Separation Process – 1

Lab Report

Submitted By:
Muhammad Talha Umar
(2023-CH-253)
Submitted To:
Madam Farah Butt

Department Of Chemical Engineering

University of Engineering and Technology Lahore

(new campus).
 Equipment Detail

CLOs For Separation-1 Lab

General Safety And Precautions For
Students In Separation-1 Lab
Personal Safety:
1. Personal Protective Equipment (PPE)
Always wear goggles, gloves, lab coat, and closed-toe shoes.
2. Appropriate Dress Code
Tie back long hair, avoid loose clothing and jewelry.
3. No Eating or Drinking in the Lab
Food and drink are strictly prohibited in lab areas.
4. General Conduct and Behavior
Maintain professionalism and avoid horseplay.
5. Emergency Exits and Evacuation Knowledge
Familiarize yourself with exit routes and assembly points.
6. First Aid Awareness
Know the location and use of the first aid kit.
7. Fire and Chemical Burn Response
Understand the use of fire blankets and eyewash stations.
8. Working Under Supervision
Never work alone; always perform experiments under guidance.
9. Health Conditions and Reporting
Report any allergies, asthma, or injuries to the supervisor.
10. Focus and Concentration
Stay alert, avoid distractions, and follow instructions carefully.

Equipment Safety:
1. Pre-Use Equipment Inspection
Check for any damage, wear, or malfunction before use.
2. Correct Setup of Apparatus
Secure glassware and align apparatus properly before starting.
3. Handling Glassware Safely
Avoid using cracked or chipped glass items.
4. Temperature and Pressure Precautions
Don’t exceed equipment limits; monitor gauges carefully.
5. Safe Use of Distillation Columns
Ensure proper sealing and venting to avoid vapor leaks.
 6. Centrifuge Operation Protocol
Always balance samples and never open while spinning.
7. Proper Use of Filtration Units
Don’t apply excessive vacuum pressure; secure filter funnels.
8. Electrical Equipment Safety
Keep devices dry, and never touch them with wet hands.
9. Post-Use Equipment Shutdown
Switch off and unplug equipment after use.
10. Reporting Equipment Malfunctions
Immediately notify the lab technician or supervisor if any issue arises.

Chemical Safety:
1. Reading and Understanding SDS/MSDS
Always review chemical data sheets before handling substances.
2. Proper Labeling of Containers
Label all chemicals with name, concentration, and hazard symbols.
3. Safe Storage of Chemicals
Store acids, bases, flammables, and oxidizers in separate, proper containers.
4. Correct Handling Techniques
Use pipettes, not hands; never smell or taste chemicals.
5. Use of Fume Hoods for Hazardous Vapors
Always conduct volatile chemical work under a fume hood.
6. Avoiding Chemical Exposure
Prevent contact with skin, eyes, and clothing.
7. Chemical Incompatibilities Awareness
Do not mix chemicals without understanding their interactions.
8. Proper Waste Disposal
Follow procedures for segregating and discarding chemical waste.
9. Spill Management and Cleanup
Use spill kits and follow emergency protocols for spills.

Lab Layout
 Equipment Detail

1.Wetted Wall Gas Absorption Column Apparatus

Diagram:

Introduction:
The wetted wall column is a classic piece of laboratory equipment
used to study the principles of mass transfer between gas and liquid phases under
controlled conditions.

In this experiment, a gas mixture containing a soluble component is passed over a

thin film of liquid that flows down the inner wall of a vertical glass tube. The
absorption process occurs as the gas contacts the wetted surface, allowing the
target component to dissolve into the liquid. The wetted wall column provides a
simplified and controlled system that eliminates complications due to packing or
trays, making it ideal for studying fundamental mass transfer coefficients and
validating theoretical models.

The primary objective of this experiment is to determine the gas-phase mass

transfer coefficient by analyzing the rate of absorption of a specific solute gas,
such as carbon dioxide (CO₂), into a suitable solvent like water or sodium
hydroxide solution. Parameters such as gas flow rate, liquid flow rate, and column
dimensions are varied or measured to study their effect on mass transfer
performance.

This experiment provides a practical understanding of film theory, mass transfer

resistance, and the influence of hydrodynamics on gas absorption, which are
crucial for the design and scale-up of industrial gas-liquid contactors.

Working Principle:
The working principle of a wetted wall gas absorption column is based on the
transfer of a gaseous solute from a gas phase into a liquid phase flowing as a thin
film along the inner wall of a vertical tube. In this setup, the liquid absorbent is
introduced from the top and flows downward, forming a uniform film that "wets"
the wall. Simultaneously, the gas mixture containing the solute (e.g., CO₂ in air) is
passed either co-currently or counter-currently through the center of the column.
As the gas flows over the liquid film, the solute diffuses across the gas boundary
layer, reaches the gas-liquid interface, and is then absorbed into the liquid film
due to the concentration gradient. The absorbed solute continues to diffuse
through the liquid film and exits with the liquid at the bottom of the column. This
mass transfer process is governed by both gas-side and liquid-side mass transfer
resistances and is typically analyzed using film theory, which assumes stagnant
boundary layers near the interface. The wetted wall column allows for precise
study of these mechanisms and is commonly used in labs to evaluate mass
transfer coefficients and validate theoretical models.

Apparatus:

1. Wetted Wall Column

 o A vertical glass tube (typically 1–2 cm in diameter and 50–100 cm in
length) where the liquid flows as a thin film along the inner wall.
2. Gas Supply System
o Source of solute-containing gas (e.g., CO₂-air mixture or pure CO₂).
o Gas flow meter or rotameter to measure and control gas flow rate.
o Pressure regulator and valves for flow control.
3. Liquid Supply System
o Water or aqueous NaOH solution as the absorbing liquid.
o Liquid feed tank/reservoir.
o Peristaltic pump or gravity feed system to control liquid flow rate.
4. Solute Gas Analyzer / Conductivity Meter / Titration Setup
o To analyze the concentration of solute gas (e.g., CO₂) in the outlet gas
or absorbed in the liquid phase.
o May include a conductivity meter (if using NaOH) or a titration setup
with phenolphthalein indicator.
5. Thermometer or Temperature Sensor
o To measure the operating temperature of the gas and liquid streams.
6. Manometer or Pressure Gauge
o To measure the pressure drop across the column (if applicable).
7. Stopwatch
o For timing the experiment during sampling.
8. Measuring Cylinders and Beakers
o For collecting and measuring liquid samples.
9. Piping and Fittings
o For safe and leak-proof connections between gas and liquid supply
lines.

Safety Equipment

 Gloves, lab coat, safety goggles.

 Fume hood (if dealing with acidic or basic solutions).

Applications
1. Academic and Research Studies
 o Used in chemical engineering labs to study mass transfer
fundamentals under controlled conditions.
o Ideal for validating theoretical models like film theory and
penetration theory.
2. Determination of Mass Transfer Coefficients
o Helps in calculating gas-phase and liquid-phase mass transfer
coefficients, essential for designing industrial absorbers.
3. Scale-up of Absorption Processes
o Provides basic data used in the design and scale-up of packed
towers, spray towers, and tray columns for gas absorption.
4. Air Pollution Control Studies
o Used in research on removal of pollutants (e.g., CO₂, SO₂, NH₃)
from industrial gas streams by absorption into a liquid.
5. Parameter Sensitivity Analysis
o Allows study of the effects of variables such as flow rates,
temperature, pressure, and concentration on mass transfer.
6. Heat and Mass Transfer Correlation Development
o Used to develop and validate empirical correlations for heat and
mass transfer in gas-liquid systems.
7. Investigation of Interfacial Phenomena
o Enables close examination of gas-liquid interface behavior, which is
difficult in packed or tray towers.
8. Study of Chemical Absorption Reactions
o Helps analyze absorption accompanied by chemical reaction, such
as CO₂ absorbed in NaOH.
9. Design of Environmental Equipment
o Used for modeling and testing equipment like scrubbers and
absorbers used in wastewater or flue gas treatment.

10 Educational Demonstration Tool

 Commonly used in undergraduate labs to demonstrate principles of gas

absorption and mass transfer visually.
 2.Distillation Unit
Figure:

Introduction:
Distillation is one of the most widely used separation techniques in chemical
engineering, employed for the purification and separation of liquid mixtures based
on differences in their boiling points. It is a thermal separation process in which a
liquid mixture is partially vaporized and the vapor is then condensed to separate
components with varying volatilities.

In a typical distillation unit, the liquid mixture is heated in a reboiler or distillation

flask. The component with the lower boiling point vaporizes first, rises through the
distillation column, and passes into a condenser, where it is cooled and collected as
the distillate. The remaining liquid, richer in the less volatile component, is called
the residue or bottom product.

Laboratory-scale distillation units are essential for studying the principles of vapor-
liquid equilibrium (VLE), mass transfer, and energy balance. They provide hands-
on experience with fundamental concepts such as reflux ratio, theoretical stages,
and separation efficiency.

This experiment is particularly important for students to understand the design and
operation of industrial distillation columns, which are extensively used in
petroleum refining, chemical manufacturing, and environmental engineering.

The objective of this experiment is to observe the distillation process, analyze the
composition of the distillate and residue, and understand the factors influencing
separation such as column design, feed composition, and operating conditions.

Working Principle:
The working principle of a distillation unit is based on the difference in boiling
points of the components in a liquid mixture.

When the mixture is heated in the distillation flask or reboiler, the component
with the lower boiling point vaporizes first.

These vapors rise through the distillation column, which may be packed or
equipped with trays to enhance separation by allowing repeated condensation
and vaporization (fractionation).
As the vapors ascend, they become richer in the more volatile component. Upon
reaching the condenser, the vapors are cooled and condensed back into liquid
form and collected as distillate in a receiving flask.

The less volatile components remain in the boiling flask as the residue or
bottoms. The efficiency of separation can be improved by using a fractionating
column and adjusting the reflux ratio (the portion of condensed vapor returned
to the column). This principle is widely applied in both laboratory and industrial
settings to purify solvents, separate chemical compounds, and analyze liquid
mixtures.

Apparatus:
1. Distillation Flask / Reboiler
A round-bottom or flat-bottom flask where the liquid mixture is initially
heated.
Acts as the vapor generation chamber.
2. Heating Source
Heating mantle, hot plate, or water/oil bath used to supply heat to the
flask.
May include a magnetic stirrer for uniform heating.
3. Thermometer with Thermowell
Measures the temperature of vapors leaving the column or flask.
Helps determine when components are being separated.
4. Distillation Column / Fractionating Column
A vertical glass column where multiple vapor-liquid contact stages
occur.
Often packed with glass beads, Raschig rings, or sieve trays for
enhanced separation.
5. Condenser
Usually a Liebig, Vigreux, or Graham condenser.
Cools the vapors back into liquid using circulating cold water.
6. Cold Water Supply and Tubing
Provides continuous cooling for the condenser.
Includes inlet and outlet for water circulation.
7. Receiving Flask / Distillate Collector
Collects the condensed distillate product after separation.
 Usually a clean conical flask, beaker, or measuring cylinder.
8. Vacuum Adapter (Optional)
Used in vacuum distillation to reduce system pressure.
Allows distillation of high-boiling or heat-sensitive substances.
9. Support Stand and Clamps
Retort stands, clamps, and rings to hold the glassware securely in
position.
Prevent accidents and ensure stability during operation.
10.Reflux Condenser (for Fractional Distillation)
Allows part of the condensed vapor to return to the column, improving
separation.

Essential when reflux ratio control is needed.

11.Vacuum Pump (Optional)

Reduces pressure for vacuum distillation, lowering the boiling points of
components.

Schematics of Batch Distillation Process.

Applications:
1. Purification of Chemicals in Laboratories

 Used to purify solvents, organic compounds, and recover

chemicals after reactions.
 Petroleum Refining
 Separates crude oil into useful products like gasoline, diesel,
kerosene, and lubricants through fractional distillation.
 Pharmaceutical Industry
 Helps in the purification of active pharmaceutical ingredients
(APIs) and intermediates.
 Alcohol and Beverage Production
 Used in the distillation of alcoholic beverages like whiskey,
vodka, and ethanol.
 Essential Oil Extraction
 Steam distillation is used to extract essential oils from plants
and herbs.
 Environmental Applications
 Employed in water purification and solvent recovery in
environmental testing labs.
 Perfume and Cosmetic Industry
 Used for the separation and purification of fragrance
components.
 Food Industry
 Helps in extracting flavors and aromas and in concentration of
natural extracts.
 Chemical Process Industry
o Essential in the large-scale separation of chemical feedstocks and final
products.
 Educational and Research Laboratories
 Used in teaching principles of separation processes, phase equilibrium, and
thermodynamics.

3. Liquid-Liquid Extraction
Figure:

Introduction:
 Liquid-liquid extraction (LLE) is a mass transfer-based separation technique
used to separate components of a liquid mixture by utilizing the differences
 in their solubilities in two immiscible liquids, typically an aqueous phase
and an organic solvent.
 The basic principle involves transferring a solute from one liquid phase
(usually water) into another immiscible liquid phase (the solvent), where it is
more soluble.
 This process is especially useful for separating compounds that cannot be
efficiently separated by distillation, such as heat-sensitive substances or
mixtures with close boiling point.
 The equipment used in liquid-liquid extraction varies depending on the
scale and application, ranging from simple separating funnels in the lab to
more complex equipment like mixer-settlers, spray columns, packed
columns, centrifugal extractors in industrial processes.
 In typical lab setup, the two liquids are mixed to allow mass transfer of the
solute, and then allowed to settle into two distinct layers due to differences
in density. The extracted phase is then separated and analyzed. Liquid-liquid
extraction is widely applied in chemical, pharmaceutical, and environmental
industries for purification, separation, and recovery of valuable or hazardous
components.

Working Principle:

 Liquid-liquid extraction involves the separation of components based on

their differing solubilities in two immiscible liquids.
 When a mixture containing a desired solute is brought into contact with a
second liquid (usually an organic solvent) that does not mix with the first
(usually water), the solute partitions between the two phases.
 The extent to which the solute transfers to the solvent phase depends on its
affinity for that phase, described by the distribution or partition coefficient.
 By mixing the two liquids, the surface area for mass transfer is increased,
allowing the solute to move from the feed phase to the extracting solvent.
After mixing, the two liquids are allowed to settle into separate layers, with
the solute now concentrated in the solvent phase. This technique is widely
used for separating, purifying, or recovering compounds from mixtures that
are difficult to separate by other means like distillation.
Apparatus of Liquid-Liquid Extraction Unit
a) Separating Funnel
a. A conical or pear-shaped glass container with a stopcock at the
bottom.
b. Used to mix and then separate the two immiscible liquid layers
(extract and raffinate).
b) Beakers or Conical Flasks
a. Used for preparing the feed solution and collecting the separated
phases after extraction.
c) Mechanical Stirrer or Shaker (Optional)
a. Helps in mixing the two immiscible liquids thoroughly to increase
contact and improve mass transfer.
d) Measuring Cylinders
a. Used to accurately measure volumes of feed solution and solvent.
e) Pipettes or Droppers
a. Used for transferring small amounts of liquids for testing or analysis.
f) Thermometer (Optional)
a. Monitors temperature during extraction, especially if the process is
temperature-sensitive.
g) Support Stand with Clamp
a. Holds the separating funnel securely in a vertical position during
settling and separation.
h) Glass Rod or Magnetic Stirrer
a. For manual or automatic stirring of liquids before pouring into the
separating funnel.
i) Solvent (Extracting Liquid)
a. An immiscible liquid with high affinity for the desired solute (e.g.,
ether, chloroform, hexane).
j) Feed Solution
k) The original liquid mixture containing the solute that needs to be extracted
(usually aqueous).

 Applications For liquid – liquid Extraction.

 Pharmaceutical Industry
 Extraction of active pharmaceutical ingredients (APIs) from plant
materials or reaction mixtures.
 Purification of heat-sensitive drug intermediates.
 Chemical Industry
 Separation and purification of organic acids, amines, and other specialty
chemicals.
 Recovery of solvents and valuable compounds from mixtures.
 Petroleum Industry
Removal of sulfur compounds and aromatics from hydrocarbon fuels.
Extraction of impurities during lubricant and fuel processing.
 Food and Beverage Industry
Extraction of essential oils, flavors, and natural colorants.
Isolation of bioactive compounds from fruits, vegetables, and herbs.
 Environmental Engineering
 Removal of toxic or hazardous chemicals from industrial wastewater.
 Recovery of reusable or valuable components from waste streams.
 Nuclear Industry
o Separation and recovery of radioactive isotopes such as uranium and
plutonium.
o Purification of nuclear fuel components during reprocessing.
 Biotechnology and Biochemistry
o Extraction of enzymes, proteins, and vitamins from fermentation
broths.
o Purification of biological compounds in research labs.
 Cosmetic and Fragrance Industry
o Extraction of natural fragrances, oils, and plant extracts for perfumes
and creams.
 Analytical Chemistry
o Sample preparation and pre-concentration before chromatographic or
spectroscopic analysis.
Research and Academic Labs
 Demonstration of phase equilibrium and separation techniques.
 Used in practicals to study distribution coefficients and solute behavior .
 4.Ion Exchange Appratus

Figure:

Introduction:
 Ion exchange apparatus is an essential piece of equipment used in the
separation process laboratory to study the removal, recovery, or separation
of ionic species from solutions through a reversible chemical exchange
process. The principle of ion exchange involves the replacement of
undesirable ions in a solution with desirable ions from a solid ion-exchange
resin. These resins are typically made of organic polymers that carry fixed
ionic groups capable of exchanging cations or anions with the surrounding
liquid phase. The apparatus is generally composed of a vertical glass or
acrylic column filled with ion exchange resin, through which the ionic
 solution is passed. As the solution flows through the resin bed, targeted
ions are selectively exchanged and removed from the solution. This
technique is widely used in water softening, deionization, purification of
pharmaceuticals, recovery of valuable metals, and wastewater treatment.
In a laboratory setting, the ion exchange apparatus helps in understanding
the kinetics, capacity, and selectivity of ion exchangers under controlled
flow and concentration conditions.

Appratus :
 Ion Exchange Column
o A vertical glass or acrylic tube filled with ion exchange resin.
o It allows the ionic solution to pass through and interact with the resin.
 Ion Exchange Resin
o The core material used for exchanging ions (either cationic or
anionic).
o Common resins include sulfonated polystyrene for cation exchange
and quaternary ammonium resins for anion exchange.
 Support Screen / Filter Mesh
o Placed at the bottom and sometimes top of the column to hold the
resin in place and prevent it from washing out.
 Feed Reservoir
o A container holding the ionic solution to be treated (the influent).
o Usually connected to the inlet of the column.
 Inlet and Outlet Tubing
o Connects the feed reservoir to the column and directs treated water to
the collecting flask.
 Flow Control Valve / Rotameter
o Regulates and monitors the flow rate of the solution through the
column.
 Effluent Collector / Receiving Flask
o Collects the treated (ion-exchanged) solution that exits the column.
 Regenerant Reservoir
o Holds the chemical solution used to regenerate the exhausted resin
(e.g., HCl for cation resin, NaOH for anion resin).
 Stopwatch / Timer
 o Used to monitor the contact time and residence time of the solution in
the column.
 pH Meter or Conductivity Meter
 Measures the quality of the effluent and indicates the completion of ion
exchange or breakthrough point.

Working Principle:
 The working principle of an Ion Exchange Apparatus relies on the
process of ion exchange, where unwanted ions in a liquid are replaced by
desirable ions from a solid phase, typically an ion-exchange resin. The ion-
exchange resin, which is usually made of synthetic polymers, contains fixed
ionic groups (such as sulfonate or quaternary ammonium groups) that attract
and hold onto either cations (positively charged ions) or anions (negatively
charged ions). When an ionic solution is passed through the ion-exchange
column, the ions from the solution are attracted to the resin. The resin
releases equivalent amounts of the desired ions (such as sodium or chloride
ions) into the solution, while simultaneously binding the unwanted ions
(such as calcium, magnesium, or harmful anions) to its functional groups.

 This process occurs due to the selective affinity of the resin for specific ions,
and it is governed by factors like ion concentration, resin type, and flow rate.
Over time, the resin becomes saturated with the unwanted ions, and the ion
exchange process slows down. At this point, the resin needs to be
regenerated by passing a regenerant solution (such as a strong acid or base)
through the column to remove the accumulated ions and restore the resin’s
ion-exchange capacity. The apparatus operates in a continuous or batch
mode, and the performance is monitored by measuring parameters like pH,
conductivity, and ion concentration in the effluent. Ion exchange is widely
used for applications such as water softening, deionization, and separation of
valuable metals or compounds.

Applications:

1. Water Softening
 Industry Use: Ion exchange is widely employed in domestic and
industrial water softening systems to remove calcium and magnesium
ions that cause hardness in water, thereby preventing scale buildup in
pipes, boilers, and machinery.
2. Demineralization of Water
Industry Use: In power plants, laboratories, and pharmaceutical
industries, ion-exchange is used to produce ultra-pure water by removing
virtually all mineral ions, ensuring high-quality water for sensitive
applications.
3. Wastewater Treatment
Industry Use: Ion-exchange technology is applied in the treatment of
wastewater, particularly in the removal of heavy metals, radioactive ions,
and other contaminants, to meet environmental discharge standards or
recycle water for reuse.
4. Separation and Recovery of Metal Ions
Industry Use: In the mining and metallurgy industries, ion exchange is
used to extract and recover valuable metals like uranium, gold, and silver
from ores or process streams. It’s also used in the recovery of metals
from industrial effluents.
5. Pharmaceutical Industry
Industry Use: Ion-exchange is applied for the purification of
pharmaceutical compounds and the separation of active ingredients. It is
particularly useful for isolating specific ions or compounds in drug
formulations.
6. Food and Beverage Industry
Industry Use: Ion-exchange is used to purify liquids, such as sugar
syrups and fruit juices, by removing impurities like metals and
undesirable ions, improving the clarity and quality of the final product.
7. Nuclear Industry
Industry Use: In the nuclear industry, ion exchange is employed for the
treatment of radioactive waste and water purification, as well as the
recovery of valuable isotopes like uranium and plutonium during nuclear
reprocessing.
8. Chemical Manufacturing
Industry Use: Used in the chemical industry for the purification of
chemicals by removing unwanted ionic species. It is also used for
separating and concentrating rare or valuable ions in chemical reactions
or processes.
9. Aquarium and Fish Tank Maintenance
 Industry Use: Ion-exchange resins are used in aquariums to maintain
water quality by removing unwanted ions, such as ammonia, nitrate, and
phosphate, which can be toxic to aquatic life.
10.Cosmetic and Fragrance Industry
Industry Use: Ion-exchange equipment is utilized in the purification of
ingredients for cosmetics and fragrances, ensuring the removal of trace ionic
impurities that could affect the product's stability or safety.

5. Solid-Liquid Extraction

Figure:
 Introduction:
Solid-liquid extraction is a powerful and versatile technique that plays a crucial
role in separating and isolating valuable substances from solid materials using a
liquid solvent. The process is grounded in the principle of solubility: the solvent
selectively dissolves the target components, leaving behind unwanted impurities in
the solid matrix.
At its core, the process begins when the solid material (which could be plant
biomass, ores, or other materials) is exposed to a solvent. The solvent's chemical
properties allow it to dissolve specific substances from the solid, such as essential
oils, bioactive compounds, or metals. These dissolved compounds then transfer
into the liquid phase, where they can be further purified or concentrated.

The efficiency of solid-liquid extraction depends on several key factors:

1. Solvent Selection: The solvent must have a high affinity for the compounds
of interest, but not for others. For instance, a polar solvent like water is good
for extracting polar compounds, while non-polar solvents like hexane are
more suitable for extracting oils or lipids.
2. Temperature: Heating the solvent can help increase the rate of extraction,
as higher temperatures generally accelerate the dissolution of compounds
from the solid matrix.
 3. Time: The longer the solid is in contact with the solvent, the greater the
amount of material that can be extracted. However, excessive extraction
time may lead to the extraction of unwanted compounds, so it’s a balance.
4. Particle Size: Smaller particle sizes provide more surface area for the
solvent to act upon, improving extraction efficiency

Equipment:
1. Extraction Vessel (Extraction Tank)
o This is the container where the solid material and solvent are mixed
together. It can be a batch or continuous system, depending on the
setup. The vessel is usually made of stainless steel, glass, or other
inert materials to resist corrosion by solvents.
2. Solvent Reservoir
o A container that holds the solvent before it is introduced to the solid
material. It is an essential part of ensuring a consistent and controlled
solvent supply during the extraction process.
3. Stirring Mechanism (Agitator)
o Often a mechanical stirrer or agitator, it helps mix the solid material
with the solvent to increase the contact surface area and improve the
efficiency of the extraction. This is particularly important in batch
extractions to ensure thorough mixing.
4. Heating Source
o Some solid-liquid extraction processes require heating to increase the
rate of extraction. This could be a heating mantle, water bath, or a
jacketed vessel with controlled temperature for more accurate heat
management.
5. Filtration Unit
o After the extraction process, the mixture is often filtered to separate
the liquid extract from the solid residue. Filtration equipment can
include filter paper, vacuum filtration setups, or centrifuges for
separating solids from the solvent.
6. Solvent Recovery System
o In large-scale operations, a solvent recovery system is used to
condense and recover the solvent for reuse. This often involves a
distillation unit or a rotary evaporator, which separates the solvent
from the extracted liquid based on differences in boiling points.
7. Centrifuge
 o Used in some solid-liquid extraction processes, especially when high-
speed separation of the solid and liquid phases is required. The
centrifuge uses rotational force to separate the components based on
density differences.
8. Rotary Evaporator (Rotavap)
o A common tool in laboratory-scale extraction, the rotary evaporator is
used to efficiently remove the solvent from the extract under reduced
pressure, minimizing heat damage to the extract and allowing for
solvent recovery.
9. Cooling System
o Cooling systems, such as a condenser or cold trap, are used to
condense vapors back into the liquid phase, especially when solvents
need to be recycled. This is particularly useful when working with
volatile solvents in solvent recovery.
10.Flow Control Valve

 This regulates the flow of the solvent into the extraction vessel. Proper flow
control ensures that the solvent is added at a steady rate, maintaining optimal
conditions for extraction and preventing overflow or inefficiencies.

Working Principle:
The working principle of solid-liquid extraction involves transferring soluble
components from a solid material into a liquid solvent. The solid material, such as
plant matter or ores, is mixed with a solvent that dissolves the desired
compounds.

The solvent must have a high affinity for the target compounds to extract them
effectively. Once the solid and solvent are in contact, the soluble compounds
diffuse from the solid into the solvent due to the concentration gradient, where
the concentration of the compound is higher in the solid than in the solvent. As
the solvent penetrates the solid, it dissolves the target compounds, causing them
to move into the liquid phase. After a certain period, the liquid solvent containing
the dissolved compounds is separated from the solid residue, often through
filtration, centrifugation, or decantation. In some cases, the solvent can be
recovered and reused, typically by processes like evaporation or distillation,
where the solvent is separated from the extracted compounds. The efficiency of
the extraction depends on factors such as the solvent choice, temperature, time,
and the particle size of the solid material.

Software Main Screen:

 Modern solid-liquid extraction equipment often integrates multiple software

systems, allowing for data sharing between process control, simulation, and
monitoring tools. This integration enhances process efficiency, helps reduce
operational costs, and ensures the extraction process is executed according to
the desired parameters.
 In summary, software for solid-liquid extraction equipment includes process
control, simulation, data acquisition, and maintenance tools. These software
 systems work together to optimize extraction efficiency, ensure safety, and
provide detailed data for analysis and reporting.

SCADA (Supervisory Control and Data Acquisition) and PID Control interface for
a process control system, most likely used in a lab or industrial setup for
educational purposes (e.g., by Edibon, a company known for training equipment).
Here's a breakdown of the key components labeled in the image:

1. SCADA Panel (Top Left)

SCADA (Edibon SCADA software) is used for control and data acquisition.

Includes buttons for:

START / STOP: Start or stop the process.

CALIBRATE: Calibrate sensors.

QUIT: Exit the program.

VIEW DATA: Access logged or real-time data.

2. Process Diagram (Center)

 Central schematic of a control system, likely involving air flow, temperature,
or pressure.

 Shows a motor with adjustable vanes or fans, and sensors placed in different
sections (SEC-1 to SEC-4).

 Arrows show the flow of material or air.

 Components:
  PRODUCT CONDUCT

 FEED ADJUSTMENT

3. Sensors Panel (Top Right)

 Displays sensor readings for different sections (SEC-1 to SEC-4):

 Could represent temperature, pressure, or flow rates.
 Sensor data is shown in real-time.
 Useful for monitoring how process variables change.

4. PID Control Panel (Bottom Right)

 PID (Proportional-Integral-Derivative) Controller setup.

 Parameters:
 Setpoint: Desired value of the process variable.
 Actual Value: Current value.
 Error: Difference between the setpoint and actual value.
 Buttons to activate and adjust PID control.

5. Graph Area (Bottom Center)

 Two real-time plotting graphs labeled Graph A and Graph B.

 Used to display trends of sensor readings and controller outputs.

6. Sensor Selection (Bottom Left)

 Allows user to select which sensor data to plot.

  Options from Sensor 1 to Sensor 6.

 Option to reset the graph.

Applications:

 Pharmaceutical Industry
 Solid-liquid extraction is widely used to extract active pharmaceutical
ingredients (APIs) from natural sources like medicinal plants. It's a key step
in the production of herbal medicines, tinctures, and nutraceuticals.

 Food and Beverage Industry

 SLE is used to extract flavors, colors, caffeine, and essential oils from plant
materials such as tea leaves, coffee beans, vanilla pods, and spices. It's also
used in sugar extraction from sugarcane and sugar beets.

 Chemical Industry
 This technique helps extract valuable chemicals, dyes, and organic
compounds from solid raw materials. It’s also used in the recovery of
catalysts or residual reactants from solid reaction mixtures.

 Biotechnology
 Solid-liquid extraction plays a role in extracting enzymes, proteins, and
secondary metabolites from microbial biomass or plant tissues in various
biotechnological applications.

 Agriculture and Agro-Industry

 Used in extracting natural pesticides, fertilizers, or growth hormones from
organic or plant-based materials. It's also applied in oil extraction from
seeds and nuts.

 Cosmetic Industry
 Essential oils, natural colors, and fragrances used in cosmetics are often
extracted from herbs and flowers using solid-liquid extraction methods.
 Environmental Engineering
 Applied in extracting pollutants or hazardous compounds from soil or solid
waste samples for environmental testing and remediation purposes.

 Metallurgical Industry
 Used for leaching valuable metals from ores and minerals — such as gold,
copper, or uranium — using suitable solvents.

Experiments of Separation process-1.

Experiment 1

(Wetted Wall gas Absorption column)

Objective:
To calculate rate of absorption of air (Oxygen) into water from analysis of
liquid water flowing down wetted wall gas absorption column

Equipment Setup / Apparatus:

 Wetted Wall Gas Absorption Column Apparatus

 DO meter

Reagents:
 Water
 Air

Procedure:
  Fill the liquid reservoir tank at the base of the column to approximately
threequarters full with (preferably) deionized water. Note the volume
added [VT liters].
 Start the liquid pump and adjust the water flow through the column to
approx. 6 liters/minute on flowmeter F1 by adjusting flow control valve C1.
 Start the air blower and adjust control valve C2 to give an air flow of
approx. 10% of full scale on flowmeter F2.
 After 5 minutes of steady operation, take samples at 5 minute intervals
from water outlet. Take 150ml samples at known times in each case.
 Analyze the samples using DO meter. 6. Repeat the above process for
different flow rate of water and air. 7. Compare the results for different
flow rates and draw the graph.

Data Analysis:

Water flow rate = _____________

Air flow rate = _____________

Air flow rate = 6 L/min

Sr No. Air Flow Rate Water Flow Dissolve O2 Time Air Humidity
rate
1 6 4 7.1 3
2 6 6 3.5 6
3 6 8 3 9

At Water Flow Rate = 6 L/min

1 7 4 21.6 85 69
2 8 4 32.5 86 68
3 9 4 38.9 86 68
 Experiment 2.
Objective:
To determine the regeneration efficiency of cation resin and an anion resin.

Equipment Setup / Apparatus:

Ion Exchange Unit , Beaker 500 ml , Glass Stirrer.

Figure:
Reagents:

Cation Exchange Resin, Anion Exchange Resin, HCl, NaOH, Test Water
containing dissolved solids, Distilled or Demineralized Water .

 Theory: (DEMINERALIZATION);
 Theory of Ion Exchange Experiment

 What is Ion Exchange?

 Ion exchange is a reversible chemical process in which ions from a liquid
solution are exchanged with ions attached to an insoluble solid resin. This
process is selective, meaning that certain ions are more easily exchanged
than others depending on their charge and size.

 Types of Ion Exchange Resins

 There are two primary types of ion exchange resins:
 Cation Exchange Resins: Replace positive ions (e.g., Ca²⁺, Mg²⁺) with H ⁺
or Na⁺ ions.
 Anion Exchange Resins: Replace negative ions (e.g., Cl⁻, SO₄²⁻) with
OH⁻ or other anions.

 How It Works
 When a solution passes through a column filled with ion exchange resin, the
resin captures the target ions from the solution and releases its own ions in
return. For example, in water softening, calcium and magnesium ions are
replaced with sodium ions.

 What Happens in the Experiment

 In this experiment, a known ion-containing solution is passed through the
ion exchange column. The change in ion concentration is monitored before
and after the exchange, showing the resin’s efficiency and capacity.

 Regeneration of Resin
 Once the resin becomes saturated with exchanged ions, it can be
regenerated by washing it with a strong solution of the original ions (e.g.,
NaCl or HCl). This restores the resin’s ability to perform future exchanges.

 Selectivity of Ions
 Not all ions exchange at the same rate. Resins have selectivity — some ions
are exchanged more easily due to their valency, size, and hydration energy.

 Applications Demonstrated
 The experiment models real-world uses like water softening, deionization,
and removal of heavy metals from wastewater.

 Important Parameters Observed

 During the experiment, key observations include:
 Breakthrough curve
 Exchange capacity
 Ion concentration changes
 Efficiency of resin

 Purpose of the Experiment

 The main goal is to understand how ion exchange works practically and to
evaluate the resin’s ability to purify or alter the composition of a solution.
Procedure:
A. For Cation Resin Regeneration Efficiency
 Fill cation column to a depth of 300mm with a cation exchanger resin in the
hydrogen ion form.
 Fill anion column to a depth of 300mm with an anion exchange resin in the
hydroxyl form.
 Fill tank A with 100ml of a 10% HCl solution.
 Fill tank B with 100ml of a 5% NaOH solution.
 Fill tank C with test water containing 800 to 1000 mg/liter of dissolved solids.
 Fill tank D with distilled or demineralized water.
 If tap water is used, the concentrations of the principal cations and anions, as
well as the total dissolved solids, must be determined if not already known.
 From a knowledge of the concentrations of the main cations and anions in the
water to be used, calculate the total strength in meq/liter.
 This will be used in calculating the regeneration efficiency of the two resins. The
electrical conductivity should also be measured.
 Backwash: Select tank D, open valves 3 and 6.
 Regenerate: Select tank A, open valves 2 and 10. Collect whole of the solution.

B. For Anion Resin Regeneration Efficiency

 To determine the regeneration efficiency of the anion resin it will be necessary
to carry out the full demineralization experiment.
 Since the exchange capacities of cation resins are generally greater than those
of anion resins, it is expected that the anion resin will be first to be exhausted

Data Analysis:
Final Depths:

CATION = _______________

ANION = _______________

Sodium ion concentration (meq/ml) =

Volume of solution used (ml) = (π × 15 × 10−3) ^2/ 4 × Final Depth.

Exchange capacities can now be calculated.

Exchange Capacity = sodium ion / Volume of wet Bed.

Actual Exchange Capacity = real quantity – Actual Quantity.

Experiment 3
(Solid Liquid Extraction Unit)
Objective:
Use of the conductivity meter for determining mixture composition.
Equipment Setup/ Apparatus:
Solid liquid extraction unit, Conductive-meter, Measuring Cylinder 100ml.
Reagents:
Sodium Bicarbonate, Water.
Procedure:

1) Measure the conductivity of pure Water.

2) Make up small quantities of 0.2M, 0.4M, 0.6M, 0.8M and 1M sol. of sodium
bicarbonate.
3) Find out the conductivity of different solutions.

Molarity of sodium bi carbonate solution Conductivity

0.0 0
0.2 14.2
0.4 25.7
0.6 35.8
0.8 45.7
1.0 50.7

Graph:

Experiment 4
Objective:
To demonstrate how a mass balance is performed on the extraction column, and to
measure the mass transfer coefficient and its variation with flowrate with the aqueous
phase as the continuous medium.

Equipment Setup / Apparatus:

Liquid-Liquid Extraction Apparatus, 250ml Conical Stoppered Flask, 250ml Measuring
Cylinder, Pipette with Rubber Bulb, Burette.
Figure:

 The solvent metering pump is calibrated in percentage of maximum flow which

varies slightly from pump to pump
 The pump should be calibrated initially by setting F2 to 100%, setting valve V8 to
the calibrate position and measuring the flow from the pump, using a measuring
cylinder and stopwatch.
 Calculate the flow rate produced settings of 10% intervals (ml per minute), then
plot a graph of ml per minute against percentage of metering pump stroke.
Thereafter any selected flow may be obtained by using the graph.

Reagents:
0.1 Molar NaOH Solution, Phenolphthalein, Propionic Acid, Trichloroethylene, Water .

Procedure:
WARNING:

 Concentrated Sodium Hydroxide can form explosive volatile products when in contact with
Trichloroethylene. Ensure that diluted Sodium Hydroxide (NaOH) is used when performing this
experiment.
 1) Add 100ml of propionic acid to 10 liters of trichloroethylene. Mix well to ensure an even
concentration then fill the organic phase feed tank (bottom tank) with the mixture.
  2) Switch the level control to the bottom of the column (electrode switch S2)
 3) Fill the water feed tank with 15 liters of clean de-mineralized water, start the water feed
pump and fill the column with water at a high flow rate.
 4) As soon as the water is above the top of the packing, reduce the flow rate to 0.2 liters/min.
5) Start the metering pump and set at a flow rate of 0.2 liters/min.
 6) Run for 15-20 minutes until steady conditions are achieved, monitor flow rates during this
period to ensure that they remain constant.
 7) Take 15ml samples from the feed, raffinate and extract streams.
 8) Titrate 10ml of each sample against 0.1M NaOH using phenolphthalein as the indicator. (To
titrate the feed and raffinate they may need continuous stirring using a magnetic stirrer).
 9) Repeat the experiment with both the water and trichloroethylene flow rates being
increased to 0.3 1iters/min

Data Analysis:

Separation Initial Point Final Point

Dark Blue 0 39
Total Separation
CCL4 , Water , 0 94.5
Iodine

Experiment 5
Objective:
To study the demineralization of water and to determine the exchange capacities of a
hydrogen ion cation exchanger and an anion exchanger.

Equipment Setup / Apparatus:

Ion Exchange Unit, Beaker 500 ml, Glass Stirrer.

Figure:
Reagents:
Cation Exchange Resin, Anion Exchange Resin, HCl, NaOH, Test Water containing
dissolved solids, Distilled or Demineralized Water.

Theory:

 Water demineralization is a process used to remove dissolved minerals and

impurities from water by using ion exchange resins. In the process, water
passes sequentially through two types of resins—a cation exchanger and an
anion exchanger—that replace dissolved ions with hydrogen (H ⁺) and
hydroxide (OH⁻) ions, respectively, resulting in the formation of pure water
(H₂O). This experiment not only purifies water but also demonstrates how
to evaluate the exchange capacities of these resins.

Principle of Ion Exchange

Cation Exchange:

A hydrogen ion form cation exchanger contains fixed sulfonate (–SO₃⁻) groups. When
mineral-rich water flows through the resin, metal cations (e.g., Ca²⁺, Mg²⁺, Na⁺) are
exchanged for H⁺ ions according to the reaction:

Resin–H+ + Mn+ → Resin–M(n)+ + nH+

Anion Exchange:
An anion exchanger in the hydroxide form contains fixed quaternary ammonium
(–NR₃⁺) groups. It replaces anions (e.g., Cl⁻, SO₄²⁻, NO₃⁻) with OH⁻ ions:

Resin–OH− + X− → Resin–X− + OH−

Overall Reaction for Demineralized Water:

When water passes through both resins in series, the H⁺ ions released by the cation
exchanger and the OH⁻ ions released by the anion exchanger combine to form water :

H+ + OH− → H2O

3. Reaction Mechanism and Efficiency

 Sequential
The water first flows through the cation exchanger where metal cations are
replaced by H⁺. Then, as it passes through the anion exchanger, anions are
removed by exchanging with OH⁻.
 Breakthrough
The point at which the conductivity of the effluent begins to rise indicates
that one of the resins is reaching saturation. Simultaneously, changes in pH
provide clues about whether the cation or anion resin is exhausted.
 Exchange
The exchange capacity is defined as the maximum amount of ions that the
resin can capture. It is determined by measuring the volume of water
treated until breakthrough occurs and calculating the total moles of ions
exchanged per unit weight of the resin

Determination of Exchange Capacities

For the Cation Exchanger:

Once the effluent's pH rises (indicating excess H⁺ release), you can calculate the
cation exchange capacity by assessing the total quantity of metal ions removed :

For the Anion Exchanger:

If instead the conductivity increases while the pH remains low (indicating anion
exchange failure), the anion exchanger’s capacity is calculated from the total
moles of anions removed:

In both cases, the moles exchanged can be determined using titration or

conductivity data against known concentration standards.

5. Applications and Significance:

This process is critical for producing high-purity water required in industries such
as power generation, pharmaceuticals, and electronics. The experiment also
provides valuable insights into resin performance and regeneration, helping in
designing more efficient water treatment systems.

Procedure:
A. Preliminary Requirements
 Fill cation column to a depth of 300mm with a cation exchanger resin in the
hydrogen ion form.
 Fill anion column to a depth of 300mm with an anion exchange resin in the
hydroxyl form.
 Fill tank A with 100ml of a 10% HCl solution
Fill tank B with 100ml of a 5% NaOH solution.
 Fill tank C with test water containing 800 to 1000 mg/liter of dissolved solids.
 Fill tank D with distilled or demineralized water.
 If tap water is used, the concentrations of the principal cations and anions, as
well as the total dissolved solids, must be determined if not already known.
 From a knowledge of the concentrations of the main cations and anions in the
water to be used, calculate the total strength in meq/liter.
 This will be used in calculating the exchange capacities of the two resins. The
electrical conductivity should also be measured.

C. Demineralization:

 Select tank C, open valves 2, 13 and 15. Set flow rate to between 50 and 70
ml/min
Note time at which flow is started and take conductivity readings at 5 minute
intervals.
 At 20 minute intervals draw off samples from valve 10 and measure pH value.
 Note the time when the conductivity of the demineralized water begins to rise,
i.e. the breakthrough point at which one of the resins has become exhausted.
 As soon as possible after this point, take another small sample from valve no. 16
and measure its pH. 6) If this pH is higher than the values previously recorded, it
indicates that the cation exchanger has become exhausted.
 It is advisable to confirm this by drawing one or two further samples for pH
determination.
 The experiment should be stopped at this point, and the exchange capacity of the
cation exchanger calculated.
 It is then possible to determine the exchange capacity of the anion exchanger in
this experiment.
 If, on the other hand, the pH of the cation exchanger effluent continues at a low
value, the rising conductivity of the final effluent indicates that the anion
exchanger is exhausted, and its capacity can be calculated.
 In the latter event, the exchange capacity of the cation exchanger can be
determined by continuing the flow of water through the first column only,
collecting the water which passes through it and measuring pH values until the
breakthrough point, when the pH begins to rise.
 D. Backwashing:
 Each column should be separately backwashed.
 In each case, the rate of backwashing should be controlled to give not more
than 50% expansion of the bed.
 Measure the final depths of the two beds.

D. Cation Regeneration:
o Regenerate the cation exchanger.
o Select tank A, open valves 2 and 12. Follow the acid with distilled
 demineralized water from tank D, to flush out any surplus acid.
o Check pH of effluent and continue flushing until pH has returned to above
5.0.
E. Anion Regeneration
1) Regenerate the anion exchanger.

2) Select tank B, open valves 1 and 15, followed by distilled or demineralized water
from tank D until pH of the effluent has returned to below 9.0

Data Analysis:
In the demineralization experiment, the breakthrough point is detected by
readings of pH (for the cation exchanger) or conductivity (for the anion
exchanger) instead of by direct measurement of concentrations.

Time(min 0 3 6 9 12 15 18
)
Cation 123.1 1.4 29.8 33.9 62.4 86.1 98.9
 Anion 16 0.2 0.9 1.5 1.9 2.4 3.1

In order to calculate the exchange capacities in terms of milli-equivalents (meq), it is

necessary to convert pH or conductivity readings to meq/liter.

To convert Conductivity values to meq/liter

If pH reading is “x”

Hydrogen ion concentration = 10-x moles/liter

= 103-x meq/liter

(B )To convert conductivity values to meq/liter.

 For a water with a given content of salts, the electrical conductivity is closely
proportional to the concentration of total dissolved solids.
 Although these solids consist of several salts of varying electrolytic properties, it
is sufficiently accurate to assume that electrical conductivity is also proportional
to the the total concentration in terms of meq/liter.
 The constant of proportionality was established by determination of the electrical
conductivity and the strength of meq/liter of the raw water.
 Hence the electrical conductivity of the demineralized water can be converted to
meq/liter. In any event these figures should be very low .

Other Calculations:

Final Depths:

CATION = _______________

ANION = _______________