Experiment:

Water treatment by Ozonation

Objective:
To study water treatment/color removal by passing ozone over a sample of water.
Equipment:
Ozone generator, dye, magnetic stirrer, Beakers, Conical Flask, spectrophotometer:
Procedure:
Step 1: Making Dye:
• Take the dye sample and make 1000mg/L solution.
• Run tests for different wavelengths with a spectrophotometer and check for maximum wave
length absorbed by the solution.
• Fix this wavelength for the experiment.
Step 2: Making Calibration chart.
• Prepare solutions of different concentrations from the parent solution (of step 1).
• Check absorbance for every solution
• Make a calibration chart.
Step 3: Ozonation.
• Take a beaker and fill 250ml of distilled water.
• Add random small amount of dye in it.
• Insert the ozone probe in the water.
• Turn on the magnetic stirrer.
• Switch on the ozone generator.
• Take sample after every 10 minutes and check for light absorption using a spectrophotometer.
• Use calibration chart to determine percent color removal and concentration.

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 Reverse Osmosis
Introduction:

Reverse osmosis is a membrane separation process and is one of the physical / chemical
processes. This procedure can be used to remove dissolved organic and inorganic
substances from water. These substances can be, for example
viruses or ions.

Unit Description:

The complete device consists of a supply unit and a trainer. The supply unit and
trainer are connected to each other hydraulically and electrically.
The supply unit contains the raw water tank, the rinse water tank and the permeate tank. The raw
water tank and the rinse water tank each contain a float switch. The two taps V7 and V8 are fitted
with limit switches. The float switch and limit switch are components of the safety system
intended to protect the pump from dry running.
The trainer contains all other components and control elements.

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Process Diagram:

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Complete Device:

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Principle and Theory:
Fundamental principles of reverse osmosis
In order to understand reverse osmosis, first of all osmosis is explained. Osmosis
refers to the diffusion of the solvent via semi-permeable membranes from a less
concentrated solution into a more concentrated solution. This leads to the concentrations
being equalized. Semi-permeable means that the membrane is permeable for the solvent
and not permeable for the solutes. Diffusive transport is triggered by different
concentrations at different locations. A solution with a high concentration and a low
concentration of a solute is considered. The two solutions are separated by a semi-
permeable membrane. The concentration difference cannot be balanced by transporting
the solute, since the solute cannot pass through the membrane. The molecules of the
solvent on the other hand, can penetrate the membrane. The molar fraction for the solvent
is higher in the solution with the lower concentration of solute than in the solution with the
higher concentration of the solute.

Membrane separation process

In comparison to filtration, membrane separation processes can remove significantly
smaller substances (such as viruses and dissolved ions) from the water. Driving forces for
separation may be, for example concentration or pressure differences between the two
sides of the membrane. Water treatment uses the following membrane separation
processes:
1. Microfiltration
2. Ultrafiltration
3. Nanofiltration
4. Reverse osmosis
The pressure difference, the so-called transmembrane pressure, increases in the order
stated above. At the same time, the separation limit – i.e. the size of the smallest separable
substances – decreases. The cleaned raw water is called permeate, the retained portion of
the raw water is called retentate.

Wound membrane module design

The spiral wound membrane module consists of several membrane envelopes. A
membrane
envelope consists of two membranes, between which lies a porous spacer. The membrane
envelope is closed on three sides and connected to the perforated permeate collecting tube
at the fourth, open side. There are more spacers between the envelopes, which ensure the
solution flows axially. These spacers are wound spirally around the permeate collecting
tube, together with the membrane envelopes. The solution enters at the front face of the
module and flows axially between the envelopes through to the raw water side. The
semi-permeable membrane is permeable for the water (permeate), but hardly permeable
for the solute. The applied pressure forces the solvent through the membrane into the
envelopes. There it flows spirally to the permeate collecting tube (see Fig. below) and leaves
the module in the axial direction. The solution (raw water) is concentrated by removing the
water as it passes through the module. It leaves the module as retentate.

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Composite membranes are usually used for spiral wound membrane modules. Composite
membranes consist of three layers:

1. semi-permeable separation layer

2. microporous supporting layer

3. stable carrier layer.

The very thin semi-permeable separation layer is permeable for the water (permeate), but
hardly permeable for the solute. It consists of polyamide. The thicker polysulphone
supporting layer, covered with micro pores, provides the necessary strength and resists
compression at high operating pressures. The stable carrier layer gives the entire membrane
the necessary structure and strength.

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Important characteristics
When operating membrane modules, there are some important characteristics:
• Recovery
• Rejection
• Passage

Recovery (or Yield)

This is the portion of water to be cleaned (raw water), which leaves the membrane
system as product (permeate). The flow rates are usually set so that the recovery is greatest.
High recovery, however, increases the contamination of the membrane by precipitated low-
solubility salts (scaling).

Rejection
The separation efficiency of a membrane is called rejection. This is the portion of the
concentration of solute that has been removed from the raw water using the membrane
system.

R Rejection in %
cP Concentration of the solute in the permeate in g/L or w%
cF Concentration of the solute in the raw water in g/L or w%

Passage
Passage indicates the opposite of rejection. This is the portion of the concentration of the
solute from the raw water which has passed through the membrane.

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Factors influencing the efficiency of the separation process
The two most important variables for describing the separation efficiency are
• Flow rate of the permeate
• Rejection
These two variables are mainly influenced by the following parameters:
• Pressure
• Temperature
• Recovery
• Concentration in the raw water
Below we will consider the theoretical influence of each separate parameter on the flow
rate of the permeate and on rejection. To do so, the other three parameters are assumed to
be constant. In practice, this is not the case, since two or more effects usually overlap. The
following illustration is based on the solution-diffusion model.

Pressure
With increasing pressure in the raw water, the flow rate of the permeate increases. On the
other hand, the concentration of the solute in the permeate declines with increasing
pressure. This corresponds to an increase in rejection.

Temperature
The flow rate of the permeate increases with increasing temperature, if all other parameters
remain constant. Rejection on the other hand decreases with increasing temperature. This
means that more solute passes through the membrane.

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Recovery
The flow rate of the permeate decreases with increasing recovery. The flow rate of
the permeate ends when the concentration of solute in the retentate leads to an osmotic
pressure in the retentate, which is as large as the pressure in the raw water.

Raw water concentration

Rejection and the flow rate of the permeate decrease with increasing concentration
of solute in the raw water.

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 Experiments

1) Creating Calibration Curve:

Objective: To create a calibration curve for determination of concentration from observed
conductivity.

Procedure:

1) To determine the calibration curve, it is necessary to prepare NaCl solutions by

dilution with different concentrations.
2) Make Nacl solutions of following concentrations. 0.25wt%, 0.50wt%, o.75wt%, 1 wt%, 2
wt%.
3) Determine the conductivity of all solutions by using a conductivity meter or use the
conductivity probe of reverse osmosis unit. Make sure conductivity meter reading is in
agreement with reverse osmosis unit conductivity readings.
4) Make a calibration curve and use to determine unknown concentrations from observed
conductivities in future experiments.
Analysis:
Plot concentration against the conductivities.

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 2) Investigate the influence of raw water Pressure on
Reverse osmosis process.
Objective:
To investigate the influence of pressure in the raw water on permeate and rejection.
Procedure:

1. Add a specific weight of NaCl in supply tank.

2. Turn trainer on at the main switch.
3. Turn on stirring machine R.
4. Wait until the NaCl is completely dissolved.
5. Turn stirrer off.
6. Make following configuration of Valves and taps at the beginning:
• V1 fully open
• V2 fully open
• V3 closed
• V4 open
• V5 open
• V6 closed
• V7 closed
• V8 closed
• V9 non-return valve: non-adjustable
• V10 closed
• V11 closed
• V12 closed
• V13 closed
• V14 safety valve: non-adjustable
7. Open V8.
8. Switch on the pump.
9. Put on ear defenders. Strong vibrations occur in the transition area from the
unpressurised state to the operating state, because this is out of the working range of
the pulsation damper.
10. Simultaneously turn valves V1 and V2 quickly clockwise, in order to quickly exceed
the transition area. Set a pressure of about 15 bar.
11). Start taking readings after running machine for 5 mins. Take readings every 3 minutes.
12). Repeat the process by varying pressure to 20, 25 and 30 bars respectively.
`

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Observation and Analysis:

Plot permeate flow rate against the pressure and observe the trend.
Plot rejection against the varying pressure and observe the trend.
Draw a graph between recovery and time for all the pressure values.

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 3) Investigate the influence of raw water concentration on
Reverse osmosis process.
Objective:
To investigate the influence of concentration in the raw water on permeate and rejection.
Procedure:

1. Make a 0.05 wt% NaCl solution in supply tank initially.

2. Turn trainer on at the main switch.
3. Turn on stirring machine R.
4. Wait until the NaCl is completely dissolved.
5. Turn stirrer off.
6. Make following configuration of Valves and taps at the beginning:
• V1 fully open
• V2 fully open
• V3 closed
• V4 open
• V5 open
• V6 closed
• V7 closed
• V8 closed
• V9 non-return valve: non-adjustable
• V10 closed
• V11 closed
• V12 closed
• V13 closed
• V14 safety valve: non-adjustable
7. Open V8.
8. Switch on the pump.
9. Put on ear defenders. Strong vibrations occur in the transition area from the
unpressurised state to the operating state, because this is out of the working range of
the pulsation damper.
10. Simultaneously turn valves V1 and V2 quickly clockwise, in order to quickly exceed
the transition area. Set a pressure of about 20 bar.
11). Start taking readings after running machine for 5 mins. Take readings every 3 minutes.
12). Repeat the process by varying initial concentration to 0.10, 0.15, 0.20 and 0.25wt% NaCl
solutions respectively.
`

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Observation and Analysis:

Feed/Raw water initial pressure: 20bar.

Feed/Raw Water initial concentration: ........... wt%

Plot permeate flow rate against the concentration and observe the trend.
Plot rejection against the varying concentration and observe the trend.
Draw a graph between recovery and time for all the concentration values.

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 4) Investigate the influence of raw water Temprature on
Reverse osmosis process.
Objective:
To investigate the influence of concentration in the raw water on permeate and rejection.
Procedure:

1. Make a specific wt% NaCl solution in supply tank initially.

2. Turn trainer on at the main switch.
3. Turn on stirring machine R.
4. Wait until the NaCl is completely dissolved.
5. Turn stirrer off.
6. Record the initial temperature of raw water.
7. Make following configuration of Valves and taps at the beginning:
• V1 fully open
• V2 fully open
• V3 closed
• V4 open
• V5 open
• V6 closed
• V7 closed
• V8 closed
• V9 non-return valve: non-adjustable
• V10 closed
• V11 closed
• V12 closed
• V13 closed
• V14 safety valve: non-adjustable
8. Open V8.
9. Switch on the pump.
10. Put on ear defenders. Strong vibrations occur in the transition area from the
unpressurised state to the operating state, because this is out of the working range of
the pulsation damper.
11. Simultaneously turn valves V1 and V2 quickly clockwise, in order to quickly exceed
the transition area. Set a pressure of about 20 bar.
12). Start taking readings after running machine for 5 mins. Take readings every 3 minutes.
13). Repeat the process by varying initial temperature. Making an increment of 5 degree
Celsius rise in temperature. Take readings at atleast 5 different temperature.
`

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Observation and Analysis:

Feed/Raw water initial pressure: 20bar.

Feed/Raw Water initial Temperature: ...........

Plot permeate flow rate against the temperature and observe the trend.
Plot rejection against the varying temperature and observe the trend.
Draw a graph between recovery and time for all the different temperatures.

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