Experiment Instructions

CE 600 Continuous Rectification

 CE 600 CONTINUOUS RECTIFICATION
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

Experiment Instructions
Dipl.-Ing. (FH) Klaus Schröder

Last modification by: Dipl.-Ing. (FH) Peter Mittasch

This manual must be kept by the unit.

Before operating the unit:

- Read this manual.
- All participants must be instructed on
handling of the unit and, where appropriate,
on the necessary safety precautions.

Version 2.9 Subject to technical alterations

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 CE 600 CONTINUOUS RECTIFICATION

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Table of Contents

1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
1.1 Proper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
1.2 Teaching instructions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3

2 Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
2.1 Intended use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
2.2 Structure of safety instructions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
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2.3 Safety instructions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

3 Unit Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
3.1 Process diagram . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
3.2 Layout . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
3.3 Equipment Functions and Components . . . . . . . . . . . . . . . . . . . . . . 14
3.3.1 Components for the thermal process . . . . . . . . . . . . . . . . . . 14
3.3.2 Control cabinet . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
3.4 Data acquisition program. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
3.4.1 Installing the program . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
3.4.2 Operating the program . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
3.5 Commissioning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
3.6 Shutdown. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23

4 Theory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
4.1 Basic principles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
4.1.1 Distillation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
4.1.2 Rectification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
4.1.3 Azeotropic mixtures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33

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5 Experiments - Preparations, variants, instructions for performing . . . . . . . 35

5.1 Preparing the unit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
5.1.1 Tank volumes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
5.1.2 Refitting the columns . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
5.2 Accessories for performing experiments . . . . . . . . . . . . . . . . . . . . . . 41
5.2.1 Tanks, measuring cups. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
5.2.2 Measuring instruments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
5.3 Experiment variants. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
5.4 Experiments - batch mode. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43
5.4.1 Notes on performing experiments - operation at
ambient pressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43
5.4.2 Notes on performing experiments - operation with vacuum . 45
5.5 Experiments - continuous mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48
5.5.1 Notes on performing experiments. . . . . . . . . . . . . . . . . . . . . 48
5.6 Practical tips . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
5.6.1 Requirements for the water / water hardness. . . . . . . . . . . . 52
5.6.2 Pumping from the feed tanks into the evaporator . . . . . . . . . 52
5.6.3 Bottom product cooling at the end of an experiment . . . . . . 53
5.6.4 Reuse of input substances . . . . . . . . . . . . . . . . . . . . . . . . . . 55
5.6.5 Hose lengths . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56

6 Experiments - with ethanol/water mixture . . . . . . . . . . . . . . . . . . . . . . . . . 57

6.1 Recommended ethanol/water mixture. . . . . . . . . . . . . . . . . . . . . . . . 57
6.1.1 Material values . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
6.1.2 Determining concentration by density and temperature . . . . 61
6.1.3 Mixing behaviour. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62

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6.2 Definition of background conditions, experiment series . . . . . . . . . . 63

6.2.1 Method of operation of the unit . . . . . . . . . . . . . . . . . . . . . . . 64
6.2.2 Comparative experiments, experiment series . . . . . . . . . . . 68
6.2.3 Example of a batch experiment series . . . . . . . . . . . . . . . . . 69
6.2.4 Example of a continuous experiment series . . . . . . . . . . . . 72
6.3 Example of a batch experiment, V3. . . . . . . . . . . . . . . . . . . . . . . . . . 74
6.3.1 Experiment aims . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74
6.3.2 Experimental setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74
6.3.3 Performing the experiment . . . . . . . . . . . . . . . . . . . . . . . . . . 75
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6.3.4 Measured values . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77

6.3.5 Evaluation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82
6.3.6 Comments, assessment . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91
6.4 Example of a continuous experiment, V7 . . . . . . . . . . . . . . . . . . . . . 97
6.4.1 Experiment aims . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
6.4.2 Experimental setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
6.4.3 Performing the experiment . . . . . . . . . . . . . . . . . . . . . . . . . . 97
6.4.4 Measured values . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101
6.4.5 Evaluation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 106
6.4.6 Comments, assessment . . . . . . . . . . . . . . . . . . . . . . . . . . . 115

7 Appendix . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119
7.1 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119
7.2 Worksheets . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 120
7.3 Abbreviations and symbols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 123
7.3.1 Abbreviations used . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 123
7.3.2 Symbols used . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 124

8 Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 125

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1 Introduction

In physical-chemical engineering, liquid mixtures

that consist of mutually soluble fluids are often
separated by thermal processes. The main
processes are distillation and rectification.
The Continuous Rectification CE 600 experi-
mentation unit enables liquid mixtures to be
thermally separated by means of rectification in
the experiment.
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The unit consists of an electrically heated evapo-

rator in which the initial liquid mixture is heated
and evaporated. The steam rises through a
column and is subsequently condensed in a
water-cooled condenser. From here, all of the
condensate can be drained off as the top product,
or all or part of it can be returned to the column.
Either a sieve plate column or a packed column
can be used for the experiments. The column
head incorporates a port for the return flow of
distillate.
A pump can be used to pump mixture into the
column, permitting continuous running of experi-
ments. For that purpose, the sieve plate column
features three ports at different heights. The
separation behaviour varies depending on which
port is chosen. The packed column features a port
half way up.
A heat exchanger enables the pumped-in liquids
to be pre-heated.
A water jet pump can be used to generate a
vacuum in the entire tube system for vacuum
rectification.

1 Introduction 1
CE 600 CONTINUOUS RECTIFICATION

The unit can be operated locally from the control

cabinet. It is a good idea, however, to control the
unit from a self-supplied PC using software
supplied with the unit. This enables the available
measurements to be automatically recorded and
documented.

The range of experiments covers the following

variants:
• Discontinuous (batch) or continuous
• Sieve plate column or packed column
• Sieve plate column, 3 different infeed heads
selectable
• Reduction in the number of plates in the sieve
plate column
• Operation at ambient pressure or under
vacuum
• Operation with or without feed preheating

The instruction manual provides detailed

instructions on performing the experiment. The
method of operation is described in order to
illustrate the possibilities and limits of the unit.
Potential series of experiments for the
recommended ethanol/water material mix are
demonstrated. Two experiments from the series
are demonstrated, evaluated and commented
upon in detail by way of example.

2 1 Introduction
 CE 600 CONTINUOUS RECTIFICATION

1.1 Proper use

The Continuous Rectification experimentation

unit CE 600 is intended solely for educational
purposes and not for industrial production.

1.2 Teaching instructions

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The unit is designed so that all operations are

mostly visible and can be observed. The unit is for
educational use in the field of thermal process
engineering and apparatus construction.

A suitable laboratory facility is required to operate

the unit (for water quality see Chapter 5.6.1,
Page 52; for required cooling water flow see
Chapter 7.1, Page 119). Control of the unit
requires sound experience in the performance of
experiments.

Areas of application of the unit are:

• Demonstration experiments
The tutor operates the prepared system while a
small group of five to eight students observes.
The reaction of the unit to changing conditions
is demonstrated. The main effects can be
demonstrated in one hour’s operation.

1 Introduction 3
CE 600 CONTINUOUS RECTIFICATION

• Practical experiments
Small groups of two to three students can also
perform experiments independently. The esti-
mated time required to perform an experiment
is between four and five hours (from charging
the unit and putting it into operation, recording
data, determining the masses and concen-
trations through to draining the unit at the end).
• Project work
The unit is especially well suited to carrying out
project work. The influence of changing
conditions on the measurement results can be
determined by way of experiment series.
In continuous mode, the experiments should
be performed by two students. For batch
experiments, a single, experienced student
may also operate the unit.

Because of the complexity of the experimentation

unit and the demanding subject, detailed training
by a specialist GUNT engineer may be necessary
and useful.

4 1 Introduction
 CE 600 CONTINUOUS RECTIFICATION

2 Safety

2.1 Intended use

The unit is to be used only for teaching purposes.

2.2 Structure of safety instructions

The signal words DANGER, WARNING or

CAUTION indicate the probability and potential
severity of injury.
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An additional symbol indicates the nature of the

hazard or a required action.

Signal word Explanation

Indicates a situation which, if not avoided, will result in

DANGER death or serious injury.

Indicates a situation which, if not avoided, may result in

WARNING death or serious injury.

Indicates a situation which, if not avoided, may result in

CAUTION minor or moderately serious injury.

Indicates a situation which may result in damage to

NOTICE equipment, or provides instructions on operation of
the equipment.

2 Safety 5
CE 600 CONTINUOUS RECTIFICATION

Symbol Explanation

Electrical voltage

Explosive materials

Flammable materials

Hazard (general)

Materials hazardous to health

Hot surface

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 CE 600 CONTINUOUS RECTIFICATION

2.3 Safety instructions

WARNING
Risk of electric shock when working on the
control cabinet
Have work on the control cabinet carried out only
by a qualified electrician. Prior to opening the
control cabinet, unplug the mains power plug.
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WARNING
Risk of electric shock due to wetness and
moisture on the control cabinet
Do not allow the control cabinet to get wet.

WARNING
There is a risk of explosion if the wrong
chemicals are selected.
Select chemicals such that ignition temperatures
cannot be reached during operation. This applies
to the single input materials and to mixtures of
them.

WARNING
If the level in the evaporator is too low the risk
of explosion will be increased.
Make sure the level in the evaporator is sufficiently
high before switching on the electric heater.
Do not open the ball valve on the evaporator drain
during rectification.

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CE 600 CONTINUOUS RECTIFICATION

WARNING
Ethanol
Risk of explosion / detonation
Naked flames or smoking when handling ethanol
can cause severe injury
• No naked flames
• No smoking
• Keep the area well ventilated.

WARNING
Potential health hazard when handling
chemicals.
Follow the relevant health and safety instructions,
particularly with regard to charging and draining
the unit.

WARNING
Risk of burns by touching the apparatus, in
particular the evaporator, the column and the
pipes.
Do not touch hot surfaces.

WARNING
Risk of scalding when removing the heated
bottom product.
Drain the heated bottom product only into a heat-
proof container, and wear heat-resistant gloves
while doing so.

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 CE 600 CONTINUOUS RECTIFICATION

NOTICE
The choice of chemicals for rectification is limited
by the resistance of the materials used in the
construction of the equipment. Use only
chemicals which do not attack VITON, PVDF,
PTFE and stainless steel!

NOTICE
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During operation, ensure a sufficient flow of cool-

ing water to the condenser to prevent deactivation
of the heater.

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3 Unit Description

3.1 Process diagram

Fig. 3.1, Page 12 shows the process diagram for

the rectification unit CE 600.
This chapter sets out more information on the
design of the unit and its components.
Information on the unit circuitry and instructions
for performing the experiment in its different vari-
ants are provided in chapter 5.
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3 Unit Description 11
CE 600 CONTINUOUS RECTIFICATION

Media
Top Product
Feed Instrumentation and Control
Bottom Product FI01 Cooling Water Flowmeter
Cooling Water FSL01 Flow Switch
LSL01 Evaporator Level Switch
Main Components Valves and Fittings LI02 Evaporator Level
B1,B2 Feed Tank V01,V02 Solenoid Valves for Reflux Ratio PDI01 Column Pressure Loss
B3 Phase Separation Tank V03,V04 3-Way Ball Valves for Bottom Product Cooling PI02 Relative System Pressure
B4 Top Product Tank V05-V09 Regulating Valves TI01,TI02 Feed Temperatures
B5,B6 Bottom Product Tank V11-V34 Ball Valves TI03 Evaporator Temperature
B7 Solvent Tank V40 Non-return Valve TI04-TI11 Column Temperatures
D1 Evaporator V41 Safety Valve TI12 Column Top Temperature
H1 Heater TI13 Top Product Temperature
K1 Sieve Plate Column, Packed Column TI14 Bottom Product Temperature
P1 Feed Pump TI15 Cooling Water Inlet Temperature
P2 Water Jet Pump TI16 Cooling Water Outlet Temperature
W1 Top Product Condenser TI17 Solvent Temperature
W2 Bottom Heat Exchanger TSH18 Temperature Switch

Fig. 3.1 Process diagram of rectification unit CE 600

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 CE 600 CONTINUOUS RECTIFICATION

3.2 Layout

11 10 9 8 7 6

12 5

4
13
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14

Item Name

1 Feed pump
3
2 Feed tank
3 Control cabinet
4 Top product tank
2 5 Water jet pump
15
6 Pressure gauge
7 Solenoid valve
8 Phase separation tank
9 Top product condenser
1
10 Solenoid valve
11 Differential pressure sensor

12 Solvent tank
13 Column
14 Flowmeter for cooling water

15 Evaporator
16 17
16 Bottom heat exchanger

17 Bottom product tank

Fig. 3.2 CE 600, Continuous Rectification, Overview

3 Unit Description 13
CE 600 CONTINUOUS RECTIFICATION

3.3 Equipment Functions and Components

3.3.1 Components for the thermal process

The Continuous Rectification CE 600 experi-

Feed connections
mentation unit is used to separate homogeneous
liquid mixtures by means of rectification on an
experimental scale.
A steel tank with a built-in electric heater acts as
an evaporator (15) for the liquid mixture. The
tank has level indicator tube on its front.
The evaporator is charged by means of the feed
pump (1). The liquid mixture is pumped into the
column from one of the two independent feed
tanks (2).
One of the columns (13) in which the separation
takes place is mounted on top of the evaporator.
Either a packed column or a sieve plate column
with eight plates can be used (see Fig. 3.3 and
Fig. 3.3 Sieve plate column Fig. 3.4).
The pressure loss above the column is recorded
by a differential pressure sensor (11).
The steam passes along a metal tube at the top of
the column into the water-cooled top product
condenser (9). The distillate occurring at this
point flows into a phase separation tank (8).
From there, a tap enables it to be discharged
directly into a top product tank (4). Using two
electric solenoid valves (7, 10), the distillate
downstream of the phase separation tank can
also be split into reflux and top product with a
defined reflux ratio. The reflux returns to the unit
by way of the column head.

Fig. 3.4 Packed column

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 CE 600 CONTINUOUS RECTIFICATION

The cooling water for the condenser must be

supplied from an external source via a laboratory
connection (for position of connection see Fig.
3.5). The cooling water volumetric flow can be
read from the flowmeter (14). This volumetric
flow is regulated by way of the regulating valve
V05 above the flowmeter (see Fig. 3.5).
V05

The residue which is enriched in the evaporator

during the experiments is called the bottom
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product. The bottom product can be drained

directly into a suitable vessel by way of a tap on
the front of the evaporator. Alternatively, it can be
discharged into one of the bottom product tanks
(17). In doing so, it passes through the bottom
heat exchanger (16). This can be used to
V06 preheat the feed (mixture infeed) with the waste
Water connection heat of the draining bottom product when the unit
Fig. 3.5 Cooling water connection
is operating in continuous mode. If this feed
preheating is not required, the bottom heat
exchanger can be operated with cooling water
from the laboratory connection to cool the bottom
product.

A water jet pump (5) is used to perform

experiments with vacuum. The pump reduces the
pressure throughout the system. The pump is
also operated with water from the laboratory
supply. The regulating valve V06 (see Fig. 3.5) is
used to regulate the flow of water through the
pump. The level of vacuum can be read from the
pressure gauge (6).

3 Unit Description 15
CE 600 CONTINUOUS RECTIFICATION

Cap To prevent impermissibly high temperatures, the

Cover electric heater has a temperature switch TSH
(measuring point TSH18). The temperature
switch serves as a safety temperature limiter. If
the permissible temperature is exceeded the
heater cut-out is automatically tripped.
When the heater cut-out has been tripped, the
heater cannot be restarted as normal. The
temperature switch on the heater must first be
reset.
Fig. 3.6 Evaporator with electrical
Heater The adjacent photos show the rear of the evapo-
rator, indicating the cover of the electric heater.

Cap, removed When the cap is unscrewed the temperature

Temperature switch switch is accessible and can be pressed to
perform a reset.

Fig. 3.7 Evaporator with electrical

Heater, Temperature switch
accessible

16 3 Unit Description
 CE 600 CONTINUOUS RECTIFICATION

3.3.2 Control cabinet

Some switching and monitoring functions can be

provided by the electrical control cabinet (3).
All available data can be measured and recorded,
and all control functions can be implemented, by
means of the separate program on PC.
(see Chapter 3.4.2, Page 21).

Item Name
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20 USB port

21 Master switch
26 25
22 Local/Auto selector switch

23 Display for the differential pressure of the column

27 24 24 Controls for the reflux ratio

25 Temperature display T13-T16 with

23 measuring point selector switch

26 Temperature display T1-T12 with

28
measuring point selector switch
29 22
27 Controls for the heater
30
28 Controls for the feed pump
31 21
29 „Level too low“ warning lamp
32
30 „Temperature too high“ warning lamp
20 31 „Flow cooling water too low“ warning lamp
33
32 „PC-Control out of order“ warning lamp
33 Emergency Stop button

Fig. 3.8 Control cabinet, front view

3 Unit Description 17
CE 600 CONTINUOUS RECTIFICATION

The following unit components can be operated

from the control cabinet:
• Heater (27)
• Feed pump (28)
• Reflux ratio (24)
The controls listed below are provided for the
purpose:
• I/O switch
• Adjusting knob
The Local/Auto selector switch (22) determines
whether these unit components are controlled
from the control cabinet (locally) or from the PC
(Auto).
Digital displays are installed for these unit
components and for the differential pressure and
the temperatures.

On the rear of the control cabinet there are sock-

ets to connect the temperature sensors T4-T11 of
the column (see Fig. 3.9).

Fig. 3.9 Control cabinet, rear panel

18 3 Unit Description
 CE 600 CONTINUOUS RECTIFICATION

The warning lamps make it easier to identify the

causes of faults:
• “Level too low” warning lamp (29).
The evaporator is fitted with the level switch
(LSL). To prevent overheating, if the level falls
below the minimum (~3L), the heater is auto-
matically deactivated. The warning lamp is also
activated.
• “Temperature too high” warning lamp (30).
The temperature switch (TSH) prevents
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unacceptably high temperatures on the heater

(see also Fig. 3.7, Page 16). If the temperature
switch trips, the heater is automatically deacti-
vated and the warning lamp is switched on.
• “Flow cooling water too low” warning lamp (31).
For safe operation, it is necessary to condense
the vapours produced in the system (the
FI01
vapours should not get into the ambient air).
Therefore, the flow of cooling water to the con-
denser (9) is monitored. If the minimum cooling
water flow is not reached, the flow switch FSL
(measuring point FSL01) trips, resulting in the
heater being shut down and this warning lamp
FSL01 being switched on.
• “PC-Control out of order” warning lamp (32),
signals failure of the external controller.

Fig. 3.10 Flow switch FSL

3 Unit Description 19
CE 600 CONTINUOUS RECTIFICATION

3.4 Data acquisition program

3.4.1 Installing the program

The following is needed for the installation:

• An fully operational PC, laptop or notebook
with USB port (see Appendix for minimum
requirements).
• G.U.N.T. - CD-ROM
All components necessary to install and run the
program are contained on the CD-ROM,
delivered by G.U.N.T. along with the CE 600.
After starting, the installation runs automatically.
During the course of the installation, various
program components are loaded onto the PC
• Software for PC-based data acquisition
• LabVIEW-runtime program and driver routines
• G.U.N.T. - Libraries

Installation procedure

NOTICE
Connect nothing to the USB port during the instal-
lation of the program. Only after the software has
been installed can the USB hardware be connected.

• Boot the PC
• Load the G.U.N.T. - CE 600 CD-ROM
• Start the installation software "Start.bat".

20 3 Unit Description
 CE 600 CONTINUOUS RECTIFICATION

• Follow the installation procedure on the screen.

• Reboot the PC after the installation is finished.

3.4.2 Operating the program

• The program for the CE 600 is selected and

started by choosing:
Start / All Programs / G.U.N.T. / CE 600
• The language can subsequently be changed at
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any time in the "Language" menu.

• Various pull-down menus are provided for
additional functions.
• For detailed instructions on use of the program
refer to its Help function. You can access the
help function via the "?" button.

Saved measurement data can be imported into a

spreadsheet program (such as Microsoft Excel)
where it can be edited.

After the program starts, the system diagram for

the continuous rectification CE 600 will appear on
the screen (see Fig. 3.11).
It shows the available system data along with the
associated measuring point positions.
The following elements can also be controlled
from the PC:
• Heater (T3)
• Reflux ratio (0...100%)
• Feed pump (0...100%)

3 Unit Description 21
CE 600 CONTINUOUS RECTIFICATION

Fig. 3.11 Process diagram, System diagram

One of two modes can be selected:

• Manual:
The desired value is directly entered
(0...100%)
• Automatic:
The PC functions as a controller. Setpoint
values and control parameters are entered on
the PC.
Note regarding Automatic mode:
The actual set of control parameters will be
stored. If required, the default set of control
parameters can be activated again (therefor click
„Controller“ and „Load Default Values“).

The feed pump cannot be controlled automati-

cally. It features only the Manual mode.

22 3 Unit Description
 CE 600 CONTINUOUS RECTIFICATION

3.5 Commissioning

• Ensure that all hose connections are secure

and free from leaks
• Connect the cooling water supply and reflux
lines (see Fig. 3.5, Page 15), reflux
unpressurized
• Connect the unit to the mains electricity supply
• Install the data acquisition and control program
on the PC (see Chapter 3.4.1, Page 20)
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• Plug the unit into the PC

For more information and detailed instructions for
performing the experiment refer to Chapter 5 and
Chapter 6.

3.6 Shutdown

• Shut down the PC

• Switch off the unit at the master switch
• Shut off the water supply and isolate the unit
from the water main
• Leave unit to cool
• Check the positions of the valves, prevent
unintentional leakage of liquids
• If the unit is being shut down for a lengthy
period of time, drain all tanks completely

3 Unit Description 23
CE 600 CONTINUOUS RECTIFICATION

24 3 Unit Description
 CE 600 CONTINUOUS RECTIFICATION

4 Theory

The basic principles set out in the following make

no claim to completeness. For further theoretical
explanations, refer to the specialist literature.

4.1 Basic principles

Distillation and rectification are thermal processes

used to separate or purify liquid mixtures whose
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

constituents are wholly miscible with one another.

Both processes work by the basic operations of
evaporating a liquid and then condensing the
resulting vapours.

1
When a liquid mixture AB is brought to the boil,
Molar fraction y1 of substance A

wherein the substance A has the molar fraction

0.8 x1, vapour arises from it. But substance A now
has a different molar fraction y1 in the steam than
0.6 it does in the liquid mixture AB.
0.52

0.4
If we enter the corresponding values for the
vapour for all possible mixture ratios of AB in a
in vapour AB

0.2 diagram, we obtain the curve of equilibrium (see

Fig. 4.1). This curve indicates the mixture ratio of
0
0 0.2 0.4 0.6 0.8 1
the steam given off by the boiling liquid.
0.3

Curves of equilibrium are different for different

Molar fraction x1 of sub-
stance A in liquid mixture AB
substance mixtures. The more the curve arcs
away from the diagonal of the diagram, the
Fig. 4.1 Example of a curve of
greater is the increase in concentration of
equilibrium
substance A from liquid to vapour.

4 Theory 25
CE 600 CONTINUOUS RECTIFICATION

The collected condensate is therefore richer in

low-boiling constituents compared with the initial
mixture. The proportion of high-boiling constitu-
ents in the residual mixture is correspondingly
higher.
In distillation/rectification therefore, the vapour
phase has a different mixture ratio than the liquid
phase. This fact is the basis of both processes.

4.1.1 Distillation

In distillation, a liquid mixture is brought to the boil

and the resulting vapour is drawn off and
condensed. This condensed liquid is known as
the distillate. The remaining mixture is the
residue.

Distillation apparatus consists of:

Condenser
• an evaporator to heat the initial mixture and
Evaporator

collect the high-boiling component (residue).

• a condenser to condense the low-boiling
component (distillate).
• one or more tanks to collect the distillate.
Residue

Distillation does not produce a complete separa-

Distillate tion of the initial mixture. It just divides the initial
mixture into two mixtures with different concen-
trations (see Chapter 4.1, Page 25).
Fig. 4.2 Distillation, schematic
In simple distillation, all of the distillate is
collected.

26 4 Theory
 CE 600 CONTINUOUS RECTIFICATION

There is also the process in which the condensate

is collected in different vessels, known as
fractions, as distillation time passes. This is
known as fractional distillation.
To protect temperature-sensitive substances dur-
ing distillation, their mixtures are distilled in a
vacuum where boiling points are lower. This
method is known as vacuum distillation.
This process is essentially just the same as con-
ventional distillation. A vacuum pump
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downstream of the condenser maintains a

vacuum throughout the system.

There are two basic types of distillation:

• Batch distillation (discontinuous, batch-by-
batch):
The evaporator is charged and the distillation is
continued until no more distillate occurs for
example.
• Continuous distillation:
Distillate and residue are continuously
discharged. To compensate for the discharge,
a corresponding amount of additional initial
mixture (feed) is pumped into the evaporator.

4 Theory 27
CE 600 CONTINUOUS RECTIFICATION

4.1.2 Rectification

y4
The result of the separation obtained by
distillation is not sufficient in all cases.
y3

To improve separation, the collected distillate

y2 should be distilled again. This process should be
repeated until the required material is satisfacto-
rily enriched. Multiple-stage distillation of this
y1
type is expensive and energy-intensive.
Consequently, rectification is applied (for a
schematic view see Fig. 4.4 and Fig. 4.5).
In rectification, the released vapour is first passed
x1 x2 x3 x4 x5
through a vertical tube called the column before
it reaches the condenser. Instead of all of the
Fig. 4.3 Equilibrium diagram for distillate collected in the condenser being drawn
multi-stage distillation
off straight away, part of it is returned to the
column as the so-called reflux.
The difference between rectification and
distillation is that the rising vapour mixture and
returning condensate flow counter to one another.
The process is therefore also known as reverse
flow distillation.
The returned condensate now runs down the
column and, at the next level down, is forced into
contact with the rising vapours on suitable
internals for the purposes of material exchange.
The result is an exchange of material and heat
between the rising vapours and the falling liquid.

28 4 Theory
 CE 600 CONTINUOUS RECTIFICATION

The high-boiling component condenses first from

the rising vapours.
The resulting condensation heat causes more
low-boiling component to evaporate in turn. The
result is that the liquid flowing back to the bottom
of the column is enriched with high-boiling compo-
Top nents. The vapours at the top of the column are
Top product

correspondingly richer in low-boiling components.

Rectification can be understood as being multi-
stage distillation, but with just one evaporator
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and one condenser. This improves efficiency,

Reflux

because at the transition from one stage to the

next the vapour does not have to be first
Column condensed and then reheated and evaporated.

Thus the number of stages in rectification is

comparable to the number of series-connected
distillation stages.
If the column is a sieve plate column (for
Bottom illustration see Fig. 3.3, Page 14 and Fig. 5.8,
Page 39), each sieve plate represents one sepa-
ration stage. The number of sieve plates in the
Bottom product
column is the plate count.
A common alternative to the sieve plate column is
the packed column. It is filled with packing. The
purpose of the large number of packing blocks is
to provide the material mixture with a large
Fig. 4.4 Rectification, schematic
surface area. This intensifies the material
exchange in the column. The contact between the
liquid and gaseous phases occurs throughout the
packed bed.
Packing blocks are small, regularly shaped pieces
of plastic, ceramics or metal.

4 Theory 29
CE 600 CONTINUOUS RECTIFICATION

There is a wide variety of different packing blocks

to suit different separation applications.
The packed column, with its homogeneous
packed bed, has no direct plate count. To be able
to characterise and design packed columns
despite this, the concept of theoretical transfer
units has been devised. In this, NTU (Number of
Transfer Units) represents a theoretical number of
transfer units and HTU (Height of Transfer Unit) is
the height of the packed bed of such a unit.

At the top of the column, the distillate is divided

into one part reflux and one part top product. The
ratio of reflux to top product is called the reflux
ratio. It is an important characteristic value for
operation of the unit. The reflux ratio v may
assume values from zero to infinity.
As already described in Chapter 3.3.1, Page 14,
the CE 600 unit separates distillate into reflux and
top product by cycling two electric solenoid
valves. In this process, the solenoid valves 7 and
10 are alternately opened and closed.
Differing from the usual definition, an adjusted
definition is used as the reflux ratio R for this unit.
Here R is the ratio of the opening time of solenoid
valve 10 to the sum total of the opening times of
solenoid valves 7 and 10. The value range for R is
0 to 100%.

The following examples illustrate this reflux ratio R:

30 4 Theory
 CE 600 CONTINUOUS RECTIFICATION

The following examples illustrate this reflux ratio

R:
• R=100%: Solenoid valve 10 is permanently
open, solenoid valve 7 permanently closed.
The entire condensate flows back into the
column.
• R=0%: Solenoid valve 10 is permanently
closed, solenoid valve 7 permanently open.
The entire condensate flows into the top
product tank.
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• R=50%: Solenoid valves 10 and 7 are alter-

nately opened and closed, and for the same
amount of time. The condensate flow is
divided. One portion flows back into the
column, the other is routed to the top product
tank.

Condenser

Column head
Reflux

Aftercooler
Reflux divider
Column with
internals

Top product
Evaporator
(low-boiling)
Initial
Column bottom
mixture

Bottom product
Aftercooler (high-boiling)

Fig. 4.5 Rectification unit, schematic representation

4 Theory 31
CE 600 CONTINUOUS RECTIFICATION

Rectification can also be carried out in two

different ways:
• Batch rectification (discontinuous, batch-by-
batch):
The evaporator is charged and the rectification
is continued until no more top product occurs
for example.
• Continuous rectification:
The top and bottom products are continuously
discharged. To compensate for the discharge,
a corresponding amount of additional initial
mixture (feed) is pumped through the column.
Liquid mixtures can be separated virtually
completely by rectification. Even mixtures with
curves of equilibrium close to the diagram
diagonal are separated much more effectively
than in single-stage distillation.

32 4 Theory
 CE 600 CONTINUOUS RECTIFICATION

4.1.3 Azeotropic mixtures

A special case occurs with regard to many liquid

mixtures when they reach a certain concentration.
The vapour arising from the mixture has the same
composition as the liquid phase. Such mixtures
are called azeotropic.
This means that the curve of equilibrium
intersects the diagram diagonal.

Azeotropic point
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100
95,6

80
Low-boiling mass fraction in the vapour

Azeotropic mixture,
e.g. ethanol/water

60

40
al
on
ag
di

20
am
gr
ia
D

20 40 60 80 100
95,6
Low-boiling mass fraction in the liquid

Fig. 4.6 Curve of equilibrium of an azeotropic mixture

Normal rectification can only separate such

mixtures down to their azeotropic point.

4 Theory 33
CE 600 CONTINUOUS RECTIFICATION

The closer the separation gets to that point, the

more similar the compositions of the liquid and
vapour become. Consequently, no further enrich-
ment of the lower-boiling component in the
condensate is possible. For an ethanol/water
mixture for example, this concentration is
95,6%m (mass fraction).

Two methods can be applied to obtain a pure

component:
• Altering the working pressure in the column by
vacuum or high-pressure distillation. This
enables the azeotropic point to be shifted or
eliminated in many cases.
• Addition of an ancillary substance to the
mixture. This substance forms a low-boiling or
high-boiling mixture together with one of the
components. This likewise enables the
azeotropic point to be shifted.
This process is termed azeotropic rectification.
For an ethanol/water mixture for example,
cyclohexane is a suitable ancillary substance. It is
intermingled with the product containing approxi-
mately 95%m ethanol. The product is separated
into the now higher-boiling ethanol, which is
enriched in the bottom of the column, and the now
lower-boiling water/cyclohexane mixture.
Water and cyclohexane are not miscible. Owing
to their different densities, they are separated in
the phase separation tank. The lighter
cyclohexane floats to the top and is fed back into
the column. This means the ancillary cyclohexane
circulates around the system.

34 4 Theory
 CE 600 CONTINUOUS RECTIFICATION

5 Experiments - Preparations, variants, instructions for performing

The following provides instructions for carrying

out rectification with the CE 600 unit.
This section occasionally refers to CE 600
components without showing the process
diagram adjacent to the text. For clarification,
please refer to the process diagram in Fig. 3.1,
Page 12.
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5.1 Preparing the unit

First run through the commissioning procedure as

detailed in Chapter 3.5, Page 23.

5.1.1 Tank volumes

When performing the experiments, it is useful to

be able to obtain a quick estimate of the levels in
the various tanks.
This is why the following tanks have level markers
(Fig. 5.1 to Fig. 5.4, Page 36):
• feed tank
• evaporator
• top product tank
• bottom product tank

5 Experiments - Preparations, variants, instructions for performing 35

CE 600 CONTINUOUS RECTIFICATION

Fig. 5.1 Feed tank (B1,B2) volume Fig. 5.2 Top product tank (B4) volume

Fig. 5.3 Bottom product tank (B5,B6) Fig. 5.4 Evaporator (D1) volume
volume

36 5 Experiments - Preparations, variants, instructions for performing

 CE 600 CONTINUOUS RECTIFICATION

5.1.2 Refitting the columns

5.1.2.1 Replacing the columns

To convert between a sieve plate and packed

column, run through the following steps (see
adjacent photos in Fig. 5.5).
• Make sure the unit has cooled down
sufficiently.
• On the rear panel of the control cabinet, detach
and unplug the connectors of the measuring
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cables for temperature sensors T4 to T11.

• Reel up and tie the cables in pairs, using a
cable tie for example.
• Detach the hoses from the column hose
couplings.
• Release the clamp around the column head.
Then slide the column head slightly upwards
and re-tighten the clamp.
• Unscrew and remove the screws on the top
and bottom column flanges.
• With the aid of a second person, remove the
column. Store the column carefully, so that the
temperature sensors are not bent.
• Clean the two flange seals (see Fig. 5.6) and
coat them on both sides with water
(for explanatory notes see below).
• With the aid of a second person, carefully fit the
replacement column with the flange seals.
• Loosen the clamp around the column head and
lower the column head.
Fig. 5.5 Column photos • Fit the screws, retaining rings and nuts on the
top and bottom column flanges and tighten
them evenly.

5 Experiments - Preparations, variants, instructions for performing 37

CE 600 CONTINUOUS RECTIFICATION

• Clamp around column head.

Upper flange seal
• Unreel the tied-up measuring cables.
• On the rear panel of the control cabinet, insert
and secure the connectors of the measuring
cables for temperature sensors T4 to T11.
Keep to the assignments labelled on the
connectors and on the rear panel socket.
Lower flange seal • Connect the hoses to the column by their
couplings.
Fig. 5.6 Flange seals
The flange seals tend to adhere more strongly to
the flanges as the service life advances. This
makes removing them more difficult. The
adhesion can be reduced by coating the flange
seals with water prior to fitting.

5.1.2.2 Sieve plate column, plate removal

For the sieve plate column, it is useful to

investigate the influence of the number of plates.
The following section explains how individual
plates can be removed from the column and re-
inserted into it.
Fig. 5.7 shows how the disassembled sieve plate
column can be clamped to a bench.
The following photos in Fig. 5.8 and Fig. 5.9 the
actions required. The following steps must be run
through to remove a sieve plate:
• Clamp the sieve plate column to the bench
• Slacken and remove the flange screws at the
desired separation point

Fig. 5.7 Sieve plate column mounting

38 5 Experiments - Preparations, variants, instructions for performing

 CE 600 CONTINUOUS RECTIFICATION

• Detach the upper section of the column

• Release the temperature sensor mount (1)
• Pull back the temperature sensor (2)
• Remove the sieve plate (3)
• Assemble the distance washer (see Fig. 5.9,
item 4), replacing the removed sieve plate (3)
• Return the temperature sensor (2) to its original
position, and tighten the union nut
• Moisten the O-ring (see Fig. 5.9, item 5) and
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ensure it is firmly seated

1 2
• Carefully slot the upper section of the column
at the correct angle (not twisted) into the
bottom section (without tilting it).
• Fit the screws, retaining rings and nuts. Tighten
the nuts carefully and evenly.
Purpose of the distance washer: Five dis-
2
tance washers are part of the accessories. The
assembled distance washer replaces the
removed sieve plate, in order to get the identi-
cal overall height of the column, and to avoid
damages of the temperature sensor (without
distance washer, there is a risk that the temper-
ature sensor between the upper and lower sec-
tions of the column may be crashed).
3

To add a single sieve plate, follow the above

procedure in reverse.

Fig. 5.8 Photos: Disassembling a sieve

plate column

5 Experiments - Preparations, variants, instructions for performing 39

CE 600 CONTINUOUS RECTIFICATION

Fig. 5.9 Photos: Assembling a sieve plate column

The photos illustrate that the space between the flanges is required for
removal and fitting of the sieve plates. Consequently, there is no room for
insulation on a sieve plate column. By contrast, a packed column is supplied
with insulation, so as to reduce heat loss.

40 5 Experiments - Preparations, variants, instructions for performing

 CE 600 CONTINUOUS RECTIFICATION

5.2 Accessories for performing experiments

To perform the experiments, a number of

accessories are required in addition to the actual
unit and the material mixture under investigation
(accessories not included in the scope of
delivery).

5.2.1 Tanks, measuring cups

• Three measuring cups, e.g. 2000ml capacity

All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

• Two lockable canisters, e.g. 25L capacity, for

interim storage of the substances and mixing
• A shallow cup, e.g. 500ml, for removing bottom
product from the bottom product tanks.

5.2.2 Measuring instruments

• A weighing scale, measuring range up to at

least 2,5kg
• A concentration meter for the material mixture
(e.g. density spindle/areometer, with upright
cylinder)
• A thermometer to measure the sample
temperature

5 Experiments - Preparations, variants, instructions for performing 41

CE 600 CONTINUOUS RECTIFICATION

5.3 Experiment variants

The unit offers a wide range of options for carrying

out experiments under widely varying conditions.
The possible modes include:
• Discontinuous (batch) or continuous
• Sieve plate column or packed column
• Sieve plate column, three different infeed
heads selectable
• Reduction in the number of plates in the sieve
plate column
• Operation at ambient pressure or under
vacuum
• Operation with or without feed preheating
• Operation of heater and reflux ratio via fixed
values, or regulated

The key difference in terms of operating mode is

between discontinuous (batch) and continuous.
This differentiation also determines the basic
method of performing the experiment.

42 5 Experiments - Preparations, variants, instructions for performing

 CE 600 CONTINUOUS RECTIFICATION

5.4 Experiments - batch mode

The batch experiments differ primarily in that the

unit is operated at ambient pressure or under
vacuum. The differences with regard to perform-
ing experiments are set out in the following
subsections.

5.4.1 Notes on performing experiments - operation at

ambient pressure
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Fig. 5.10, Page 44 is a variant of the actual

process diagram in Fig. 3.1, Page 12, and the
flow through the unit for batch experiments at
ambient pressure in colour-coded form.
The unit components, pipe lines and hoses are
colour-coded. The meanings of the various
colours are indicated by the key.
Before performing an experiment, the valves must
be set to produce the flow shown during sub-
sequent operation.

5 Experiments - Preparations, variants, instructions for performing 43

CE 600 CONTINUOUS RECTIFICATION

Closed

Open

Closed

Media
Top Product
Bottom Product
Cooling Water

Fig. 5.10 Process diagram for a batch experiment at ambient pressure

44 5 Experiments - Preparations, variants, instructions for performing

 CE 600 CONTINUOUS RECTIFICATION

The process diagram Fig. 5.10 also specifies the

V33
positions of the two small ball valves close to the
pressure gauge. They are shown in the adjacent
photo Fig. 5.11 (V33 and V34).
For operation at ambient pressure it is
important to open the manual ball valve V34.
This equalises the pressure relative to the
atmosphere.
If the unit was operated with the ball valve V34
V34 closed, the entire system may be pressurised
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because of the rising steam pressure. The

Fig. 5.11 Ambient pressure circuit
consequence of the higher pressure would then
be a higher boiling point, meaning that the
V17 temperature level throughout the system would
also rise. Such an increased temperature level
may result in the destruction of unit components.
For the same reason, it is advisable to open the
ball valve V24 in order to vent the top product tank
(B4).

The ball valve V17 shown in Fig. 5.12 at the feed

connection of the column should be closed so as
to avoid unnecessary thermal loading on the
hose.
Fig. 5.12 Column, feed connection

5.4.2 Notes on performing experiments - operation with vacuum

Fig. 5.13, Page 46 is also a variant of the actual

process diagram in Fig. 3.1, Page 12, and
represents the flow through the unit for batch
experiments under vacuum in colour-coded form.
Before performing an experiment, the valves must
be set to produce the flow shown during sub-
sequent operation.

5 Experiments - Preparations, variants, instructions for performing 45

CE 600 CONTINUOUS RECTIFICATION

Open

Closed

Closed

Media
Top Product
Bottom Product
Cooling Water
Vacuum lines

Fig. 5.13 Process diagram for a batch experiment under vacuum

46 5 Experiments - Preparations, variants, instructions for performing

 CE 600 CONTINUOUS RECTIFICATION

The water jet pump P2 (see Fig. 5.14) generates

vacuum. When the regulating valve V06 is
opened the flow passes through the water jet
pump from bottom to top. The water jet effect
causes air to be drawn in at the left side pump
connection, producing a vacuum.
The vacuum can be influenced by altering the
water flow. A higher vacuum is produced by
increasing the water flow.
Take care to have reflux water flow by gravity
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(connection unpressurized; pressure in the reflux

line could result in insufficient vacuum).
The process diagram Fig. 5.13 specifies the
positions of the two small ball valves close to the
pressure gauge. They are shown in the adjacent
photo Fig. 5.15 (V33 and V34).
For operation under vacuum it is important to
Fig. 5.14 Water jet pump close the manual ball valve V34. This prevents the
pressure being equalised with the atmospheric
pressure. For the same reason, the ball valve V24
V33
must be closed for venting of the top product tank
(B4).
When the water jet pump (P2) is in operation, the
ball valve V33 is opened so that air can be
extracted from the system.

As already explained in Chapter 5.4.1, Page 43,

V34 the ball valve V17 at the feed connection of the
Fig. 5.15 Ball valves on the pressure
column should be closed so as to avoid unneces-
gauge sary thermal loading on the hose.

5 Experiments - Preparations, variants, instructions for performing 47

CE 600 CONTINUOUS RECTIFICATION

5.5 Experiments - continuous mode

5.5.1 Notes on performing experiments

Here, too, a variant of the actual process diagram

is used to illustrate the flow through the unit - see
Fig. 5.16, Page 49.
Before performing an experiment, the valves must
be set to produce the flow shown during sub-
sequent operation.

48 5 Experiments - Preparations, variants, instructions for performing

 CE 600 CONTINUOUS RECTIFICATION

Closed

Open
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

Open

Media
Top Product
Feed
Bottom Product
Cooling Water

Fig. 5.16 Process diagram for continuous experiments at ambient pressure,

example with feed preheating

5 Experiments - Preparations, variants, instructions for performing 49

CE 600 CONTINUOUS RECTIFICATION

The positions of the ball valves close to the

pressure gauge apply here as set out in
Chapter 5.4.1, Page 43.
The ball valve at the column feed connection
already mentioned initially remains closed. It is
not opened until immediately before the feed
pump is switched on.
Attention must also be paid to the following
details:
Vent plug
1.) Tank breathing:
Fig. 5.17 Venting the feed tanks (B1,B2)
In continuous mode, the levels in the top product,
feed and bottom product tanks change. To enable
unhindered charging and draining of those tanks,
they must be vented.
For the top product tank (B4) this is done by
opening the top ball valve V24.
For the feed and bottom product tanks it is
necessary to unscrew the filler neck drain plugs.
The drain plugs next to the filler necks are shown
in the photos in Fig. 5.17.
2.) Bottom heat exchanger circuit:
Vent plug
The process diagram Fig. 5.16 specifies the posi-
Fig. 5.18 Venting the bottom product
tanks (B5, B6) tions of the two 3-way ball valves V03 and V04. In
this setting feed flows through the jacket of the
bottom heat exchanger.
It is important to adjust the two 3-way ball valves
and the ball valve V15 in the same way.
If only one of the two 3-way ball valves is
adjusted, either water will flow into the column or
feed will enter the cooling water return.

50 5 Experiments - Preparations, variants, instructions for performing

 CE 600 CONTINUOUS RECTIFICATION

V03 V04 V08

V15
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Fig. 5.19 Bottom heat exchanger circuit

Fig. 5.19 shows the installation situation.

There is a 90° tap in the 3-way ball valves. The
hand lever can be rotated 180°. In the mid-
position no flow is open. At the end positions the
direction of the hand lever indicates the open flow.

It must also be ensured that the feed route from

the tank into the column is open (see Fig. 5.16).
To protect the pump, pumping against closed
valves should be avoided.

3.) Adjusting the level in the evaporator:

The regulating valve V08 is used for fine adjust-
ment of the level in the evaporator in continuous
operation.

5 Experiments - Preparations, variants, instructions for performing 51

CE 600 CONTINUOUS RECTIFICATION

5.6 Practical tips

5.6.1 Requirements for the water / water hardness

To flush through the unit and for test purposes,

water is generally used. Water is also a
component of the recommended ethanol/water
substance mixture.
The quality of the water used is one of the key
factors determining the durability of the unit. The
harder the water, the more deposits and scaling
will form in the apparatus and the pipework. The
behaviour of the unit will change even before the
narrowest cross-section is blocked. This will
impair the reproducibility of experiments.
Consequently, the use of water with a hardness
< 5°dH is recommended for the cooling and
motive water.
For the separation mixture we recommend using
distilled water.

5.6.2 Pumping from the feed tanks into the evaporator

To charge the evaporator, the initial mixture is fed

into the feed tanks. Where a sieve plate column is
installed, it is advisable to connect the hose (1) to
the bottom infeed connection of the column
(see Fig. 5.20).
1
If it is connected to one of the higher fittings, the
column may be flooded. The reason is that then,
with the larger number of plates, the displaced air
from below impedes the feed from above.

Fig. 5.20 Charging with sieve plate

column

52 5 Experiments - Preparations, variants, instructions for performing

 CE 600 CONTINUOUS RECTIFICATION

5.6.3 Bottom product cooling at the end of an experiment

At the end of an experiment there is bottom product

at boiling temperature in the evaporator (D1).
If there is enough time, the unit can be allowed to
cool overnight with the bottom product in it. The
next day the bottom product is then drained off so
as to perform the outstanding measurements
(mass, density, temperature).
If the bottom product is drained off immediately,
however, there is a risk of scalding.
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WARNING
Risk of scalding when removing the heated
bottom product.
Use the facility to cool the bottom product (see
below).

So what is needed is a method of cooling the

entire evaporator content, also to save time and
enable a second experiment to be conducted on
the same day.
The bottom heat exchanger (W2) could, in
principle, be used for cooling, if configured so that
cooling water flows inside the jacket. However,
the siphon in the evaporator prevents the
remaining approximately 6l of bottom product
from flowing through (see also Chapter 6.2.1,
Page 64).

An elegant solution to the problem is to “short-

circuit” the siphon.

5 Experiments - Preparations, variants, instructions for performing 53

CE 600 CONTINUOUS RECTIFICATION

Evaporator Fig. 5.21 shows normal operation with continu-

V25 V26 ous rectification. The ball valve V25 beneath the
siphon is open. The ball valve V26 on the drain is
closed.
The siphon is operational, and the bottom
product volume in the evaporator does not fall
below the minimum (approximately 6 litres). The
electric heater in the evaporator is completely
surrounded by liquid bottom product. The gener-
ated heat is evenly absorbed by the liquid bottom
product, while the surface temperature of the
electrical heater remains constant.
It is important to ensure that the siphon is contin-
uously in use during rectification (ball valve V26
remains closed). This is one of three safety
Fig. 5.21 Circuit Evaporator, for
devices to prevent the upper heater rods from
continuous rectification drying out and an impermissible temperature
increase occurring (entailing an increased risk of
V25 V26 explosion). The other two safety devices ensuring
prompt deactivation of the heater are the level
switch LSL and the temperature switch TSH
(see Chapter 3.3, Page 14 ff).

Fig. 5.22 shows the evaporator with switched ball

valves V25 and V26, for bottom product cooling
when the experiment is ended. The siphon is
short-circuited. The evaporator content is com-
pletely drained into the bottom product tank by
way of the bottom heat exchanger, with the
bottom product being cooled in the process (see
also process diagram in Fig. 3.1, Page 12.

Fig. 5.22 Circuit Evaporator, for bottom

product cooling at end of
experiment

54 5 Experiments - Preparations, variants, instructions for performing

 CE 600 CONTINUOUS RECTIFICATION

5.6.4 Reuse of input substances

It is possible to discard the top and bottom

products after each experiment and apply a new
mixture of input substances for each new
experiment.
However, large quantities of input material can be
saved by remixing product after performing an
experiment. This mixture can be reused as the
initial mixture for the subsequent experiment.
A certain loss of liquid while the experiment is
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being performed is inevitable (due to transfers,

spillage when pouring, sampling, evaporation,
and so on). Consequently, each new mixture
should be composed of a larger initial mix
quantity, so as to ensure there is adequate
volume for each new experiment.
It is likely that the concentration of the mixture will
change in the course of the experiments. The
reason is that the more volatile substance
evaporates and is lost to a greater extent. So the
concentration should be checked every time prior
to use. The mixture must be reset to the desired
concentration as necessary.

5 Experiments - Preparations, variants, instructions for performing 55

CE 600 CONTINUOUS RECTIFICATION

5.6.5 Hose lengths

Most of the lines interconnecting components of

the CE 600 unit are pipes. It is, however,
necessary to use hoses with couplings at some
points.
This relates primarily to moving parts (such as the
column head) or parts which can be removed and
replaced (such as the column). It also relates to
the alternative circuits (three infeeds into the
sieve plate column).
1 Sagging of hoses, creating a sack effect, is not
Fig. 5.23 Reflux hose always avoidable. This does not usually entail any
negative consequences. Problems do, however,
arise if liquid collects in the “sack” and affects the
process. This may happen at the following points:
• Reflux hose (item 1 in Fig. 5.23). Here liquid
deposits may impair the flow of the top product
2 completely (see also Chapter 6.2.1, Page 64,
Reflux).
• Hoses between the column and the differential
pressure sensor (items 2 and 3 in Fig. 5.24).
Here liquid deposits may cause incorrect
measurements.
The liquid may occur due to process events, such
as flooding of the column. Often, though, it
condenses from the system, during cooling after
3 the unit has been in use.
It is advisable to detach the hoses in question and
drain them before starting a new experiment. If
problems persist, the hoses in question should be
shortened to a minimum length.

Fig. 5.24 Hoses for differential pressure

measurement

56 5 Experiments - Preparations, variants, instructions for performing

 CE 600 CONTINUOUS RECTIFICATION

6 Experiments - with ethanol/water mixture

The selection of experiments makes no claims of

completeness but is intended to be used as a
stimulus for your own experiments.
The results shown are intended as a guide only.
Depending on the construction of the individual
components, experimental skills and environmen-
tal conditions, deviations may occur in the experi-
ments. Nevertheless, the laws can be clearly
demonstrated.
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All the experiments on which this section is based

were conducted using an ethanol/water mixture.
The density was measured in order to determine
the concentration. An areometer (measuring
range 0,8 to 1,0kg/L), together with an upright
cylinder (capacity 500mL) was used to measure
the density. As a result, the sample volume has
been specified and the number of possible
samples limited.

This section occasionally refers to CE 600

components without showing the process
diagram adjacent to the text. For clarification,
please refer to the process diagram in Fig. 3.1,
Page 12.

6.1 Recommended ethanol/water mixture

An ethanol/water mixture is recommended for

operation of the unit, for safety reasons.

6.1.1 Material values

The concentration of a material mixture can be

determined from the mixture’s density.

6 Experiments - with ethanol/water mixture 57

CE 600 CONTINUOUS RECTIFICATION

Knowledge of the densities of the input sub-

stances alone is not sufficient however, because
the ratio between the concentration and the
density of an ethanol/water mixture is not linear.
The reason is that the ethanol and water
molecules in the mixture influence each other and
create additional binding forces (hydrogen
bonding).
Consequently, the molecules may take up a
smaller overall space, so the volume of the
mixture is less than the sum of the individual input
substance volumes (volume contraction).
In view of that, table values have to be applied
across the entire concentration range.
The concentration of an ethanol/water mixture is
not only dependent on the mixture density, but
also the mixture temperature.
Tables are frequently to be found which set out
the density and concentration for a fixed
reference temperature. The reference tempera-
ture quoted is often 20°C, sometimes 15°C.
Tables for reference temperatures above 20°C
are difficult to find.
However, extensive material values are provided
by the Organisation Internationale de Métrologie
Légale (OIML) in the form of “International
Alcoholometric Tables” (link: www.oiml.org). They
set out the correlations between density and
concentration for the reference temperatures -20
to +40°C, for both volumetric and mass fractions.
Extracted from those extensive material data
listings, the following tables set out the densities,
dependent on the ethanol mass fraction, for the
temperatures +20 to +30°C.

58 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION
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Tab. 6.1 For the ethanol/water mixture: Density ρ in kg/m³ as a function of the ethanol
mass fraction p and temperature t , 0 ≤ p ≤ 50% , 20 ≤ t ≤ 30°C

6 Experiments - with ethanol/water mixture 59

CE 600 CONTINUOUS RECTIFICATION

Tab. 6.2 For the ethanol/water mixture: Density ρ in kg/m³ as a function of the ethanol
mass fraction p and temperature t , 50 ≤ p ≤ 100% , 20 ≤ t ≤ 30°C

60 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

6.1.2 Determining concentration by density and temperature

The object of density measurement is to

determine the concentration of the mixture.
Common concentrations quoted for the ethanol/
water mixture are the ethanol volumetric fraction
and mass fraction.
Any indication of the volumetric fraction is only
unambiguously specific in conjunction with the
associated reference temperature. So a more
suitable quantity for comparison and balancing
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purposes is the ethanol mass fraction in the

mixture.
To determine this mass fraction, the tables from
Chapter 6.1.1 can be used.
A comparison of the densities at different tempe-
ratures shows that the concentration is
substantially dependent on the sample tempera-
ture as well as the density.
If possible, the samples should be appropriately
temperature-controlled prior to measuring the
density, such as to the reference temperature
20°C. Then the concentration can be read directly
from the table with the measured density at the
relevant temperature.
No such temperature control was available for the
experiments on which this chapter is based.
Consequently, the density and temperature of the
sample were measured for each concentration
calculation. Allowance is made for the influence of
the temperature by means of linear interpolation
(see Evaluation, Chapter 6.3.5.2, Page 84 ff).
The major influence of small changes in density
on the ethanol mass fraction is illustrated in
Chapter 6.3.6, Page 91 ff. under item 5., based
on a concrete example.

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CE 600 CONTINUOUS RECTIFICATION

6.1.3 Mixing behaviour

Ethanol and water are mutually soluble. Solubility

exists across the complete concentration range.
Nevertheless, mixing problems are to be
expected!
Example: At the end of the experiment approxi-
mately 8L of mixture remain in the CE 600
evaporator, with 20%m ethanol, temperature
90°C. When the experiment is complete the top
products are collected and fed by way of a feed
tank into the evaporator, 2L, 90%m ethanol,
25°C.
This mixture remains in the evaporator overnight.
Result the next morning: The stratification in the
insulated evaporator is retained. There are still
major differences in temperature, density and
concentration between the mixture at the top and
bottom of the evaporator!
Result: To determine the density and
temperature of the mixture, the entire evaporator
content must be drained off and mixed.

62 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

6.2 Definition of background conditions, experiment series

As already described in Chapter 5.3, Page 42,

there is a wide variety of experiment variants, with
different background conditions. This also applies
to the ethanol/water mixture.
Depending on the object of the experiment, a
distinction can be made between three different
categories of usage:
1. Spontaneous experiments, with frequently
changing conditions
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2. Automatic mode, using the

various control loops
3. Comparative experiments, recording the
influence of a change
Re 1. Spontaneous experiments: Spontaneous
experiments rapidly convey a feel for the unit and
for the material mixture. While the unit is running,
immediately after altering a condition, the reaction
of the unit is observed (change in temperatures,
differential pressure, boiling behaviour, ...). The
limits of the unit are plotted. An estimation can be
quickly obtained as to whether stable operation is
to be expected under specific conditions.
Re 2. Automatic mode: Operating the unit in
automatic mode is useful when the object of the
experiment is to prepare for practical production
operations. The behaviour of the various control
loops can be observed. And the associated
measured values can be recorded. The reaction
to changes in control parameters can be
investigated. Two different temperature control
systems are also possible here.

6 Experiments - with ethanol/water mixture 63

CE 600 CONTINUOUS RECTIFICATION

Either the temperature T3 in the evaporator or the

temperature T12 in the column head can be
controlled.

Re 3. Comparative experiments: The object of

comparative experiments is to determine the
influence of one change on the measurement
results. To do this, the individual experiments
must be reproducible. Reproducibility is improved
when disturbances to the experiment are mini-
mised. Consequently, there are advantages in
avoiding automatic mode when performing
comparative experiments. Instead fixed values
should be used for the heater and for the reflux
ratio.

These instructions primarily relate to comparative

experiments.

6.2.1 Method of operation of the unit

In contrast to large-scale production units, the

CE 600 is not optimised for a specific application.
Rather, attention was paid to covering a large
number of different experiment variants at rea-
sonable expense, including in terms of the control
engineering.
The restricted height means that some infeed
heads and supply pressures are limited.
Another factor is the interaction of thermal and
hydraulic influences throughout the system.

64 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

In spontaneous experiments, changes sometimes

do not lead to the intended result.
So at this point the method of operation of the
unit for an ethanol/water mixture is depicted:
• Column differential pressure: The differential
pressure is a measure of the boiling intensity
and separation efficiency in the column. We
recommend setting the heater to produce a
differential pressure of around 10 to 20mbar. If
the pressure falls below 10mbar, the boiling
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intensity is low and the experiment takes an

unnecessarily long time. If the pressure
exceeds 20mbar the boiling intensity is high.
The volume of steam in the column is then
sometimes so great that the downward flow of
condensate is too severely impaired. The result
is then unstable operation.
• Liquid level in evaporator (D1) in batch
experiments: The minimum is given by the
switching point of the level switch (at just over
3L). For safety reasons, the heater is switched
off if the level falls below the minimum.
The maximum is based on preventing flooding
of the evaporator. The interface between the
liquid and the steam/air should always remain
visible in the level indicator tube. This results in
the practical maximum of around 10L.
• Liquid level in evaporator in continuous
experiments: A siphon is installed in the
evaporator upstream of the outlet.

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CE 600 CONTINUOUS RECTIFICATION

If the siphon was not installed, the evaporator

would quickly be completely drained as the
flow passes from the evaporator to the bottom
product tanks (B5, B6). The driving force in this
is not only the liquid head at the outlet, but also
the higher operating pressure in the evapora-
tor, referred to the ambient pressure in the bot-
tom product tank.
If the level falls below about 6L, the siphon
restricts the flow from the evaporator to the
bottom product tank at ambient pressure. This
means the range for the usable volume at
ambient pressure is limited to 6 to 10L. This
requires careful observation of the evaporator
level during operation and regular adjustment
of the regulating valve V08 (see Fig. 5.19,
Page 51).
However, the range for the usable volume is
extended during operation in accordance with
the prevailing operating pressure.
• Reflux: The reflux flows when the solenoid
valve (V01) is open owing to the difference in
height between the phase separation tank (B3)
and the column head. This difference in height
must overcome the pressure difference built up
between the column head and the phase sep-
aration tank during operation (ambient pres-
sure). If the pressure difference is too large the
reflux will be impaired, or even prevented
altogether. Conversely, the flow from the phase
separation tank to the top product tank (B4) is
not impeded when the solenoid valve (V02) is
open (both tanks are at ambient pressure). In
the case of high reflux ratios it is even possible
that top product may back-up in the phase
separation tank.

66 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

In such cases this pressure difference should

be reduced, such as by reducing the heat
output.
• Vacuum mode: During operation, minor
changes in pressure have a significant
influence on the boiling temperature. By chang-
ing the pressure a few hundredths of a bar, the
boiling intensity in the column can be greatly
increased, or may virtually disappear entirely.
This in turn influences the pressure in the
system. Regulating the pressure by altering the
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water flow into the water jet pump (P2) requires

some practice. So CE 600 enables relatively
stable operation in vacuum mode during batch
experiments. However, vacuum mode in
continuous experiments cannot run perma-
nently stable because the overall system
responds too sensitively to fluctuations.
• Infeed heads of the sieve plate column: The
choice of infeed to the sieve plate column
influences the stability and reproducibility of the
experiment. Top infeed can result in
inadequate stability and uniformity.
• Production factors, fluctuations in ambient
conditions and changes during operation of the
unit may cause the unit properties to change
and so shift the optimum parameter over time.
• The experiments described below were carried
out using an earlier version of the unit. The
modifications made to individual components
since then may result in slightly different meas-
ured results in some experiments.

6 Experiments - with ethanol/water mixture 67

CE 600 CONTINUOUS RECTIFICATION

6.2.2 Comparative experiments, experiment series

When defining the conditions for comparative

experiments and experiment series, the difficulty
is in safeguarding continuous, stable and
reproducible operation for all the planned experi-
ments. Without practical testing, there is a severe
risk that any unsuitable choice of conditions will
only be identified during the actual running of the
experiments. That is why it is advisable to check
a planned new series of experiments in advance
by means of spontaneous experiments and
correct them as necessary.
It is conceivable that a large number of different
experiment series could be developed over time.
In the following chapters two experiment series
are presented in which the conditions of the
individual experiments are coordinated.

It is possible to discard the top and bottom

products after each experiment and apply a new
mixture of input substances for each new
experiment.

However, for the experiments on which this

chapter is based the products were remixed after
each experiment (see also Chapter 5.6.4,
Page 55). The experiment reports, worksheets,
analyses and suchlike detailed in the following
relate to this method.

68 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

6.2.3 Example of a batch experiment series

The batch experiment series comprises

experiments V1 to V5.
Tab. 6.3 lists the common conditions applicable to
all experiments V1 to V5.
The heating power is indicated as a percentage of
the maximum 4,0kW, in line with the input prompt
on the PC.
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Condition type Name Symbol/unit Value

Volume V in L 10
Initial mixture
Ethanol mass fraction wE in %m 25
·
Cooling water quantity Volumetric flow V in L/h 150

Reflux ratio R in % 100

Start with
Heating power Pel in % 100

At T3 ≥ TWarm , Reflux ratio R in % 100

Continue with Heating power Pel in % 20

At Tx = constant, Reflux ratio R in % 50

operation with Heating power Pel in % 30

At T3 ≥ TEnd , Reflux ratio R in % 50

Cancel with Heating power Pel in % 0

After t = 5 min, Reflux ratio R in % 100

sampling Heating power Pel in % 0

Tab. 6.3 Common conditions for batch experiment series

6 Experiments - with ethanol/water mixture 69

CE 600 CONTINUOUS RECTIFICATION

The “variable” conditions by which experiments

V1 to V5 differ are set out in Tab. 6.4.

Condition type Symbol, Experiment

Unit V1 V2 V3 V4 V5

Column type: Pd, SP-8, SP-4 SP-8 SP-8 SP-8 Pd SP-4

Operation at ambient pressure or p = atm or

atm 0,5 atm atm atm
vacuum p in bar abs.

Reflux ratio,
R in % 0 0 50 50 50
in operation

Evaporator temperature,
TWarm in °C 70 50 70 70 70
after warm-up

Evaporator temperature,
TEnd in °C 92 75 92 92 92
at end of operation

Key: Pd: Packed column

SP-8: Sieve plate column with 8 plates
SP-4: Sieve plate column with 4 plates
atm: Atmospheric pressure / Ambient pressure
Tab. 6.4 Variable conditions for batch experiment series

After performing these five experiments, the

following comparisons are possible:
• Sieve plate column / Packed column
• Sieve plate column, 8 plates / Sieve plate
column, 4 plates
• Vacuum mode / Operation at ambient pressure
• Reflux ratios 0, 50 and 100%
Experiment V3 is described in detail and
evaluated by way of example for this experiment
series in Chapter 6.3, Page 74.

70 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

The abort condition with “TEnd = Evaporator

temperature, at end of operation, designated in
the table as T3 ≥ TEnd requires some explanation.
It is necessary to adjust the abort condition
because the boiling points of the input substances
and mixtures are pressure-dependent. As the
absolute pressure falls the boiling points drop. An
identical abort temperature for experiments in
vacuum mode and at ambient pressure would
make it difficult to compare the experiments.
In fact, an unchanged abort temperature of 92°C
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would make no sense for the experiment V2

described. Then the abort temperature would be
greater than the boiling temperature of the high-
boiling water component (around 81°C at 0,5 bar
abs.). That means 92°C in the evaporator cannot
be reached at 0,5 bar abs.
That is why the numeric values for the abort tem-
perature TEnd are defined here as the mean value
of the initial mixture boiling temperature and the
boiling temperature of pure water, referred to the
respective pressure.
Similarly with regard to the feed-forward condition
“Evaporator temperature, after warmup”, desig-
nated in the tables as TWarm. These tempera-
tures, too, are selected so that the experiments
are roughly comparable for vacuum mode and
operation at ambient pressure (temperature gap
between reduced heating power after warm-up
and attainment of boiling temperature).

6 Experiments - with ethanol/water mixture 71

CE 600 CONTINUOUS RECTIFICATION

6.2.4 Example of a continuous experiment series

The continuous experiment series comprises

experiments V6 to V8.
Tab. 6.5 lists the common conditions applicable to
all experiments V6 to V8.

Condition type Name Symbol/unit Value

Initial mixture Volume V in L 9

in the evaporator Ethanol mass fraction wE in %m 25

Initial mixture Volume V in L 10

in the feed tanks Ethanol mass fraction wE in %m 25
·
Cooling water quantity Volumetric flow V in L/h 300

Reflux ratio R in % 100

Start with
Heating power Pel in % 100

Reflux ratio R in % 100

At T3 ≥ 80°C , Continue with
Heating power Pel in % 25

Reflux ratio R in % 25

5 min after first reflux, Heating power Pel in % 25

operation with Start feed pump n in % 21

Start B.pr. in B.pr.tank ------- ----

Reflux ratio R in % 25

After feed volume 5L, Heating power Pel in % 0

abort with Stop feed pump n in % 0

Stop B.pr. in B.pr.tank ------- ----

After t = 5 min, sampling Reflux ratio R in % 100

Key: B.pr.: Bottom product

B.pr.tank: Bottom product tank
T3: Evaporator temperature
Tab. 6.5 Common conditions for continuous experiment series

72 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

The heating power is indicated as a percentage of

the maximum 4,0kW, in line with the input prompt
on the PC.
The percentage speed presetting for the feed
pump is referred to the maximum speed.

Experiments V6 to V8 are intended for operation

at ambient pressure. The sieve plate column is
used in each, to enable comparisons with the
batch experiments V1 to V3.
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The abort condition “After feed volume 5L” is a

compromise between the time and measurement
commitment and the additional expected results.
If required, the experiment can of course be
prolonged by likewise pumping the remaining 5L
feed into the column.

The “variable” conditions by which experiments

V6 to V8 differ are set out in Tab. 6.6.

Condition type Experiment

V6 V7 V8

Feed preheating Yes/No No Yes Yes

Infeed to sieve plate column

Bottom Bottom Centre
Centre/Bottom

Tab. 6.6 Variable conditions for

continuous experiment series

Experiment V7 is described in detail and

evaluated by way of example for this experiment
series in Chapter 6.4, Page 97 ff.

6 Experiments - with ethanol/water mixture 73

CE 600 CONTINUOUS RECTIFICATION

6.3 Example of a batch experiment, V3

Experiment V3 originates from the batch

experiment series (see also Chapter 6.2.3,
Page 69). Conditions for this experiment are:
• Initial mixture 10L, ethanol fraction 25%m
• Sieve plate column
• Operation at ambient pressure
• Cooling water flow 150L/h
• Operation at heating power 30%,
Reflux ratio 50%
• Rectification aborted (heater off) on reaching
evaporator temperature T3 = 92°C

6.3.1 Experiment aims

Experiment aims are:

1. To concentrate the ethanol
2. To record the measured value using the data
acquisition program (temperature and
pressure profiles)
3. To determine the ethanol concentration in the
initial mixture, top product and bottom product
4. To depict the change over time of the ethanol
concentration in the top product
5. To check the concentrations by means of mass
balances

6.3.2 Experimental setup

Connected CE 600 unit, with accessories as set

out in Chapter 5.2, Page 41.

74 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

6.3.3 Performing the experiment

• Observe the safety instructions (see Chapter 2,

Page 5)
• Prepare the unit as set out in Chapter 5.4.1,
Page 43. Open the ball valve V34 underneath
the pressure gauge.
• The requirement is a canister containing more
than 10L of initial mixture, ethanol: 25%m,
water: 75%m (new addition, e.g. for 12L, with
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

2885g ethanol and 8655g water).

• Mix the initial mixture in the canister.
• Identify the density and temperature of the
initial mixture. Check the concentration.
• Transfer the initial mixture from the canister
into the two feed tanks (B1,B2). Use measuring
cups for this, and weigh the content of each cup
(net weight of each). Fill the feed tanks up to
their 5litre marks. Also weigh the residue in the
measuring cup.
• Transfer the initial mixture from the feed tanks
through the column into the evaporator (see
Chapter 5.6.2, Page 52). To do so, open the
ball valve on the column during pumping.
• Press Reset on the differential pressure display
(item 23 in Fig. 3.8, Page 17 ).
• Unit operation by PC. Set and start the meas-
urement data acquisition.
• Set the reflux ratio to 100% initially
• Open the condenser water supply and adjust it
to about 150L/h

6 Experiments - with ethanol/water mixture 75

CE 600 CONTINUOUS RECTIFICATION

• Switch on the heater. Initial fixed value 100%

• When evaporator temperature T3 = 70°C is
reached, reduce the heater to the fixed value
20%
• Wait for distillate to appear at the phase
separation tank (B3), reflux begins and the
system reaches a state of equilibrium
(temperatures constant about 20minutes after
first appearance of distillate).
Then changes to operating conditions:
- Heater from 20 to 30%
- Reflux ratio from 100 to 50%
• When the minimum sample volume is reached,
withdraw the top product from the top product
tank (B4). Determine the mass, density and
temperature. Keep the sample (for a later
mixed sample). Perform a new measurement
as soon as the minimum sample volume has
been reached again.
• Abort on reaching T3 = 92°C
• 5 minutes after aborting, change reflux ratio to
100%. Shut off the water supply.
• Measure the remaining top product (residue
from top product tank together with residue
from phase separation tank); determine the
mass, density and temperature.
• Pour together and intermingle the previous top
product samples and measure the total mass,
density and temperature.
• Cool the bottom product from the evaporator
(see also Chapter 5.6.3, Page 53). Drain off
the cooled bottom product, weigh it and mix it
in the second canister.

76 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

Take a sample of the bottom product mixture,

determine density and temperature.
• Fill canister with unused initial mixture and with
top and bottom product. Mix well.
This provides a new initial mixture for the next
experiment.

6.3.4 Measured values

6.3.4.1 Measurement data from the data acquisition program (experiment

All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

aim 2)

The data acquisition program saves the measured

values in files. This measured value file contains
a chronological sequence of measured data
records. A measured data record is a snapshot
of all the measured values at the given point in
time.
For this experiment an interval of 30 seconds was
selected (representing the time between
recording of two measured data records). Based
on a minimum recording period of 100 minutes,
this produces more than 4200 measured values
(two measured data records per minute, each
with 21 measured values).
A tabular representation of the complete
measured value file, with all measured data
records, would be too extensive to set out at this
point. Consequently, a selection was made to
depict the most informative time bands.
The measured values for the selected time bands
are imported into MS-Excel (see measured value
tables Tab. 6.7 to Tab. 6.9).

6 Experiments - with ethanol/water mixture 77

CE 600 CONTINUOUS RECTIFICATION

The MS-Excel Import function is used to import

the measured values.
The selected time bands are:
• Column start-up until production of the first
distillate
• Start of rectification under operating conditions
• End of rectification under operating conditions

Alongside the differential pressure dp1 and the

temperatures T1 to T16, these measured value
tables also contain the three control variables Y1
to Y3. In the experiment described here, fixed
values were programmed on PC rather than using
the software controllers. Using the defined
operating conditions (heater Y1=30% and reflux
ratio Y2=50%), this enables the start and end of
the actual experiment (here 14:30 and 15:06
hours) to be determined from the measured value
tables.

The differential pressure and selected tempera-

tures are presented graphically in
Chapter 6.3.5.1, Page 82.

78 6 Experiments - with ethanol/water mixture

 All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

W 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7GS<3HO <5 <Q

KKPPVV ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& PEDU   

Tab. 6.7
                    
CE 600
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    

6 Experiments - with ethanol/water mixture

                    
                    
                    
                    
                    

V3, measured values at column start-up

                    
                    
                    
CONTINUOUS RECTIFICATION

                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    

7HPSHUDWXUHVDQGGLIIHUHQWLDOSUHVVXUHDFFRUGLQJWRIORZGLDJUDPPV\VWHPGLDJUDP
<<<&RQWUROOHU2XWSXWVIRUKHDWHU5HIOX[UDWLRSXPSVSHHG

79
80
W 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7GS<3HO <5 <Q
KKPPVV ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& PEDU   

Tab. 6.8
                    
CE 600
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    

V3, measured values at start of rectification

                    
                    
CONTINUOUS RECTIFICATION

                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    

7HPSHUDWXUHVDQGGLIIHUHQWLDOSUHVVXUHDFFRUGLQJWRIORZGLDJUDPPV\VWHPGLDJUDP
<<<&RQWUROOHU2XWSXWVIRUKHDWHU5HIOX[UDWLRSXPSVSHHG

6 Experiments - with ethanol/water mixture

 All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

W 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7GS<3HO <5 <Q

KKPPVV ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& PEDU   

Tab. 6.9
                    
CE 600
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    

6 Experiments - with ethanol/water mixture

                    
                    
                    
                    
                    
                    

V3, measured values at end of rectification

                    
                    
CONTINUOUS RECTIFICATION

                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    

7HPSHUDWXUHVDQGGLIIHUHQWLDOSUHVVXUHDFFRUGLQJWRIORZGLDJUDPPV\VWHPGLDJUDP
<<<&RQWUROOHU2XWSXWVIRUKHDWHU5HIOX[UDWLRSXPSVSHHG

81
CE 600 CONTINUOUS RECTIFICATION

6.3.4.2 Self-recorded measured values (without PC assistance)

The self-recorded measured values are primarily

the masses, densities and temperatures of the
various mixtures/products. In the course of the
experiment they were entered by hand on the
“Batch worksheet” (see Tab. 7.1, Page 121).
These measured values are presented, together
with the evaluation, in Chapter 6.3.5.2, Tab. 6.10,
Page 85.

6.3.5 Evaluation

6.3.5.1 Presentation of automatically recorded measurement data (experiment

aim 2)

The bases of the following diagrams are the measured value tables Tab. 6.7,
Page 79 to Tab. 6.9 . Please note that the diagrams have differing tempera-
ture and pressure ranges.

90 15

Differential pressure in mbar

80 13

70 11
Temperature in °C

60 9

50 7

40 5

30 3

20 1

10 -1
13:55 13:57 13:59 14:01 14:03 14:05 14:07 14:09 14:11 14:13 14:15
Time
T3, Evaporator temperature T4, Plate 1 temperature
T6, Plate 3 temperature T8, Plate 5 temperature
T10, Plate 7 temperature T12, Top temperature
dp1, Column pressure loss

Fig. 6.1 V3, Temperature and pressure profile at column start-up

82 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

Differential pressure in mbar

Temperature in °C
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

Time
T3, Evaporator temperature T4, Plate 1 temperature
T6, Plate 3 temperature T8, Plate 5 temperature
T10, Plate 7 temperature T12, Top temperature
dp1, Column pressure loss

Fig. 6.2 V3, Temperature and pressure profile at start of rectification

Differential pressure in mbar

Temperature in °C

Time
T3, Evaporator temperature T4, Plate 1 temperature
T6, Plate 3 temperature T8, Plate 5 temperature
T10, Plate 7 temperature T12, Top temperature
dp1, Column pressure loss

Fig. 6.3 V3, Temperature and pressure profile at end of rectification

6 Experiments - with ethanol/water mixture 83

CE 600 CONTINUOUS RECTIFICATION

6.3.5.2 Evaluation of self-recorded measured values

The following Tab. 6.10, Page 85 presents the

measured masses, densities and temperatures,
together with the total masses and concentrations
calculated from them.

The individual mixture masses at the start and

end of the experiment have been added together.
In determining the total mixture mass at the start
of the experiment, the “residue” - here 8,0g - must
be taken into account. This “residue” results from
the fact that when transferring from the last meas-
uring cup into the feed tank, the total volume of
10,0L is reached before the measuring cup is
completely empty. The “residue” is thus the mass
of the mixture remaining in the measuring cup.

Re experiment aim 3 - To determine the

ethanol concentrations:
For all the samples, the ethanol mass fraction E
wE was determined from the density and tempe-
rature by means of linear interpolation. The
procedure is explained here in respect of the first
sample (mixture at start of experiment) by way of
example:
The measured values of the first top product
sample are:
Total density ρM = 962 kg/m³ at mixture tempera-
ture TM = 22,8°C (index M for measured value).

84 6 Experiments - with ethanol/water mixture

6 Experiments - with ethanol/water mixture All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

CE 600
Measurement Evaluation
Clock Product/measurement Mass Tempera- Density Level Comments Mass Mass fraction
no. net ture in Evap net Ethanol, wE

CONTINUOUS RECTIFICATION
g °C kg/L L g %m
13:15 Start, mixture, Evap ----- 22,8 0,962 10,0 9695,0 23,8
14:41 T.pr., 1. 430,5 24,0 0,825 9,3 ----- 85,9
14:52 T.pr., 2. 370,5 22,7 0,832 9,0 ----- 83,6
15:06 T.pr., 3. 429,0 22,8 0,836 9,0 ----- 82,0
----- End, T.pr., mixture 1392,5 22,8 0,832 ----- ----- 83,6
----- End, B.pr., Evap ----- 22,1 0,974 ----- 8219,0 15,3

Measurement
Start, Fill feed tank, 1945,0 1932,5 1930,5 1942,0 1953,0
Individual masses in g (-8,0g residue, when 10L reached)
End, B.pr., from Evap, 2022,0 2046,0 1904,0 1788,5 458,5
Individual masses in g

Key: T.pr.: Top product; B.pr.: Bottom product; Evap: Evaporator

Tab. 6.10 V3, Self-recorded measured values, with evaluation

85
CE 600 CONTINUOUS RECTIFICATION

Consequently, wE cannot be read directly from

Tab. 6.1, Page 59 because there ρ is listed only
for integer wE and integer T. The four ρ values for
measured value 962kg/m³ belonging to the next
highest and next lowest integer values wE and T
can be read however:
ρA = ρ(23%m, 22°C) = 963,51 kg/m³
ρB = ρ(23%m, 23°C) = 963,01 kg/m³
ρC = ρ(24%m, 22°C) = 962,05 kg/m³
ρD = ρ(24%m, 23°C) = 961,53 kg/m³
As a result, ρ23 = ρ(23%m, 22,8°C) is produced
by linear interpolation as:

23C – T
 23 =  B + ---------------------------------
M
-   A – B 
23C – 22C
23C – 22, 8C 3
 23 = 963,01 + ---------------------------------------   963,51 – 963,01  = 963, 11 kg  m
23C – 22C

Correspondingly, for ρ24 = ρ(24%m, 22,8°C)

the value 961,63 kg/m³ is obtained.
The value wE being sought is obtained by linear
interpolation with the aid of ρ23 and ρ24 as per:

 23 –  M
w E = 23 + -----------------------   24 – 23 
 23 –  24
963,11 – 962
w E = 23 + -----------------------------------------   24 – 23  = 23 75 %m
963,11 – 961,63

After rounding, this produces the desired ethanol

mass fraction of wE = 23,8%m.

86 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

Re experiment aim 4. To present the change

over time in the ethanol concentration in the
top product
Fig. 6.4 shows the progression over time of the
ethanol concentration in the top product:
wE in %m
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

Time

Clock Ethanol mass fraction

wE in %m

14:41 85,9

14:52 83,6

15:06 82,0

Fig. 6.4 V3, Progression over time of the ethanol concentration in the top product

6 Experiments - with ethanol/water mixture 87

CE 600 CONTINUOUS RECTIFICATION

Re experiment aim 5. To check the concen-

trations by means of mass balances
It is useful to check the measured values with the
aid of mass balances. Any conflicts arising from
the mass balances indicate errors in evaluation or
inaccurate measurement data.
At this point the mixture and ethanol masses at
the start and end of the experiment are compared:
The following examples illustrate the graphical
symbols used below:

m: Mixture mass, general

m E: Ethanol mass, general
wE : Ethanol mass fraction, general
m(Start): Mixture mass, at start of experiment
mE(End): Ethanol mass, at end of experiment
wE(T.pr.): Ethanol mass fraction in top product
m(T.pr.): Mixture mass, top product

Mixtures mass balance:

To be checked:
m Start  = m End  (6.1)
where
m  End  = m  T.pr.  + m  B.pr.,Evap  (6.2)

The following table consolidates the values from

Tab. 6.10, Page 85 and adds them together
according to the formula (6.2):

88 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

Mass, net, in g

m(Start) m(End)

m(Start) 9695,0 ------

m(T.pr.) ------ 1392,5
m(B.pr.,Evap) ------ 8219,0
Total 9695,0 9611,5

Tab. 6.11 V3, Mixture balancing

The comparison of the two values shows that at

the end of the experiment there is still 99,1% of
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

the original mixture mass present.

Ethanol mass balance:

In line with the mass balances for the mixtures,
(6.1) and(6.2), the resultant ethanol mass
balances are:
To be checked:
m E  Start  = m E  End  (6.3)
where
m E  End  = m E  T.pr.  + m E  B.pr.,Evap  (6.4)

The ethanol mass fraction wE is defined as the

ratio of the ethanol mass mE to the mixture mass
m. This enables the individual ethanol masses to
be expressed as the product of the mixture mass
and the mass fraction, e.g. for:

m E  T.pr. = m  T.pr.  w E  T.pr. (6.5)

The following table summarises how the values

from Tab. 6.10, Page 85 and Tab. 6.11, Page 89
are evaluated using the equations (6.4) and (6.5):

6 Experiments - with ethanol/water mixture 89

CE 600 CONTINUOUS RECTIFICATION

Designation ... Start End

m(...) wE(...) mE(...) m(...) wE(...) mE(...)

g %m g g %m g

Start 9695,0 23,8 2307,5 ------ ------ ------

T.pr. ------ ------ ------ 1392,5 83,6 1164,0
B.pr.,Evap ------ ------ ------ 8219,0 15,3 1257,5
Total 9695,0 ------ 2307,5 9611,5 ------ 2421,5

Tab. 6.12 V3, Ethanol balancing

The comparison of the two values shows that at

the end of the experiment there is still 104,9% of
the original ethanol mass present.
This surprising result is commented upon in
Chapter 6.3.6 under item 5.

90 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

6.3.6 Comments, assessment

The comments and assessment are based on the

pre-defined experiment aims:
Re 1. To concentrate the ethanol and
Re 3. To determine the ethanol concentration
in the initial mixture, top product and bottom
product
The initial mixture was separated into the top
product, with increased ethanol content, and the
bottom product, with reduced ethanol content.
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

The ethanol mass fraction in the top product is

greater than in the initial mixture by a factor of
3,51.

Re 2. To record the measured value using the

data acquisition program (temperature and
pressure profiles)
Fig. 6.1, Page 82 shows the profiles at column
start-up. The temperature rise in the individual
plates from bottom to top is clearly traceable.
Some of the temperature curves have a kink in
them during heat-up. A kink of this kind can be
interpreted as forming the equilibrium between
vapour and liquid, on occurrence of the first
condensate.
While the equilibriums are being created, the
pressure loss in the column increases steadily.
The time between reaching the boiling tempera-
ture in the column head and the initial distillate in
the phase separation tank (B3) is about 5minutes
under the selected conditions. When the first
distillate occurs, the equilibriums have formed
and the differential pressure in the column
increases much less markedly.

6 Experiments - with ethanol/water mixture 91

CE 600 CONTINUOUS RECTIFICATION

Fig. 6.2, Page 83 shows the differential pressure

and temperatures at the start of rectification. At
14:30 hours the operating conditions are adjusted
(reflux ratio R from 100 to 50%, heater from 20 to
30%). The effect of the increase in heating power
is felt only slowly, identifiable by the flat rate of rise
of the curve for the evaporator temperature T3.
A rapid reaction does occur, however, because of
the reduced reflux. The temperatures on the
upper plates 5 and 7, in particular, rise rapidly.
The cause of this is the halving of the much cooler
reflux flow into the column head (reflux tempera-
ture T13 at 14:30 around 25°C). That is to say, the
mixture of cooler reflux and newly formed
condensate on the plates becomes warmer. New
equilibriums are formed.

Fig. 6.3, Page 83 shows the profiles at the end of

rectification. Operations are aborted by switching
off the heater (0%) at around 15:06 hours. The
reaction of the temperatures in the column and
column head is rapid. An initial rapid drop in
temperatures by 4 to 8°C is detected. The fastest
reaction is on the column head and the upper
plates. At the same time the steam pressure falls,
so the column loses condensate.
The reflux ratio R was changed from 50 to 100%
at 15:11 hours. The purpose of this delay 5
minutes after the actual abort is to obtain as much
top product as possible under conditions similar to
those during operation.

92 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

Then the last top product sample is taken.

As a reaction to the larger flow of cooler reflux (at
15:11 hours around 27°C) into the column head,
an accelerated fall in the temperatures in the
upper area of the column is detected.

Re 4. To present the change over time in the

ethanol concentration in the top product
Fig. 6.4, Page 87 shows the decrease in the
ethanol mass fraction wE in the top product. It is
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

seen that wE decreases by 3,9 percentage points

in the course of the experiment.
At first glance that appears a substantial
decrease.
The reason for this decrease is that there is a
greater proportion of ethanol in the newly created
top product than in the bottom product in the
evaporator. As a result, the bottom product in the
evaporator loses ethanol in the course of the
experiment. The decreasing concentration in the
evaporator then results in a reduced concen-
tration in the top product.

6 Experiments - with ethanol/water mixture 93

CE 600 CONTINUOUS RECTIFICATION

Re 5. To check the concentrations by means

of mass balances
Evaluation of the experiment shows that at the
end of the experiment there is still 99,1% of the
original mixture mass present.
Taking into account the losses during sampling
and transfer, and due to evaporation, these
values are of a realistic magnitude.
By contrast, it is surprising that at the end of the
experiment there is still 104,9% of the original
ethanol mass present.
There cannot be an actual increase in ethanol
mass, because no chemical conversion takes
place in the rectification unit. A similar loss as in
the case of the mixture masses would be
expected.
Consequently, an investigation is conducted as to
whether a realistic value is produced when
measurement inaccuracies are taken into
account.
Of importance to the balancing operation are
masses and mass fractions. The accuracy in
determining masses is extremely high.
The influence of the mass fractions on the
balancing result is much more marked, because
both the temperature and the density are incorpo-
rated into the calculation of mass fractions.
Of these two measured values, the density has
the greater influence.
To measure the density, the areometer shown
adjacent was used. The measurement error for
this areometer is composed of the actual
instrument error
Fig. 6.5 Areometer used

94 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

(Scale does not precisely match the actual

penetration depth) and the read error (meniscus
formation on the scale, parallax).
The measurement error for the areometer used is
unfortunately not specified. Consequently, only
the effect of the read error is investigated here:

The measuring range of the areometer is 0,800 to

1,000kg/L. The difference in density between two
graduations on the scale is 0,002kg/L.
Consequently, the read error is estimated as
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

± 0,001kg/L.

The following Tab. 6.13 shows how the variation

in density by 0,001kg/L affects the ethanol mass
fraction wE (corrected values are shown here in
blue).

Designation ... Values Corrected values

ρ(...) wE(...) ρK(...) wE,K(...)

kg/L %m kg/L %m

Start 0,962 23,8 0,961 24,4

T.pr. 0,832 83,6 0,833 83,2
B.pr.,Evap 0,974 15,3 0,975 14,6
Tab. 6.13 V3, Influence of density measurement error on ethanol mass fraction

6 Experiments - with ethanol/water mixture 95

CE 600 CONTINUOUS RECTIFICATION

These corrected values result in the following

balance (see Tab. 6.14):

Designation ... Start End

m(...) wE,K(...) mE,K(...) m(...) wE,K(...) mE,K(...)

g %m g g %m g

Start 9695,0 24,4 2366,0 ------ ------ ------

T.pr. ------ ------ ------ 1392,5 83,2 1158,5
B.pr.,Evap ------ ------ ------ 8219,0 14,6 1200,0
Total 9695,0 ------ 2366,0 9611,5 ------ 2358,5

Tab. 6.14 V3, Ethanol balancing, with influence of density measurement error

The comparison of the two values shows that at

the end of the experiment there is now still 99,7%
of the original ethanol mass present.
The apparent contradiction can thus be explained
solely by the areometer read error.
The influence of the densities here is so great that
a change in density of 0,001kg/L alters the
balance by more than 5 percentage points.

96 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

6.4 Example of a continuous experiment, V7

6.4.1 Experiment aims

Experiment aims are:

1. To concentrate the ethanol
2. To record the measured value using the data
acquisition program (temperature and
pressure profiles)
3. To determine the ethanol concentration in the
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

initial mixture, top product and bottom product

4. To present the change over time in the ethanol
concentration in the top and bottom products
5. To check the concentrations by means of mass
balances

6.4.2 Experimental setup

Connected CE 600 unit, with accessories as set

out in Chapter 5.2, Page 41.

6.4.3 Performing the experiment

• Observe the safety instructions (see Chapter 2,

Page 5)
• Prepare the unit as set out in Chapter 5.5.1,
Page 48. Open the ball valve V34 underneath
the pressure gauge.
• The requirement is a canister containing more
than 19L of initial mixture, ethanol: 25%m,
water: 75%m (new addition, e.g. for 20L, with
4808g ethanol and 14425g water).

6 Experiments - with ethanol/water mixture 97

CE 600 CONTINUOUS RECTIFICATION

• Mix the initial mixture in the canister.

• Identify the density and temperature of the
initial mixture. Check the concentration.
• Transfer the initial mixture from the canister
into the two feed tanks (B1,B2). Use measuring
cups for this, and weigh the content of each cup
(net weight of each). Fill the feed tanks up to
their 5litre marks. Also weigh the residue in the
measuring cup (after pumping out, pour into
feed tank).
• Transfer 9 of the 10L of initial mixture from the
feed tanks through the column into the
evaporator (see Chapter 5.6.2, Page 52).
While transferring, open the ball valve on the
column. Switch the pump off when the 9L level
is reached according to the markings on the
feed tanks.
• Transfer additional initial mixture from the
canister into the two feed tanks. Use measur-
ing cups for this, and weigh the content of each
cup (net weight of each). Fill the feed tanks up
to their 5L marks. Also weigh the residue in the
measuring cup.
• Check whether the heat exchanger (W2) is
switched for feed heating.
• Press Reset on the differential pressure display
(item 23 in Fig. 3.8, Page 17 ).
• Unit operation by PC. Set and start the meas-
urement data acquisition.
• Set the reflux ratio to 100% initially
• Open the condenser water supply and adjust it
to about 300L/h.

98 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

• Switch on the heater. Initial fixed value 100%.

• When evaporator temperature T3 = 80°C is
reached, reduce the heater to the fixed value 25%.
• Wait until distillate appears at the top tube of
the phase separation tank (B3) and reflux
begins. After waiting 5minutes, change
operating conditions:
– Start feed in column, pump (P1) on at 30%
– Reflux ratio from 100 to 25%
– In the line from the evaporator to the front
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

bottom product tank, open the ball valve V25

completely and the regulating valve V08
slightly (see Chapter 5.5.1, Page 48, and
Fig. 5.19, Page 51).
– In the line from the evaporator to the front bot-
tom product tank, open the regulating valve
completely and the regulating valve slightly.
– Note down the volume in the evaporator
– Keep the level in the evaporator as constant
as possible, adjusting the regulating valve
setting as necessary.
• When the minimum sample volume is reached,
withdraw the top product from the top product
tank (B4). Determine the mass, density and
temperature. Keep the sample (for a later mixed
sample). Note down the volume in the evaporator.
Perform a new measurement as soon as the min-
imum sample volume has been reached again.
• When the minimum sample volume is reached,
withdraw the bottom product from the bottom
product tank (B5). Determine the mass, density
and temperature.
Keep the sample (for a later mixed sample). Note
down the volume in the evaporator. Perform a
new measurement as soon as the minimum
sample volume has been reached again.

6 Experiments - with ethanol/water mixture 99

CE 600 CONTINUOUS RECTIFICATION

• Abort e.g. after adding 5L feed:

– Pump off
– Heater off
– Close valve from evaporator to bottom
product tank
• 5minutes after aborting, change reflux ratio to
100%. Shut off the water supply.
• Measure the remaining bottom product (totally
drain bottom product tank); determine mass,
density and temperature.
• Pour together and intermingle the previous
bottom product samples and measure the total
mass, density and temperature.
• Measure the remaining top product (residue
from top product tank together with residue
from phase separation tank); determine the
mass, density and temperature.
• Pout together and intermingle the previous top
product samples and measure the total mass,
density and temperature.
• Cool the bottom product from the evaporator
(see Chapter 5.6.3, Page 53). Drain off the
cooled bottom product, weigh it and mix it in the
second canister. Take a sample of the bottom
product mixture, determine density and
temperature.
• Fill canister with unused initial mixture and with
top product and the two bottom products. Mix
well.
This provides a new initial mixture for the next
experiment.

100 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

6.4.4 Measured values

6.4.4.1 Measurement data from the data acquisition program (experiment

aim 2)

The data acquisition program saves the measured

values in files. This measured value file contains
a chronological sequence of measured data
records. A measured data record is a snapshot
of all the measured values at the given point in
time.
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

For this experiment an interval of 30 seconds was

selected (representing the time between
recording of two measured data records). Based
on a minimum recording period of 120 minutes,
this produces more than 5040 measured values
(two measured data records per minute, each
with 21 measured values).
A tabular representation of the complete
measured value file, with all measured data
records, would be too extensive to set out at this
point. Consequently, a selection was made to
depict the most informative time bands.
The selected time bands are identical to the batch
experiment:
• Column start-up until production of the first
distillate
• Start of rectification under operating conditions
• End of rectification under operating conditions

6 Experiments - with ethanol/water mixture 101

CE 600 CONTINUOUS RECTIFICATION

The measured values for the selected time bands

are imported into MS-Excel (see measured value
tables Tab. 6.15 to Tab. 6.17). The MS-Excel
Import function is used to import the measured
values.

Alongside the differential pressure dp1 and the

temperatures T1 to T16, these measured value
tables also contain the three control variables Y1
to Y3. In the experiment described here, fixed
values were programmed on PC rather than using
the software controllers. Using the defined
operating conditions (heater Y1=25%, reflux ratio
Y2=25%, pump Y3=30%), this enables the start
and end of the actual experiment (here 16:35 and
17:44 hours) to be determined from the measured
value tables.

The graphical view is presented in

Chapter 6.4.5.1, Page 106.

102 6 Experiments - with ethanol/water mixture

 All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

W 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7GS<3HO <5<Q

KKPPVV ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& PEDU   
                    
CE 600

Tab. 6.15
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    

6 Experiments - with ethanol/water mixture

                    
                    
                    
                    
                    

V7, measured values at column start-up

                    
                    
                    
CONTINUOUS RECTIFICATION

                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    

7HPSHUDWXUHVDQGGLIIHUHQWLDOSUHVVXUHDFFRUGLQJWRIORZGLDJUDPPV\VWHPGLDJUDP
<<<&RQWUROOHU2XWSXWVIRUKHDWHU5HIOX[UDWLRSXPSVSHHG

103
 W 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7GS<3HO <5 <Q

104
KKPPVV ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& PEDU   
                    
CE 600

Tab. 6.16
                    
                   
                   
                    
                   
                   
                   
                   
                   
                   
                   
                   
                   
                   
                   
                   
                   
                   
                   
                   

V7, measured values at start of rectification

                   
CONTINUOUS RECTIFICATION

                   
                   
                   
                   
                   
                   
                   
                   
                   
                   
                   
                   
                   
                   
                   
                   
                   

7HPSHUDWXUHVDQGGLIIHUHQWLDOSUHVVXUHDFFRUGLQJWRIORZGLDJUDPPV\VWHPGLDJUDP
<<<&RQWUROOHU2XWSXWVIRUKHDWHU5HIOX[UDWLRSXPSVSHHG

6 Experiments - with ethanol/water mixture

 All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

W 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7GS <3HO <5 <Q
KKPPVV ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& ƒ& PEDU   
                   
CE 600

Tab. 6.17
                   
                   
                   
                   
                   
                   
                    
                    
                    
                    
                    
                    
                    
                    
                    

6 Experiments - with ethanol/water mixture

                    
                    
                    
                    
                    
                    

V7, measured values at end of rectification

                    
CONTINUOUS RECTIFICATION

                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    
                    

                    

7HPSHUDWXUHVDQGGLIIHUHQWLDOSUHVVXUHDFFRUGLQJWRIORZGLDJUDPPV\VWHPGLDJUDP
<<<&RQWUROOHU2XWSXWVIRUKHDWHU5HIOX[UDWLRSXPSVSHHG

105
CE 600 CONTINUOUS RECTIFICATION

6.4.4.2 Self-recorded measured values (without PC assistance)

The self-recorded measured values are primarily

the masses, densities and temperatures of the
various mixtures/products. In the course of the
experiment they were entered by hand on the
“Continuous worksheet” (see Tab. 7.2,
Page 122).
These measured values are presented, together
with the evaluation, in Chapter 6.4.5.2, Tab. 6.18,
Page 109.

6.4.5 Evaluation

6.4.5.1 Presentation of automatically recorded measurement data

(experiment aim 2)

The bases of the following diagrams are the measured value tables
Tab. 6.15, Page 103 to Tab. 6.17 . Please note that the diagrams have
differing temperature and pressure ranges.

90 15

Differential pressure in mbar

80 13

70 11
Temperature in °C

60 9

50 7

40 5

30 3

20 1

10 -1
16:10 16:12 16:14 16:16 16:18 16:20 16:22 16:24 16:26 16:28 16:30
Time

T3, Evaporator temperature T4, Plate 1 temperature

T6, Plate 3 temperature T8, Plate 5 temperature
T10, Plate 7 temperature T12, Top temperature
dp1, Column pressure loss

Fig. 6.6 V7, Temperature and pressure profile at column start-up

106 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

92 26

Differential pressure in mbar

90 24
Temperature in °C

88 22

86 20

84 18

82 16

80 14

78 12
16:34 16:36 16:38 16:40 16:42 16:44 16:46 16:48 16:50 16:52 16:54
Time
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

T3, Evaporator temperature T4, Plate 1 temperature

T6, Plate 3 temperature T8, Plate 5 temperature
T10, Plate 7 temperature T12, Top temperature
dp1, Column pressure loss

Fig. 6.7 V7, Temperature and pressure profile at start of rectification

100 14

Differential pressure in mbar

12

90 10
Temperature in °C

80 6

70 2

60 -2
17:40 17:42 17:44 17:46 17:48 17:50 17:52 17:54 17:56 17:58 18:00
Time

T3, Evaporator temperature T4, Plate 1 temperature

T6, Plate 3 temperature T8, Plate 5 temperature
T10, Plate 7 temperature T12, Top temperature
dp1, Column pressure loss

Fig. 6.8 V7, Temperature and pressure profile at end of rectification

6 Experiments - with ethanol/water mixture 107

CE 600 CONTINUOUS RECTIFICATION

6.4.5.2 Evaluation of self-recorded measured values

The following Tab. 6.18, Page 109 presents the

measured masses, densities and temperatures,
together with the total masses and concentrations
calculated from them.
The individual mixture masses at the start and
end of the experiment have been added together
(details follow in this chapter under item 5.).

Re experiment aim 3 - To determine the

ethanol concentrations:
For all the samples, the ethanol mass fraction E
wE was determined from the density and
temperature by means of linear interpolation (for
description of procedure see Chapter 6.3.5.2,
Page 84).
The material values originate from Tab. 6.1,
Page 59 and Tab. 6.2, Page 60.

108 6 Experiments - with ethanol/water mixture

6 Experiments - with ethanol/water mixture All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

CE 600
Measurement Evaluation
Clock Product/measurement Mass Tempera- Density Level Comments Mass Mass fraction
no. net ture in Evap net Ethanol, wE
g °C kg/L L g %m
----- Start, mixture, Evap ----- 24,0 0,9635 9,0 8744,5 22,3

CONTINUOUS RECTIFICATION
16:52 B.pr., 1. 477,5 23,1 0,970 9,1 ----- 18,0
16:58 T.pr., 1. 402,5 23,5 0,825 9,1 ----- 86,1
17:02 B.pr., 2. 448,5 23,9 0,970 9,2 ----- 17,7
17:10 B.pr., 3. 430,0 24,3 0,970 9,1 ----- 17,6
17:16 T.pr., 2. 424,5 23,7 0,830 9,1 ----- 84,1
17:19 B.pr., 4. 475,0 25,0 0,970 9,1 ----- 17,4
17:29 B.pr., 5. 455,5 25,3 0,975 9,2 ----- 13,7
17:44 B.pr., 6. (+7.) 923,5 26,6 0,975 9,2 Total drainage ----- 13,4
17:44 T.pr., 3. 636,5 23,5 0,835 ----- Total drainage ----- 82,2
----- End, T.pr., mixture 1620,0 23,0 0,833 ----- ----- 83,1
----- End, B.pr., mixture 3204,5 24,2 0,972 ----- ----- 16,2
----- End, B.pr., from Evap ----- 21,8 0,977 ----- 8580,0 13,1

Measurement
Start, Fill feed tank, 1939,5 1939,5 1935,0 1929,5 1945,5
Individual masses in g (-24,5g residue 1, when 10L reached)
Start, Fill feed tank, 1941,0 1937,0 1944,5 1925,0 979,5 (24,5g see above;
Individual masses in g -7g residue 2, when 10L reached)
End, B.pr., from Evap, 1930,0 1866,5 1855,0 1660,0 1268,5
Individual masses in g

Key: T.pr.: Top product; B.pr.: Bottom product; Evap: Evaporator

109

Tab. 6.18 V7, Self-recorded measured values, with evaluation

CE 600 CONTINUOUS RECTIFICATION

Re experiment aim 4. To present the change over time in the ethanol

concentration in the top and bottom product
Fig. 6.9 shows the progression over time of the ethanol concentration:

Top product
wE in %m

Time

20,0
Bottom product
18,0
wE in %m

16,0

14,0

12,0

10,0
16:50 17:00 17:10 17:20 17:30 17:40
Time

Clock Ethanol mass fraction

Top product Bottom product

wE in %m wE in %m

16:52 ----- 18,0

16:58 86,1 -----
17:02 ----- 17,7
17:10 ----- 17,6
17:16 84,1 -----
17:19 ----- 17,4
17:29 ----- 13,7
17:44 82,2 13,4

Fig. 6.9 V7, Progression over time on the ethanol concentration in the top and bottom products

110 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

Re experiment aim 5. To check the concen-

trations by means of mass balances
It is useful to check the measured values with the
aid of mass balances. Any conflicts arising from
the mass balances indicate errors in evaluation or
inaccurate measurement data.
At this point the mixture and ethanol masses at
the start and end of the experiment are compared:
The following examples illustrate the graphical
symbols used below:
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m: Mixture mass, general

m E: Ethanol mass, general
wE : Ethanol mass fraction, general
m(Start): Mixture mass, at start of experiment
mE(End): Ethanol mass, at end of experiment
m(Evap): Mixture mass in evaporator
mE (Feed): Ethanol mass in feed tanks
wE (T.pr.): Ethanol mass fraction in top product
m(B.pr.): Mixture mass, bottom product

Mixtures mass balance:

To be checked:
m  Start  = m  End  (6.6)
where
m Start  = m Start, Evap  + m Start, Feed  (6.7)
and
m End  = m T.pr. + m B.pr. + m B.pr.,Evap  + m End, Feed  (6.8)

6 Experiments - with ethanol/water mixture 111

CE 600 CONTINUOUS RECTIFICATION

The following table illustrates how the values for

m(Start,Feed), m(Start,Evap) and m(B.pr.,Evap)
are produced by adding together the individual
mixture masses from Tab. 6.18, Page 109:

Mass, net, in g

m(Start,Feed) m(Start,Evap) m(B.pr.,Evap)

1. Measuring 1939,5 1941,0 1930,0

2. Measuring 1939,5 1937,0 1866,5
3. Measuring 1935,0 1944,5 1855,0
4. Measuring 1929,5 1925,0 1660,0
5. Measuring 1945,5 979,5 1268,5
Residue 1 -24,5 24,5 ------
Residue 2 ------ -7,0 ------
Total 9664,5 8744,5 8580,0

Tab. 6.19 V7, Addition of mixture masses

The “residue 1”, 24,5g, is included. This “residue 1”

results from the fact that when transferring from
the last measuring cup into the feed tanks (B1, B2),
the total volume of 10,0L is reached before the
measuring cup is completely empty. The residue
is thus the mass of the mixture remaining in the
measuring cup. After pumping the 9,0L into the
evaporator, this “residue 1” is transferred into the
feed tanks.

In the course of the experiment, 5,0L of the 10,0L

feed is pumped into the column. The other 5,0L
remain in the second feed tank. Consequently:
m(End,Feed) = m(Start,Feed) / 2 =
9664,5 / 2 = 4832,3 g

112 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

The following table consolidates the mixture

masses calculated above and adds them together
according to the formulae (6.7) and (6.8):

Mass, net, in g

m(Start) m(End)

m(Start,Evap) 8744,5 ------

m(Start,Feed) 9664,5 ------
m(T.pr.) ------ 1620,0
m(B.pr.) ------ 3204,5
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

m(B.pr.,Evap) ------ 8580,0

m(End,Feed) ------ 4832,5
Total 18409,0 18237,0

Tab. 6.20 V7, Mixture balancing

The comparison of the two values shows that at

the end of the experiment there is still 99,1% of
the original mixture masses present.

Ethanol mass balance:

In line with the mass balances for the mixtures,
(6.6) to(6.8), the resultant ethanol mass balances
are:
To be checked:
m E Start  = m E End  (6.9)
where
m E Start  = m E Start, Evap + m E Start, Feed  (6.10)
and
m E End  = m E T.pr. + m E B.pr. + m E B.pr.,Evap  + m E End, Feed  (6.11)

6 Experiments - with ethanol/water mixture 113

CE 600 CONTINUOUS RECTIFICATION

The ethanol mass fraction wE is defined as the

ratio of the ethanol mass mE to the mixture mass
m. This enables the individual ethanol masses to
be expressed as the product of the mixture mass
and the mass fraction, e.g. for:

m E T.pr. = m T.pr.  w E T.pr. (6.12)

The following table summarises how the values

from Tab. 6.18, Page 109 and Tab. 6.20,
Page 113 are evaluated using the equations
(6.10) to (6.12):

Designation …
.. Start End

m(...) wE(...) mE(...) m(...) wE(...) mE(...)

g %m g g %m g

Start,Evap 8744,5 22,3 1950,0 ------ ------ ------

Start,Feed 9664,5 22,3 2155,0 ------ ------ ------
T.pr. ------ ------ ------ 1620,0 83,1 1346,0
B.pr. ------ ------ ------ 3204,5 16,2 519,0
B.pr.,Evap ------ ------ ------ 8580,0 13,1 1124,0
End,Feed ------ ------ ------ 4832,5 22,3 1077,5
Total 18409,0 ------ 4105,0 18237,0 ------ 4066,5

Tab. 6.21 V7, Ethanol balancing

The comparison of the two values shows that at

the end of the experiment there is still 99,1% of
the original ethanol mass present.

114 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

6.4.6 Comments, assessment

The comments and assessment are based on the

pre-defined experiment aims:
Re 1. To concentrate the ethanol and
Re 3. To determine the ethanol concentration
in the initial mixture, top product and bottom
products
The initial mixture was separated into the top
product, with increased ethanol content, and the
two bottom products, with reduced ethanol
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

content.
The ethanol mass fraction in the top product is
greater than in the initial mixture by a factor of
3,73.
Comparison with the factor 3,51 from the batch
experiment V3 (see also Chapter 6.3.6, Page 91)
shows that in experiment V7 in continuous mode
a better concentration was achieved.

Re 2. To record the measured value using the

data acquisition program (temperature and
pressure profiles)
Fig. 6.6, Page 106 shows the profiles at column
start-up. The curves run similarly to those in batch
experiment V3.
The temperature rise in the individual plates from
bottom to top is clearly traceable. Some of the
temperature curves have a kink in them during
heat-up. A kink of this kind can be interpreted as
forming the equilibrium between vapour and
liquid, on occurrence of the first condensate.
While the equilibriums are being created, the
pressure loss in the column increases steadily.

6 Experiments - with ethanol/water mixture 115

CE 600 CONTINUOUS RECTIFICATION

The time between reaching the boiling tempera-

ture in the column head and the initial distillate in
the phase separation tank (B3) is about 5 minutes
under the selected conditions. When the first
distillate occurs, the equilibriums have formed
and the differential pressure in the column now
changes only to a minor extent.

Fig. 6.7, Page 107 shows the differential pressure

and temperatures at the start of rectification.
Around 16:35 hours the operating conditions are
adjusted (start pump at 30%, bottom feed, feed
heating, start bottom product from evaporator to
bottom product tank, reflux ratio R from 100
to 25%).
The many simultaneous changes take effect at
different rates, and influence each other.
As a reaction, it is seen that the temperatures in
the column initially fall - most rapidly in the upper
section. At the same time the differential pressure
rises. After about 10 minutes the complete
system has adjusted to the new equilibriums, and
the temperatures slowly rise. The rise is in line
with the rising boiling point at reduced ethanol
concentrations.

Fig. 6.8, Page 107 shows the profiles at the end of

rectification. Around 17:44 hours operations are
aborted by: Stop pump, stop bottom product from
evaporator to bottom product tank, switch off
heater.

116 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

The reaction of the temperatures in the column

and column head is rapid. An initial rapid drop in
temperatures by 2 to 5°C is detected. At the same
time the differential pressure falls, so the column
loses condensate.
Compared to the corresponding profile in the
batch experiment (see Fig. 6.3, Page 83), the
cooling process is slower here. However, the
differential pressure in the column is reduced
roughly twice as fast.
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

Re 4. To present the change over time in the

ethanol concentration in the top and bottom
product
Fig. 6.9, Page 110 shows the decrease in the
ethanol mass fraction wE in the top product. It is
seen that wE decreases by 3,9 percentage points
in the course of the experiment. This decrease
corresponds to the result from batch experiment
V3 (see Chapter 6.3.6, Page 91).

At first glance that appears a substantial

decrease.
The reason for this decrease is that there is a
greater proportion of ethanol in the newly created
top product than in the bottom product of the
evaporator. As a result, the bottom product in the
evaporator loses ethanol in the course of the
experiment. The decreasing concentration in the
evaporator then results in a reduced concen-
tration in the top product.

6 Experiments - with ethanol/water mixture 117

CE 600 CONTINUOUS RECTIFICATION

Fig. 6.9 also shows the decrease in the ethanol

mass fraction wE in the bottom product. As
expected, wE steadily decreases in the course of
the experiment.
In the second half of the experiment - in the time
band from 17:19 to 17:29 hours - a major
decrease in wE is seen. This particular curve trend
should not be expected by way of reproducibility
in any subsequent repetitions of the experiment.
Alongside the known inaccuracies of the density
measurement, there is another reason for
variations here:
The measured bottom product flows permanently
out of the evaporator. This discharging bottom
product is always a mixture of existing evaporator
content and newly arriving, differently concen-
trated condensate from the column. The inter-
mingling of the evaporator content with the
condensate varies in intensity.

Re 5. To check the concentrations by means

of mass balances
Both regard to the mixtures and to ethanol,
comparison of the two values shows that at the
end of the experiment there is still 99,1% of the
original mass present (see above).
In view of the losses during sampling and transfer,
and due to evaporation, these values are of a
realistic magnitude.
This confirms the measured values and the
evaluation of the experiment.

118 6 Experiments - with ethanol/water mixture

 CE 600 CONTINUOUS RECTIFICATION

7 Appendix

7.1 Technical data

Overall unit: lxwxh: 1300 x 750 x 2300 mm

Weight: approx. 210 kg
Electrical supply: 3 x 400V / 50 Hz
Optional alternatives, see rating plate
Cooling water flow: min. 400 L/h
In-house water supply (p ≥ 1,5 bar g, T ≤ 25°C)
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

Sieve plate column: Øxh 50 x 765 mm

Material: Stainless steel
Number of plates: 8

Packed column: Øxh 50 x 765 mm

Material Stainless steel
Packing Raschig rings
Material Soda glass
Øxh 4 x 4 mm

Evaporator: Heating power 4,0 kW

Capacity max. 10 L
Minimum fill 3 L
Safety cut-out at approx. 110 °C

Feed pump: Type: Hose pump

Capacity approx. 0...420 ml/min
Internal electrical supply 24 VDC

Temperature sensors T1 ... T16 : Pt100 0...150 °C

Differential pressure sensor: piezoresistive 0 ... 0,25 bar

Experiment mixture: ethanol/water ~ 25 : 75 %m

7 Appendix 119
CE 600 CONTINUOUS RECTIFICATION

Volumes: Feed tanks each ~ 5 L

Bottom product tanks each ~ 5 L
Top product tank ~ 1,5 L
Phase separation tank ~ 0,5 L
Solvent tank ~ 0,9 L

Data acquisition: USB communication

Program environment: LAB-VIEW Runtime
System requirements:
• PC with Pentium IV processor, 1 GHz
• Min. 1024 MB RAM
• Min. 1 GB available memory on hard disk
• 1 x USB port
• Graphics card resolution min.
1024 x 768 pixels, True Color
• Windows Vista / 7 / 8

7.2 Worksheets

The following pages set out a series of

worksheets. The worksheets can be used to enter
self-recorded measurements by hand during
experiments.
The “Batch” worksheet in Tab. 7.1 can be used for
experiments from the “Batch” series.
The “Continuous” worksheet in Tab. 7.2 is
intended for experiments in the “Continuous”
series.

120 7 Appendix
7 Appendix All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

CE 600
Experiment no.: Date: Participants:
Measurement Evaluation
Clock Product/measurement Mass Tempera- Density Level Comments Mass Mass fraction
no. net ture in Evap net Ethanol, wE

CONTINUOUS RECTIFICATION
g °C kg/L L g %m
Start, mixture, Evap -----
T.pr., 1. -----
T.pr., 2. -----
T.pr., 3. -----
----- End, T.pr., mixture ----- -----
----- End, B.pr., Evap ----- -----

Measurement
Start, Fill feed tank,
Individual masses in g
End, B.pr., from Evap,
Individual masses in g

Key: T.pr.: Top product; B.pr.: Bottom product; Evap: Evaporator

Tab. 7.1 “Batch” worksheet for self-recorded measurements in the “Batch” experiment series
121
122

CE 600
Experiment no.: Date: Participants:
Measurement Evaluation
Clock Product/measurement Mass Tempera- Density Level Comments Mass Mass fraction
no. net ture in Evap net Ethanol, wE
g °C kg/L L g %m

CONTINUOUS RECTIFICATION
Start, mixture, Evap -----
-----
-----
-----
-----
-----
-----
-----
-----
-----
----- End, T.pr., mixture ----- -----
----- End, B.pr., mixture ----- -----
----- End, B.pr., from Evap ----- -----

Measurement
Start, Fill feed tank,
Individual masses in g
Start, Fill feed tank,
Individual masses in g
End, B.pr., from Evap,
Individual masses in g
7 Appendix

Key: T.pr.: Top product; B.pr.: Bottom product; Evap: Evaporator

Tab. 7.2 “Continuous” worksheet for self-recorded measurements in the “Continuous” experiment series
 CE 600 CONTINUOUS RECTIFICATION

7.3 Abbreviations and symbols

7.3.1 Abbreviations used

B.pr. Bottom product

B.pr.tank Bottom product tank
Evap Evaporator
HTU Height of Transfer Unit
FSL Flow Switch Low
LSL Level Switch Low
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

NTU Number of Transfer Units

Pd Packed column
SP Sieve plate column
T.pr. Top product
T.pr.tank: Top product tank
TSH Temperature Switch High

7 Appendix 123
CE 600 CONTINUOUS RECTIFICATION

7.3.2 Symbols used

m Mass, mixture mass g, kg

mE Ethanol mass g, kg
n Speed min-1
p pressure bar, mbar
Pel Electrical Power Output kW
R Reflux ratio %
t Time min, s
T Temperature °C
V Volume L
·
V Volumetric flow L/h
w Mass fraction %m
wE Ethanol mass fraction %m
x1 Molar fraction in the liquid mixture %
y1 Molar fraction in the steam %

ρ Density kg/L, kg/m³

124 7 Appendix
 CE 600 CONTINUOUS RECTIFICATION

8 Index

A
Areometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41, 94
Automatic mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22, 63
Azeotropic mixture . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
Azeotropic rectification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34

B
Batch experiment series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
Batch rectification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32, 43, 69
Batch worksheet . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 121
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

Bottom . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
Bottom heat exchanger . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Bottom product . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15, 31, 53

C
CE 600 process diagram . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12, 22
Column . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
Column differential pressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14, 65
Condenser . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14, 26
Continuous experiment series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72
Continuous rectification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32, 48, 72
Continuous worksheet . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 122
Curve of equilibrium . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25

D
Data acquisition . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77, 101, 123
Density measurement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61, 94
Density of ethanol/water mixture . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
Distillate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
Distillation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
Distillation, reverse flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

E
Evaporator . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14, 53, 119
Experiment series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68

8 Index 125
CE 600 CONTINUOUS RECTIFICATION

F
Feed . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Feed pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14, 119
Feed tank . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14, 35
Flow switch . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
Fractional distillation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27

H
HTU . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30

I
Interpolation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84

L
Level . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
Level switch . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19

M
Mass balance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 88, 94, 111
Mass fraction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
Measured data record . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77, 101
Measured value file . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77, 101
Method of operation of the unit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
Multi-stage distillation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28, 29

N
NTU . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30

P
Packed bed . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
Packed column . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14, 29, 119
Phase separation tank . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14, 34, 120

R
Rectification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1, 28
Reflux . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
Reflux ratio R . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
Residue . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
Reverse flow distillation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

126 8 Index
 CE 600 CONTINUOUS RECTIFICATION

S
Sieve plate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29, 39
Sieve plate column . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14, 38, 119
Spontaneous experiments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63

T
Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119
Temperature switch . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16, 19
Theoretical transfer units . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30

V
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 04/2018

Vacuum distillation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
Volume contraction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58

W
Warning lamp . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
Water jet pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15, 47
Worksheets . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 120

8 Index 127
CE 600 CONTINUOUS RECTIFICATION

128 8 Index