ULTRAFILTRATION (UF) MEMBRANE RETENTION (Short Report)

Student Name Nur Fathinatul Akmal Binti Saharudin Group Members Tan Xiang Yi Chong Pin Jia

School of Engineering Taylors University Malaysia 8th October 2012

Date of Experiment:8th Oct. Report due date: 15th Oct Report submission date: 15th Oct. Checked by: Dr. Rajesh Item/marks Format/10 Abstract and Introduction/10 Figures and Diagrams/15 Materials and Method/10 Results Discussions/45 References/10 Total

Table of Contents
1.0 INTRODUCTION..............................................................................................................................................4 2.0 Experiment design..............................................................................................................................................6 3.0 RESULTS ..........................................................................................................................................................8 DISCUSSION........................................................................................................................................................11 CONCLUSIONS AND RECOMMENDATIONS.................................................................................................12 REFERENCE.........................................................................................................................................................13

ABSTRACT This Ultrafiltration Membrane Retention experiment is carried out to determine the values of ultrafiltration membrane resistance (Rm), membrane retention (R) and permeate flux (J) for ultrafiltration process of Bovine Serum Albumin (BSA) protein solution. 1.0 INTRODUCTION Membrane filtration processes are defined as separations, based primarily on size differences, between two or more components in the liquid phase. Their spectrum ranges from the millimeter (for coarse filters) to the Angstrom () scale (for reverse osmosis and gas separation membranes). The membrane in this case, acts as a selective barrier (an interface) that permits passage of certain components and retains others. The main criterion for separation is size, although other factors, such as surface charge, or shape of the molecule or particle may have an effect. The material that passes through the membrane is the permeate stream, which is depleted with respect to the retained components. The fraction that is retained by the membrane is known as the concentrate or, more correctly, the retentate stream, which is enriched in the non-permeable components. The major pressure driven membrane separation processes are microfiltration (MF), ultrafiltration (UF), nanofiltration (NF) and reverse osmosis (RO). There are no precisely defined boundaries between them, conceptually they are similar to each other, the distinction between them being their degree of semi-permeability and consequently their separation characteristics . [1] Ultrafiltration membranes are usually anisotropic structures made by the Loeb Sourirajan process. They have finely porous surface layer or skin supported on much more open micro porous substrate. The finely porous surface layer performs the separation; the micro porous substrate provides mechanical strength. [2] The mode of operation used in this experiment is dead-end flow.
Feed + Pressure

Filter Filtrate

Figure 1.Dead End Flow Ultrafiltration

However, filtration performance is often limited due to a few resistances such as concentration polarization, formation of a cake at the membrane surface and also hydraulic membrane resistance, Rm. it is a constant which characterizes membrane property and does not depend on the feed composition or the applied pressure. [3] The permeate flux J, passing through the membrane can be described by equation: J = LpP ----------------- Equation 1 Where, is the hydraulic membrane permeability. is the trans-membrane pressure. The value of Where, is the viscosity of water (Cp) Rm is the membrane resistance Retention in ultrafiltration can be calculated from equation: --------------------- Equation 3 Where, is the concentrations in the bulk feed is the concentrations in the permeate can be found by equation: Lp = 1/(Rm) ------------ Equation 2

2.0 EXPERIMENT DESIGN

Figure 2. Ultrafiltration experiment setup 2.1. Materials Materials and Apparatus 1. Ultrafiltration membrane sheet (14650-47-D, Satorius Germany) 2. Bovine Serum Albumin (BSA)
3.

Ultrafiltration apparatus

4. Stopwatch 5. Clean couvette cells 6. UV-spectrophotometer 7. Lowry protein assay kit

2.2. Methods The absorbance values of different concentrations of BSA are measured by using spectrophotometer. The value of membrane resistance is measured first by the ultrafiltration of distilled water. Then the permeate flux J is obtained by measuring the volumetric flow rate of permeate from BSA ultrafiltration. The values of the retention of the protein are then calculated by using equation 3.

2.3. Procedure 1. Membrane Resistance Measurement (Rm)

i. ii.

The ultrafiltration membrane disc are cleaned and rinsed with distilled water. The ultrafiltration membrane disc is inserted on the membrane housing to prepare the apparatus for distilled water flux. 200 ml distilled water is fed into the ultrafiltration and the feed port is fastened. The pressure is set to 1 bar and the permeate volume for each 10 minute is recorded. The experiment is repeated for different pressures (2, 3, 4 and 6 bars).

iii. iv.

v.

2. Permeate Flux
i. ii.

A solution of 100ppm of Bovine Serum Albumin (BSA) is prepared. The prepared solution is fed into the filtration apparatus and the feed port is fastened. The pressure is set to 1 bar and the permeate volume for each 1 minute is recorded. The experiment is repeated for different pressures (2, 3, 4 and 6 bars).

iii.

iv.

3. BSA standard curve i. ii.

iii.

Five solution of BSA is prepared by containing 400, 300, 200, 100 and 0 ml of BSA into test tubes. The 300, 200, 100 and 0 ml samples are then top up with distilled water to make 400 ml solution. 400 l of solution B is then mix with 200 l of solution C, vortex. Then 2 ml of the mixed solution is then added into each tube. The solution is then mixed and allowed to settle for 10 minutes at room temperature. After 10 minutes, 400l of folin solution is added to each of the test tube and the solution is allowed to settle for another 30 minutes. The absorbance vale for each tube is measured at 750nm using spectrophotometer. The BSA standard curve is then plotted for absorbance against concentration.

iv.

v.
vi.

vii.

3.0 RESULTS 3.1. The tabulation of data Table 1: BSA standard curve (calibration data) Sample
Volume of BSA (l) Volume of Distilled water (l) 400 350 300 250 200 Absorbance (OD) 0.026 0.055 0.079 0.107 0.135 Concentration (ppm) 0 12.5 25 37.5 50

1 2 3 4 5

0 50 100 150 200

Table 2.The flowrate of distilled water at different pressure

Pressure (bar) 1 2 3 4 6

Time (min) 10 10 10 10 10

Time (sec) 600 600 600 600 600

Volume of water out (m3) 2.30E-05 2.90E-05 3.50E-05 4.10E-05 5.20E-05

Volumetric flow rate (m3/sec) 3.833E-08 4.833E-08 5.833E-08 6.833E-08 8.667E-08

Flux (m/s)

2.21E-05 2.78E-05 3.36E-05 3.94E-05 4.99E-05

Table 3.The flowrate of BSA solution at different pressure Pressure (bar) 1 2 3 4 6 Pressure (bar) Time (sec) 600 600 600 600 600 Volume of BSA (m3) Volumetric Flowrate (m3/sec) Flux (m/s) Absorbance after filtration (OD) 0.219 0.296 0.232 0.209 0.18

1.15E-05 1.91667E-08 1.1043E-05 1.00E-05 1.66667E-08 9.60259E-06 1.10E-05 1.83333E-08 1.05628E-05 1.20E-05 2.00E-08 1.15231E-05 1.55E-05 2.58333E-08 1.4884E-05 Table 4.The table of data for permeate of BSA Absorbance value of permeate (OD) Permeate concentration (ppm)

Flux (m/s)

Retention

1 2 3 4 6

1.1043E-05 9.60259E-06 1.05628E-05 1.15231E-05 1.4884E-05

0.219 0.296 0.232 0.209 0.18

87.55 122.55 93.45 83.00 69.82

0.12 -0.23 0.07 0.17 0.30

Table 5: The values of membrane resistance Pressure (bar) 1 2 3 4 6 3.2. Graph Figure 3.The graph of concentration against absorbance of BSA Volumetric Flowrate (ml/min) 2.3 2.9 3.5 4.1 5.2 Flux (L/hm2) 79.50944483 100.2510391 120.9926334 141.7342277 179.760484 Membrane Resistance (1/m) 0.012577122 0.019949918 0.024794898 0.028221835 0.033377747

Figure 4.The graph of permeate flux of distilled water against pressure

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Figure 5.The graph of permeate flux of BSA against pressure

3.3 Calculation Useful data: Area of ultrafiltration membrane = Viscosity of water @25C = 1 cP Water flux @ 4 bar = 0.2 mL/min/cm2 = 120 (L/hm2) Ultrafiltration Membrane Resistance @ 4 bar = 0.03333 m-1 J = P/(Rm) Experimental Rm @4bar = 0.0282 m-1 Percentage error = (0.03333-0.0282)/0.03333*100 = 15.39 % = 0.001735643 m2

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DISCUSSION The membrane resistance obtained from this experiment at 4 bar is 0.0282 m-1 while the theoretical value is 0.03333 m-1 with percentage error of 15.39 %. There are few factors that contributed to this error. The ultrafiltration membrane used for the experiment might contain trapped particle inside it due to improper cleaning. The pressure gauge used in this experiment also is not consistent throughout of the experiment and has lower sensitivity. From Figure 4, during ultrafiltration of distilled water, it is shown that the permeate flux is increases when the pressure is increases. However, in Figure 5, it is shown that the flux decreases at first but after pressure at 2 bar, the flux of permeate started increases as the pressure increases. From literature point of view, it might be expected that permeate flux would increase with increasing pressure difference and this is indeed the case until a critical pressure is reached at which the flux levels out. Also, at any given transmembrane pressure, the flux decreases with time of operation. These decreases begin immediately and the flux can fall to 59% of the original value. Three mechanisms may be responsible for these phenomena: fouling, compaction and concentration polarization. Fouling is characterized by an irreversible decline in permeate flux due to the accumulation of macromolecular particles on the membrane surface of the crystallization of smaller solutes within the pores of the membrane. [4] Concentration polarization or external fouling is a phenomenon in which a higher concentration of particle or molecules is retained on membrane surface compared to that of the bulk of the feed stream. Concentration polarization is the result of the separation function of the membrane, and hence cannot be prevented completely. This phenomenon has a very important influence on the economy of the process because it lowers permeate flux and results in an interaction between retained components and the membrane which leads to pore blocking of the membrane. [5] Fouling which refers to the adsorption and deposition of feed components on and within the membrane is the main reason for decrease in permeate flux and hence productivity in an ultrafiltration process. In some cases, fouling can adversely affect product quality. For a given membrane feed system, fouling is influenced by concentration polarization, the more severe the concentration polarization, the more severe is the fouling. Hence, controlling concentration polarization helps in reducing fouling. Concentration polarization and subsequent fouling can be reduced by improving the hydrodynamic conditions near the membrane surface. Various techniques, such as use of pulsatile flow, generation of secondary flow (e.g. Dean and Taylors vortices), feed flow

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obstruction using helical inserts and baffles and the use of corrugated membrane surfaces have been shown to be effective at promoting local mixing near the membrane. The consequence of membrane fouling is a reduction of permeate production rate and an increase in solute passage across the membrane with time. Fouling also causes increase in energy consumption as transmembrane pressure can increase substantially due to fouling, increases downtime and may shorten membrane lifespan. [6] Membranes represent a significant part of a plant costs, thus, maintenance of good membrane performance must be a prime objective of any membrane filtration system. Tactics to control membrane fouling take one of the following approaches: preventing fouling from accuring by pretreating the feed water to remove foulants and promoting conditions at the membrane surface to prevent their deposition, removing fouling by periodic membrane cleaning and manipulation of the filtration mechanism to improve cleaning efficiency. [7] The major advantages of ultrafiltration process over other competing separation techniques are low equipment/ operating costs, high throughput of product, relative case of scale up ease of equipment cleaning/ sanitization, no chemical additives required, no changes in pH and ionic strength and advantage in operation at ambient temperature. In this ultrafiltration experiment, the tubular module equipment is being used. This tubular module has several advantages in ultrafiltration process and often used for small scale and high value applications. The tubular moduls is often chosen for cases involving severe fouling because this structure can be easily cleaned mechanically. Nowadays, most MF/UF plants operate in dead-end filtration mode, as the energy required is lower compared to cross-flow systems, as the high cross-flow velocity required to prevent fouling results in increased head loss and energy consumption. [8]

CONCLUSIONS AND RECOMMENDATIONS In conclusion, the value of the membrane resistance for this ultrafiltration experiment is 0.0282 m-1. The permeate flux and concentration at different pressure are not increasing or decreasing consistently due to membrane fouling, membrane resistance and concentration polarization. There are few things that can be done to improve this experiment. The membrane used in this experiment should be cleaned every time the experiment is repeated. This step is to ensure there is no build up or particles that trapped in the membrane pore. This experiment should be repeated at least 2 times in order to get more accurate results and increases the chance of yielding a better result.

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REFERENCE [1] Trevor J. Britz, Advanced Dairy Science and Technology, Blackwell Publishing Ltd (2008). [2] Richard B, Membrane Technology and Applications, 3rd Edition, John Wiley and Sons Ltd (2012). [3] Marcel Mulder, Basic Principles of Membrane Technology, 2nd edition, Kluver Academic Publishers, (1996). [4] Smith P.G., Introduction to Food Process Engineering, 2nd edition, Springer Science+Business Media, LLC (2011). [5] Kaushik N., Membrane Separation Processes, Prentice Hall (2008). [6] Nazih K. S., Membrane and Desalination Technologies, Springer Science+Business Media, LLC (2011). [7] Siobhan Francesca E. B., Scaling and Particulate Fouling in Membrane Filtration Systems, Swets & Zeitlinger Publishers (2001). [8] Sanjay K. S, Handbook on Applications of Ultrasound Sonochemistry for Sustainability, CRC Press Taylor & Francis Group (2012).