MEMBRANE TEST UNIT

ABSTRACT INTRODUCTION AIMS THEORY APPARATUS PROCEDURE RESULTS DISCUSSION CONCLUSION RECOMMENDATIONS REFERENCES APPENDICES 2 3 4 5 9 9 11 12 14 16 17 18

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ABSTRACT
This experiment is conducted to study the characteristics on 4 different types of membranes which are AFC 99 (polyamide film), AFC 40 (polyamide film), CA 202 (cellulose acetate) and FP 100 (PVDF) by using membrane test unit (TR14). Membrane separation is a technology which fractionates materials through pores and minutes of gaps in the molecular arrangement of a continuous structure. Membrane separation can be classified by pore size and by the separation driving force for example Microfiltration (MF), Ultrafiltration (UF), Nanofiltration (NF), Ion-Exchange (IE) and Reverse Osmosis (RO). We need to operate the plunger pump, control the valves, and collect the samples as well as weighing the samples. After weighing the sample, graph of permeates weight versus time is plotted. Based on the graph, membrane 1 and membrane 3 used in membrane process that operates at higher pressure while membrane 2 and membrane 4 used in membrane that operates at lower pressure. Membrane 1 used in reverse osmosis process and membrane 3 is in nanofiltration which both of the tubes in these membranes are fitted with polyamide. The tubes fitted in membrane 2 is polyethersulphone which for ultrafiltration while for membrane 4 is PVDF which for microfiltration. This experiment is conducted successfully.

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INTRODUCTION
This Membrane Test Unit (Model: TR 14) has been designed to demonstrate the technique of membrane separations which has become highly popular as they provide effective separation without the use of heating energy as in distillation processes. This type of membrane is widely used biotechnology and process industry. Heat sensitive materials, such as fruit juices, can be separated or concentrated by virtue of their molecular weights. The unit consists of a test module supplied with four different membranes, namely the reverse osmosis (RO), nanofiltration (NF), ultrafiltration (UF) and microfiltration (MF) membranes, thus allowing students or researchers to carry out membrane separation processes that are most widely used in the food, dairy, pharmaceutical and chemical industries. This self-contained unit on a mobile epoxy coated steel framework, requires only connection to a suitable electricity supply and a normal cold water supply to be fully operational. It consists of a feed tank, a product tank, a feed pump, a pressure regulator, a water bath, and a membrane test module. All parts in contact with the process fluid are stainless steel, PTFE, silicone rubber or nitrile rubber. The unit comes with a high pressure feed pump for delivering the feed to the membrane unit at the desired flow rate and pressure. The retentate line can be either returned to the feed tank or straight to the drain. Appropriate sensors for flow, pressure and temperature are installed at strategic locations for process monitoring and data acquisitions. In this experiment we need to study the characteristic on 4 different types of membranes. The TR 14 unit is supplied with 4 membranes which are: Membrane 1: AFC 99 (polyamide film) Membrane 2: AFC 40 (polyamide film) Membrane 3: CA 202 (cellulose acetate) Membrane 4: FP 100 (PVDF)

The AFC 99 is rated with 99% NaCl rejection at maximum pressure and temperature which is 64 bar and 80 whereas the AFC 40 has 60% CaCl2 rejection at 60 bar and 60 Both of

these membranes use in operation of reverse osmosis. Meanwhile, the CA 202 is rated with apparent retentation of 2000 MWCO and the FP 100 is 100000 MWCO. Both of these two membranes use in ultrafiltration process which CA 202 operates at 25 bars and 30 the FP 100 is at 10 bar and 80 while

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The advantages of cross-flow membrane separations are the concentrate remains in a mobile from suitable for further processing, possible to fractionate solutes of different sizes, can prevent solid buildup on membrane surface so that higher overall liquid removal rate is achieved and solute content of the concentrate ma be varied over a wide range.

AIMS

To study the characteristics of membrane by performing a characteristic study on 4 different types of membranes.

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THEORY
Membrane separation is a technology which fractionates materials through pores and minutes of gaps in the molecular arrangement of a continuous structure. Membrane separation can be classified by pore size and by the separation driving force for example Microfiltration (MF), Ultrafiltration (UF), Nanofiltration (NF), Ion-Exchange (IE) and Reverse Osmosis (RO).

This figure is examples of different substance that correspondence to the pore size of the membrane separation method. Reverse osmosis separates aqueous ionic solutions of different concentration. There is an osmotic pressure when the solvent moves from an area of high water potential to low water potential so that equal ionic concentrations on each side of membranes. When a hydraulic pressure is applied to the concentrated solution which is greater and in reverse to the osmotic pressure, water molecules will pass to dilute solution side through the membrane. This process can separate water from ions and low-molecular weight organic constituents. Ultrafiltration enables precise separation, concentration and purification of dissolved and suspended constituents based on the relative molecular size of substance. Microfiltration membranes enable efficient and precise separation as well as concentration of suspended and colloidal particles.

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REVERSE OSMOSIS

ULTRAFILTRATION

MICROFILTRATION

The membrane separation techniques utilized in the dairy industry serve different purposes:

RO -used for dehydration of whey, UF permeate and condensate. NF -used when partial desalination of whey, UF permeates or retentate is required. UF -typically used for concentration of milk proteins in milk and whey and for protein standardization of milk intended for cheese, yoghurt and some other products.

MF -basically used for reduction of bacteria in skim milk, whey and brine, but also for defatting whey intended for whey protein concentrate (WPC) and for protein fractionation.

Many theoretical models and the identification of new factors controlling flux, J or mass transfer through membranes have been proposed. The build-up of deposited materials on the surface has introduced the terms of hydrodynamic resistance which are the best outlined basic operating patterns.

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The flux J will be given by: J= = = (1) is a variable depending on the applied pressure and time (the

For most biological materials,

compressible deposit), so that the expression requires a numerical solution. A useful method for the effects of cross-flow removal of depositing materials is to write: J= (2)

Removal of solute by cross-flow is sometime assumed constant, and equal to the convective particle transport at steady state which can be obtained experimentally or from an

appropriate model. In many situation however, steady state of filtration is seldom achieve. In such case, it is possible to describe the time dependence of filtration by introducing an efficiency factor, , representing the fraction of filtered material remaining deposit rather than being swept along by the bulk flow. This gives: RC = , where o < <1 (3)

Although deposition also occurs during ultrafiltration, an equally important factor controlling flux is concentration polarization.

a) Applied pressure

b) ln CA

c) ln (cross-flow velocity)

Figure: typical dependence of membrane flux a) applied pressure difference

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b) Solute concentration c) cross-flow velocity Solution containing molecular gel-forming solute will form a gel on the surface of the membrane. The gel formation will contribute to formation of dynamic membranes. The mechanism is as follows; Due to convective flux through the membrane a concentration of the solution at the surface CW increase and eventually reaches a gel formation concentration Cg (figure b) the flux, J through the membrane depends on a concentration according to the relation; J = k ln Combining equation (1) and (4) ln = (5) (4)

As long as concentration Cw is less than Cg, Cw will increase with pressure, but the moment Cw equals to Cg, an increase in bring about an increase of the layer resistance Rp, and the flux will no longer vary with pressure. Assuming no fouling effect, the membrane resistance Rm can be calculate from the flux equation below: J= The slope obtain from the plot of flux J vs be express by the rejection coefficient, R R= Where Cf is final macrosolute concentration in the retentate C0 is initial macrosolute concentration V0 is initial volume Vf is final retentate volume (7) is equals to (6) the retention of any solute can

This expression assumed complete mixing of retentate seldom accomplishes due to concentration polarization. The apparent rejection coefficient depends on factors affecting polarization including UF rate and mixing. For material entirely rejected, the rejection coefficient is 1 (100% rejection); for freely permeable material it is zero.
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Rejection is a function of molecular size and shape. Nominal cut-off levels, defined with model solute, are convenient indicators. Fractional rejection membrane with low MW cut-off spans a narrower range of molecular size than by more open membranes. For maximum retention of a solute, select a membrane with nominal cut-off well below the MW of the species. Many biological macromolecules tend to aggregate so that effective size may be much larger that the native molecule, causing increase rejection. Degree of hydration, counter ions and steric effect can cause molecule with similar molecular weights to exhibit very different retention behaviour.

APPARATUS
The membrane test unit (TR14) Sodium chloride solution

PROCEDURE
General start-up procedures

1. Ensure all valves are initially closed. 2. Prepare a sodium chloride solution by adding 100 gram of sodium chloride into 20 litre of water. 3. Fill up the tank with the salt solution prepared in step 2. The feed shall always be maintained at room temperature. 4. Turn on the power for the control panel. Check that all sensors and indicators are functioning properly. 5. Switch on the thermostat and make sure that the thermo oil is above the coil inside thermostat. Check that the thermostat connections are properly fitted. 6. The unit is now ready for experiments.

General shut-down procedures

1. Switch off the plunger pump (P2).

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2. Close valve V2. 3. Drain all liquid in the feed tank and product tank by opening valves V3 and V4. 4. Flush all the piping with clean water. Close V3 and V4, fill the clean water to feed tank until 90% full. 5. Run the system with the clean water until the feed tank is nearly empty.

Procedures

1. The general start-up is performed. 2. Valves V2, V5, V7, V11 and V15 are opened. 3. The plunger pump (P1) is switched on and valve V5 is slowly closed to set the maximum working pressure at 20 bars. The pressure value at pressure gauge is observed and the pressure regulator is adjusted to 20 bars. 4. Valve V5 is opened. Membrane maximum inlet pressure is set to 18 bars for membrane 1 by adjusting the retentate control valve (V15). 5. The system is allowed to run for 5 minutes. The sample is collected from permeate sampling port and the sample is weighed using digital weighing balance. The weight of permeates every 1 minutes for 10 minutes. 6. Step 1 to 5 for membrane 2, 3 and 4 are repeated. The respective valves are open and close and membrane maximum inlet pressure is adjusted for every membrane. Membrane Open valves (step 2) V2, V5, V7, V11, and V15 V2, V5, V8, V12 and V16 V2, V5, V9, V13 and V17 V2, V5, V10, V14 and V18 Sampling valves Retentate control valve V15 V16 V17 V18 Membrane maximum inlet pressure(bar) 18 12 10 8.5

1 2 3 4

Open V19 and closed V11 Open V20 and closed V12 Open V21 and closed V13 Open V22 and closed V14

7. The graph of permeate versus time is plotted.

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RESULTS
Time (min) 1 2 3 4 5 6 7 8 9 10 Membrane 1 49.21 83.43 117.27 151.59 185.40 221.04 255.55 290.83 327.34 367.77 Weight of permeates (g) Membrane 2 Membrane 3 236.63 265.43 394.11 297.60 465.75 327.29 536.07 357.81 605.49 386.91 676.01 418.09 746.12 448.69 817.00 479.79 889.99 512.76 959.10 539.92

Membrane 4 536.17 768.43 1001.07 1233.24 1465.07 1696.85 1924.43 2153.87 2393.55 2608.04

3000

2500 weight of permeates(g)

2000 Membrane 1 1500 Membrane 2 Membrane 3 1000 Membrane 4

500

0 1 2 3 4 5 6 7 8 9 10

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DISCUSSION

Membrane separation is based on separation mechanisms and size of the separated particles. The membrane processes that have been widely used are microfiltration, ultrafiltration, nanofiltration, reverse osmosis, electrolysis, dialysis, electrodialysis, gas separation, vapour permeation, pervaporation, membrane distillation and membrane contactors. Pervaporation is the only process that involves phase change. All processes except electrodialysis are pressure driven. We conduct this experiment to study the characteristics on 4 different types of membranes which are AFC 99 (polyamide film), AFC 40 (polyamide film), CA 202 (cellulose acetate) and FP 100 (PVDF). From the graph that has been plotted, the slope of the membrane 4 is the steepest compared to other membranes. This followed by membrane 2, membrane 3 and membrane 1 respectively. Based on the graph, membrane 1 is used for reverse osmosis process. This is because the weight of permeates for membrane 1 have the lightest weight. Reverse osmosis operates at very high pressure which is more than 20 bras. Reverse osmosis require the greatest operating pressure as it has the smallest pore-size range and has the ability to remove solids as small as salts. Only small amounts of very low molecular weight solute can pass through the membranes. Membrane 1 is nonporous, asymmetric, and composite with homogeneous layer which has dense pore size. Reverse osmosis is mainly applied in production of pure water. Apart from that, nanofiltration is a type of membrane process that uses membrane 3. This is also same as reverse osmosis that operates at high pressure but not as higher as pressure used in reverse osmosis. The driving force used in nanofiltration is between 4 to 20 bars. Nanofiltration is used for organic, color and contaminant removal as well as for softening. Membrane 3 is also asymmetric, microporous which has pore size between 1 to 5 nm. Main application of nanofiltration is to separate small organic compounds and multivalent ions. Membrane 2 operates in ultrafiltration. Ultrfiltration designates a membrane separation process, driven by a pressure gradient, in which the membrane fractionates components of a liquid as a function of their solvated size and structure. The membrane configuration is usually cross-flow. The feed water flows across the membrane surface by limiting the extent of particle deposition and formation on the membrane surface. The membrane pore size is
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larger allowing some components to pass through the pores with the water. Ultrafiltration operates at lower pressure compared to nanofiltration and reverse osmosis. A type of membrane 3 is asymmetric microporous and the size of pore is 5-100nm. The driving force for this membrane is between 1-9 bars. Nanofiltration is applied in separation of macromolecular solutions. The membrane process for membrane 4 is microfiltration. In microfiltration, the membrane separation process is similar to ultrafiltration but it has larger membrane pore size. Thus, this will allow particles in the range of 0.1 to 10 micrometers to pass through. The pressure used is basically lower than that of ultrafiltration process which is 0.5 to 2 bars. The membrane configuration is usually cross-flow. This membrane is symmetric and asymmetric porous. Microfiltration used in the clarification and sterile filtration.

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Reverse osmosis have been used to remove nitrate from contaminated groundwater as well as remove high concentrations of naturally occurring fluoride from deep groundwater. It is also effective in removing specific synthetic organic contaminates from contaminated groundwaters. Nanofiltration is used as an alternative treatment method to lime softening in order to reduce the level of calcium and magnesium in hard waters. NF also can remove naturally occurring color and dissolved organic species which is responsible for the formation of THMs and DBPs regulated by US EPA. Microfiltration and ultrafiltration can be used for particulate removal to comply with surface water treatment rule. Both of MF and UF can precede by pretreatment systems to precipitate or co-precipitate dissolved inorganic and dissolved organic compound. MF used in separation of bacteria and cells from solution whereas UF used in separation of protein and virus, concentration of oil-in-water emulsions.

CONCLUSION

From this experiment, it can be concluded that membrane 1 is operate in reverse osmosis process while membrane 3 is in nanofiltration process. Both of this membrane process operate at very high pressures and are typically deployed for the removal of dissolved inorganic and organic constituents. Low pressure membrane processes which are microfiltration and ultrafiltration are applied for the removal of particulate and microbial contaminants and can be operated under negative or positive pressure. Membrane 2 and membrane 4 has been used in ultrafitration and microfiltration respectively.

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RECOMMENDATIONS
In this experiment, there are some recommendations that can be done in order to get the best results which are: During taking the weight of permeates by using digital weighing balance, the reading should be taking in more significant figures so that the reading of the actual weight of permeates are more accurate and the value of true error could be minimized. The average weight of permeates should be calculated by taking the weight of permeates in three times in order to get more accurate value of weight of permeates. When collecting the sample from permeates sampling port, make sure that we used a big container to support the volume of the sample and to avoid the sample from spill out in order to get more accurate weight of permeates. The system should be run in more than 5 minutes so that the system and membrane maximum inlet pressure is more stabilized in order to get the accurate value of weight of permeates. To collect the sample, the sampling valves should be open and close simultaneously so that there is no interruption during collecting the sample from permeates sampling port.

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REFERENCES

1. (1986). Dairy Processing Handbook. In Dairy Processing Handbook (p. 125). sweeden: Tetra Pak Processing Systems AB. 2. Eliane Rodrigues dos Santos Goes,Elisabete Scolin. Mendes, Nehemias Curvelo Pereivela, Sueli Teresa Davantel de Barros. (2005). influence at different condition on the concentration by reverse osmosis. Retrieved 9 april, 2012, from Alim.Nutr.Araquara: http://serv-bib.fcfar.unesp.br/seer/index.php/alimentos/article/viewFile/489/452 3. http://www.solution.com.my/pdf/TR14(A4).pdf. (n.d.). membrane test unit. Retrieved 9 april, 2012, from solteq: http://www.solution.com.my/pdf/TR14(A4).pdf 4. membrane separation technology primer. (n.d.). Retrieved 8 april, 2012, from asahi kasei chemicals: http://www.asahi-kasei.co.jp/membrane/microza/en/kiso/index.html 5. nakagawa, o. (2012, february 12). membrane separation. Retrieved april 8, 2012, from wikipedia: http://en.wikipedia.org/wiki/Membrane_technology#Membrane_separation_processes 6. Ripperger S., Schulz G. (1986). Microporous membranes in biotechnical applications. In Bioprocess Engineering (pp. 43-49). 7. Zeman, Leos J., Zydney, Andrew L. (Inc,1996). Microfiltration and Ultrafitration, Principles and Applications. In M. Dekker, Microfiltration and Ultrafitration, Principles and Applications. New York.

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APPENDICES

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