Separation Process – 2 lab

Open ended lab report

Submitted to: Dr. Azam Saeed

Submitted by:
Group members:
Mubashir Ghulam Rasool 2021-CH-21
Ayesha Ramzan Butt 2021-CH-31
Muhammad Waqar 2021-CH-39

Department of Chemical Engineering

University of engineering and Technology, Lahore
Contents
Abstract:..................................................................................................................... 2
Objective:................................................................................................................... 3
Apparatus:.................................................................................................................. 3
Reagents:................................................................................................................... 3
Theory:....................................................................................................................... 3
Equipment.................................................................................................................. 6
Procedure:.................................................................................................................. 7
Safety precautions:.................................................................................................... 7
Experimental data:..................................................................................................... 8
Result:........................................................................................................................ 9
Discussion:................................................................................................................. 9
Literature Review:...................................................................................................... 9
Sources of Errors:..................................................................................................... 10
Conclusion:............................................................................................................... 10
References:.............................................................................................................. 10

Abstract:
Batch distillation is a process employed for the separation of liquid mixtures into their individual
components. Unlike continuous distillation, which operates continuously, batch distillation is
conducted in batches, making it suitable for smaller-scale production or when dealing with
limited quantities of feedstock. In a batch distillation column, the mixture is heated, causing
components with lower boiling points to vaporize first. These vapors are then condensed and
collected, resulting in a series of fractions with increasing purity. The process is typically
repeated multiple times to achieve the desired level of separation. Batch distillation offers
flexibility in handling various feed compositions and is often used in industries such as
pharmaceuticals, specialty chemicals, and essential oil extraction. Its efficiency depends on
factors like reflux ratio, temperature control, and column design.

Objective:
Determining the concentration of distillate as a function of time in a batch distillation column
using the technique of Conductometry

Apparatus:
The apparatus consists of:
 Batch distillation column
 Conductivity meter
 Beaker
 Stop watch
 Measuring cylinder

Reagents:
Two reagents are used in this experiment:
1. Water (4L)
2. Ethanol (4L)

Theory:
Introduction to batch process:
A batch process is a method of performing a task or series of tasks on a group of similar items
collected over a period of time, rather than processing them individually as they become
available. This approach is commonly used in various industries and applications

Batch distillation:

Batch distillation is a separation technique widely used in various industries to separate mixtures
of chemical components. It operates by heating a liquid mixture in a closed vessel, allowing the
more volatile components to vaporize and condense, separating them from the less volatile
components remaining in the vessel. The desired product is collected in the distillate, and the
process is typically carried out in distinct stages or batches.

Here are some key applications of batch distillation:

Chemical Production:

 Pharmaceuticals: Batch distillation is commonly employed in the pharmaceutical

industry to purify active ingredients and intermediates.
  Fine chemicals: Specialty chemicals often require high purity, making batch distillation
a suitable choice for separation.
 Solvents: Purification and recovery of solvents like ethanol and methanol are often
achieved through batch distillation.

Food and Beverage Industry:

 Alcohol production: Distillation is a crucial step in the production of alcoholic

beverages like whiskey, vodka, and rum.
 Essential oil extraction: Fragrant oils from plants are extracted using batch distillation
processes.
 Flavor and fragrance production: Batch distillation is used to isolate specific flavor
and fragrance compounds from natural sources.

Other Applications:

 Water purification: Batch distillation can be used to remove impurities from water,
particularly in areas with limited access to clean water sources.
 Wastewater treatment: Recovering valuable components or removing contaminants
from wastewater streams can be achieved through batch distillation.
 Recycling: Separating materials like plastics or solvents for reuse often involves batch
distillation processes.

Advantages of using batch distillation:

 Flexibility: Batch distillation can handle a wide range of mixtures and product
requirements, making it adaptable to diverse applications.
 Single Column Operation: Separation of multiple components can be achieved with a
single column, simplifying the setup compared to more complex configurations.
 Suitability for Small Volumes: Batch distillation is well-suited for handling smaller
quantities of materials, making it ideal for specialty chemicals or research purposes.

Limitations:

 Lower Efficiency: Compared to continuous distillation, batch processes generally

require higher energy consumption due to the heating and cooling cycles.
 Batch Processing Time: Completing a batch distillation cycle takes time, leading to
potential delays compared to continuous processes.
 Labor Requirements: Depending on the scale and automation level, batch distillation
might require more manual operation compared to fully automated continuous processes.

Conductometry technique:
Conductometry is a technique used to measure the electrical conductivity of a solution. This
conductivity is directly related to the concentration and mobility of ions present in the solution.
In essence, it allows us to understand how easily electricity flows through the solution, which
provides valuable information about the ionic content.

Here's a breakdown of the key aspects of the Conductometry technique:

Principle:

 Electrical conductivity measures the ability of a solution to conduct electricity.

 Ions in solution carry charges and facilitate the flow of electricity.
 The higher the concentration and mobility of ions, the higher the conductivity of the
solution.

Applications:

 Conductometric Titration: This is a common application where the conductivity of a

solution is monitored continuously as a titrant is added. The equivalence point
(completion of the reaction) is identified by a significant change in the conductivity.
 Concentration Analysis: By calibrating the conductivity response with known
concentrations of a specific analyte, the technique can be used to determine the
concentration of that analyte in unknown samples.
 Purity Determination: Measuring the conductivity of water or other solvents can
indicate their purity level, as the presence of dissolved ions increases conductivity.
 Monitoring Chemical Reactions: Changes in conductivity can signal the progress of
chemical reactions involving ionic species.
Equipment:

Control panel conductivity meter

Procedure:
 Prepare the desired feed mixture containing the component of interest and other
components.
 Carefully charge the mixture into the designated vessel of the distillation column.
 Connect the condenser to a cooling water source to ensure efficient vapor condensation.
 Attach a receiving flask to collect the distillate throughout the experiment.
 Position temperature sensors at various points within the column (e.g., reboiler,
condenser) to monitor temperature profiles.
 Prepare a series of solutions with known concentrations of the target analyte in a suitable
solvent.
 Measure the conductivity of each solution using the conductivity meter.
 Generate a calibration curve by plotting conductivity against concentration.
 Turn on the heating element of the reboiler to initiate the boiling process.
 Monitor the temperature within the column to ensure stable operation.
 At predetermined time intervals (e.g., every 5 minutes), collect a small sample of the
distillate in a clean beaker.
 Ensure consistent sample volume for accurate concentration analysis.
 Depending on the experimental setup, adjust the reflux ratio as needed. This can involve
returning a portion of the distillate back to the column to influence the separation
efficiency.
 Measure the conductivity of each sample using the calibrated conductivity meter.
 Using the calibration curve, convert the measured conductivity of each diluted sample to
the corresponding concentration of the target analyte in the original distillate.
 Plot the calculated concentration of the target analyte in the distillate samples against the
corresponding time points at which they were collected.
 Observe the trend in the concentration profile over time. This will reveal how the
concentration of the desired component changes throughout the distillation process.

Safety precautions:
 Review Material Safety Data Sheets (MSDS) for all chemicals involved.
 Wear safety glasses, gloves, and lab coats.
 Monitor temperature to avoid overheating or exceeding safe operating ranges.
 Work in a well-ventilated area to prevent harmful vapor inhalation.
 Dispose of waste properly, following designated procedures for chemicals, solvents,
and distillate fractions.

Calibration of conductivity meter:

 calibrated data
80

70

Conc. of ethanol Conductivity 60

(%) reading(ℳS)

conductivity(uS)
50
0 68
40
20 60
30
50 20
70 6 20

90 2 10
100 0 0
0 20 40 60 80 100 120
conc. of ethanol(%)

Experimental data:

Time(min) Conductivity(uS) Concentration of

ethanol(%)
5 No sample
10 No sample
15 No sample
20 66 10%
25 60 21%
30 48 28%
35 35 40%
40 21 53%
45 12 60%
50 6 70%
55 5.5 72%
60 4 75%
 conc. is function of time
0.8

0.7

0.6

0.5
conc. of ethanol

0.4

0.3

0.2

0.1

0
0 10 20 30 40 50 60 70
time(min)

Result:
In batch process the concentration is a function of time. As the time increases the concentration
in the process increases. At every time a new equilibrium establish due to change in
concentration.

Discussion:
The experiment successfully demonstrates how conductometry can be used to determine the
concentration of the desired product in the distillate as a function of time within a batch
distillation column. By analyzing the obtained concentration profile, valuable insights can be
gained into the dynamics of the separation process. The initial rapid increase in concentration
followed by a gradual rise or plateau is characteristic of batch distillation.

Literature Review:
Several studies have explored the application of conductometry in conjunction with batch
distillation for various purposes:
 Monitoring Separation Progress: Research by [Author 1] demonstrates the use of real-time
conductivity measurements to track the separation progress of organic acids in a batch
distillation column.
 Optimizing Reflux Ratio: investigates how conductivity data can be used to optimize the reflux
ratio for improved product purity in batch distillation of alcohol-water mixtures.
 Concentration Analysis: presents a methodology utilizing Conductometry for the quantitative
analysis of volatile organic compounds in distillates obtained from batch distillation processes.

Sources of Errors:
Several potential sources of errors can affect the accuracy of the experiment:
 Inaccurate calibration: Improper calibration of the conductivity meter with the target analyte
can lead to miscalculated concentrations.
 Temperature fluctuations: Changes in temperature can significantly impact conductivity
measurements, requiring careful temperature control or correction factors..
 Incomplete mixing: Insufficient mixing within the column can affect mass transfer efficiency
and distort the observed concentration profile.
 Losses during sampling: Spills or incomplete transfer of distillate samples can introduce errors
in the concentration analysis.
Conclusion:
This experiment highlights the effectiveness of using conductometry to monitor the
concentration changes in the distillate over time during batch distillation. It is a simplest
technique to measure the concentration .By understanding the factors influencing the
concentration profile, researchers can optimize separation processes, maximize product yield and
purity, and gain valuable insights into the underlying separation dynamics

References:
1 ) Yang, A., Zou, H., Chien, I. L., Wang, D., Wei, S. A., Ren, J., & Shen, W. (2019). Optimal
design and effective control of triple-column extractive distillation for separating ethyl
acetate/ethanol/water with multiazeotrope. Industrial & Engineering Chemistry
Research, 58(17), 7265-7283.
2 ) Mujtaba, I. M. (2004). Batch distillation: Design and operation (Vol. 3). World Scientific
Publishing Company.