Faculty of Engineering

Department of Chemical Engineering

Bellville Campus

Practical Manual: DISTILLATION

2016
Subject name:

CHEMICAL ENGINEERING TECHNOLOGY III

Subject Code:

CET301S

ND:

CHEMICAL ENGINEERING

NQF level:

Lecturers:

Mr. G Hangone
Dr. D De Jager

Revision No

Approved

Date

Draft 1

D De Jager

July 2016

Purpose Statement for Qualification

This qualification is intended for process or chemical engineering technicians working in the process or
metallurgical related industries. Learners achieving this qualification have the competence to apply existing
process technology to chemical engineering related problems, process design and will illustrate technical
competence thus contributing to the needs of the chemical profession.

TABLE OF CONTENTS
1.

RULES FOR ATTENDING THE PRACTICAL SESSIONS ......................................................... 1

2.

GENERAL INFORMATION ........................................................................................................ 2

3.

DECLARATION ......................................................................................................................... 2

4.

LAB SAFETY RULES ................................................................................................................ 2

5.

MARK ALLOCATION ................................................................................................................. 3

6.

DISTILLATION ........................................................................................................................... 4

1.

RULES FOR ATTENDING THE PRACTICAL SESSIONS

The following is important to attend to:

Two practicals per semester will be performed. The short report constitutes 40% of the overall
practical mark, and the long report 60%.

The contribution of the overall practical mark to the year mark is equivalent to 15% of the final
mark.

Students are required to get a minimum of 50% for the practicals to pass the subject.
It is expected of each student to do all the practicals. A student will receive a mark of NIL for
the practical if the student is absent unless the absence on medical grounds. A medical
certificate should be produced for verification purposes.

A student may not hand in a report if the student did not attend the practical.

Data generated by groups other than the students group may not be used in the report unless
provided by the Technical Officer.

A draft copy of the report must be uploaded onto the anti-plagiarism website SafeAssign via
Blackboard to detect plagiarism. Students may alter their reports if plagiarism is detected and
resubmit to SafeAssign until the report meets the requirements. Any irregularities should be
rectified before the hardcopy of the report is submitted.

A report will be regarded as not submitted if the entire report has not been uploaded to
SafeAssign and as a result can be awarded a mark of zero.

Students should understand plagiarism and the various types. Students should also heed the
seriousness of the offence and that such an offence will carry the minimum penalty of
receiving a mark of zero for parts of the report plagiarized. A mark of zero can be awarded.

The report cover page should clearly indicate the report title, students full name, student
number, group number, date performed and date submitted.

The due date for practical reports is two weeks after the practical was performed unless the
due date falls in the holidays. In such a case the due date falls on the first day of term that the
technical officer is at the campus.

Students are given the opportunity to submit the report in an allocated time slot and sign for its
submission. Reports submitted outside this time slot should be deposited in the allocated box
but will not receive verification upon receipt.

If a practical is handed in later than the due-date, 10 % will be deducted from the student's
mark for each day the practical is handed in late. After three days overdue, the report will
receive zero.

At the end of the practical program, groups may have the opportunity to present a specific
practical.

2.

GENERAL INFORMATION

Practical Scheduling
The schedule of practicals for each group is provided. Students are expected to perform each
practical on the day and between the hours specified, and will not be permitted to work outside
these hours unless prior agreement has been granted by the Practical Supervisor. Any problems
with regard to the practical schedule should be taken up with the Practical Coordinator as soon as
possible. If scheduling changes are made with the agreement of the Coordinator, hand-in dates will
also be changed; otherwise the original dates will remain in force.

Location of Equipment
Experiments will be performed at the Cape Peninsula University of Technology, Bellville Campus in
the Chemical Engineering laboratory.

3.

DECLARATION

While all experimental work will be performed in groups, the practical report must be the student's
own individual work. The following undertaking is incorporated in the cover page of each report and
must be signed by the student:

'I certify that this report is my own unaided work, except for the assistance received from the
teaching staff. I undertake not to pass this report onto any other student.

4.

LAB SAFETY RULES

Keep books, briefcases, and other property (especially jewellery) away from your work
bench.

DO NOT TASTE anything and AVOID INHALING toxic or noxious fumes.

Clean up spills as soon as possible. Wash with water to dilute.

When working with concentrated acids, take special care to AVOID SKIN CONTACT. Also
work over the sink to avoid any spillage on the bench.

When DISPOSING of LIQUIDS, do so into RUNNING WATER in the sink. Wash down with
lots of water.

Any broken apparatus must be reported immediately.

Smoking, eating or drinking will not be tolerated in the laboratory.

Unauthorized experiments are strictly forbidden.

Students are reminded that many of the experiments performed have inherent dangers
associated with them and due precaution should be observed at all time. These dangers
include the effects of rotating equipment, electrical machinery, high pressure air and steam.
First aid equipment is available chemical engineering laboratory. Fire hoses, fire
extinguishers and safety showers are placed on all levels of the building. An eye bath is
located in the analytical laboratory. Students should check to see where these items are
located. Students must wear appropriate footwear and ladies should wear jeans in place of
skirts while performing experimental work. Smoking and eating is not permitted in the
laboratory.

5.

REPORT ANY ACCIDENT, however small, to your supervisor immediately.

MARK ALLOCATION
LONG REPORT: Distillation
%
Title page

Synopsis

Introduction

Literature Review and Theory (including in-

10

Mark

text referencing)
Experimental Set-up and Procedure

10

Results and Discussion

55

Conclusions

Bibliography and personal impression

TOTAL:

100

The discussion must include intext referencing and relate the some of the results obtained
to theory.

6.

DISTILLATION

Aim
1. Acquaint the students with the concept of Continuous Distillation
2. Calculate the number of theoretical plates
3. Perform an energy balance across the condenser
Introduction
Distillation is defined as the separation of a m i x t u r e o f l i q u i d s i n t o t h e i r c o m p o n e n t s
b y u s i n g t h e r e l a t i v e v o l a t i l i t y o f t h e l i q u i d s . One of the essential requisites to carry
out distillation successfully is that substances to be separated h a v e d i f f e r e n t b o i l i n g p o i n t s .
A vapour enriched in the more volatile component (or with a lower boiling temperature) will
be formed when heat is applied to the mixture while the less volatile component will
predominate in the liquid phase.

Distillation can be done continuously and in batch.

Continuous distillation: the supply (liquid mixture to be distilled) is introduced constantly to the
reboiler, so that the quantity of liquid in the boiler will always remain constant. We obtain a
distillate from the condenser and a liquid (residue) at the lower part of the system. As the mass
balance of the system must be fulfilled, the quantity of supply introduced in the system will be
the same as the one that goes out as a distillate and as a remainder. One of the characteristics of
this type of distillation is that the composition of liquid and vapor is constant throughout the
column with respect to time.

Batch distillation: a volume of liquid to be distilled is added to the column before distillation
commences. It differs from a continuous process where feed is added continuously as products are
formed. It can be deduced that with time the volume of liquid in the distillation column will diminish
and become concentrated with the liquid/s of higher boiling point/s as the distillate is formed. The
temperature of the mixture will rise as the more volatile component evaporates thereby increasing
the amount of less volatile component in the vapour. Generally batch distillation is preferable to
continuous when small volumes are being distilled. Sporadic or infrequent availability of feed would
also prove batch distillation more feasible. Batch distillation may be more promising if operations
upstream or downstream are batch or the feed varies in quality. Another advantage of a batch
operation is the possibility to draw off various qualities of products over time

Cooling water

Cooling water

Vapour

Vapour
Condensate
Condensate
Reflux

Reflux

Distillate

Feed

Reboiler

Distillat
e
Energy
Source

Reboiler

Energy Source

Bottoms

Figure 1: Schematic of (a) a batch and (b) a continuous distillation column

Experimental procedure
1. Introduce the test solution in the boiler through the appropriate mouth using a funnel to
facilitate the process.
2. Switch on the refrigeration circuit.
3. Run the SCADA-UDDC or SCADA-UDCC program and select a name for the data file.
4. Switch on the heating mantle and program a value higher than the boiling temperature of the
most volatile component and lower than the boiling temperature of the least volatile
component as the set point.
5. Turn the reflux valve to the 100% reflux position. It must be taken into account that the reflux
ratio is expressed as outlet percentage and its variation with the percentage is linear, being
0% when all the condensed vapor returns to the column and 100% when all the condensed
vapor is extracted and distilled.
6. Let the distillate flow get stable.
7. Close the valve leading back to the column from the distillate tank and record the time it
takes to fill 100ml of distillate. Take a sample of the distillate.
8. Record the temperatures and cooling water flow rate.
Results and Calculations
1. From the distillate and bottoms concentrations, determine the number of theoretical stages
using the McCabe-Theile method and compare to the actual number.
5

2. Perform an energy balance around the condenser using the cooling water data and rate of
distillate production.

APPENDIX A: Table of liquid and vapour equilibrium data for an ethanol and water mixture.
1

YA (mole fraction ethanol in vapour phase)

0.9

0.8

0.7

0.6

0.5

0.4

0.3

0.2

0.1

0
0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

XA (mole fraction ethanol in liquid phase)

Figure 2: Chart of liquid and vapour equilibrium data for an ethanol and water mixture