Liquid-Liquid Extraction PDF

Experiment Instructions
CE 620 Liquid-Liquid Extraction

CE 620 LIQUID-LIQUID EXTRACTION
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 12/2013
Experiment Instructions
Dipl.-Ing. (FH) Klaus Schröder
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 1.2 Subject to technical alterations
i
ii
Table of Contents
1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
2 Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
2.1 Intended use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
2.2 Structure of safety instructions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
2.3 Safety instructions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
3 Description of the device . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

3.1 Objective of the extraction, designation of the substances involved . 15

3.2 Process diagram . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
3.3 Device design . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
3.4 Device function and main components . . . . . . . . . . . . . . . . . . . . . . . 19
3.4.1 Operating mode and process description . . . . . . . . . . . . . . . 20
3.4.1.1 Batch mode. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
3.4.1.2 Continuous mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
3.4.2 Extraction column . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
3.4.3 Setting the phase boundary . . . . . . . . . . . . . . . . . . . . . . . . . 30
3.4.4 Distillation unit. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
3.5 Control cabinet with controller . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
3.6 Special features of individual components . . . . . . . . . . . . . . . . . . . . 41
3.7 Accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
3.8 Inserting packing into the extraction column . . . . . . . . . . . . . . . . . . . 44
3.9 Positioning the trainer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48
3.10 Commissioning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
3.11 Decommissioning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
3.12 Care and maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
3.12.1 Vacuum grease for glass valves. . . . . . . . . . . . . . . . . . . . . . 56
3.12.2 Descaling the round-bottomed flask . . . . . . . . . . . . . . . . . . . 56
iii
4 Basic principles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
4.1 Liquid-liquid extraction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
4.2 Types of liquid-liquid extraction systems . . . . . . . . . . . . . . . . . . . . . . 63
4.3 Refining crude vegetable oil, removal of lecithin . . . . . . . . . . . . . . . . 65
4.4 Model material system for CE 620 . . . . . . . . . . . . . . . . . . . . . . . . . . 67
4.5 Distillation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
4.6 Thermophysical properties and determining concentration. . . . . . . . 70
5 Experiments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75
5.1 Beaker experiments. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77
5.2 Conducting the density measurement . . . . . . . . . . . . . . . . . . . . . . . . 78
5.3 Preliminary experiment for flow measurement . . . . . . . . . . . . . . . . . 83
5.4 Experiments with the device . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
5.4.1 Stirring feed and solvent . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86
5.4.2 Standard experiment, basic conditions,
series of experiments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 87
5.4.3 Objectives of the experiment . . . . . . . . . . . . . . . . . . . . . . . . 88
5.4.4 Experiment setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 88
5.4.5 Conducting the experiment and cleaning . . . . . . . . . . . . . . . 89
5.4.5.1 Conducting the liquid-liquid extraction experiment, batch . . 90
5.4.5.2 Conducting the distillation experiment . . . . . . . . . . . . . . . . . 96
5.4.5.3 Normal cleaning after the end of the experiment . . . . . . . . 100
5.4.5.4 Additional cleaning with methylated spirits . . . . . . . . . . . . . 102
5.4.6 Measurements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 106
5.4.7 Evaluation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 108
5.4.8 Comment and evaluation . . . . . . . . . . . . . . . . . . . . . . . . . . 110
iv
6 Appendix . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 113
6.1 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 113
6.2 Scope of delivery, accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . 116
6.3 List of abbreviations. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117
6.4 List of identification letters used in the process diagram . . . . . . . . . 117
6.5 Worksheet . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 118
v
vi
1 Introduction
Technical classification
CE 620 enables the liquid-liquid extraction of a
transition component from a liquid mixture in a
solvent.
We recommend the " Extraction of ethanol from
refined plant oil with water" model material
system for experiments with CE 620.
This model material system copies the "refined
vegetable oil and water" solvent system, in a sim-

ilar way to the real application "removal of lecithin
from crude vegetable oil."
Layout and function of the device

The liquid mixture to be extracted (feed = carrier
liquid with transition component) is pumped into
the bottom of the transparent extraction column.
There, it moves in counterflow to the solvent,
which is pumped into the top of the extraction col-
umn. In doing so, the transition component trans-
fers from the feed into the solvent. Carrier liquid
and solvent are insoluble in one another and form
a phase boundary in the extraction column.
Feed and solvent each leave the extraction
column at the side opposite the inlet.
The trainer can be operated in both discontinuous
(batch) and continuous modes.
The integrated distillation unit is used for enrich-
ing the transition component in the extract.
The distillation unit consists of a heated round-
bottomed flask with packed columns and Liebig
condenser.
1 Introduction 1
The vacuum pump installed allows distillation at

low pressure.
The learning objectives are:

• Transition of a component from a two-compo-
nent liquid mixture (feed) into a solvent by
extraction.
• Scale-up from the beaker to the pilot plant
scale.
• Enrichment of the transition component in the
extract by distillation.
• Evaluation of the separation processes via
concentration measurements and mass bal-
ances.
• Influence of experimental variations on the
separation processes.
Structure of the instructions

In addition to these experiment instructions, a
separate installation manual is included in the
delivery. In this manual you will find details on how
to install the distillation unit.
Didactic notes for teachers

CE 620 can be used to carry out practical liquid-
liquid extraction at the scale of a pilot plant.
The trainer is designed such that the processes
are largely visible and can be observed.
The field of application is education in the subject
of process engineering.
A suitable laboratory environment with water sup-
ply and water drainage is required for the opera-
2 1 Introduction
tion of the trainer. Operating the system requires

good prior experimental experience.
These experiment instructions include a descrip-
tion of the trainer and its functional principle.
A standard experiment is presented for the rec-
ommended "extraction of ethanol from refined
vegetable oil with water" model material system.
Areas where the trainer can be employed include:

• Practical experiments
Small groups of two or three students can carry
out experiments for themselves. The time
required to conduct an experiment can be esti-
mated at about five hours. Additional time is
required to clean the trainer on the following
day.
• Project work
The trainer is particularly suited to carrying out
project work.
A series of experiments can be used to work
out how changing the experimental conditions
affects the results.
The experiments can be performed by a single
experienced student after thorough instruction.
1 Introduction 3
These materials are intended to be used to help

you prepare your lessons. You can compile parts
of the materials as information for students for use
in the classroom.
We also provide you with these experiment
instructions in PDF format on a CD to support
your lessons. We grant you unlimited reproduc-
tion rights for use within the context of your teach-
ing duties.
4 1 Introduction
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.
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
Symbol Explanation
Electrical voltage
Explosive materials
Flammable substances
Hazard area (general)
Hot surface
Rotating parts
Risk of slipping
Notice
Wear eye protection
Wear gloves
Wear safety shoes
No smoking
6 2 Safety
2.3 Safety instructions
These safety instructions relate to the model

material system that is recommended for operat-
ing the CE 620 trainer:
• Refined rapeseed oil as carrier liquid,
• Ethanol as transition component,
• Water as solvent,
as well as methylated spirits, detergent and dilute
acetic acid as cleaning agents.
NOTICE
If starting materials other than those specified
are used, the customer must carry out his own
safety analysis. This applies to both the different
starting material and to any possibly resulting
intermediate and final products.
NOTICE
If starting materials other than those specified are
used, the customer must check the material com-
patibility beforehand.
2 Safety 7
WARNING
Electrical connections are exposed when the
control cabinet is open.
Risk of electrical shock.
• Disconnect the plug from the power supply
before opening the switch cabinet.
• All work must be performed by trained electri-
cians only.
• Protect the switch cabinet from humidity.
WARNING
Irritant chemicals.
Contact with ethanol, methylated spirits and
detergent irritates the eyes and skin. Repeated
contact may cause dermatitis due to the degreas-
ing effect.
Contact with acetic acid irritates the eyes and
skin.
• Wear protective gloves and protective goggles.
• In case of contact with the skin, wash with
plenty of water.
• In case of contact with the eyes, hold eyelid
open and rinse immediately with plenty of
water. Seek medical attention.
WARNING
Irritant chemical vapours.
Vapours from ethanol and methylated spirits can
cause drowsiness and dizziness.
• Do not inhale directly.
• Ensure adequate ventilation.
8 2 Safety
WARNING
Flammable solvents.
The vapours from ethanol and methylated spirits
can form explosive mixtures with air.
• Keep away from sources of ignition.
• Do not smoke.
• Do not empty ethanol and methylated spirits
into drains undiluted.
• Observe national and local regulations.
WARNING
The cylinder of the extraction column is made
of glass.
Injuries from glass splinters are possible.
• Wear safety goggles.
• Avoid water hammers. When filling the extrac-
tion column, open valve V30 for ventilation.
WARNING
Parts of the distillation unit are made of glass.
2 Safety 9
WARNING
Localised overheating is possible when heat-
ing the round-bottomed flask without suffi-
cient fill level.
• Read through the separate manufacturer's
documentation before using the heating mantle
for the first time.
• The heating mantle may not be operated unat-
tended.
• Never heat the round-bottomed flask without
liquid.
• Depending on the number of heating zones
switched on, ensure the level in the round-bot-
tomed flask remains continuously sufficient.
WARNING
Heating mantle is sensitive to moisture.
Risk of electrical shock.
• Read through the separate manufacturer's
documentation before using for the first time.
• Prevent moisture from penetrating the heating
mantle.
tended.
• Turn off moist heating mantle immediately.
• Only re-start moist heating mantle after it has
been fully dried.
10 2 Safety
WARNING
Hot surfaces of switched on heating mantle.
Burns are possible.
tended.
• Do not touch the heating mantle when it is
switched on.
WARNING
Hot liquids at the outlet of the round-bottomed
flask.
Scalds are possible.
• Do not touch during operation.
• Wear safety goggles and protective gloves
when draining.
WARNING
Rotating shaft when agitator is operated with
a hand drill.
Risk of hand injuries.
• Do not touch the shaft.
WARNING
Rapeseed oil spillages.
Possible injury from falls.
• Clean up rapeseed oil spillages immediately.
2 Safety 11
NOTICE
Upon completion of individual experiments:
• Empty the device.
• Thoroughly rinse and clean all containers and
pipe lines.
NOTICE
Operating the feed pump and the solvent pump
without liquid will cause damage to the respective
pump.
• Ensure supply with liquid when operating these
pumps.
NOTICE
Localised overheating is possible when heating
the round-bottomed flask without sufficient fill
level.
The heating mantle can be seriously damaged as
a result of localised overheating.
• Never heat the round-bottomed flask without
liquid.
• Depending on the number of heating zones
switched on, ensure the level in the round-bot-
tomed flask remains continuously sufficient.
NOTICE
Rapeseed oil residues can become rancid and
develop smells.
• Do not empty rapeseed oil into drains.
12 2 Safety
NOTICE
Frost damage is possible when the system is
stored.
• Only store the system in a frost-free location.
• Drain the tank if there is a risk of frost.
• Drain the water if the device is not going to be
used for long periods.
NOTICE
Frequently changing the packed bed fill height
should be avoided so as to prevent glass splinters
as far as possible.
Only deepen the packed bed if absolutely neces-
sary.
Glass splinters in the trainer may cause serious
damage to the components of the trainer.
2 Safety 13
14 2 Safety
3 Description of the device
3.1 Objective of the extraction, designation of the substances involved
The main objective of liquid-liquid extraction is

to transfer a transition component from a liquid
mixture into a liquid solvent.
The substances involved in liquid-liquid extrac-

tion have various common names. This can eas-
ily give rise to misunderstandings, especially
when comparing different sources.

Therefore, we shall explain here which designa-
tions are used in these experiment instructions.
More detailed information will follow in Chapter 4,
Page 59ff.
The simplest form of liquid-liquid extraction

involves three liquids:
• Transition component
• Carrier liquid
• Solvent
The liquid mixture of the transition component and

carrier liquid is called the feed. In the feed, the
transition component is dissolved in the carrier
liquid.
Carrier liquid and solvent together form the sol-
vent system. The transition component must be
soluble in both the carrier liquid and the solvent.
The carrier liquid and solvent should together
form a phase boundary in order to allow the sep-
aration of the two phases. Therefore, carrier liquid
3 Description of the device 15

and solvent should be as mutually insoluble in

each other as possible.
The two phases, which we get at the end of
liquid-liquid extraction are called the extract
and the raffinate.
The extract is essentially a solution of the transition
component in the original solvent.
The raffinate is essentially the original feed, less
the extracted proportion of the transition compo-
nent.
3.2 Process diagram
Fig. 3.1, Page 17 shows the process diagram for

the CE 620 liquid-liquid extraction unit.
The identification letters used are explained in
Chapter 6.4, Page 117f.
All main components and measuring points are
shown and labelled in the process diagram. The
flow through the trainer is illustrated.
More detailed information on the design of the
device and its functions follows in Chapter 3.3
and Chapter 3.4.
These chapters also use extracts from the pro-
cess diagram to illustrate details.
16 3 Description of the device

Media
Fig. 3.1
Feed CE 620
Solvent
Extract
Raffinate
Residue
Distillate
Cold water
3 Description of the device

Main components
B1 Solvent tank
B2 Distillate tank
B3 Extract tank
B4 Raffinate tank
B5 Feed tank
D1 Round-bottomed flask
H1 Heating mantle
K1 Extraction column
K2 Distillation column
P1 Solvent pump
LIQUID-LIQUID EXTRACTION
P2 Feed pump
P3 Vacuum pump
W1 Distillation bridge
F1 Strainer
V1-V4 Control valve
V5, V6 Relief valve
Process diagram of the CE 620 liquid-liquid extraction system

V7, V8 3-way ball valve
V10-V30 Valve
Measurement and control technol

FI01 Solvent flow
FI02 Feed flow
LI01-LI05 Fill level
PI01, PI02 Pressure
TI01 Residue temperature
TI02 Vapour temperature
TIC1 Temperature controller
17
3.3 Device design
Front view
6 5 4 3
2
8
10
1
Rear view
11 12 13 14 15 16 17
1 Distillate tank (B2) 11 Heating mantle (H1)

2 Control cabinet 12 Regulating valve for solvent return (V3)
3 Regulating valve for solvent inflow (V1) 13 Solvent tank (B1)
4 Regulating valve for feed inflow (V2) 14 Feed tank (B5)
5 Extract tank (B3) 15 Raffinate tank (B4)
6 Regulating valve for feed return (V4) 16 Feed pump (P2)
7 Distillation bridge (W1) 17 Solvent pump (P1)
8 Distillation column (K2)
9 Extraction column (K1)
10 Round-bottomed flask (D1)
Fig. 3.2 Overview of the CE 620 liquid-liquid extraction system

3.4 Device function and main components
This chapter is divided into several subsections.

Firstly, we will look at the trainer's different oper-
ating modes (continuous mode and batch mode).
In doing so, we will describe the process.
Then, we will explain the structure of the extrac-
tion column K1 (9).
Then we will explain how the phase boundary is
set up in the extraction column.
Finally, we will describe the distillation unit.
The numbers in brackets in the following text

refer:
• mainly to the position numbers in the overview
in Fig. 3.2, Page 18, as well as
• occasionally to the labels in the process dia-
gram in Fig. 3.1, Page 17. This applies to those
components that are only illustrated in the pro-
cess diagram (some of the valves and instru-
mentation).
Wherever the function of the components is
meant to be emphasised, both are added: first the
label according to the process diagram, then the
position number in brackets.

3.4.1 Operating mode and process description
The CE 620 trainer can be operated either con-

tinuously or in batch mode (i.e. discontinu-
ously).
The desired operating mode is selected using the
3-way ball valves V7 and V8. The photo opposite
shows V7 and V8 in the front view.
The following subsections describe the two oper-

ating modes using variations of the process dia-
gram from Fig. 3.1, Page 17.
In these variations of the process diagram, thicker
line widths denote the pipelines which are flowed
through. In addition, the flow through the tank
involved and through the extraction column is col-
our coded.
Fig. 3.3 3-way ball valves V7 and V8
3.4.1.1 Batch mode
Fig. 3.4, Page 21 shows the variation of the pro-

cess diagram for batch mode, without distillation.

Media
Feed
Solvent
Fig. 3.4 CE 620 process diagram, batch mode variant, without distillation
On the names of the materials and material flows

in batch mode:
The naming of materials and material flows for
batch mode requires some explanation.

Key facts:
• At the beginning of extraction, solvent is
located in the solvent tank.
Feed
• At the beginning of extraction, feed is located in
return the feed tank.
• After extraction, extract is located in the solvent
tank.
• After extraction, raffinate is located in the feed
tank.
But how long does extraction have to last to get
extract from solvent and raffinate from feed?
In these experiment instructions, the name corre-
sponds to the colour coding in Fig. 3.4, Page 21,
for batch operation during extraction. The point
where solvent is renamed as extract and feed as
raffinate is known as extraction end.
Process description for batch mode, without distil-

lation:
The mass transfer of liquid-liquid extraction takes
place in the extraction column K1(9). This is
where feed and solvent meet. When this hap-
Solvent
return pens, a part of the transition component is
Solvent inflow
Feed inflow
extracted from the feed into the solvent.

Fig. 3.5 shows the extraction column K1, as an
excerpt from the process diagram in Fig. 3.4,
Page 21.
The feed is continuously pumped from the feed
tank B5(14) by the feed pump P2(16) into the
bottom of the extraction column (feed inflow).
The feed moves upwards in the extraction col-
Fig. 3.5 CE 620 process diagram, umn.
extraction column section

From the top of the extraction column the feed

returns to the feed tank (feed return).
The solvent is continuously pumped from the sol-
vent tank B1(13) by the solvent pump P1(17)
into the top of the extraction column (solvent
inflow). The solvent moves downwards in coun-
terflow to the feed. From the bottom of the extrac-
tion column, the solvent returns to the solvent tank
(solvent return).
The driving force for the counterflow is the den-
sity difference between solvent and feed.

Therefore, the material and/or the mixture with the
lower density must be pumped into the bottom of
the extraction column.
This condition is satisfied for the recommended
Quick couplings
rapeseed oil-ethanol-water model material
system. The density of the feed (solution of etha-
nol in rapeseed oil) is less than the density of the
solvent (water).
If this condition is not satisfied for any possible
alternative material system that you may have
chosen, then the trainer can be adapted accord-
ingly.
Quick couplings
Colour coded quick couplings are installed for

this adaptation (see Fig. 3.6). These can be
uncoupled and both the inflows (feed inflow and
solvent inflow) and the returns can be swapped
with each other.
The colour coding helps when you have to restore
Fig. 3.6 Quick couplings
the normal state again (coupling and plug nipple
of the same colour belong together).

The tanks B1-B5 are available for feed, solvent,

raffinate, extract and distillate. These tanks
have a level indicator (LI01-LI05) in addition to
the drainage and the necessary inlet and outlet
nozzles. The tanks B1 and B3-B5 have a remov-
able lid.
The distillate tank B2(1) is designed with a
screwed lid and seal (see Fig. 3.7). This seal
allows distillation at reduced pressure.
Solvent pump P1(17) and feed pump P2(16)
Fig. 3.7 Distillate tank B2(1),
top view are designed as positive displacement pumps.
Recirculation lines are provided in order to allow
adjustment of the desired flow rates and to protect
the pumps. The pumps are also protected by
internal relief valves.
The following figure uses the solvent system to
illustrate the principle (excerpt from the process
diagram in Fig. 3.4, Page 21).
Solvent inflow
Solvent return
Recirculation
Fig. 3.8 Excerpt from the process diagram, solvent system

When unthrottled and with free run-off, the solvent

pump delivers with maximum flow rate. The flow
rate is reduced by the counter pressure in the
extraction column K1. In addition, flow can be
throttled using the regulating valve V1. The
relief valve V5 starts when the corresponding
response pressure is reached. From the relief
valve, the excess solvent returns to the solvent
FI01
tank B1(13) via the recirculation line. The actual
solvent flow rate is thus divided into the desired
flow to the extraction column and the excess back
Float into the solvent tank.

The flow measurement (FI01) and throttling (reg-
V1 ulating valve V1) functions are combined in a sin-
gle component (see photo opposite). FI01 is
designed as a variable-area flowmeter.
Fig. 3.9 Flow meter FI01

with regulating valve V1 The valve V27 is used to vent the suction line in the
event of any suction problems.
The valve V29 is used for emptying, cleaning and

rinsing the extraction column and solvent system
3.4.1.2 Continuous mode
Fig. 3.10, Page 26 shows the variation of the

process diagram for continuous mode, without
distillation.

Media
Feed
Solvent
Extract
Raffinate
Fig. 3.10 CE 620 process diagram, continuous mode variant, without distillation

The process description is largely similar to the

process description for batch mode (see
Chapter 3.4.1.1, Page 20ff).
The key difference is that in continuous mode,
only a single cycle of feed and solvent through the
extraction column K1(9) takes place.
The solvent return goes directly into the extract
tank B3(5) as extract. The feed return goes
directly into the raffinate tank B4(15) as raffinate.
By comparison, in batch mode multiple cycles of

feed and solvent are possible.
Therefore, in batch mode we usually obtain a bet-
ter mass transfer and a higher concentration of
the transition component in the extract.

3.4.2 Extraction column
The cylinder of the extraction column K1(9) is

transparent to allow the process to be observed.
The cylinder is made of borosilicate glass.
During extraction, solvent and feed flow through
the extraction column in counterflow.
Head
The feed passes through a guide pipe into the

bottom of the extraction column. The exiting feed
Distributor
pipe flow is directed upwards. This supports the lift of
the specifically lighter feed through the downward
directed solvent flow.
A perforated plate is positioned approximately
Perforated level with the upper edge of the inlet pipe.
plate
The perforated plate allows packing to be
Guide pipe inserted. The packed bed is then located above
the perforated plate (see also Chapter 3.8,
Page 44ff).
Base
The space between upper edge of the guide pipe
and the base of the extraction column is called the
Fig. 3.11 Extraction column K1(9), solvent stabilising zone (see Fig. 3.13, Page 29).
head and base
Purpose of the solvent stabilising zone:
• Additional separation of the liquid mixture. In
Head other words, any feed components present in
the downward solvent flow can still float.
• Avoiding a possible short circuit current where
Feed the feed that has just exited goes directly into
return
the solvent return.
Distributor
pipe
Fig. 3.12 Extraction column, showing

removed head with distributor
pipe

The specifically heavier solvent enters the extrac-

Feed tion column via a distributor pipe, coming from
stabilising zone
above and directed downwards. The distributor
pipe consists of a vertical pipe, under which a hor-
izontal pipe section is attached. This horizontal
pipe section has a few small holes on the under-
neath. Thus, the solvent inflow is divided into sev-
eral small partial flows. This improves the mass
transfer of the transition component. Fig. 3.12,
Extraction zone
Page 28 shows the removed head with distributor
pipe.
Solvent
Feed
Similar to the solvent stabilising zone, the space

between the head of the extraction column and
the lower edge of the distributor pipe is called the
feed stabilising zone.
The principles described above apply to the feed
stabilising zone accordingly (separation and
avoidance of short circuit current).
The space between solvent stabilising zone and
feed stabilising zone is called the extraction
Solvent
stabilising zone zone. The mass transfer of the transition compo-
nent from the feed into the solvent takes place in
Fig. 3.13 Extraction column zones the extraction zone.
Note on safety:
WARNING
The cylinder of the extraction column is made
of glass.
• Avoid water hammers. When filling the extrac-
tion column, open valve V30 for ventilation.

3.4.3 Setting the phase boundary
A phase boundary forms at the point where the

mutually insoluble solvents (carrier liquid and
solvent) meet.
Solvent inflow Feed return If the phase boundary moves up or down in the
· · extraction column, then this will result in
V Solv,in V Feed,out unwanted breaks. In other words, either feed
enters the solvent/the extract, or solvent enters
the feed/the raffinate.
The aim is to keep the phase boundary at a similar
level during the entire extraction time to enable
reproducible experiments.
Material balance envelope
Setting the phase boundary during the experi-

ment requires some practice. It requires an under-
standing of the hydraulic system.
A key component of the hydraulic system is the
extraction column K1(9).
The phase boundary is determined by the interac-
tion of the two incoming and two outgoing material
flows.
The material balance envelope with the volume
flows around the complete filled extraction column
is shown in Fig. 3.14.
This is based on the standard case, where the
feed has a lower density than the solvent. This
Feed inflow Solvent return
means that the feed enters the extraction column
· ·
V Feed,in V Solv,out at the bottom and the solvent enters at the top.
Fig. 3.14 Material balance envelope

around
extraction column

The balance shows: the sum of the incoming vol-

ume flows is equal to the sum of the exiting vol-
ume flows:
· · · ·
V Solv,in + V Feed,in = V Solv,out + V Feed,out (3.1)
After a long extraction time, in the steady state, if

mass transfer of the transition component from
the carrier liquid into the solvent is no longer tak-
ing place, the following also applies:
· ·
• Where V Solv,in  V Solv,out the phase boundary
moves upwards in the extraction column.

In words: an excess of solvent displaces the
phase boundary upwards.
· ·
• Where V Feed,in  V Feed,out the phase boundary
moves downwards in the extraction column.
In words: an excess of feed displaces the
phase boundary downwards.
• An excess of solvent is equivalent to a decrease
of feed in the extraction column, and vice versa.
This describes the main influence on the level of
the phase boundary. From this, we can deduce
how to respond to a shift in the phase boundary
(see below).
It should be noted here that the shift in the phase
boundary in the actual extraction process (no
steady state) is more complicated. The mass
transfer of the transition component along the
extraction path is constantly affecting the material
compositions and densities.

This results in an additional influence on the level

of the phase boundary.
Feed Fig. 3.15 repeats Fig. 3.5, Page 22 and shows the
return excerpt from the process diagram, which relates
to this material balance envelope.
We can see:
• The flow of the incoming solvent and feed
material flows is measured (FI01 and FI02).
• The volumes of the exiting material flows are
unknown.
• Both the incoming and the exiting material
flows can be throttled using regulating valves
V1 to V4.
• Any change to only one of the four regulating
valves in principle changes all four material
flows.
The values of FI01 and FI02 flow measurements

refer to water at 20°C. For materials with signifi-
cantly different properties, the value must be cor-
rected (see also Chapter 5.3, Page 83f).
Solvent
return We must also note that the exiting materials may
Solvent inflow
Feed inflow
have very different viscosities. The material flow

of the viscous material is much lower with the
same opening of the regulating valve. It therefore
makes sense to only throttle the material flow of
the less viscous exiting material.
Fig. 3.15 CE 620 process diagram,

extraction column section

We recommend the following procedure to keep

the level of the phase boundary in the extraction
column as constant as possible (assuming the
feed is much more viscous than the solvent):
• Allow inflowing material flows, set the begin-
ning of extraction and keep constant during
extraction. Readjust in the event of variances.
• During extraction, fully open regulating valve
V4 for the more viscous exiting material.
• Set phase boundary by throttling the regulating
valve V3(12) for the less viscous exiting mate-

rial.
• Regularly note down the position of this regu-
lating valve V3 and the phase boundary in the
extraction column. The change in level can
then be used to derive whether V3 should be
opened a little more or closed.
A worksheet designed for this purpose can be
found in the appendix (see Tab. 6.3, Page 119).
The photo opposite shows the mark for half the
extraction height (50%).
The distance between the mark and the phase
Fig. 3.16 Mark for the level of the phase
boundary boundary can be measured with a ruler.
• If the phase boundary is falling, close regulat-
ing valve V3 a little more.
• If the phase boundary is rising, open regulating
valve V3 a little more.

3.4.4 Distillation unit
The main components of the distillation unit that

come into contact with the product are transpar-
ent in order to allow the process to be observed.
For these components, there is risk of fracture
(glass material). Therefore, the distillation unit is
supplied in a partially disassembled state, and the
components at risk of fracture are carefully pack-
aged.
The separate installation instructions describe
how to assemble the distillation unit.
The distillation unit is integrated into the trainer

and supplements the actual liquid-liquid extrac-
tion.
In many real world applications, distillation occurs
downstream of the liquid-liquid extraction
stage.
In these cases, distillation is used to prepare the
extract. The aim is usually regeneration of the
solvent from the extract and/or the enrichment
of the transition component in the extract.
The desired change in concentration is essentially
brought about by evaporating the liquid mixture
(extract) and condensing the resulting vapours.
The following figure shows the distillation unit,

both as a photo in the trainer and schematically.

23 23
24
22
22
25
26
27 33
26
28
28
27
29 21
30
29
31
31 32 33 32
21 Heating zone switch for heating mantle

22 Distillation bridge (W1)
23 Thermometer for vapour temperature (TI02)
24 Manometer for low pressure (PI02)
25 Suction connection to vacuum pump
26 Distillation column (K2)
27 Valve (V10)
28 Temperature sensor for residue temperature (TI01)
29 Round-bottomed flask (D1)
30 Connection block for cold water
31 Heating mantle (H1)
32 Valve (V26)
33 Filling port
Fig. 3.17 Distillation unit

The round-bottomed flask D1(29) is filled:

• either directly from the extract tank B3(5), by
opening the valve V10(27)
• or via the filling port (33).
The liquid mixture is heated to boiling point in the

round-bottomed flask D1(29) by means of the
electrically operated heating mantle H1(31).
In this case, the temperature is measured using
the temperature sensor TI01(28).
It is important to prevent moisture penetrating the
heating mantle. Should moisture penetrate the
heating mantle, then the mantle may only be re-
started after being fully dried. If moisture pene-
trates the heating mantle, an RCD circuit
breaker triggers. This RCD must be reset before
re-starting the heating mantle. It is located in the
control cabinet (see wiring diagram in the control
cabinet for the marking).
The heating mantle has an upper and a lower
heating zone. The heating zone switch (21) is
shown in Fig. 3.18. It is used to select the heating
zones of the heating mantle and the intensity of
heating.
For more information and to see the safety
instructions, please refer to the documentation
from the heating mantle manufacturer provided.
Please also note the safety information in
Chapter 2.3, Page 7ff.
Fig. 3.18 Heating zone switch (21)

From the round-bottomed flask, the resulting

vapour enters the distillation column K2(26).
Here there is intensive contact between the
ascending vapour and the downward-flowing con-
densate in counterflow. During this process, the
concentrations of the transition component in the
vapour and the condensate are constantly chang-
ing in the direction of flow.
The distillation column is designed as a packed
column. The packed column contains a bed of
packing (small, regularly shaped bodies, in our
case glass cylinders). The contact between

vapour and condensate takes place throughout
the packed bed. The packed bed provides large
surface areas and intensifies the mass transfer.
The temperature of the vapour at the outlet from
the distillation column is read on thermometer
TI02(23).
The vapour exiting the distillation column enters
the distillation bridge W1(22). There, the vapour
is condensed in the Liebig condenser by means of
cold water. Cold water and vapour are fed in
counterflow.
Fig. 3.19 shows the connection block for cold
water (30). The connecting nozzles for the cold
water inflow and the cold water return are marked
on the trainer.
The liquid mixture exiting from the distillation
bridge is called distillate. The outflowing distillate
is collected in the distillate tank B2(1). After dis-
tillation ends, any liquid mixture present in the
Fig. 3.19 Connection block for
round-bottomed flask is called residue.
cold water (30)

The vacuum pump P3 is supplied separately and

Cold water inflow allows distillation at low pressure, also called vac-
uum distillation.
The vacuum pump reduces the pressure in the
entire distillation unit. It is designed as a water jet
pump and is operated with cold water from the
laboratory mains supply.
Suction
connector The low pressure is read on manometer PI02(24).
The desired low pressure is set by adjusting the
cold water volume flow through the vacuum
pump.
Valve V11 can also be used for fine adjustment.
Briefly opening V11 causes the entry of ambient
air into the distillation unit, and thus an increase in
Cold water return pressure.
Fig. 3.20 Vacuum pump connector P3
PI02(24)
V11
Suction
connector
Fig. 3.21 Manometer PI02(24)

and valve V11

3.5 Control cabinet with controller
The following figure gives an overview of the

switching and control functions of the electrical
control cabinet (item 2 in Fig. 3.2, Page 18).
46 45
44
47
43
48
42
49
41
41 Emergency off switch

42 Rotary switch for solvent pump (P1)
43 Operating light for solvent pump (P1)
44 Rotary switch for feed pump (P2)
45 Operating light for feed pump (P2)
46 Controller TIC1 for temperature TI01
47 Operating light for heating mantle (H1)
48 Rotary switch for heating mantle (H1)
49 Main switch
Fig. 3.22 Control cabinet (2)
The main switch (49) is used to turn the power sup-

ply on and off. The power supply can be instantly
interrupted at any time by pressing the emergency
off switch (41).

The solvent pump P1 and the feed pump P2 can

be operated from the control cabinet.
In each case a rotary switch (42, 44) is provided
as a control element for this purpose. The corre-
sponding operating light (43, 45) lights up when
the pump is switched on.
Controller:
Actual value
A hardware controller with display is installed (46)
for the temperature control loop.
Fig. 3.23 shows this controller TIC1 (46).
Actual value and target value are displayed.
The desired target value can be adjusted using
the two arrow keys.
The controller is released via the rotary switch
(48). When released, this is indicated by the oper-
ating light (47).
The controller TIC1 regulates the temperature T1

Arrow keys Target value of the residue. It is employed as a PID controller.
The controller controls the heating mantle H1. It
Fig. 3.23 Controller TIC1 (46)
varies the time durations for actuating and not
actuating the heating mantle, at a constant period
duration.
The controller TIC1 parameters are preset as

factory defaults (see Chapter 6.1, Page 113f for
the values).
The controller enables self-optimization. For infor-
mation, please refer to the manufacturer's docu-
mentation supplied.

3.6 Special features of individual components
The aim of this chapter is to draw your attention to

Sealing cap inserted
special features of individual components.
Both manometers (PI01 and PI02) of the trainer

are designed as Bourdon tube gauges with
glycerol filling.
The glycerol in the Bourdon tube gauge has a
damping effect. This means that the pressure
gauge remains easy to read when pressure is

fluctuating.
This damping effect is particularly important for
the manometer PI01, because the upstream sol-
vent pump P1(17), as a piston-diaphragm pump,
produces pulsating pressure fluctuations.
Fig. 3.24 Manometer PI02, with sealing
cap inserted
Both manometers are supplied with an inserted
Sealing cap raised sealing cap in order to avoid the accidental leak-
age of glycerol during transport.
The photos opposite show the manometer PI02,
with inserted and raised sealing cap.
In operation, correct pressures are only displayed
when the housing can be ventilated and bled.
There are two ways to achieve this:
• Either raise the sealing cap, as shown in Fig.
3.25, or
• cut a gap in the inserted sealing cap.
Fig. 3.25 Manometer PI02, with sealing

cap raised

3.7 Accessories
Components and accessories for the distillation

unit are described in the separate installation
instructions.
The other accessories provided are shown in the
figure below.
55 54 53 52 62 61
63
64
51 65 66 67 68
51 Hose for cold water 61 Measuring flasks 100mL, for determining density
52 Small parts 62 Measuring beaker 2 L
53 Packing for extraction column (K1) 63 Agitator, for hand drill
54 Conductivity meter 64 Hose for quick coupling, 6x8
55 Packing for distillation column (K2) 65 Hose for draining, 7x10
56 Hose for cold water (not illustrated) 66 Vacuum grease
67 Filling funnel, for round-bottomed flask
68 Quick coupling (plug nipple and coupling)
Fig. 3.26 CE 620: accessories supplied

There is no packing in the extraction column

K1(9) upon delivery (see Chapter 3.8, Page 44ff).
The packing for the extraction column (53)
included with the accessories is used for initial
filling and as a replacement. The packing for the
extraction column (53) is greater than that for the
distillation column (55).
The distillation column K2(26) is supplied with
packed bed. The packing for the distillation col-
umn (55) included with the accessories is used as
a replacement.
Fig. 3.27 Conductivity meter (54) Fig. 3.27 shows the conductivity meter in its
opened packaging.
The conductivity meter can be used to determine
concentrations for experiments using alternative
G F E D C material systems. An example of such an alterna-
tive material system is the extraction of benzoic
acid from petroleum spirit with distilled water.
For information on handling and operation of the
conductivity meter, please refer to the manufac-
turer's documentation supplied.
The photo opposite shows the small parts (52).

The stopper (A) and the wire clip (B) are used as
A B
spare parts for the distillation unit.
A Stopper
B Wire clip The hose clips (C, D) are used to secure the
C Hose clips hoses (51, 56).
D Hose clips
E Control cabinet key
The Allen wrench (G) is required when disassem-
F Adjustable wrench bling the extraction column K1 (see also
G Allen wrench Chapter 3.8, Page 44ff).
Fig. 3.28 Small parts (52)

3.8 Inserting packing into the extraction column
NOTICE
This chapter can be skipped if you are only work-
ing with the recommended model material system
(refined rapeseed oil as carrier liquid, ethanol as
transition component and water as solvent).
There is no packing in the extraction column

upon delivery. In this state, CE 620 is ready for
experiments with the recommended model mate-
rial system.
Packing is generally used to produce large sur-

face areas in columns and to improve mass trans-
fer.
If rapeseed oil is involved in the extraction, then

experience has shown that packing is more of a
hindrance (see Fig. 3.29). The rapeseed oil tends
to enclose the packing. In a packed bed, complete
column cross-sections may be covered by rape-
seed oil. This then hinders the rising of the specif-
ically lighter rapeseed oil and the falling of the
specifically heavier water. This increases the risk
of breakthrough, i.e. rapeseed oil can get into the
extract and water can get into the raffinate.
Packed beds are provided in the accessories to
CE 620 in view of the possibility of using other
mixtures of materials (item 53 in Fig. 3.26,
Page 42).
Fig. 3.29 Extraction column, packed
bed with rapeseed oil

For experiments with different material systems, it

may make sense to insert this packing into the
extraction column. The optimum height of the
packed bed also depends on the material system
used and the operating conditions.
For the alternative material system "extraction
of benzoic acid from petroleum spirit with dis-
tilled water" a bed height of about 25cm has
proven to be ideal, corresponding to 90g of pack-
ing mass.
NOTICE
Frequently changing the packed bed fill height
should be avoided so as to prevent glass splinters
as far as possible.
Only deepen the packed bed if absolutely neces-
sary.
Glass splinters in the trainer may cause serious
damage to the components of the trainer.
In the following section we will briefly describe the

Fig. 3.30 Object: extraction column with
packed bed procedure for inserted the packing. This should
clarify the key points.
You will need some tools, similar to the tools
shown below.
Sometimes a second person is required to follow
the procedure.
In the following description, "extr.col." is used to

describe the extraction column K1.

• Uncover extr.col. To do this, remove connected

pipelines.
• Loosen the four mounting screws on the
extr.col., see also Fig. 3.31 (Do not completely
unscrew mounting screws).
• Have second person hold extr.col. steady.
Then unscrew mounting screws Remove
extr.col. from the trainer and carefully put down
in a horizontal position.
• Place head side of the extr.col. slightly higher,
for example by putting a box under it, see also
Fig. 3.32, Page 47.
• On the bottom side of the extr.col., support
glass cylinder by sliding a wedge under.
• Loosen the nuts on the tensioning bolts and
remove.
Fig. 3.31 Removing the extraction col-
umn, preparations • Pull head out of the extr.col.
• Weigh out 90g of packing in the 2L beaker
(item 62 in Fig. 3.26, Page 42).
• Add approximately 1L of water to the beaker
and stir gently.
The aim is to separate out dirt and small glass
splinters from the packing. The aim is also to
not produce any new glass splinters.
• Strain off any dirt, splinters and water.
Pour packing into a smaller vessel, such as a
400 mL beaker.
• Carefully pour the packing from this beaker
through a funnel into the opened extr.col.
Again, the aim here as far as possible is not to
produce any new glass splinters.

Fig. 3.32 Inserting packing into the disassembled extraction column
• Every so often, use a slender rod to slide the

packing further down in the column to make
room for new packing.
• Mount in reverse order.
When mounting the extr.col. make sure that the
flange surfaces of the base and head are
aligned. To do this, place extr.col. on a flat sur-
face on the two flange surfaces and mount.
Ensure the glass cylinder sits centrally in the
base and head.
Fig. 3.30, Page 45 shows the assembled extr.col.,
with packing inserted.

3.9 Positioning the trainer
In general, the following conditions apply for the

operating site and storage location of the trainer:
• Enclosed space
• Free from dirt and humidity
• Level and fixed surfaces
• Frost-free
Furthermore, you should also take into account,

with which materials CE 620 is operated.
When individual materials cannot be allowed to
get into the drains then the trainer may not be
positioned over a water pit. Example: In the alter-
native material system "extraction of benzoic acid
from petroleum spirit with distilled water", the
petroleum spirit may not be allowed to get into the
drains.
For the recommended model material system

"extraction of ethanol from refined rapeseed oil
with water", positioning the trainer on a water pit
is very beneficial.
In this recommended model material system, the
cleaning at the end of the experiment is very
important in order to maintain the function of the
trainer. During this cleaning, different areas of the
trainer are emptied and rinsed separately. The
rinsing liquid must be able to drain off with the
rapeseed oil residues.
Fig. 3.33, Page 49 shows the positioning of
CE 620 over a water pit.

Fig. 3.33 CE 620 positioned over water pit
You can see that the hoses are plugged into the
drains and rinsing points. These hoses lead down
to the water pit. In this way, it is not necessary to
collect rinsing liquid in separate vessels. Such a
set-up also makes sampling easier.
The required hose material is included in the
accessories (item 65 in Fig. 3.26, Page 42).
A shallow pan placed underneath the trainer can
also be used as a replacement for a water pit.
Alternatively, the hoses can also be directed to a
low-lying water outlet.

3.10 Commissioning
Note on water quality:

We recommended avoiding the use of water with
high water hardness (>5°dH). The lower the
water hardness, the less deposits will form in the
trainer.
This is true for cold water, rinsing water and the
solvent.
Tap water can be used as the solvent. However,
we recommend using distilled water if the influ-
ence of water contents on the liquid-liquid extrac-
tion is to be excluded.
Another argument for using distilled water as sol-
vent is the tendency of tap water to cause lime-
scale deposits in the distillation unit.
Tap water was used during the experiments con-
ducted by GUNT at our factory.
Familiarisation with the trainer:

To operate the trainer, it is necessary to under-
stand the process and the operating modes in
advance. It is also very helpful to be able to find
the components in the trainer quickly and safely.
If not already done, the preparation for commis-
sioning is a good time to become familiarised with
the trainer.
It is helpful to compare process diagram and
trainer with regard to components, instruments
and pipelines.

It is useful to consider the cycles of the different

media in succession in the direction of flow.
The subsequent commissioning will then consoli-
date what has been learned.
Commissioning sequence:
• Observe the safety instructions (see Chapter 2,
Page 5 ff.)
• Observe the separate safety instructions in the
manufacturer's documentation for the heating

mantle.
NOTICE
Risk of damage to the device.
• Before connecting to the electrical power sup-
ply:
Make sure that the laboratory power supply
meets the specifications on the device's rating
plate.
• Select position of the trainer (see Chapter 3.9,

Page 48 f).
• Install distillation unit according to the installa-
tion instructions supplied separately.
• Connect hose line for cold water inflow (see
Fig. 3.19, Page 37).
• Connect hose line for cold water return and
lead to the water drain.
• Connect hose lines for cold water inflow and
cold water return to vacuum pump P3, accord-
ing to Fig. 3.20, Page 38.

• Cut hoses (item 65 in Fig. 3.26, Page 42) to

length and plug into drains and rinsing points
(see also Chapter 3.9, Page 48f).
• For manometers PI01 and PI02, raise sealing
cap (see Chapter 3.6, Page 41).
• Remove cover from tanks B1 and B3-B5.
• If possible, lead the customer supply hose for
tap water to the trainer (hose with valve).
This supply hose can also be used in later
experiments to fill the tanks.
• Fill feed tank B5 and solvent tank B1 with tap
water.
• Correct any possible leaks.
• Connect trainer to the mains power supply.
• Turn main switch (no.. 49 in Fig. 3.22, Page 39)
to "1".
• Position valves and 3-way ball valves so as to
get the flow for batch operation according to
Fig. 3.4, Page 21.
• Ensure that valve V30 is opened.
• Start solvent pump P1.
• Start feed pump P2.
• Watch as the extraction column K1 fills up.
Close valve V30 as soon as water starts to
come out.
• Position valves and 3-way ball valves so as to
get the flow for continuous operation according
to Fig. 3.10, Page 26.
• Stop solvent pump P1 and feed pump P2.

• Open valve V10 until the round-bottomed flask

D1 is sufficiently filled for both heating zones.
• Move heating zone switch (21) to "3".
• Switch on heating mantle H1. To do this,
release controller TIC1 and set target value of
90°C.
• Open cold water inflow to distillation bridge W1.
• Start vacuum pump P3 by opening the cold
water inflow.
• First close valve V11.

• Observe manometer PI02. Once p = -0,5 bar g
is reached, throttle cold water inflow to the vac-
uum pump a bit.
• Maintain the desired negative pressure p = -
0,5 bar g as steadily as possible by adjusting
the cold water inflow.
Once p = -0,5 bar g is reached, throttle cold
water inflow to the vacuum pump a bit.
• Bring water in the round-bottomed flask D1 to
boiling point.
• Ensure that the level in the round-bottomed
flask D1 is sufficient for operation with two
heating zones.
• Operate distillation until distillate is flowing into
the distillate tank B2.
• Switch off heating mantle H1.
• Slowly open valve V11 (pressure equalisation).
• Close cold water inflow to distillation bridge
W1.

• Drain trainer, except for the round-bottomed

flask (boiling liquid!)
• Seal tanks B1 and B3-B5 with their lids.
• Main switch to "0".

3.11 Decommissioning

Page 5 ff.)
mantle.
• If not already done, thoroughly rinse the entire
trainer.
• If not already done, thoroughly clean the entire
trainer (see Chapter 5.4.5.3, Page 100ff.)

• Drain trainer as far as possible. To do this,
open all valves.
• Switch over 3-way ball valves V7 and V8.
• Disconnect hoses from the trainer.
• Unscrew the cover of distillate tank B2.
• Drain any liquid remaining in the trainer as far
as possible. Wipe dry tanks from the inside with
cloth or towel.
• Disconnect trainer from mains electricity sup-
ply.
• Store trainer and accessories in a closed
space, covered, clean, dry and frost-free.

3.12 Care and maintenance
3.12.1 Vacuum grease for glass valves
There are two valves made of glass, V10 and

V26, in the distillation unit. These valves may jam
on contact with hot liquids or vapours.
The effect is significantly reduced by applying
vacuum grease on the sealing surfaces. Vacuum
grease is already applied to the sealing surfaces
on delivery.
If problems occur during operation, we recom-
mend the following procedure:
• End the experiment.
• Thoroughly clean the distillation unit, according
to Chapter 5.4.5.3, Page 100ff.
• Drain the distillation unit.
• Remove valves V10 and V26.
• Lubricate sealing surfaces with the vacuum
grease from the accessories (item 66 in Fig.
3.26, Page 42).
• Install valves V10 and V26.
3.12.2 Descaling the round-bottomed flask
The recommended model material system is

intended to use water as the solvent. Depending
on the hardness of the water used, over time lime-
scale deposits will form in the distillation unit (see
notes on water quality, Chapter 3.10, Page 50).

The reason for this is that the significant tempera-

ture changes in the distillation unit affect the solu-
bility of dissociated calcium salts. Furthermore,
there is an increase in concentration in the resi-
due, as a result of evaporation. In this case the
residue can be supersaturated, resulting in the
formation of limescale deposits in the round-bot-
tomed flask D1(29).
If these limescale deposits interfere with the

experiments, then we recommend descaling with

dilute acetic acid. Approximately 5L of diluted
acetic acid is required (Concentration roughly
2...5 %):
Page 5 ff.)
• Thoroughly clean the distillation unit, according
to Chapter 5.4.5.3, Page 100ff.
• Drain the distillation unit.
• Close valves V10 and V26.
• Place funnel from the accessories (item 67 in
Fig. 3.26, Page 42) on the inlet nozzle of the
round-bottomed flask.
• Pour approximately 5L of diluted acetic acid
(2...5 %) into the round-bottomed flask and
leave to work overnight.
• Empty the round-bottomed flask.
• Finally, thoroughly clean the distillation unit
once more.


4 Basic principles
The basic principles set out in the following make

no claim to completeness. For further theoretical
explanations, refer to the specialist literature.
In extraction we differentiate between:

• Solid phase extraction and
• Liquid-liquid extraction
Solid phase extraction refers to the process of

dissolving out soluble components from solid mix-
tures using a solvent.
An example of solid phase extraction is the prep-
aration of coffee, i.e. the dissolving out of coffee
ingredients from ground coffee with hot water.
4.1 Liquid-liquid extraction
Liquid-liquid extraction refers to the dissolving

out of one or more components of a liquid mixture
using a solvent.
Examples of liquid-liquid extraction are:
• Separation of aromatic compounds from crude
oil fractions.
• Separation of vitamins from aqueous solutions.
• Removal of lecithin from vegetable oil.
Therefore liquid-liquid extraction involves at
least three liquids.
Names such as solution, solvents, etc. often lead
to misunderstandings, especially in comparison to
different sources.
4 Basic principles 59
As already described in Chapter 3.1, Page 15f,

these experiment instructions use the following
designations for the liquids involved:
• Transition component
• Carrier liquid
• Solvent
The illustration in Fig. 4.1, Page 61 symbolises

liquid-liquid extraction in a beaker, with the fol-
lowing simplifications:
• Only three liquids are involved.
• The transition component transfers completely
from the carrier liquid into the solvent.
On the left is the beaker with two liquid phases.

Carrier liquid and solvent together form the sol-
vent system.
The carrier liquid and solvent together form a
phase boundary. They are insoluble in one
another. This is the condition so that separation
into two phases can occur after the actual extrac-
tion. Also required is a clear density difference
between the carrier liquid and solvent.
60 4 Basic principles
Before Mixing Settling After

Liquids involved Abbreviation

Transition component T
Carrier liquid C
Solvent S
Fig. 4.1 Simplified representation of liquid-liquid extraction
In this example, the solvent is specifically heavier

than the carrier liquid. Therefore the carrier liquid
floats on the solvent.
The carrier liquid "carries" the transition
component, the transition component is dis-
solved in the carrier liquid.
The next step shows is the mixing of the two liq-
uid phases. Droplets are formed, the specific sur-
face area increases and the three liquids are
brought into intensive contact. In doing so, the
transition component transfers from the carrier liq-
uid into the solvent. Another condition for extrac-
tion is that the transition component is soluble in
the solvent.
After mixing, two further liquid phases form.
The specifically heavier solvent settles down-

wards (settling). The transition component is dis-
solved in the solvent. The carrier liquid floats.
Finally, the two liquid phases are transferred into
separate beakers.
In process engineering we are often interested in

the incoming and outgoing materials and material
flows. Fig. 4.2 expands the graphical
representation from Fig. 4.1, Page 61 with the
corresponding terms.
Feed Raffinate
Solvent Extract
Fig. 4.2 Liquid-liquid extraction, identification of incoming and outgoing materials
The following terms are common in liquid-liquid

extraction:
The liquid mixture of the transition component and
carrier liquid is called the feed.
The two liquid phases, which we get at the end of
liquid-liquid extraction are called the extract
and the raffinate.
The extract is essentially a solution of the transi-

tion component in the original solvent.
The raffinate is essentially the original feed, less
the extracted proportion of the transition compo-
nent.
This results in:
• From solvent and feed we get raffinate and
extract.
• The aim of liquid-liquid extraction is to trans-
form as high a proportion of the transition com-

ponent from the feed into the extract as possi-
ble.
4.2 Types of liquid-liquid extraction systems
There are a variety of different types of liquid-liq-

uid extraction systems.
One simple model is the mixer-settler extraction
system.
In the mixer-settler extraction system, the sepa-
rate steps of mixing and settling take place in sep-
arate tanks. The mixing is done in a stirred tank,
the settling in a downstream settling tank.
The process is similar to the simplified represen-
tation of liquid-liquid extraction in Fig. 4.1,
Page 61.
Liquid-liquid extraction is particularly suitable for

continuous operation, especially since all phases
are liquid.
The most commonly used liquid-liquid extrac-
tors for continuous operation are extraction col-
umns. They are available in a variety of designs.
The figure opposite shows a schematic view of

the trainer's extraction column (see also Fig. 3.13,
Page 29). Feed and solvent meet each other in
the extraction column. When this happens, a part
of the transition component is extracted from the
feed into the solvent.
This assumes that the feed has a lower density
than the solvent. The feed inflow therefore enters
the bottom of the extraction column and moves
upwards. The solvent enters the top of the extrac-
tion column and moves downwards in counterflow
Solvent
Feed
to the feed.
The driving force for the counterflow is the den-
sity difference between solvent and feed.
In contrast to the mixer-settler extraction system,

both the mixing and settling take place in the
same apparatus, i.e. in the extraction column.
Fig. 4.3 Extraction column,

schematic
4.3 Refining crude vegetable oil, removal of lecithin
Vegetable cooking oils are obtained by pressing

oil-bearing seeds and fruits. After pressing, there is
still a large quantity of vegetable oil in the press
residue, which is also obtained by extraction.
The crude vegetable oil obtained in this way still
contains undesirable additional constituents.
The removal of these unwanted additional constit-
uents is known as refining.
Fig. 4.4 shows the individual steps of refining
crude vegetable oil.
Crude vegetable oil

Add: Remove:
Water Removal of lecithin Lecithin
Phosphoric acid, heat Degumming Turbidity, mucilage
Caustic soda Deacidification Free fatty acids
Bleaching clay, activated Bleaching Pigments, heavy metals

carbon
Water vapour Deodorisation Odourants,

flavourings
Refined vegetable oil
Fig. 4.4 Refining crude vegetable oil
Often, refining begins with the second step of deg-

umming.
The first step of removal of lecithin is chosen if
lecithin is to be obtained as a by-product of veg-
etable oil production.
Crude vegetable oils from soy and rapeseed are

used for the removal of lecithin due to their high
lecithin content.
When removing lecithin a bit of hot water is added
to the crude vegetable oil. This causes the lecithin
to swell, and it falls out of the oil. This swollen lec-
ithin has a higher density than the vegetable oil,
so that it can be divided out in separators. We get
the lecithin sludge from the raw lecithin obtained
by evaporation.
The material group of lecithins is a component of

cell membranes of all living things. Lecithins have
a bipolar molecular structure, in other words they
are both lipophilic ("fat friendly") and hydro-
philic ("water-friendly"). They therefore permit the
mixing of liquids that are not miscible (e.g. oil and
water). Lecithins act as a natural emulsifier.
In many countries lecithins are approved as

emulsifiers and dispersing agents in the food
industry. They are almost indispensable in many
industries.
In addition to the food industry there are further
applications of lecithins, including in the pharma-
ceutical and cosmetic industries, and the animal
feed industry.
4.4 Model material system for CE 620
The actual process of lecithin removal described

in Chapter 4.3, Page 65f consists of several basic
processes (unit operations). The separation of
carrier liquid and solvent in separators is a key
component of this process.
As is common at the production scale, this pro-
cess cannot be transferred to CE 620. Moreover,
the lecithin transition component itself is a mixture
of various materials, only present in crude vegeta-
ble oil in low concentrations and is expensive. In

addition, it is quite difficult to determine the con-
centration of lecithin.
We therefore recommend using a model mate-
rial system for CE 620.
According to the actual process of lecithin
removal, the same solvent system is used (veg-
etable oil as carrier liquid, water as solvent). Eth-
anol is used as transition component in place of
lecithin. Thus with the model material system
we get the extraction of ethanol from vegetable
oil with water.
The density change relative to pure water is used
as a measure of the concentration of the ethanol
in the extract (mixture of ethanol in water) (details
below in Chapter 4.6, Page 70ff).
Crude vegetable oils from soy and rapeseed are
used for the removal of lecithin due to their high
lecithin content. The proliferation of various vege-
table oils varies between regions. In Northern
Europe, rapeseed oil is more widespread than
soybean oil.
Therefore, refined rapeseed oil was used for the

experiments carried out by GUNT at our factory.
It is also possible to use refined soybean oil.
It is important that refined vegetable oil is used
(refining: separating out of unwanted additional
constituents from the crude vegetable oil). Advan-
tages of refined vegetable oil compared to crude
vegetable oil:
• Increased durability and chemical stability of
the vegetable oil during the experiment.
• Better reproducibility of the measurements.
• Easier final cleaning of the trainer.
In addition to the "ethanol from refined rapeseed

oil with water" model material system, CE 620 is
also suitable for experiments with the following
material system:
• Petroleum spirit as carrier liquid.
• Benzoic acid as transition component.
• Distilled water as solvent.
Details on the necessary introduction of packing

in the extraction column can be found in
Chapter 3.8, Page 44ff.
4.5 Distillation
In many real world applications, distillation occurs

downstream of the liquid-liquid extraction
stage.
In general, distillation is used to prepare the
extract.
Typical objectives of this distillation are:
• Regeneration of the solvent from the extract.
• Enrichment of the transition component in
the extract.
Distillation is a thermal process for the separa-

tion or purification of liquid mixtures whose com-
ponents are completely soluble in each other.
The desired change in concentration is essentially
brought about by evaporating the liquid mixture (in
this case the extract) and condensing the resulting
vapours.
The collected condensate is called distillate. The
remaining mixture is called the residue. The dis-
tillate is richer in low-boiling constituents com-
pared to the initial mixture. Accordingly, the pro-
Fig. 4.5 Distillation, schematic portion of high-boiling components is greater in
the residue.
In order to protect temperature-sensitive products

during distillation, corresponding mixtures are dis-
tilled at reduced pressure. This results in lower
boiling temperatures. This method is called vac-
uum distillation.
4.6 Thermophysical properties and determining concentration
When studying the mass balance of liquid-liquid

extraction, it is necessary to determine the con-
centration of the transition component in the
extract and/or raffinate.
For the recommended "extraction of ethanol from
refined rapeseed oil with water" model material
system, it is useful to determine the concentra-
tion of ethanol in the extract.
The mixture density can be used as a measure
of the concentration of ethanol in the extract (a
mixture of ethanol in water).
Ethanol and water are soluble in each other. The

solubility exists for the complete range of
concentration.
However, knowledge of just the pure material
densities does not help in this case, because the
relationship between concentration and density of
an ethanol/water mixture is not linear. The reason
is that the ethanol and water molecules affect
each other in the mixture and form additional bind-
ing forces (hydrogen bonding).
Therefore, the molecules overall may occupy a
smaller space, so that the volume of the mixture is
less than the sum of the pure component volume
(volume contraction).
Therefore, we have to refer to tabulated values
over the entire concentration range.
The concentration of an ethanol/water mixture is
dependent not only on the mixture density, but
also on the temperature of the mixture.
We often find tables where density and concen-

tration for a fixed reference temperature are con-
trasted. Often 20°C is used as the reference
temperature, occasionally it is 15°C. Tables for
reference temperatures greater than 20°C are dif-
ficult to find.
However, the International Organization of Legal

Metrology (OIML) provides comprehensive ther-
mophysical properties as "International Alcoholo-
metric Tables" (link: www.oiml.org). These tables
show the relationship between density and

concentration for the reference temperatures -20
to +40°C for both volume and mass fractions.
The information about the volume fraction is only
unambiguous in combination with the associated
reference temperature. In our case, the mass
fraction of ethanol in the mixture of wE was
chosen as a measure of concentration since it is
better for comparisons and mass balance studies.
As an excerpt from this extensive collection of
materials data, the tables below specify the den-
sities depending on the mass fraction of ethanol,
for the temperatures +10°C to +30°C.
These tables make it easier to determine the

concentration, because the samples do not have
to be brought to the correct temperature (which
saves time during the experiment). The tempera-
ture dependence comes from the table values.
 = f  wE  T 
T
wE
Fig. 4.6 For the ethanol/ water mixture: Density  in kg/m³ as a function of mass fraction of
ethanol wE and temperature T , 0%  wE  50% , 10°C  T  20°C
 = f  wE  T 
T
wE
Fig. 4.7 For the ethanol/ water mixture: Density  in kg/m³ as a function of mass fraction of
ethanol wE and temperature T , 0%  wE  50% , 20°C  T  30°C
5 Experiments
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.
In terms of the material system the previous

chapters are largely worded to be generally valid.
The terms transition component, carrier liquid and
solvent are frequently used.
This chapter describes experiments with the rec-
ommended model material system of
" extraction of ethanol from refined rapeseed
oil with water."
The experiments use:
• Refined rapeseed oil as carrier liquid,
• Ethanol as transition component,
• Water as solvent,
as well as methylated spirits, detergent and dilute
acetic acid as cleaning agents.
This chapter uses the material names water, eth-
anol and rapeseed oil (as a short form for refined
rapeseed oil). The associated function (carrier liq-
uid, transition component, solvent) is often not
mentioned.
Fig. 5.1 shows the materials used by GUNT dur-
ing our experiments.
5 Experiments 75
The materials were purchased in a supermarket,

with the exception of ethanol.
Ethanol Washing-up liquid Dilute acetic acid

Rapeseed oil Methylated spirits
Materials used Note

Ethanol Purity > 99,5%. Pro analysi.
Rapeseed oil Commercially available. Refined rapeseed oil.
Commercially available. Notes such as "high fat dissolving power" are
Washing-up liquid
desired.
Methylated spirits Commercially available. Ethanol volume fraction of about 95%.
Dilute acetic acid Commercially available. Vinegar essence, acetic acid about 25%.
Fig. 5.1 Materials used
Water is also required. Tap water was used for

cold water, rinse water and solvent during the
experiments conducted by GUNT at our factory.
For notes on water quality please refer to
Chapter 3.10, Page 50.
76 5 Experiments
5.1 Beaker experiments
We recommend that you perform a few beaker

experiments before the first experiment with the
device.
These beaker experiments should be based on
the subsequent experiments using the device,
including with respect to:
• Ethanol mass fraction in the rapeseed oil.
• Mass ratio between feed and solvent.
This allows a comparison with the experiments

using the device.
In addition, these beaker experiments serve as

familiarisation with the model material system
and the materials involved.
In addition, the density measurement to deter-
mine the ethanol mass fraction in the extract is
practised (details below in Chapter 5.2,
Page 78ff).
Various laboratory equipment is required to con-

duct the beaker experiments, including:
• A few beakers, nominal volume 400mL.
• Magnetic agitator.
• Analytical balance.
• Pipette.
5 Experiments 77
5.2 Conducting the density measurement
The density measurement is used to determine

the mass fraction of ethanol in extract, distillate
and residue. In doing so, you are advised to take
an accurate measurement of density, because
the density only varies slightly with the change of
the mass fraction of ethanol.
In principle, a measuring spindle is suitable for
measuring the density, see figure opposite. It
floats in the liquid mixture to be measured. The
immersion depth is a measure of the density.
Disadvantages of the measuring spindle:
• Too inaccurate.
• The required sample volume too great at about
0,5L. Removing 0,5 L of extract disrupts the
ongoing experiment too much.
Fig. 5.2 Measuring spindle In the experiments carried out by GUNT, the den-
sity measurement was carried out using a volu-
metric flask (100mL).
Two pieces of this 100mL volumetric flask are
included in the delivery. The photo in Fig. 5.3,
Page 79 shows the two volumetric flasks
(100mL). They are standing on an analytical bal-
ance. You can also see an Eppendorf pipette and
a hand-held thermometer.
The volumetric flasks have a narrow neck. The
100mL mark is located about half way up the
neck. The small cross section at the level of the
mark means the volume of 100mL is defined rea-
sonably accurately. It is based on the sample tem-
perature of 20°C and deaerated water.
78 5 Experiments
Fig. 5.3 Volumetric flask (100mL) with analytical balance, Eppendorf pipette and hand-held ther-
mometer
The measuring principle is to fill the volumetric

flask with 100mL of the liquid mixture and to
determine the corresponding mass of the tare.
Looking at the photo in Fig. 5.3 we can see an

additional mark next to the 100mL mark, written in
waterproof marker on masking tape.
This additional mark takes into account that nei-
ther the tap water nor the samples from the trainer
are deaerated. The gas fraction would thus simu-
late too low a density.
The higher "corrected" mark compensates for this
effect.
5 Experiments 79
Determining the height of the corrected mark:

• Remove the stopper from the volumetric flask.
• Half way up, stick masking tape around the
existing marking line.
• Heat tap water to 20°C.
• Place volumetric flask on the analytical balance
and tare.
• Pour 99,83g into the volumetric flask, accord-
ing to the water density of 0,9983 kg/L.
In doing so, just before you reach the mark, add
99,83g water with the Eppendorf pipette.
• Indicate the corrected mark with a waterproof
marker.
• Repeat the previous steps for the second volu-
metric flask.
80 5 Experiments
Taking a measurement:
• Pour a sample of just over 100mL of liquid mix-
ture into a beaker.
• Use a hand-held thermometer to determine the
temperature of the sample and note it down.
• Place clean, dry volumetric flask on the
analytical balance.
• Tare analytical balance.
• Take the volumetric flask in one hand and the
beaker in the other.

Pour liquid mixture into the volumetric flask to
about 1cm below the mark.
• Place volumetric flask back on the analytical
balance.
• Use the Eppendorf pipette to add sample into
the volumetric flask, until you reach the cor-
rected mark.
• Read mass of the tare and note it down.
• Pour sample from the volumetric flask back into
the beaker.
• Pour sample from the beaker back into the
trainer.
• Thoroughly clean beaker and volumetric flask.
To do so:
– Put on gloves.
– First rinse beaker and volumetric flask with
water.
– Create a detergent solution.
– Rinse out beaker and volumetric flask with
detergent solution, then rinse with water and
drain.
5 Experiments 81
This removes any rapeseed oil.

– Rinse out volumetric flask with methylated
spirits and drain.
This removes any rapeseed oil still present.
This also encourages the evaporation of liq-
uid residues in the volumetric flask.
The dirty glassware does not have to be thor-
oughly cleaned after every measurement.
However, the aim is to provide enough usable
glassware for the next measurement.
You can use the measurement method suggested

here if there isn't any alternative, more accurate
measuring method for smaller sample volumes.
Before using any such alternative measuring
method to sample the extract, you must ensure
that any rapeseed oil residues present in the sam-
ple will not cause damage.
82 5 Experiments
5.3 Preliminary experiment for flow measurement
The flowmeters for solvent and feed, FI01 and

FI02, are designed as variable area flowmeters.
The values shown relate to water at 20°C.
Therefore, when using water as the solvent we
should only expect small variances between the
· ·
displayed flow V Solv and actual flow V Solv,real .
The process is different when using ethanol dis-

solved in rapeseed oil as a feed. In this liquid mix-

ture the properties of the rapeseed oil are pre-
dominant.
Compared with water, rapeseed oil has a lower
density and a considerably greater viscosity.
Therefore there are large variances between the
· ·
displayed flow V Feed and actual flow V Feed,real .
Preliminary experiment to test FI02:

With this preliminary experiment, it is advisable to
wait until the real experiment (before filling the
extraction column). Then, the required feed is pre-
sent and separate cleaning is not required after
the preliminary experiment.
• Disconnect feed inflow from the quick coupling.
• Attach hose to quick coupling from the acces-
sories, and affix the quick coupling.
• Hold hose in beaker (400mL) and start feed
pump P2.
• Using the regulating valve V2, adjust the flow-
meter FI02 so that 600mL/min is displayed.
Fig. 5.4 Draining the feed inflow line
• Start stopwatch as soon as the beaker is
100mL full.
5 Experiments 83
• Watch the beaker fill up.

Note down the time at which the beaker is
300mL full.
• Stop feed pump P2.
• Drain beaker into the feed tank B5.
·
• Calculate actual flow V Feed,real .
During the standard experiment carried out by

GUNT using refined rapeseed oil with 10%
mass fraction of ethanol, we got a real flow
·
V Feed,real of roughly 60mL/min.
·
By comparing displayed flow V Feed and actual
·
flow V Feed,real we get:
·
V Feed
--------------------
· - = 10 (5.1)
V Feed,real
The effect is therefore significant and must be

taken into consideration when conducting the
experiments.
84 5 Experiments
5.4 Experiments with the device
For experiments with the model material system,

the liquid-liquid extraction has priority.
In this case distillation does not provide any
practical benefit to the regeneration of the water
from the extract (mixture of ethanol and water).
The water is not so valuable that regeneration and
use in the subsequent experiments is worthwhile.
In addition, we would need several distillation
steps until the residue consists of pure water with-
out any ethanol content.
The aims of distillation for experiments with the

model material system are:
• Enrichment of the transition component of eth-
anol in the extract.
The mass fraction of ethanol in the distillate is
greater than that in the extract.
• Use of the distillate for cleaning purposes.
Furthermore, methylated spirits are needed for
additional cleaning (see Chapter 5.4.5.4,
Page 102ff). The distillate can replace a portion
of the methylated spirits required.
5 Experiments 85
5.4.1 Stirring feed and solvent
An agitator for a hand drill is included in the

accessories supplied. The hand drill itself is not
included.
Applications for stirring are:
1. At the start of the experiment, by mixing
ethanol and rapeseed oil to produce feed.
2. During the ongoing experiment, before sam-
pling, to mix solvent.
Stirring is not absolutely necessary for the first

application of "creating feed". Agitation has a sup-
porting effect of dissolving ethanol in the rape-
seed oil and producing a homogeneous liquid
mixture.
The photos opposite show stirring being carried
Fig. 5.5 Stirring in the feed tank out in practice.
For the second application, "mixing solvent", stir-

ring is important for obtaining reproducible meas-
urement results. The solvent flow circulating
through the extraction column is small at about
0,4 L/min compared to the volume of solvent in
the trainer (about 5 L).
By stirring, we can assume that the mass fraction
of ethanol throughout the solvent tank is the same
size.
86 5 Experiments
5.4.2 Standard experiment, basic conditions,

series of experiments
The following section describes the standard

experiment for liquid-liquid extraction with
CE 620.
The experimental conditions are:
• Extraction of ethanol from rapeseed oil with
water.
• Mass fraction of ethanol in the feed 10%.
• Equal masses of feed and solvent, each

5000g.
• Extraction time 180min.
• Solvent flow 400 mL/min.
• Feed flow 800 mL/min (display value).
A series of experiments can be used to work out

how changing experimental conditions affects the
results.
For example, variations can be:
• Reduction of the solvent mass to 3000g.
• Halving the solvent flow to 200mL/min.
If the time required to conduct an experiment has

to be reduced, for example for practical work:
In some experiments the extraction time can be
reduced. You can get meaningful results even
after 120min.
In addition, the distillation of the produced extract

is treated at ambient pressure.
5 Experiments 87
Please observe the notes from Chapter 3, if devi-

ating from the standard experiment. For example,
this applies to:
• Liquid-liquid extraction in continuous operat-
ing mode.
• Vacuum distillation.
5.4.3 Objectives of the experiment
1. Transition of a component from a two-compo-

nent liquid mixture (feed) into a solvent by
extraction.
2. Enrichment of the transition component in the
extract by distillation.
5.4.4 Experiment setup
Connected CE 620 liquid-liquid extraction

trainer, commissioning already carried out in
accordance with Chapter 3.10, Page 50ff.
The accessories required are listed in
Chapter 6.2, Page 116.
88 5 Experiments
5.4.5 Conducting the experiment and cleaning
During the experiments, rapeseed oil flows

through most of the components of the trainer
and/or the components come into contact with the
constituents of the rapeseed oil.
After contact with water and ambient air, some of
the constituents of the rapeseed oil tend to
undergo chemical changes. Rapeseed oil resi-
dues can become rancid and cause disturbing
odours.
In addition, if cleaning is inadequate it can lead to

deposits of solids building up in the trainer, caus-
ing malfunctions.
It is therefore important to remove as much

rapeseed oil from the trainer as possible after
each experiment.
The rapeseed oil residues remaining in the trainer
must be removed by normal cleaning after the
end of the experiment (see Chapter 5.4.5.3,
Page 100ff).
For interruptions of more than two rest days we
recommend additional cleaning with methyl-
ated spirits (see Chapter 5.4.5.4, Page 102ff).
5 Experiments 89
5.4.5.1 Conducting the liquid-liquid extraction experiment, batch
• Observe the safety instructions (cf. Chapter 2,

Page 5 ff.)
• Copy worksheet (see Tab. 6.3, Page 119).
• Remove cover from tanks B1 and B3-B5.
• Connect trainer to the mains power supply.
• Turn main switch (no. 49 in Fig. 3.22, Page 39)
to "1".
• Pour 5000g tap water into solvent tank B1.
To do this, the measuring beaker (2 L) provided
can be used several times. The respective
mass of tap water can be weighed out on the
analytical balance.
• Pour 500g of ethanol into feed tank B5.
• Under circulation, add 4500g of rapeseed oil
into feed tank B5 in doses. To do so:
– Close regulating valve V2 in the feed inflow.
– Start feed pump P2.
– At first slowly, then a little more quickly, add
rapeseed oil to the feed tank B5 (total mass
4500g, see above).
– Start stopwatch.
– Stir occasionally (see Chapter 5.4.1, Page 86).
– Circulate feed for 25min (roughly equivalent
to four cycles of the feed).
– Then stop stopwatch and feed pump P2.
First, ethanol is added to the feed tank and then
rapeseed oil. If added in a different order the
lighter ethanol would float on top. Only rape-
seed oil would get to the feed pump from the
90 5 Experiments
deep-lying suction nozzle and circulate, without

mixing effect.
• If desired, conduct preliminary experiment for
flow measurement according to Chapter 5.3,
Page 83f.
• Measure and note down temperatures of ambi-
ent air, solvent and feed.
• Position 3-way ball valves so as to get the flow
for batch operation according to Fig. 3.4,
Page 21.

• Fully open regulating valve V4 for feed return.
• Close regulating valve V3 for solvent return.
• Start solvent pump P1.
If there are suction problems, vent suction
hose. To do this, open valve V27 briefly.
• Using regulating valve V1, adjust solvent flow
to about 80 mL/ min.
• Using regulating valve V2, set feed flow to
about 800 mL/min (display value, not actual
flow).
In real terms, the rapeseed oil and water flows
are now the same (see Chapter 5.3, Page 83).
Therefore, the phase boundary will form at the
start of extraction at approximately half the
height of the extraction column.
5 Experiments 91
• Watch as the extraction column K1 fills up.

Close valve V30 as soon as liquid starts to
come out.
This is the start of extraction.
• Start stopwatch.
• Using regulating valve V1, increase solvent
flow to about 400 mL/ min.
• Open regulating valve V3 for solvent return about
one turn.
• Check that the feed flow is about 800 mL/min.
Readjust with V2 if it is different.
• Measure the position of the phase boundary,
based on half the extraction height (see Fig.
3.16, Page 33), using a ruler or tape measure.
• Note down position of the phase boundary and
opening of V3 on the worksheet.
• At regular intervals, for example after every
10min, re-record the values and note down on the
worksheet, including information on the time.
• By comparing with the previous value on the
worksheet, determine whether the phase
boundary has fallen or risen.
If the phase boundary deviates significantly from
half the extraction height, adapt the opening of
regulating valve V3 for solvent return:
– If the phase boundary is falling, close
regulating valve V3 a little more.
– If the phase boundary is rising, open reg-
ulating valve V3 a little more.
– Note down new position of the regulating
valve V3 on the worksheet.
Fig. 5.6 CE 620,
liquid-liquid extraction
92 5 Experiments
Adjusting the phase boundary is described in

Chapter 3.4.3, Page 30ff in more detail.
• After about 20min extraction time, carry out a
density measurement for the solvent. To do
so:
– Stir solvent in the solvent tank B1 (see
Chapter 5.4.1, Page 86).
– Pour solvent sample from solvent tank B1
into a beaker by opening the valve V21.
Empty this first sample back into B1.
– Repeat sampling. A little more than 100mL

of solvent is required.
– Carry out the density measurement in
accordance with Chapter 5.2, Page 78ff and
note down on the worksheet.
• Repeat density measurement of the solvent
after 20min, and for the last time after 180min
of extraction time.
• After 180min of extraction time, stop pumps P1
and P2.
This is the extraction end.
• Close regulating valves V1- V4.
• Open valve V30.
Now the oil phase settles on the water phase.
• By opening the regulating valve V3, the solvent
from the extraction column can flow back into
solvent tank B1.
Close V3 as soon as the phase boundary
reaches the base of the extraction column.
• By opening valve V28, pour feed from the extrac-
tion column into the measuring beaker (2 L).
5 Experiments 93
Then, by opening valve V29, the remaining

feed can flow from the extraction column into
the measuring beaker.
• Drain measuring beaker into the feed tank B5.
• Now, extract is in the solvent tank and raffi-
nate is in the feed tank (see Chapter 3.4.1.1,
Page 20ff).
• In order to make it easier to study the mass bal-
ance, determine the total mass of raffinate. To
do so:
– Let the raffinate flow from feed tank B5 into
a tare-weighted measuring beaker.
– Determine the net mass of raffinate and note
down on the worksheet.
– Empty measuring beaker into a separate
vessel, for example a metal can.
NOTICE
Rapeseed oil residues can become rancid and
develop smells.
• Do not empty rapeseed oil into drains.
– Repeat until the feed tank B5 is empty.

– Finally, drain the raffinate from the feed
inflow line into the tare-weighted measuring
beaker. To do this, disconnect the feed
inflow from the quick coupling. Then attach
hose to quick coupling from the accessories,
and affix the quick coupling (see photo
opposite).
Fig. 5.7 Draining the feed inflow line
– Hold hose in the measuring beaker and start
feed pump P2.
94 5 Experiments
– Stop pump P2 after emptying the feed inflow

line.
– Determine the net mass of raffinate and note
ance, determine the total mass of extract. To
do so:
– Let the extract flow from solvent tank B1 into
a tare-weighted measuring beaker.
– Determine the net mass of extract and note

– Repeat until the solvent tank B1 is empty.
– Finally, drain the extract from the solvent
inflow line into the tare-weighted measuring
beaker. To do this, start solvent pump P1.
– Stop P1 as soon as solvent stops entering
the extraction column.
– By opening valve V29, the remaining extract
can flow into the tare-weighted measuring
beaker. Determine the net mass of extract
and note down on the worksheet.
This concludes the actual experiment.
Never leave the trainer in an uncleaned state.
• Be sure to perform regular cleaning after
the end of the experiment, according to
Chapter 5.4.5.3, Page 100ff
5 Experiments 95
5.4.5.2 Conducting the distillation experiment
We do not recommend conducting the distillation

experiment simultaneously with the extraction
experiment.
The ideal times for conducting distillation are
either after the end of extraction at the same time
as cleaning, or on the following day.
Page 5 ff.)
mantle.
• Pour 4000g of extract into round-bottomed
flask D1.
To do this, the measuring beaker (2 L) provided
can be used several times. The respective
mass of extract can be weighed out on the
analytical balance.
It is easier to fill the round-bottomed flask if you
use the filling funnel provided (see Fig. 5.8).
The extract in the round-bottomed flask is then
distilled and thereby changes its composition.
Therefore, the liquid mixture in the round-bot-
tomed flask is now called the residue.
• If not already done, turn the main switch (no. 49
in Fig. 3.22, Page 39) to "1".
• Slowly open valve V11 (ambient pressure).
• Move heating zone switch (21) to "3".
Fig. 5.8 Filling round-bottomed flask • Switch on heating mantle H1. To do this,
D1 release controller TIC1 and set target value of
95°C.
• Start stopwatch.
96 5 Experiments
• Read off and note down residue temperature

T1 and vapour temperature T2.
• At regular intervals, for example after every
5min, re-record the temperatures and note
down including information on the time.
• Open cold water inflow to the distillation bridge
W1 well before boiling starts.
• Bring the residue in the round-bottomed flask
D1 to boiling point.
• Ensure that the level in the round-bottomed

flask D1 is sufficient for operation with two
heating zones.
• Increase the setpoint on controller TIC1 as boil-
ing activity drops off. Note down changed set-
point with information on the time.
The cause for the rising boiling temperature is
that the proportion of lower-boiling component
in the residue decreases.
• Interrupt distillation as soon as the vapour tem-
perature T2 reaches the value of 98°C.
Eventually, just as little ethanol is present in the
residue that continuing distillation reduces the
mass fraction of ethanol in the distillate.
If you intend to compare several distillation
experiments, then we recommend stopping
according to a fixed rule.
One such rule may be, for example: Stop upon
reaching 2°C temperature difference between
vapour temperature T2 and the boiling temper-
ature of pure water.
• Switch off heating mantle H1.
5 Experiments 97
• Close cold water inflow to distillation bridge

W1.
ance, determine the total mass of distillate.
To do so:
– Lift the hose between distillation bridge W1
and distillate tank B2, so that distillate resi-
due can flow out.
– Let the distillate flow from distillate tank B2
into a tare-weighted measuring beaker.
– Determine the net mass of the distillate and
note it down.
• Carry out the density measurement for the
distillate, according to Chapter 5.2, Page 78ff.
Note down the readings.
• Store distillate in a resealable container if you
intend to use it later for cleaning purposes.
The residue in the round-bottomed flask D1 is still
very hot (boiling liquid!).
WARNING
Hot liquids at the outlet of the round-bottomed
flask.
Scalds are possible.
• Do not touch during operation.
• Wear safety goggles and protective gloves
when draining.
To prevent risk of scalding, it is recommended to

only remove residue after it has sufficiently cooled
(for example, the following day).
98 5 Experiments
• Determine total mass of the residue in order

to allow the mass balance to be studied. To do
so:
– Let the residue flow from round-bottomed
flask D1 into a tare-weighted measuring
beaker.
– Determine the net mass of the residue and
note it down.
– Repeat until the round-bottomed flask is
empty.
– Carry out the density measurement for the

residue, according to Chapter 5.2,
Page 78ff. Note down the readings.
5 Experiments 99
5.4.5.3 Normal cleaning after the end of the experiment
For normal cleaning, tap water is used amongst

others. If available, use warm tap water to
improve the cleaning effect.
Page 5 ff.)
• Rinse all of the trainer's dirty components and
lines with water. To do so:
– Close all dirty valves, with the exception of
V30.
– Fill tanks B1 and B5 with tap water, then
drain.
– Fill tanks B1 and B5 with tap water once
more.
– As in the actual experiment, start pumps P1
and P2 and fill extraction column with tap
water.
– Leave the tap water to circulate in the trainer
for about 5min.
– Stop pumps P1 and P2.
– Empty trainer.
lines with detergent solution. To do so:
– Close all dirty valves, with the exception of
V30.
– Fill tanks B1 and B5 roughly half full with tap
water.
– Add detergent to tanks B1 and B5. The for-
mation of foam is desired.
– Fill tanks B1 and B5 up with tap water.
100 5 Experiments

and P2 and fill extraction column with deter-
gent solution.
– Leave the detergent solution to circulate in the
trainer for about 10min.
– Close regulating valves V1- V4.
– Open valve V30.
– Fill tanks B1 and B5 up with tap water until
completely full, see Fig. 5.9, Page 102.

– Leave the detergent solution to soak in the
trainer for at least an hour.
Here, it is useful to take a break from the cleaning.
The rest of the cleaning can be completed the fol-
lowing day. Then, the detergent solution can be
left to soak in the trainer overnight.
If you choose this method, turn the main switch to
"0" and back to "1" the next morning.
• Then empty the trainer.
lines with water twice, as described above.
• Open all "formerly dirty" valves.
• Empty trainer.
• If rapeseed oil residue is visible in the round-
bottomed flask:
Leave detergent solution to soak and rinse with
water, in a similar way to cleaning the liquid-
liquid extraction.
5 Experiments 101
Fig. 5.9 CE 620 with detergent solution
5.4.5.4 Additional cleaning with methylated spirits
The "additional cleaning with methylated spirits"

is not a substitute for "normal cleaning after the
end of the experiment."
It is carried out if necessary (see Chapter 5.4.5,
Page 89) subsequent to the "normal cleaning
after the end of the experiment."
The aim is to rinse all of the trainer's dirty compo-
nents and lines with methylated spirits.
102 5 Experiments

Page 5 ff.)
It should be emphasized:
WARNING
Flammable solvents.
• Keep away from sources of ignition.
• Do not smoke.

• Do not empty ethanol and methylated spirits
into drains undiluted.
• Close the drainage valves.

• If rapeseed oil residue is visible in the round-
bottomed flask D1:
– Insert filling funnel into the filling port (see
Fig. 5.8, Page 96).
– Pour approximately 4,5 L of methylated spir-
its into the round-bottomed flask.
– Leave to soak for about 10 min.
– Allow the methylated spirits to flow out of the
round-bottomed flask into a measuring
beaker.
– Empty the measuring beaker into solvent tank
B1.
– Repeat until the round-bottomed flask has
been emptied.
If it is not necessary to fill the round-bottomed
flask with methylated spirits, then 3,5 L of methyl-
5 Experiments 103
ated spirits is sufficient for the cleaning of the

actual liquid-liquid extraction.
Then start to fill the 3,5 L methylated spirits
directly into the solvent tank B1.
• Position 3-way ball valves so as to get the flow
for batch operation according to Fig. 3.4,
Page 21.
• Close regulating valve for feed inflow (V2) and
feed return (V4).
• Open regulating valve for solvent inflow (V1)
• Fill extraction column K1. To do this, start sol-
vent pump P1.
• Open regulating valve for solvent return (V3) a
little.
• Watch as the extraction column fills up. Close
valve V30 as soon as liquid starts to come out.
• Leave the methylated spirits to circulate in the
solvent system for about 5min.
• Pump over from the feed tank B1 into the sol-
vent tank B5. To do so:
– Open feed return regulating valve (V4).
– Close solvent return regulating valve (V3).
– Observe the level in the solvent tank. Stop
solvent pump P1 as soon as the solvent tank
is emptied.
– Close solvent inflow regulating valve (V1).
• Open feed inflow regulating valve (V2).
104 5 Experiments
• Leave the methylated spirits to circulate in the

feed system for about 5min.
• Stop feed pump P2.
• Empty trainer. To do so, collect any methylated
spirits that runs off in the measuring beaker.
Do not open all drains at the same time,
especially if CE 620 is positioned over a water
pit (see Fig. 3.33, Page 49).
The distribution of methylated spirits onto a
large surface and the formation of ethanol

vapours should be avoided.
• Rinse all of the trainer's components and lines
that have been wetted by methylated spirits with
water. To do so:
– Close all wetted valves, with the exception of
V30.
– Fill tanks B1 and B5 with tap water.
and P2 and fill extraction column with tap
water.
– Leave the tap water to circulate in the trainer
for about 5min.
– Empty trainer.
5 Experiments 105
5.4.6 Measurements
At the start of extraction 10kg of liquid were added

to the trainer (sum of solvent and feed).
At the end of extraction approximately 9,2kg of
liquid were removed from the trainer (sum of
extract and raffinate).
A large part of the measured values were entered

by hand into a copy of the worksheet Tab. 6.3,
Page 119 during the experiment (measured val-
ues for the phase boundary and for the density
measurement).
Tab. 5.1, Page 107 shows these measured val-
ues.
106 5 Experiments
Phase boundary
· ·
 t Extr V Feed V Solv V4 V3 Level
Extrac- Opening Opening, Phase Notes
tion time chg to... boundary
min mL /min mL /min % Turns cm
0 800 400 100 1,5 +2 Start of extraction
3 800 400 100 1,0 -5
6 800 400 100 1,1 +1
8 800 400 100 1,2 +4
16 800 400 100 1,3 +3
26 800 400 100 1,2 -4
39 800 400 100 1,1 -16
51 800 400 100 1,0 -23

59 800 400 100 (1,0) -14
66 800 400 100 (1,0) -10
78 800 400 100 (1,0) -3
86 800 400 100 1,1 +11
93 800 400 100 1,2 +12
105 800 400 100 (1,2) +10
116 800 400 100 (1,2) +7 Phase boundary expansion
136 800 400 100 (1,2) -3
146 800 400 100 1,1 -9
161 800 400 100 1,0 -13
173 800 400 100 (1,0) -5
180 800 400 100 (1,0) +1 Extraction end
Measurement Evaluation Notes

 t Extr T m /100mL wE (Tx ) wE (Tx+1) wE (T )
min °C g % % %
20 18,7 99,51
40 18,7 99,39
60 18,8 99,42
80 18,8 99,37
100 18,7 99,20
120 18,5 99,20
140 18,5 99,20
160 18,5 99,10
180 18,6 99,11
Key: Chg: Change; T: Temperature; wE : Mass fraction of ethanol
Tab. 5.1 Worksheet: standard liquid-liquid extraction experiment, batch mode. Measurements.
5 Experiments 107
5.4.7 Evaluation
The mass loss during extraction is roughly 8%.
Tab. 5.2, Page 109 supplements the data from

Tab. 5.1, Page 107. In addition to the measure-
ments, the mass fractions of ethanol are listed
here and highlighted in yellow.
The table in Fig. 4.6, Page 72 was used and line-
arly interpolated for the evaluation.
After extraction end, the mass fraction of ethanol

in the extract is 4,1%.
Taking into account the mass losses, the extrac-

tion effect is 44%.
In other words: Overall, about 44 percent by mass
of the ethanol present in the feed transfers from
the rapeseed oil into the water during extraction.
108 5 Experiments
Phase boundary
· ·
0 800 400 100 1,5 +2 Start of extraction
3 800 400 100 1,0 -5
6 800 400 100 1,1 +1
8 800 400 100 1,2 +4
16 800 400 100 1,3 +3
26 800 400 100 1,2 -4
39 800 400 100 1,1 -16
51 800 400 100 1,0 -23

59 800 400 100 (1,0) -14
66 800 400 100 (1,0) -10
78 800 400 100 (1,0) -3
86 800 400 100 1,1 +11
93 800 400 100 1,2 +12
105 800 400 100 (1,2) +10
116 800 400 100 (1,2) +7 Phase boundary expansion
136 800 400 100 (1,2) -3
146 800 400 100 1,1 -9
161 800 400 100 1,0 -13
173 800 400 100 (1,0) -5
180 800 400 100 (1,0) +1 Extraction end

min °C g % % %
20 18,7 99,51 1,88 1,78 1,8
40 18,7 99,39 2,56 2,44 2,5
60 18,8 99,42 2,39 2,28 2,3
80 18,8 99,37 2,67 2,59 2,6
100 18,7 99,20 3,66 3,55 3,6
120 18,5 99,20 3,66 3,55 3,6
140 18,5 99,20 3,66 3,55 3,6
160 18,5 99,10 4,20 4,08 4,1
180 18,6 99,11 4,20 4,08 4,1
Tab. 5.2 Worksheet: standard liquid-liquid extraction experiment, batch mode. Measurements and evaluation.
5 Experiments 109
5.4.8 Comment and evaluation
Causes for the mass loss during extraction are:

• Losses during sampling and density measure-
ment.
• Losses during removal of the extract and
raffinate.
• Liquid remaining in the trainer after the end of
the experiment.
·
With the flows V Solv = 400 mL/min and
·
V Feed = 800 mL/min (display value) we get a
roughly fivefold water surplus in real terms, i.e.:
·
V Solv,real
--------------------
· - = 5 (5.2)
V Feed,real
This excess water primarily acts in the upper half

of the extraction column. Occasionally we can
observe how pulsating water moves upwards in
the centre of the rapeseed oil column.
This effect cannot be observed at significantly
reduced water surplus.
110 5 Experiments
In terms of production, a contact time of rape-

seed oil and water of 180min (extraction time) is
not tenable. The quality of the rapeseed oil suf-
fers.
Therefore, extraction columns are rather rare in

rapeseed oil production. Instead, it is thoroughly
mixed. The phases separate very effectively in
separators or decanters. The result is significantly
better yields with very short contact times.
However, the benefits of using the "extraction of

ethanol from rapeseed oil with water" model
material system for demonstrating the practical
operation of an extraction column are considera-
ble:
• Relatively harmless materials.
• Relatively simple disposal of the extract and
raffinate.
• Well-formed and clearly visible phase bound-
ary in the transparent extraction column.
• Simple principle of measurement for determin-
ing the concentration.
• Actual background in terms of industrial pro-
duction, with the rapeseed oil carrier liquid and
the water solvent as solvent system.
5 Experiments 111
112 5 Experiments
6 Appendix
6.1 Technical data
Dimensions:
Length x width x height: approx. 1350 x 750 x 2100 mm
Weight: approx. 220 kg
Connection values:
Electrical power supply: 230 V; 50 Hz
Rated input (power) approx. 1,75 kW
Alternatives optional, see rating plate

Cold water, primary pressure: recommended p > 2 bar g
Cold water, temperature: recommended T < 20 °C
Extraction column:
Material: Borosilicate glass (DURAN ®)
Inner diameter: 43 mm
Cylindrical height: 1500 mm
Packing, glass cylinders,
outer diameter x length: 10 x 10 mm
Solvent tank, distillate tank, extract tank:

Nominal volume: each approx. 15 L
Raffinate tank, feed tank:

Nominal volume: each approx. 30 L
Feed pump:
Type: Gear pump, magnet-coupled,
with integrated relief valve.
Maximum flow rate for water: 1,1 L/min
Permitted overpressure: 10 bar g
6 Appendix 113
Solvent pump:
Type: Piston diaphragm pump,
with integrated relief valve.
Maximum flow rate for water: 1,2 L/min
Permitted overpressure: 1 bar g
Heating mantle for distillation unit:

Heat output: approx. 1,2 kW
Max. heating element temperature: approx. 450 °C
Number of heating zones: 2
Round-bottomed flask for distillation unit:

Material: Glass
Nominal volume: approx. 5 L
Distillation column:
Material: Glass
Inner diameter: approx. 26 mm
Cylindrical height: approx. 350 mm
Packing, glass cylinders,
outer diameter x length: 4 x 4 mm
Vacuum pump:
Type: Water jet pump
Temperature controller:
Hardware controller with display,
used as a PID controller.
Defaults are: Pb1 =1,78 , rt =88 s , dt =22 s
Measuring the vapour temperature:

Type: Thermometer
Measuring range: 0...150 °C
114 6 Appendix
Measuring the residue temperature:

Type: Pt100
Setpoint temperature range: 0...120 °C
Measuring the solvent pressure:

Type: Bourdon tube manometer,
Glycerol case filling.
Measuring range: 0...2,5 bar g
Measuring the pressure in the distillation unit:

Type: Bourdon tube manometer,

Glycerol case filling.
Measuring range: -1...+0,6 bar g
Measuring the feed and solvent flow:

Type: Variable area flowmeter
Measuring range for water at 20°C: 100...850 mL/min
Measuring the conductivity:

Type: Hand-conductivity meter,
combined measurement of conductivity
and temperature. Automatic
temperature compensation of
conductivity.
Conductivity measuring range: 0...3999 S  cm
Temperature measuring range: 0...60 °C
6 Appendix 115
6.2 Scope of delivery, accessories
• Trainer.
• Packing for extraction column.
• Packing for distillation column.
• One set of hoses.
• One set of small parts.
• One conductivity meter.
• One measuring beaker 2 L.
• Two volumetric flasks 100mL.
• One filling funnel.
• Vacuum grease.
• One stirrer.
• One quick coupling
(plug nipple and coupling).
• One set of documentation for components.
• Experiment instructions.
• Installation instructions.
Not included in the scope of delivery:

• Refined rapeseed oil, ethanol, methylated spir-
its, detergent and dilute acetic acid.
• Ruler or tape measure.
• Hand drill.
• Stopwatch.
• Various laboratory supplies, such as analytical
balance, magnetic stirrer, hand-held thermom-
eter, beakers, measuring beakers, pipettes,
metal can, etc.
116 6 Appendix
6.3 List of abbreviations
Abbreviation Meaning
C Carrier liquid
chg change
i.e. that is (id est)
poss. possible
Extr.col. Extraction column K1
RCD Residual current device
usu. usually
S Solvent
s. see
s.a. see also
v.s. see above (vide supra)
T Transition component
etc. et cetera
6.4 List of identification letters used in the process diagram
Identification Name
Equipment and machinery
B Tank
D Vapour generator, heated round-bottom flask
K Column
P Pump
W Heat exchanger, distillation bridge
Fittings
F Filter, strainer
V Valve, general
Tab. 6.1 Identification letters for equipment, machinery and fittings
6 Appendix 117
Identifi- Measurand or other input variable, actuator Processing

cation
letter as first letter as supplementary as subsequent letter
letter (sequence I, R, C)
C Feedback control
F Flow rate, flow capacity Ratio
I Display
L (Fill) level Lower limiting value
P Pressure
T Temperature
Tab. 6.2 Identification letter for measurement points
6.5 Worksheet
The following worksheet can be used to note

down measurements you take yourself in an
experiment.
The worksheet is also used to facilitate the evalu-
ation after the experiment has ended. Fields for
the mass fractions of ethanol are provided along-
side the measured values for temperature and
density.
118 6 Appendix
Phase boundary
· ·
0 Start of extraction

min °C g % % %

Tab. 6.3 Worksheet for liquid-liquid extraction, batch mode
6 Appendix 119
120 6 Appendix

Liquid-Liquid Extraction PDF

Uploaded by

Copyright:

Available Formats

You might also like

Liquid-Liquid Extraction PDF

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Liquid-Liquid Extraction PDF

Uploaded by

Copyright:

Available Formats

Experiment Instructions

CE 620 Liquid-Liquid Extraction

This manual must be kept by the unit.

Before operating the unit:

Version 1.2 Subject to technical alterations

3 Description of the device . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

3.1 Objective of the extraction, designation of the substances involved . 15

vegetable oil and water" solvent system, in a sim-

Layout and function of the device

The vacuum pump installed allows distillation at

The learning objectives are:

Structure of the instructions

Didactic notes for teachers

tion of the trainer. Operating the system requires

Areas where the trainer can be employed include:

These materials are intended to be used to help

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

An additional symbol indicates the nature of the

Signal word Explanation

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

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

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

Indicates a situation which may result in damage to

Hazard area (general)

Wear eye protection

Wear safety shoes

2.3 Safety instructions

These safety instructions relate to the model

• Observe national and local regulations.

3 Description of the device

3.1 Objective of the extraction, designation of the substances involved

The main objective of liquid-liquid extraction is

The substances involved in liquid-liquid extrac-

when comparing different sources.

The simplest form of liquid-liquid extraction

The liquid mixture of the transition component and

3 Description of the device 15

and solvent should be as mutually insoluble in

3.2 Process diagram

Fig. 3.1, Page 17 shows the process diagram for

16 3 Description of the device

3 Description of the device

Process diagram of the CE 620 liquid-liquid extraction system

Measurement and control technol

3.3 Device design

1 Distillate tank (B2) 11 Heating mantle (H1)

Fig. 3.2 Overview of the CE 620 liquid-liquid extraction system

18 3 Description of the device

3.4 Device function and main components

This chapter is divided into several subsections.

Finally, we will describe the distillation unit.

The numbers in brackets in the following text

3 Description of the device 19

3.4.1 Operating mode and process description

The CE 620 trainer can be operated either con-