[1] Introduction Diffusion is the process by which molecules, ions, or other small particles spontaneously mix, moving from

the regions of relatively high concentration into regions of lower concentration. This process can be analyzed in two ways. First, it can be described with Ficks law and a diffusion coefficient, a fundamental and scientific description used in the first two parts of this book. Second, it can be explained in terms of a mass transfer coefficient, an approximate engineering idea that often gives a simpler description. Analyzing diffusion with mass transfer coefficient requires assuming that changes in concentration are limited to that small part of the systems volume near its boundaries. For example, in the absorption of one gas into a liquid, it is assumed that gases and liquids are well mixed, except near the gas-liquid interface. Such an analysis is sometimes called a lumped-parameter model to distinguish it from the distributedparameter model using diffusion coefficients. Both models are much simpler for dilute solutions (Cussler, 2007). The definition of mass transfer is based on empirical arguments like those used in developing Ficks law. Imagine we are interested in the transfer of mass from some interface into a well-mixed solution. The mass transfer flux is proportional to the concentration difference, N1=k(C1i-C1) [1]

where k is called the mass transfer coefficient, A is the area of the interface, N1 is the flux at the interface, C1i and C1 are the concentration at the interface and the bulk solution, respectively. The flux N1 includes both diffusion and convection. The concentration C1 is at the interface but in the same fluid as the bulk concentration C1. It is often in equilibrium with the concentration across the interface in a second, adjacent phase. The physical meaning of the mass transfer coefficient is clear: it is the rate constant for moving one species from the boundary into the bulk of the phase. A large value of k implies fast mass transfer coefficient, and a small one means slow mass transfer (Cussler, 2007). Gas absorption is a unit operation in which soluble components of a gas mixture are dissolved in a liquid (Perry, et al, 1997). Most gas absorption aims at separation of acidic
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impurities from mixed gas streams. These acidic impurities include carbon dioxide (CO2), hydrogen sulfide (H2S), sulfur dioxide (SO2), and organic sulfur compounds. The most important of these are CO2 and H2S, which occur at concentration of five to fifty percent. Gas absorption at an industrial scale is most commonly practiced in packed towers. A packed tower is essentially a piece of pipe set on its end and filled with inert material or tower packing. Liquid poured into the top of the tower trickles down through the packing; gas pumped into the bottom of the tower flows counter currently upward. The intimate contact between gas and liquid achieved in this way effects the gas absorption. In the absorption of dilute gases in a packed tower, the important equations relating the characteristics of the packed tower (i.e. tower height, diameter, etc.) and the overall mass transfer coefficient of the liquid phase, Ky and of the gas phase, Kx are:
Ky=Gza11-mGL lny1-mx1y2-mx2

[2]

Kx=Lza11-LmGlnx1-y1mx2-y2m

[3]

where the subscripts 1 and 2 refer to the bottom and top of the tower, respectively; G and L are the molar flux of the gas and liquid phase, respectively; z is the height of the packed tower, a is the specific area of the packing material, x and y are the mole fractions of liquid and gas, respectively and m is the Henrys law constant divided by the total pressure (Cussler, 2007). The mass transfer is dominated by either the liquid phase overall-mass transfer coefficient, Kx or the gas phase overall-mass transfer coefficient, Ky whichever of the two has the greater value. [2] Objectives of the experiment

To determine the mass transfer coefficient for the absorption of CO 2 in the water in a packed column To carry out a mass balance over the packed absorption column
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[3] Methodology
[3.1]Materials

1 pc. 2L plastic graduated cylinder 2 pcs. 100mL graduated cylinder 0.029N NaOH 1.0N NaOH 0.1N NaHCO3 Phenolphthalein indicator 4 pcs. Erlenmeyer flasks Stop watch Base burette

[3.1]Equipment and apparatus

Packed absorption column CO2 Gas cylinder

[3.1]Procedure

Preliminary preparation Before the start of the first part of the experiment, the air and CO 2 flow control valves and the sampling cocks were closed. The sump tank was then filled with about 25-30L of distilled water and the temperature of distilled water in the sump tank was measured. The absorption globe in the HEMPL apparatus which was used in the analysis of the mole fraction of the CO2 present in the air stream was filled with 1N NaOH. Three gas samples were analyzed, using the HEMPL apparatus, before the experiment started to take into the account the CO2 initially present in air. The analyses of CO2 absorbed
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in the water stream were done through titration of the liquid samples with 0.029N NaOH. To visualize clearly the endpoint of titration, a reference sample was made by mixing 100mL NaHCO3 with 3 drops of phenolphthalein. This was done with 2 trials. Three 100mL samples of the liquid in a sump tank were taken before the experiment started and were titrated each with 0.029N NaOH with phenolphthalein as the endpoint indicator and the result gave the concentration of CO2 that was initially present in the sump tank. Absorption of CO2 in water (part 1) The air compressor and water pump switches were turned on and their flow rates were set to 30L/min and 3L/min, respectively. The working pressure of the CO2 cylinder was adjusted to 1 bar and then the flow controller of the CO 2 gas were then adjusted to 1.5L/min. The time when the CO2 was adjusted to its specified flow rate was the start time of the experiment. 100mL samples of the liquid were collected at 5 minute intervals alternately from the sump tank and from the down coming tube for 50 minutes. The amount of CO2 absorbed in the water was analyzed by titrating each of the samples with 0.029N NaOH. The gas samples were also taken simultaneously with the liquid samples at 5 minute intervals for 50 minutes and the CO2 absorbed in the gas was analyzed in the HEMPL apparatus. After 50 minutes, the CO2 flow controller was closed and the air and water flow rate were adjusted to 30 and 5 L/min, respectively. This was done for 20 minutes to remove most of the CO2 absorbed in the water in the first part of the experiment. Absorption of CO2 in water (part 2) The sump tank was added with 8L of distilled water. Afterwards, three liquid samples were taken and were analyzed to determine the initial concentration of the CO2 in the sump tank. The air and water flow rates were then set to 30 and 5 L/min, respectively. The CO2 flow was then set to 1.5
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L/min and this marked the start time of the second experiment, air and water samples were taken simultaneously at 5 minute intervals for 50 minutes. The 100mL water samples were taken alternately from the sump tank and from the down coming tube every 5 minutes. The concentration of CO2 absorbed in the water was analyzed by titration of each sample with 0.029N NaOH. The CO2 in the air stream was analyzed using HEMPL apparatus. After 50 minutes, the CO2 flow rate was set to zero and the CO2 gas cylinder was closed-the working pressure is set back to zero. Then the air and water flow rates were set back to zero and air compressor and the pump are switched off. Lastly, the distilled water in the sump tank was drained.

[4.] Results and Discussions

Figure 1. Plot of the outlet air stream mole fraction of CO 2 with respect to time (air=30L/min, CO2=1.5L/min and H2O=3L/min)

Figure 2. Plot of the inlet (x2) and outlet (x1) liquid stream mole fraction of CO2 with respect to time (air=30L/min, CO2=1.5L/min and H2O=3L/min)

In the experiment, the mole fractions of the outgoing gas phase and incoming (sump tank) and outgoing liquid phase (downcoming tube) were measured with respect to time. This was done in order to obtain a steady state value in which we could base our calculations for the overall mass transfer coefficients. The mole fractions of CO2 in the outlet gas stream were analyzed in the HEMPL apparatus. The HEMPL apparatus made use of Amagats law which states that the volume fraction of CO2 in the gas mixture is equal to the mole fraction of the CO2 in that mixture. The mole fractions of CO2 in the inlet and outlet streams were measured by taking water samples in the sump tank (the tank is assumed to be ideally mixed) and the downcoming tube, respectively. Figure 1 shows the variation of the mole fraction of CO2 in the outlet gas stream with volumetric flowrate of 30L/min of air, 1.5 of CO2, and 3L/min of water flowrate, respectively. As shown in figure 1, the mole fraction of CO2 in the outlet gas stream increased from time zero to about 30 minutes from the start of the experiment and reached a constant value at about 40 minutes. The water in the sump tank is initially unsaturated with CO2. As more CO2 is being absorbed in the liquid phase, the capacity of
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water to dissolve CO2 decreases and it eventually becomes saturated. Thus, the graph in figure 1 reaches a constant value of the CO2 mole fraction at time equal to 40 minutes. Figure 2 shows the mole fractions of CO2 in the inlet and outlet water streams as a function of time. It shows that the mole fraction of CO2 in the inlet and outlet liquid streams increases at the start of the absorption of CO 2 and approaches a steady state value when the liquid is already saturated with CO2.

Figure 3. Plot of the outlet air stream mole fraction of CO 2 with respect to time (air=30L/min, CO2=1.5L/min and H2O=5L/min)

Figure 4. Plot of the inlet (x2) and outlet (x1) liquid stream mole fraction of CO2 with respect to time (air=30L/min, CO2=1.5L/min and H2O=5L/min)

As shown in Figure 3, the steady state mole fraction of CO2 in the second part of the experiment is slightly greater than the first part of the experiment (also see Table 2). This indicates that the removal of CO2 prior to the start of part 2 of the experiment was not effective. There is no significant difference in the mole fraction of CO2 that is absorbed in the liquid in part 1 (H2O=3L/min) and part 2 (H2O=5L/min) of the experiment (see Table 2).

Table 1. The volumetric flow rates of water, air, and CO2 and their corresponding Reynolds number in a packed bed absorption column.
Flowrates H2O CO2 + air L/min 3 5 31.5 m3/s 0.00005 8.33E-05 0.000525 Nre=Dpv'/(1-) 85066 141777 49071

Table 2. The calculated overall mass transfer coefficients for the absorption of CO 2 in a packed column.
overall mass transfer coefficient Experim ent 1 2
air=30L/min)

x1 0.0001 9 0.0001 9

x2 0.0001 5 0.0001 5

y1 0.0485 3 0.0485 3

y2 0.025 0.026

Kx 0.000289 5 0.000576 3

Ky -0.0000001699 -0.0000003382

Note: Expt 1 (H2O=3L/min, CO2=1.5L/min, air=30L/min); Expt 2 (H2O=5L/min, CO2=1.5L/min,

In calculating for the overall mass transfer coefficients, we used equations 2 and 3 for the absorption of dilute vapour in the liquid phase since the concentration of CO2 in the incoming gas stream is relatively dilute (see Table 2). The equation also makes use of the moles of CO2 in the gas phase at equilibrium aside from the actual number of moles of CO2 in the gas phase. In finding the number of moles of CO2 at equilibrium, Henrys constant is used (H=1682 atm, m=1704.28 at 1 bar and 27C). The flow of water becomes even more turbulent when the flow rate was increased from 3 to 5 L/min as shown in Table 1. Table 2 shows that the liquid-side overall mass transfer coefficient, Kx is relatively greater than the gas phase overall mass transfer coefficient, Ky. This indicates that the absorption of CO2 in water is dominated by the liquid-side resistance. Table 2 also shows that the overall mass transfer coefficients, Kx and Ky, increase when the flow rate of water is increased because the thickness of the
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boundary layer is decreased in the process of increasing the turbulence of the flow of water. The mass transfer of CO2 across the boundary layer between the gas and liquid phase increases when the thickness of the boundary layer decreases. As a consequence, the moles of CO2 in the liquid phase increases about twice as much when the water flow rate is increases from H2O=3L/min to H2O=5L/min keeping both flow rates of air and CO2 constant (see Table 3). Most of the values of mass transfer coefficient in literature have positive values but our data in Ky has a negative value which is quite strange. Ky is calculated using equation 2.

Table 3. The mass balance over the packed column.

Overall Mass Balance % Experim ent 1 2 moles of CO2 lost in the gas stream 0.07152 0.06848 moles of CO2 absorbed by water 0.02613 0.04626 differe nce 63.46 32.44

The mass balance is taken over the whole packed column. Because the concentration of CO2 in the inlet air stream is relatively dilute, the molar flux of the air and the molar flux of water are constant over the length of the column. By taking a solute mole balance on both liquid and gas, we arrived at this equation: L(x1-x2) = G(y1-y2) [4]

The subscripts 1 and 2 refer to the bottom and top portion of the absorption column. Equation 4 means that the amount of CO2 lost in the gas phase must be equal to the amount of CO2 absorbed by the liquid phase. Table 3 shows that the mole fraction of the CO2 absorbed in water does not equal with the moles of CO2 lost from the gas stream. The % difference of the moles of CO2 lost in the gas stream and absorbed in the liquid of both experiments 1 and 2 are relatively high.
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The inequality of the moles of CO2 lost in the gas phase and the moles of CO2 absorbed in the liquid phase is attributed to the 10% accuracy inherent to the method of analysis in the determination of the concentration of CO2 in the liquid phase. [5] Conclusion The liquid phase and gas phase mass transfer coefficients for the absorption of CO2 in water are Kx= 0.2895 mol/m2.s, Ky= -1.669 x 10-4 mol/m2.s, respectively at H2O=3L/min, CO2=1.5L/min, air=30L/min and Kx= 0.5763 mol/m2.s and Ky= -3.382 x 10-4 mol/m2.s, respectively at H2O=5L/min, CO2=1.5L/min, air=30L/min. The number of moles of CO2 absorbed in the liquid phase is not equal to the number of moles of CO2 lost in the liquid phase due to the 10% accuracy inherent of the method of analysis of CO2 in the liquid phase.

[6] References Geankoplis, C.J. (2003) Transport Processes and Unit Operations, 4th Edition, Prentice Hall, New Jersey. Cussler, E.L. (2007) Diffusion: Mass Transfer in Fluid Systems, 3rd Edition, Cambridge University Press, New York. Perry, R.H.et Al. (1997) Perrys Chemical Engineers Handbook, 7th Edition, McGraw Hill, Inc.,New York.

[7.] Appendices
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(Please see attached pages)

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