flasks each containing 150 ml of hard water. A fourth flask containing 150 ml hard

19 water with no adsorbent added was also included to serve as a point of reference for subsequent comparisons. The media were then allowed to come in contact with the test water for about the value of the minimum contact time, which is determined from kinetic experiment. The media were then filtered out and the effluent water was tested using different analytical procedures presented in Table 3.

Raw Water

1 g Resin

1 g CHF

14.9 g Resin

Figure 3. Color Comparison Test Experimental Set-up

The following are the test done and analytical procedure used to compare the effluent characteristics of CHF to the commercial zeolite.

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Table 3. Analytical Techniques

Analytical Parameter Effluent pH Effluent Color Hardness Removal Capacity

Analysis Method ASTM D1293- 99 EPA Method 110.3 Isotherm Test

A simple cost comparison was then prepared to compare the cost of softening using CHF and synthetic resin as cation exchange media, respectively. Data Analysis The capacity of CHF is the maximum q value that was determined through the plot of the traditional isotherm curve. The isotherm curve is a plot of concentration, C, versus q, where q represents the ratio of the mass of metal ions adsorbed by CHF to the mass of CHF. The capacity was then estimated as the value at which the isotherm curve is approximately horizontal. This was done by first determining the appropriate isotherm for CHF adsorption, which data fit with the linearized equation of the given isotherm. The following are the adsorption isotherms and their corresponding plots, where k is a constant:
Table 4. Data Analysis for Isotherm Test

Adsorption Isotherm

Equation

Linearized Equation

Linear Plot

1. Linear 2. Freudlich

3. Langmuir

21 Linear regression was then used to test which equation fits the data well and to compare the regression coefficient for each isotherm that would determine the appropriate isotherm for the adsorption of ions to CHF. For the adsorption kinetic tests, the equation used in understanding the dynamics of the exchange of ions in CHF ion exchanger came from rate law equation. The rate of disappearance of A+ from the aqueous solution as it is exchanged to the CHF is given in its integrated form as:

where a and b are constants. As with the isotherm test, linear regression will be used in the analysis of data and in the determination of parameters a and b. The linearized equation for the above form is:

The bed depth-service time (BDST) equation was specifically used to determine the service life of the bed in the breakthrough experiments. It is given by the equation:

For the performance comparison, ANOVA was employed to determine if there were significant differences in the values obtained. If it is found that there is at least one inequality, a test on the equality of variances using F-test is then employed. After which, t-test is used to compare the means of the experimental values obtained.

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