1.

0 INTRODUCTION (1-2, 6) Microfiltration is a mechanical process in which the impurities as well as the contaminants (in the form of solid particles) in a fluid, either a gas or a liquid, are removed by allowing the fluid to undergo diffusion through a semi-permeable membrane.

In contrast with dead-end microfiltration, the flow of the feed is parallel to the surface of the semi-permeable membrane in cross-flow microfiltration. As compared to the dead-end microfiltration, cross-flow microfiltration is much preferable among the two main processes of microfiltration while designing a process plant.

In both processes, the continuous build-up of the filter cake layer contributes to the increasing hydraulic resistance experienced by the feed while diffusing across the semi-permeable membrane. However, in cross-flow microfiltration, the build-up of the filter cake layer is limited by the flow of the feed into the system as the solid particles deposited on the semi-permeable membrane are being swept away by the feed flow continuously.

After an initial rapid increase in the thickness of the filter cake layer, as the process progresses, the growth of the filter cake layer ceases and eventually achieves steady state condition. Correspondingly, the volumetric flow rate of the filtrate will therefore remain constant after an initial rapid decrease during the start-up of the process.

On the other hand, for dead-end microfiltration, the continuous build-up of the filter cake layer across the semi-permeable membrane may result in clogging of the system and the filtration process will eventually halt.

One of the major applications of cross-flow microfiltration in the industry nowadays is the clarification of wine. The process of clarification of wine is very important as to remove all the yeast, bacteria as well as grape solids from the wine.

As a matter of fact, wine clarification can be operated in both dead-end and cross-flow microfiltration. However, the advantages offered by the process of crossflow microfiltration weigh out those offered by the process of dead-end microfiltration.

First of all, dead-end microfiltration requires several procedures in order to get to the same clarification level achieved by only one single procedure in crossflow microfiltration. In addition to that, there is also minimal loss of wine in crossflow microfiltration as compared with the dead-end microfiltration.

Unlike dead-end microfiltration, in cross-flow microfiltration, back flushing can be used to maintain a constant throughput as well as to optimize the filtration process. On the other hand, the process of cross-flow microfiltration is preferred for wine processing as the quality and the colour intensity of the wine are easily preserved.

In short, the report presented is to verify the effect of different pump power on the quality of the filtrate by assembling the cross-flow microfiltration unit using QuixStand Benchtop System. A detailed analysis on the background theory of the process of cross-flow microfiltration is presented in Theory and Working Equation section. The experimental procedure is outlined in Materials and Methods section while the findings of the experiment can be found in the Results and Discussion section. Finally, the summary of the major findings of the experiment as well as the recommendation on how to improve the experiment are included in the Conclusions and Recommendation section.

2.0 OBJECTIVE The objectives of the experiment are: 1. To assemble the cross-flow microfiltration unit. 2. To investigate the effect of different pump power on the quality of the filtrate.

3.0 THEORY AND WORKING EQUATION (1, 3-4) In contrast with dead-end microfiltration, the flow of the feed is tangential to the surface of the semi-permeable membrane in cross-flow microfiltration. During the microfiltration process, the continuous growth of the thickness of the filter cake layer results in an increasing hydraulic resistance faced by the feed while diffusing across the semi-permeable membrane. However, in cross-flow microfiltration, the build-up of the filter cake layer is restricted by the flow of the feed into the system as the solid particles deposited on the semi-permeable membrane are being washed away by the feed flow continuously.

After an initial rapid increase in the thickness of the filter cake layer, as time progresses, steady state condition is eventually achieved as the growth of the thickness of the filter cake layer ceases. Respectively, the volumetric flow rate of the filtrate will therefore remain constant after an initial rapid decline during the start-up of the process.

Due to the difference in the particle size of the water molecules and the particles of the green colouring, the smaller water molecules can diffuse through the semi-permeable membrane very easily. On the other hand, some of the particles of the green colouring may not able to diffuse through the semi-permeable membrane while the other particles of the green colouring undergo diffusion through the semipermeable membrane without much resistance as not all the particles of the green colouring having the same particle size.

As a result, the filtrate being collected in the conical flask still preserves a certain intensity of the green colour as not all the particles of the green colouring are being filtered out. As mentioned earlier, the filtrates were going to be collected in the conical flask over a fixed duration of 1 minute. Hence, the volumetric flow rate of the filtrate collected is calculated using the equation as shown below.

Volumetric flow rate, V

Volume of filtrate collected Time taken

(1)

In order to identify the relationship between the quality of the filtrate collected and the pump power, the refractive index of the filtrate collected is measured using a refractometer. The refractometer used in this experiment is very sensitive to small changes in the refractive index and it can measure the refractive index of the sample up to 5 decimal places. Based on Snells Law, the refractive index of a sample is defined as

Refractive index, n

speed of light in vacuum c , speed of light in medium, v

(2)

8 Since the speed of light in vacuum is a constant, which is 3 10 m / s , hence

the refractive index of the sample is said to be inversely proportional to the speed of light in medium.

1 v

(3)

The refractive index obtained in this experiment is being compared to the theoretical refractive index of water, which is 1.33 in value. Thus, the relationship between the refractive index and the quality of the filtrate is deduced.

4.0 MATERIALS AND METHODS 4.1 Equipment and Materials 1. QuixStand Benchtop System 2. Xampler Cartridge 3. Green-coloured solution

4.2 Experimental Procedure a) Initial start-up and adding feed into reservoir 1. The sampling/drain valve was closed. The cartridge was secured in upper and lower manifolds. The pump tubing was ensured to be positioned and tensioned correctly within the pump head. 2. The flexible tubing was confirmed to be connected from the retentate outlet on the upper manifold to one of the tubing barbs on the reservoir cap. A retentate downcomer was ensured to be pressed into the reservoir cap for the retentate line if the process solution were to foam. 3. The flexible tubing was directed from the upper permeate line to a collection flask. 4. The sanitary clamp was removed from the reservoir cap and the reservoir cap was slide to one side. 5. The feed solution was added to the reservoir. 6. The reservoir cap was repositioned on the silicone gasket and was clamped in place using the sanitary clamp. 7. The backpressure tubing valve was open by turning the valve counter clockwise for several turns. 8. A suitable container was prepared to collect the filtrate.

b) Experiment 1. The unit was started by setting the pump speed to 80 rpm. 2. The feed was allowed to run through the unit until the feed entered the cartridge. 3. The stopwatch was started when the filtrate started to flow out and the sample was collected for duration of 1 minute. 4. The experiment was repeated by increasing the pump speed by 80 rpm increment until the maximum pump speed allowed. 5. The volumetric flow rate and refractive index were measured for each sample. The data collected was tabulated.

5.0 RESULTS AND DISCUSSION The experiment was conducted to determine the effect of different pump power on the quality of the filtrate by assembling the cross-flow microfiltration unit using QuixStand Benchtop System. The experimental data collected was tabulated as below.

Table 5.1: Table of volumetric flow rate and refractive index at different pump power Pump power (rpm) 80 160 240 320 400 Volumetric flow rate (10 m/s) 7.333 7.000 7.667 8.333 10.667 Refractive index 1.34220 1.34221 1.34220 1.34218 1.34217

Graph of Volumetric Flow Rate against Pump Power

12.000

Volumetric Flow Rate (10 m/s)

10.000 8.000 6.000 4.000 2.000 0.000 80 160 240 320 400

Pump Power (rpm)

Figure 5.1: Graph of Volumetric Flow Rate against Pump Power

As suggested by the graph above, as the pump power increases, the volumetric flow rate increases as well. The velocity of the feed flowing tangentially to the membrane increases as the feed flows into the system with a much higher velocity, resulting in the self-cleaning process of the system as the layer of larger particles deposited on the membrane being swept away by the feed flow, leaving a relatively thin layer of filter cake behind.

Hence, with the only presence of the thin layer of filter cake, the feed is allowed to diffuse through the membrane without much resistance. Thus, as the volume of the filtrate collected over a fixed duration of 1 minute increases, the volumetric flow rate of the filtrate increases.

Graph of Refractive Index against Pump Power

1.34222

Refractive Index

1.34221 1.34220 1.34219 1.34218 1.34217 1.34216 80 160 240 320 400

Pump Power (rpm)

Figure 5.2: Graph of Refractive Index against Pump Power

Due to some errors occurred during the experiment, the experimental data collected do not coincide with the theoretical data perfectly. However, as shown in the graph above, generally, the refractive index of the filtrate decreases as the pump power increases.

As the pump power increases, the amount of the larger particles deposited on the membrane decreases, forming a relatively thinner layer of the filter cake. Thus, a greater amount of the feed is allowed to diffuse through the membrane without much resistance, resulting in a larger amount of the particles of the green colouring being filtered out.

Based on the observation made using naked eyes, as the amount of impurities in the filtrate decreases, the intensity of the green colour in the filtrate collected decreases, the filtrate therefore appears much clearer as compared to the original feed. Due to the decrease in the amount of the impurities in the filtrate, light is able to pass through the filtrate with a higher velocity, contributing to a lower refractive index of the filtrate.

As compared with the theoretical refractive index of water, which is 1.33 in value, as the intensity of the green colour in the filtrate collected decreases, the clearer the appearance of the filtrate collected, the smaller the difference between the refractive index of the filtrate collected and the water.

There are various factors that may lead to such deviation between the theoretical value and the experimental value. Parallax error is among the vital factors as the position of the eyes was not perpendicular to the scale of the measuring cylinder during the recording of the measurements of the volume of the filtrate collected.

Besides, the duration for collecting the filtrate might not fixed as 1 minute as proposed in the experimental procedure due to the unawareness of the appearance of the first drop of the filtrate being collected in the conical flask.

In addition, due to insufficient time allocated for this particular experiment, the membrane was not fully cleaned during the self-cleaning process of the system, leaving a certain amount of the particles of the green colouring deposited on the membrane, resulting in the mixing of the consecutive feed with the previous one.

On the other hand, improper way of cleaning the refractometer will also affect the measurement of refractive index of the filtrate collected significantly. The filtrate being tested using the refractometer might mix with the previous sample if the refractometer was not rinsed properly before use.

Furthermore, the bubble formed within the sample of the filtrate being tested using the refractometer might as well result in a considerable change in the refractive index of the sample due to the heterogeneous condition of the sample.

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6.0 CONCLUSIONS AND RECOMMENDATION 6.1 Conclusions In conclusion, as determined from the experiment conducted, as the pump power increases, the volumetric flow rate of the filtrate collected increases while the refractive index as well as the intensity of the green colour in the filtrate collected decreases, resulting in a higher quality of the filtrate collected.

6.2 Recommendation There are various recommendations that should be taken account in order to obtain a much more accurate result from this particular experiment. First and foremost, before the initial start-up as well as the repetition of the experiment, make sure that the Xampler cartridge being used is rinsed thoroughly with distilled water to ensure no deposits on the membrane of the Xampler cartridge.

Next, all the instruments, such as the dropper being used to transfer the sample of the filtrate and the measuring cylinder being used to measure the volume of the filtrate collected, should be rinsed properly with distilled water every time before use.

Moreover, during the transfer of the sample of the filtrate from the conical flask to the refractometer, make sure that there is no any bubble formed in the sample. In addition to that, the surface of the refractometer should be wiped clean using dry and clean cloth to ensure that there are no impurities left on it.

Furthermore, while taking the measurement of the volume of the filtrate collected, the position of the eyes should be perpendicular to the scale of the measuring cylinder in order to avoid parallax error.

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7.0 REFERENCES 1. Cross-flow filtration. (18th May 2010). Retrieved on 19

th

from August

http://en.wikipedia.org/wiki/Cross-flow_filtration#Operation 2010

2. Microfiltration.

(31st

July

2010).

Retrieved

from

http://en.wikipedia.org/wiki/Microfiltration on 19th August 2010

3. Refractive

index.

(19th

August

2010).

Retrieved

from

http://en.wikipedia.org/wiki/Refractive_index on 19th August 2010

4. Refractometer.

(22nd

July

2010).

Retrieved

from

http://en.wikipedia.org/wiki/Refractometer on 19th August 2010

5. QuixStand

benchtop

system.

(2006).

Retrieved

from

http://www.gelifesciences.co.jp/catalog/pdf/18116807.pdf on 19th August 2010

6. Wine Clarification & Filtration. (2010). Retrieved from http://www.liquiflux.com/Wine_clarification.cfm on 19th August 2010

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APPENDICES Appendix A Raw Data Table A1: Raw data of volume of filtrate collected and refractive index for different pump power Pump power (rpm) 80 160 240 320 400 Volume of filtrate collected (ml) 4.40 4.20 4.60 5.00 6.40 Refractive index 1.34220 1.34221 1.34220 1.34218 1.34217

Calculations When pump power = 80 rpm, volume of filtrate collected = 4.40ml,

Volumetric flow rate, V

Volume of filtrate collected Time taken

4.40 ml 60 s 7.333 10 8 m 3 / s

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Appendix B (4-5)

Figure B1: QuixStand Benchtop System

Figure B2: Xampler Cartridges

Figure B3: Refractometer

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