Laboratory of Chemical Engineering II

Laura Alejandra Estupian Ariza, 201313394

Juan Ignacio Crdoba Martnez, 201320329
16/03/2017

PRACTICAL REPORT REVERSE OSMOSIS

ABSTRACT

The application of the case indicates that it is desired to test the new reverse osmosis equipment found in the
laboratory in order to determine the state of the membrane. The tests were made for pressures of 10, 12 and 14
bar taking 4 samples with small flow and 6 with large flow in each of the tests. It was determined that the best
working pressure to completely desalinate the water was 14 bar because the permeate and retenoate
concentrations were the lowest. Furthermore, for all the tests, permeability and membrane resistance values were
calculated, which for the pressure chosen as the best resulted in a value of 41.3158 and 0.9980. finally, the delta
of pressure to be so small was what allowed the procedure in general to yield successful results.

INTRODUCTION

Reverse osmosis is one of the techniques of separation through membranes. In this process, non-liquid (solvent)
of a concentrated solution passes through a semipermeable membrane thus allowing the passage of solvent
molecules and non-solute molecules. This transfer is done up to the pressure that is observed in the difference of
level of both liquids of the sea to stop it. (Hernandez , Tejerina, & Martinez , 1990)

Membranes in general act as selective permeable barriers that allow some sources (such as water) to
permeate through them while retaining other dissolved substances (such as ions). RO offers the finest
filtration available today, recharging most of the discarded and suspended solids, all the time that prevents
the passage of bacteria and viruses, obtaining pure and sterilized water. (Marco, 2010). Waters with a high
sales content such as sodium, calcium, boron, iron, chlorides, sulfates, nitrates and bicarbonates, can be
treated with reverse osmosis until reaching water limits as acceptable for use. (Wankat, 2011)

1. EXPERIMENTAL

Based on Case Study III (see Annex I), the way in which the practice was developed consisted of basically three
parts:

Part I: Preparation of solutions and calibration curve

Since it was necessary to use a calibration curve as a guide, sodium chloride solutions were prepared, based on
the suggestions in the manual, the concentration ratios to be handled were up to a maximum molarity of 0.1, To
the dissolution equation, the volumes necessary to carry out the preparation were calculated (see 4 table).
Report Case III: Reverse Osmosis

Then, with the help of a conductivity meter, it was possible to take measurements of the conductivity that will allow
us to perform the calibration curve. This procedure took approximately half an hour, since the calculations were
immediately entered into the excel program, as this would allow a better development of practice.

Part III: Case study development

To carry out the complete development of the practice, basically three tests were carried out throughout this one
in order to determine the behavior of the reverse osmosis. Initially, the feed tank was filled to the top with the help
of water faucets that facilitate filling. Then the pump of the equipment was turned on and with the help of the keys
of the permeate and retenoate it was possible to move them to locate the desired value of the pressure, in this
way, both the values of the flows of each key and the value of the pressure, then every minute samples of the
permeate and retenoate hoses were taken and the conductivities of the same were read. (See tables1,2 and 3).

With the help of the previously developed calibration curve, the values of the conductivities were interpolated in
the equation of the line in order to obtain the concentrations of each sample. Finally, for each of the samples at
the proposed pressures, the values of osmotic pressures, membrane resistance and permeability of the membrane
together with the flux of these membranes (see tables 5-7)

2. RESULTS

Considering that the configuration of the equipment does not vary, the results are based on the samples taken in
each dish. The following is an outline of the equipment and the points where these measures were taken:

Figure 1. Diagram of the equipment with zones where the measurements are taken

Where:

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Valve Nomenclature

V1 Pump supply V8 Power Supply Cooling Tank Circuit

V2 Recirculation of the fed solution V9 Water supply to tank
V3 Feeding the reverse osmosis membrane V10 Isolation of the general water supply
V4 Concentrated Flow Regulation V11 Discharge of the storage tank of the retentate
V5 Retention sample collection V12 Discharge of the permeate storage tank
V6 Permeate sample collection V13 High fluxes in the permeate circuit (rotameter selection)
V7 Feed Tank Discharge V14 High fluxes in the permeate circuit (rotameter selection)

1 Water
2 Permeate
3 Retentate
4 Feed Tank
5 Permeate flow measuring valve
6 Retentate flow measuring valve

The results obtained in practice are shown below:

10 bar
Permeato Reteneato Flow rates
T (min) Temperature C [ ] M Permeato [ ] M Reteneato
S S QP (L/h) QR (L/h)
1 249,00 73,00 200,00 600,00 19,4 0,02421 0,00534
2 247,00 58,00 200,00 600,00 19,6 0,02399 0,00373
3 115,80 49,30 200,00 600,00 19,5 0,00993 0,00280
4 73,70 48,80 200,00 600,00 19,7 0,00541 0,00274
5 65,00 47,90 350,00 680,00 19,5 0,00448 0,00265
6 57,20 45,00 350,00 680,00 20,3 0,00364 0,00234
7 40,30 42,00 350,00 680,00 20,4 0,00183 0,00202
8 39,50 41,40 350,00 680,00 20,4 0,00175 0,00195
9 38,40 41,00 350,00 680,00 20,4 0,00163 0,00191
10 37,40 38,00 350,00 680,00 20,4 0,00152 0,00159

Table 1. Conductivity and concentrations obtained in the first sample at 10 bar

12 bar
Permeato Reteneato Flow rates
T (min) Temperature C [ ] M Permeato [ ] M Reteneato
S S QP (L/h) QR (L/h)
1 198,40 82,00 350,00 500,00 19,7 0,01878 0,00630
2 193,60 81,00 350,00 500,00 19,7 0,01827 0,00620
3 190,50 78,90 350,00 500,00 19,7 0,01794 0,00597
4 180,60 77,50 350,00 500,00 19,5 0,01687 0,00582
5 173,20 76,00 400,00 600,00 19,6 0,01608 0,00566
6 165,50 68,90 400,00 600,00 20,3 0,01526 0,00490
7 160,40 67,50 400,00 600,00 19,7 0,01471 0,00475
8 131,40 65,40 400,00 600,00 19,5 0,01160 0,00452
9 89,70 59,40 400,00 600,00 19,6 0,00713 0,00388
10 75,70 55,50 400,00 600,00 19,6 0,00563 0,00346

Table 2. Conductivity and concentrations obtained in the second sample at 12 bar

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14 bar
Permeato Reteneato Flow rates
T (min) Temperature C [ ] M Permeato [ ] M Reteneato
S S QP (L/h) QR (L/h)
1 409 156,00 260,00 500,00 19,7 0,04136 0,01424
2 309 134,80 260,00 500,00 19,7 0,03064 0,01196
3 211 104,50 260,00 500,00 19,7 0,02013 0,00872
4 101 96,50 260,00 500,00 19,5 0,00834 0,00786
5 95 83,00 350,00 600,00 19,6 0,00770 0,00641
6 85 67,00 350,00 600,00 20,3 0,00663 0,00470
7 74,2 54,00 350,00 600,00 19,7 0,00547 0,00330
8 62,3 43,00 350,00 600,00 19,5 0,00419 0,00212
9 54,3 35,60 350,00 600,00 19,6 0,00333 0,00133
10 35,6 30,10 350,00 600,00 19,6 0,00133 0,00074

Table 3. Conductivity and concentrations obtained in the third sample at 14 bar

0,04500 0,01600
0,04000 0,01400
0,03500 0,01200
0,03000 0,01000
0,02500
[]M
[]M

10 bar 0,00800 10 bar

0,02000 12 bar 12 bar
0,00600
0,01500 14 bar 14 bar
0,00400
0,01000
0,00200
0,00500
0,00000
0,00000
0 1 2 3 4 5 6 7 8 9 10 0 2 4 6 8 10
Time min Time min

figure 2 Concentration profile obtained to permeate and retenoate respect.

figure 3. Temperature profiles obtained to threes samples

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2.1THEORETICAL RESULTS

Selectivity of the reverse osmosis

The selectivity of the reverse osmosis membrane is characterized by the ratio of rejection rate (RT), this rejection
rate depends on the working conditions of the equipment such as: feed flow and pressure applied by the
membrane. The closer the rejection rate to 1, the higher the permeate quality, the concentration of sodium chloride
in the permeate being small compared to the feed. (Hernandez , Tejerina, & Martinez , 1990)

The equation describing the rejection rate is:

1)
= =1

Cf = concentration of solution in the feed.

Cp = concentration of solution in the permeable zone.

Filter membranes are the key and responsible for separating salts from water. Such membranes can be considered
as molecular filters. The pore size of these membrane filters is extremely small, so considerable pressure is
required to pass water through them. The choice of the most appropriate membrane model is per the water being
treated and its subsequent use, determining the type of installation More suitable.
To carry out the practice, it is important to perform the calibration of the potentiometer with which the equipment
counts, for them it is important to know the minimum and maximum concentrations in the permeate using the
equation already mentioned. (Wankat, 2011)

The maximum rejection rate that can be had in a reverse osmosis system is 1 and the feed concentration we have
is the one chosen for sodium chloride which was 8 grams / liters so we can find the concentration in the permeable
zone with respect to the maximum rejection cup. (Himmelblau, 2006)

Cp
TRmx = 1 2)
Cf

1=1
8 /

= 0 /

The minimum rejection rate that can be had in a reverse osmosis system is 0 and the feed concentration we have
is the one chosen for sodium chloride which was 8 grams / litter so we can find the concentration in the permeable
zone with respect to the minimum rejection cup.

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Report Case III: Reverse Osmosis

Cp
TRmin = 1
Cf

0=1
8 /

= 8 /

In the same way was performed for an average rejection cup.

Cp
TRprom = 1 Cf
4)

0,5 = 1
8 /

= 4 /

Calculation of membrane permeability

In order to know the permeability of the membrane to the solvent, the flux is calculated by means of this equation

= 5)

Where:

Jv: flux of solvent through the membrane

Qp: Permeate flow
SM: membrane filtering surface. It is determined in the technical chart as 7.6 m2

This calculation was performed for each of the flows in the pressures worked See tables 5-7

Calculation of membrane resistance

Knowing that the calculation of fouling in the membrane is done directly and indirectly has to:

Calculation of Reversible insulation resistance

( ) = 5.15104 () 0.158 6)

Where:

p= conductivity

Irreversible fouling resistance

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Report Case III: Reverse Osmosis

= + 7)

= ( ) = 6.04104 () 0.314 8)

Which means that the total resistance of the membrane would be defined by:

9)
=
+ +

Based on these equations it is possible to determine the flux calculation from:

=
+ + 10
8)

Where: )

PT= Total pressure in feed

= Osmotic pressure
Rm= Resistance of the membrane
RCF= Irreversible fouling resistance
Rcp = Reversible insulation resistance

As the pressure was varying to different flow conditions the calculation of this is:

= ln ( ) 11)

Where:

R= Gas constant in K, Bar, L, mole

T= temperature (k)
PvSolvent= 0.000057581 bar
Pvsolution = 0.02338865 bar

These data were obtained from the guide book (Wankat, 2011)

2.2 ANALYSIS AND EXPERIMENTAL RESULTS

2.2.1 Calibration curve

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Report Case III: Reverse Osmosis

The results obtained during the practice were based on the calibration curve performed at the beginning
of the practice, as reference were taken 5 points of molar concentrations that were calculated with the
dissolution formula.

Calibration Curve
[] M mS S
0,1000 9,440 944
0,0750 7,270 727
0,0500 5,090 509
0,0250 2,530 253
0,0000 0,150 15

Table 4. concentrations to perform calibration curve

figure 4 Calibration curve

Based on the equation of the line obtained, it was possible to interpolate the conductivities obtained to determine
the molar concentrations in each of the selected samples and sections (see tables 1-3)

This cross showed a very close coefficient of correlation to 1, which indicates a good linearization consistent with
the expected linear trend, the deviation that is presented could be due to errors of experimental and human type
at the time of the preparation of the solution or When reading the values in the conductivity meter. It is important
to clarify that these values were read in two different units S and mS this because the apparatus thus yielded the
results, however the change of unit can be observed in the 4 table. Because by practical effects it was decided to
work in the first unit.

2.2.2 Experimental results of the membrane.

From the results obtained on the basis of the experimental practice of Table 1 to 3, it was possible the values of
conductivities that allowed us to determine coefficients of theory based on theoretical calculations (equations 5 to
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11). These formulas were applied with the help of the Microsoft excel program in order to optimize the calculation
process. The results of this are shown below.

10 bar
osmotic pressure
QP (L/h) RCP (g/L) QR (L/h) CR (g/L) RCR (g/L) Jv Rm Flux T (k) P
(bar)
200,00 0,02977 600,00 0,26991 167,898 26,3158 0,99822 0,86444 292,4 14,60 4,60
200,00 0,03080 600,00 0,27897 173,540 26,3158 0,99822 0,83707 292,6 14,61 4,61
200,00 0,09836 600,00 0,28422 190,206 26,3158 0,99799 0,76359 292,5 14,61 4,61
200,00 0,12004 600,00 0,28452 194,724 26,3158 0,99793 0,74640 292,7 14,62 4,62
350,00 0,12453 680,00 0,28507 237,430 46,0526 0,99828 0,61234 292,5 14,61 4,61
350,00 0,12854 680,00 0,28682 240,027 46,0526 0,99827 0,60740 293,3 14,65 4,65
350,00 0,13725 680,00 0,28863 244,306 46,0526 0,99826 0,59699 293,4 14,65 4,65
350,00 0,13766 680,00 0,28899 244,696 46,0526 0,99826 0,59604 293,4 14,65 4,65
350,00 0,13822 680,00 0,28924 245,059 46,0526 0,99826 0,59516 293,4 14,65 4,65
350,00 0,13874 680,00 0,29105 246,471 46,0526 0,99826 0,59176 293,4 14,65 4,65

Table 5. Calculation of the pressure membrane of 10 bar

12 bar
osmotic pressure
QP (L/h) RCP (g/L) QR (L/h) CR (g/L) RCR (g/L) Jv Rm Flux T (k) P
(bar)
350,00 0,05582 500,00 0,26447 151,774 46,0526 0,99789 0,95648 292,7 14,62 2,62
350,00 0,05830 500,00 0,26508 152,942 46,0526 0,99789 0,94921 292,7 14,62 2,62
350,00 0,05989 500,00 0,26634 154,135 46,0526 0,99789 0,94190 292,7 14,62 2,62
350,00 0,06499 500,00 0,26719 156,342 46,0526 0,99788 0,92803 292,5 14,61 2,61
400,00 0,06880 600,00 0,26810 188,378 52,6316 0,99821 0,77134 292,6 14,61 2,61
400,00 0,07277 600,00 0,27238 192,538 52,6316 0,99821 0,75656 293,3 14,65 2,65
400,00 0,07539 600,00 0,27323 194,096 52,6316 0,99821 0,74897 292,7 14,62 2,62
400,00 0,09033 600,00 0,27450 200,831 52,6316 0,99819 0,72344 292,5 14,61 2,61
400,00 0,11180 600,00 0,27812 211,595 52,6316 0,99816 0,68699 292,6 14,61 2,61
400,00 0,11901 600,00 0,28048 215,893 52,6316 0,99815 0,67336 292,6 14,61 2,61

Table 6. Calculation of the pressure membrane of 12 bar

14 bar
osmotic pressure
QP (L/h) RCP (g/L) QR (L/h) CR (g/L) RCR (g/L) Jv Rm Flux T (k) P
(bar)
260,00 0,05264 500,00 0,21978 123,573 34,2105 0,99780 1,17174 292,4 14,60 0,60
260,00 0,00114 500,00 0,23258 116,586 34,2105 0,99800 1,24316 292,7 14,62 0,62
260,00 0,04934 500,00 0,25088 138,268 34,2105 0,99783 1,04889 292,6 14,61 0,61
260,00 0,10599 500,00 0,25571 155,413 34,2105 0,99768 0,93330 292,5 14,61 0,61
350,00 0,10908 600,00 0,26387 196,497 46,0526 0,99811 0,73949 292,6 14,61 0,61
350,00 0,11423 600,00 0,27353 204,098 46,0526 0,99810 0,71257 292,8 14,62 0,62
350,00 0,11979 600,00 0,28138 210,756 46,0526 0,99810 0,68992 292,7 14,62 0,62
350,00 0,12592 600,00 0,28803 216,887 46,0526 0,99810 0,67004 292,5 14,61 0,61
350,00 0,13004 600,00 0,29250 221,011 46,0526 0,99809 0,65781 292,6 14,61 0,61
350,00 0,13967 600,00 0,29582 226,375 46,0526 0,99808 0,64228 292,6 14,61 0,61

Table 7 Calculation of the pressure membrane of 14 bar

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4,66 2,65 0,63 Promedio 41

2,65
4,65
2,64 0,62
4,64 2,64
2,63 0,62
P

4,63

P
2,63
4,62 0,61
2,62
4,61 2,62
0,61
2,61
4,60 2,61 0,60
0 2 4 6 8 10 0 2 4 6 8 10 0 2 4 6 8 10
Time (min) Time (min) Time (min)

figure 5. Change in pressure drop with respect to osmotic pressure for pressures of 10, 12 and 14 bar respectively

figure 6.Variation in the resistance of the membrane for each pressure over time

figure 7. Change in membrane permeability throughout the practice

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Pressure (bar) Jv Rm

10 38,1579 0,9982
12 50,0000 0,9981
14 41,3158 0,9980
Table 8 Membrane data obtained in each test

3. ANALYSIS OF RESULTS

The preparation of the calibration curve was performed to determine the concentration of sodium chloride solutions
throughout the practice by conductivity. The solutions prepared to realize the curve were carried out with the use
of water provided by the municipal red to obtain a better criterion and precision. This is due to the feed in the
osmosis system. The linearization factor R2 of the calibration curve gave a value very close to 1, as can been seen
in the figure 4, so the results of the linear interpolation from the equation of the line will be quite accurate.

The concentration profiles with respect to time were determined at three different pressures. To perform the
practice, the equipment was configured to recirculate the entire permeate to obtain less concentrated outlets and
decrease the feed concentration with respect to time in all cases. Taking different samples every 2 minutes the
conductivity of permeate and retenoate was measured at the exit for later by means of the calibration curve
prepared to find the concentrations of the different samples. As shown in Figure 2, three operating pressures were
selected to see which was optimal. When the equipment operates at 14 bars, it is observed that the concentration
decreases notoriously compared to the other two pressures, and that it takes less time to reach a low
concentration, as can be corroborated in the tables 1,2 and 3. If it is desired to obtain a specific concentration, the
time it takes for the team to reach that concentration is known. It is important to emphasize that the balance of the
equipment is affected by the concentration of the recirculation, so the time calculated to arrive at the desired
concentration will be an approximation. In this case, it will not be possible to reach equilibrium because the
recirculation will have a lower concentration and will affect the feed until it is partially pure and does not get
retained. In figure 2, it is also observed that the permeate concentration profile is higher than that of the retentate,
which means that it was the retentate that most influenced the desalination of the mixture. Although the profile of
the three operating pressures for the permeate clearly shows that at low concentrations the profiles tend to stabilize
and as stated above no more desalinated water can be obtained.

From Figure 3, we affirm that the change in operating pressure will not present a significant change in temperature
change, since the maximum change between operating pressures is 0.6 C. Although it is observed that an
increase in pressure implies an increase in temperature. Although the profiles were expected to stabilize, this may
not occur because the conductometer thermometer is not properly calibrated, and is also due to temperature
changes in the samples before recording their conductivity.

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Then using the equations from 6 to 11, the polarization coefficient was determined for the pressures of 14, 12 and
10 bars as a function of time. The actual flux and the osmotic pressure were also found to determine the pressure
delta in each case, as can be seen in detail in Tables 5, 6 and 7. With the determined concentrations taking the
feed concentrations as constants, assuming that the concentration change is negligible by the volume used which
generates margin of error. However, the behaviour of the polarization coefficient must follow the same behaviour.

Figure 5 shows the change in pressure as a function of time for each pressure. The behavior shows that the
smaller the operating pressure, the system tends to stabilize at less time. According to (Wankat, 2011), a high-
pressure difference allows the separation to be more effective so it is recommended to work at a pressure that
produces a high-pressure differential to ensure the high performance of the equipment and have a separation
efficiency.

As shown in Figure 6, the membrane resistance over time was expected, because the theory states that it is
necessary to overcome the osmotic pressure of the substance, and it is observed that the separation efficiency
Reduces dramatically when operating at low pressures. This is because the membrane has a considerable
resistance so when the equipment operates at low pressures it is more difficult to overcome this resistance, which
in turn makes separation difficult. As shown in Figure 6 the selected pressure was the highest.

The permeability of the membrane was adequate due to the linear behaviour with a linear factor close to 1 and a
good correlation. It is observed that the linear behaviour of the permeability agrees with the theory about its linear
behaviour (Wankat, 2011) As it relates to the ability of the membrane to allow the permeate to pass and the
retenoate to remain on the contact surface.

Due to the resistance and permeability of the membrane, the optimum operating pressure is 14 bars, as can be
seen in Table 8 since at this point the maximum separation efficiency is obtained.

CONCLUSIONS

It was verified that even with the pressure changes, the temperature has a very small change so the
temperature change in the equipment over time is negligible
It is demonstrated that the pressure drop is the fundamental basis of this type of practice because this is
the reason by which the membrane can desalinate the problem mixture. Consequently, for this practice it
is shown that the most effective pressure to obtain the least amount of salt, is to decide the highest degree
of purity of water was at the highest pressure of 14 bar.
The operation of the equipment at the optimum operating point (14 bars) shows the maximum separation
efficiency, however the osmotic pressure of the substance is much lower. The fact that it requires a
pressure higher than the osmotic pressure, means that the membrane may be saturated, and wear can
affect the separation.

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REFERENCES

Hernandez , A., Tejerina, F., & Martinez , L. (1990). Microfiltracion ultrafiltracion y osmosis inversa.
Recuperado el 15 de Marzo de 2017
Himmelblau, D. (2006). Principios Basicos y Calculos en Ingenieria Quimica. Prentice -Hall.
Recuperado el 07 de Marzo de 2017
Pabby, K., & Sastre, M. (2010). Handbook of Membrane Separations. Recuperado el 13 de Marzo de
2017
Seader, D. J., Ernest, J., Henley, D., & Roper, K. (2011). Separation Process Principles. Wiley & Sons
Inc. Recuperado el 08 de Marzo de 2017
Wankat, P. (2011). Separation Processes Engineering (thirt ed.). Prentice Hall. Recuperado el 19 de
Febrero de 2017

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ANNEX I

_______________________________________________________
To: Junior Engineers

From: Senior Engineer

Reference: Reverse Osmosis

As you might know, the company has acquired a new reverse osmosis apparatus. We need
to verify the membrane operativity. For that, you have been assigned to evaluate the
membranes concentration polarization modulus of the new piece of equipment. Please
follow the equipment manual to avoid early damages (Section 6.7). Use the salt solution
already loaded in the feed tank of the equipment.

Do not forget to bring your theoretical calculations before the experiment.

Our lab people have been instructed to help you run up the experiment at conditions
selected by you. Please feel free to talk to our lab people for details of the experimental setup
and its limitations.

I expect your results as soon as they are available. Please give this matter the highest
priority.

Goodluck.

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