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Experiment Instructions

CE 602 Discontinuous Rectification


07/2014

CE 602 DISCONTINUOUS RECTIFICATION


All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 07/2014

Experiment Instructions

Please read and follow the safety regulations before the first installation!

Publication-no.: 918.000 00 D 602 02 (A) DTP_4

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Table of Contents
1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

2 Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3

2.1 Equipment Layout . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3


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2.2 Equipment Functions and Components. . . . . . . . . . . . . . . . . . . . . . . 4


2.2.1 Components for the Thermal Process . . . . . . . . . . . . . . . . . 4
2.2.2 Control Cabinet. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
2.3 Commissioning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
2.3.1 Preparing the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
2.4 Shutting Down . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

3 Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

3.1 Health hazards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10


3.2 Hazards for Equipment and Function . . . . . . . . . . . . . . . . . . . . . . . 11

4 Theory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12

4.1 Basic Principles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12


4.1.1 Distillation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
4.1.2 Rectification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

5 Experiments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

5.1 Distillation Experiment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16


5.1.1 Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
5.1.2 Test Results, Pure Distillation . . . . . . . . . . . . . . . . . . . . . . . 17

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5.2 Rectification Experiments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18


5.2.1 Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
5.2.2 Test Results, Rectification I . . . . . . . . . . . . . . . . . . . . . . . . 19
5.2.3 Test Results, Rectification II . . . . . . . . . . . . . . . . . . . . . . . . 20
5.3 Method with Vacuum, Vacuum Distillation. . . . . . . . . . . . . . . . . . . . 22
5.4 Notes on Further Experiments. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
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6 Appendix . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23

6.1 Technical Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23


6.2 Tables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
6.3 Specimen Report Sheet . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
6.4 Items Supplied. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27

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1 Introduction

In physical-chemical engineering, liquid mixtures


that consist of mutually soluble fluids are usually
separated by thermal processes. The main pro-
cesses used are distillation and rectification.
The CE602 Discontinous Rectification can be
used to thermally separate liquid mixtures for ex-
perimental purposes using these two processes.
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The system consists of an electrically heated


evaporator in which the initial liquid mixture is
heated and evaporated. The steam rises through a
column and is subsequently condensed in a wa-
ter-cooled condenser. From here, all of the con-
densate can be drained off as the top product, or
all or part of it can be returned to the column.
A sieve tray column and a packed column are pro-
vided for use in experiments as required. A con-
nection is fitted at the head of each column to allow
the return of distillate.

A glass filter pump can be used to generate a


vacuum in the entire tube system for vacuum-
distillation.

The range of experiments covers the following areas:


- Batch operation with or without reflux to sieve
tray or packed column
- Comparison of separation efficiency and
separation quality between packed column
and sieve tray column
- Vacuum distillation

The equipment has been designed to allow most


operations to be observed. The system is for edu-

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cational use in the field of thermal process
engineering and apparatus construction.

The CE 602 Discontinous Rectification it in-


tended solely for educational purposes and not
for industrial production.
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1 Introduction 2
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2 Description

2.1 Equipment Layout


4 5 6 7
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1
10

1 Evaporator 11
2 Column
3 Hand valve and flowmeter 12
for cooling water
4 Differential pressure gauge
5 Condenser
6 Reflux divider
7 Vacuum gauge
8 Vacuum pump
9 Top product container
10 Control cabinet with 13
system diagram
11 Water outlet
12 Hand valve for regulating
the vacuum pump
13 Water inlet

Fig. 2.1 CE 602 Batch Distillation System, General View

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2.2 Equipment Functions and Components

2.2.1 Components for the Thermal Process

The CE 602 Discontinous Rectification is used


to separate homogenous liquid mixtures by distil-
lation or rectification on an experimental scale. A
mixture of ethanol and water is used in the experi-
ments.
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A steel tank with a built-in electric heater acts as an


evaporator (1) for the liquids. On the front of the
tank is a riser to indicate the liquid level.
The evaporator can be filled through its top cap.

A column (2) in which the mass separation takes


place when the equipment is in operation is
mounted on top of the evaporator. Either a packed
column or a sieve plate column with 8 plates can
be used.
Fig. 2.2 Sieve plate column The drop in pressure that occurs over the column
can be measured with a differential pressure
gauge (4).

The steam passes along a tube at the top of the col-


umn into the water-cooled condenser (5). The distil-
late that collects here flows into the reflux divider (6)
from where it can be drained off directly by means of a
hand valve.
By using two electrically operated valves, the distil-
late downstream of the reflux divider can be di-
vided into reflux and top product with a defined
reflux ratio which is controlled electronically. The
reflux then returns to the system across the col-
umn head. The diverted top product flows into the
top product tank (9).
Fig. 2.3 Packed column

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The cooling water for the condenser must be sup-


plied externally from a mains water supply.
The cooling water volume can be read off the
flowmeter (3). The flow can be controlled with the
corresponding hand valve under the flow meter.

The residue which is enriched in the evaporator


during the experiments is called the bottom prod-
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uct. It can be drained directly into a suitable vessel


through a drain valve at the front of the evaporator.

A glass filter pump (8) is used to perform experi-


ments with vacuum. This makes it possible to re-
duce the atmospheric pressure throughout the
system. This pump is also operated with water
Water outlet
from the mains water supply. The hand valve (12)
Water inlet
is used to regulate the flow of water through the
Fig. 2.4 Water connections pump. The level of vacuum can be read off on the
vacuum gauge (7).

All switching and monitoring functions are pro-


vided by the electrical control cabinet (10).

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2.2.2 Control Cabinet

The control cabinet contains all the switchgear


necessary to control the system and conduct mea-
surements.

14 Emergency Stop button


19 20 15 Reflux divider ON/OFF
16 Reflux ratio indicator in %
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21 17 Display and measuring point selector


for temperatures T1 - T12
18
22 18 Heater ON/OFF
19 Controller for head temperature T13
17
20 Heater indicator lamp
21 „Low Level“ warning lamp
16
23 22 System Diagram
15
23 Reflux ratio selector
24 24 Master switch
14

Fig. 2.5 Control cabinet, Front view

The following functions are available:


· A selector switch (17) for temperature mea-
suring points T1 - T12 with display.
The measuring points are selected simply by
turning the knob

· Controls for the reflux ratio:


- ON/OFF switch (15)
- Selector for reflux ratio 0 - 100%
- Reflux ratio display.
Displays the % of distillate that is
returned to the column.

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· Heater controls:
- ON/OFF switch (18)
- The indicator lamp (20) lights up when
the heater is on.
- „Low Level“ warning lamp (21)
The evaporator tank is fitted with a
level switch. If the evaporator does not
contain at least the minimum amount
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of liquid, the heater cuts out automati-


cally and the warning lamp lights up.
- Controller (19) for the head temperature T13.
This is a continuous industrial controller
which the user can configure and program.
The controller is set to a suitable basic setting
at the factory. Further settings are not neces-
1 sary. Please refer to the separate controller
5 instructions for further information.
2 4

1 Actual value
2 Setting value · Setting temperature T13 on the controller
3 Operating buttons
4 „Manual operation“ indicator lamp When it is switched on the controller is in normal
5 Unit
display mode.
Operating the „EXIT“ button toggles between the
Fig. 2.6 Temperature Controller controller’s automatic and manual modes.

Exit button
The indicator LED (5) lights when the
controller is in manual mode.
Arrow buttons In this mode the control ratio of the controller can
be adjusted directly using the two „arrow keys“.
PGM button

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If the indicator LED (5) does not light up, the con-
troller is in automatic mode.
1
5
2
In this mode the required setpoint can be adjusted
4
using the two „arrow keys“.
3
REMARK: The controller only updates the new
setpoint after approx. 2 seconds!
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1 Actual value
2 Setting value
3 Operating buttons
5 „Manual operation“ indicator lamp
6 Unit

Fig. 2.7 Temperature Controller

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2.3 Commissioning

2.3.1 Preparing the System

· Ensure that all hose connections are secure


and free from leaks
· Check the status of all hand valves,
close valves if necessary
· Select the required column and mount it on
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the evaporator
· Fill the evaporator with a suitable test liquid.
Make sure that the minimum liquid level is
reached.
Warning! The heater will not activate if the
evaporator is underfilled.
Observe the „Low Level“ warning lamp
min. 2 litres to ensure that the heater activates
min. 5 litres to allow a meaningful experiment without
the heater cutting out prematurely
· Open the water supply and provide a suitable
runoff for the cooling water
· Connect the unit to the mains electricity supply

2.4 Shutting Down

- Switch off the system at the master switch


- Shut off the water supply and isolate the sys-
tem from the water main
- CAUTION:
Allow the system to cool down for approx.
1 hour,
erect a warning sign if necessary
- Now drain the bottom tank
- Check the status of the hand valves to
prevent spillage

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3 Safety

The Instruction Manual in general and the safety information in particu-


lar must be read carefully before the equipment is used. The safety
aspects and the safe and proper handling of the apparatus must be
explained to the participants before any experiments commence.

3.1 Health hazards


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RISK of electric shock!


Only technically qualified personnel may open the
control cabinet or work on the electrical equipment
Unplug the system from the mains prior to opening
the switch cabinet and working on the electrics.
Protect the electrical system from water and moisture.

DANGER of burns!
The evaporator, column and pipes get hot during
experiments due to the nature of the process.
Do not touch system components when in operation.
When emptying the hot bottom product be sure to
drain it into suitable heat-resistant containers and
wear protective gloves at all times.

DANGER, health risk!


Follow the appropriate hazard information and
safety instructions when handling the chemicals
which are used. This applies particularly when fill-
ing and emptying the system.

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3.2 Hazards for Equipment and Function

WARNING!
The choice of chemicals for distillation and rectifi-
cation is limited by the resistance of the materials
used in the construction of the equipment. Use
only those chemicals which do not attack
- VITON,
-
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PVDF,
- PTFE and
- stainless steel 1.4305!

WARNING!
The electrical components and the control cabinet
must be protected from moisture and humidity and
especially from aggressive media.

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4 Theory

4.1 Basic Principles

Distillation and rectification are thermal processes


used to separate or purify liquid mixtures whose
constituents are wholly miscible with one another.

Both processes work by the basic operations of


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evaporating a liquid and then condensing the re-


sulting vapours.
When a liquid mixture AB, in which substance A
Fraction y1 of substance A

1
has the fraction x1, is brought to the boil, it will give
0.8 off steam. Substance A has a different fraction y1
0.6
in the steam than it does in the liquid mixture AB.
0.52
If we enter the corresponding values for the vapour
0.4
in steam

for all possible mixture ratios of AB in a diagram,


0.2 we obtain the equilibrium curve. This curve indi-
cates the mixture ratio of the steam given off by the
0
0 0.2
0.3
0.4 0.6 0.8 1 boiling liquid.
Equilibrium curves are different for different sub-
Fraction x1 of substance A
in the liquid mixture
stance mixtures. The more the curve bends away
from the diagonal in the diagram, the greater is the
difference in the ratio of substance A to substance
Fig. 4.1 Example of an
Equilibrium Curve B in liquid and vapour.
The collected condensate is therefore richer in
low-boiling constituents compared with the initial
mixture. The proportion of high-boiling constitu-
ents in the residual mixture is correspondingly
higher.
In distillation/rectification therefore, the vapour
phase has a different mixture ratio than the liquid
phase. This fact is the underlying principle of these
processes.

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4.1.1 Distillation

In distillation, a liquid mixture is brought to the boil


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

Evaporator Distillation apparatus consists of:


Condenser
-
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an evaporator to heat the initial mixture and


collect the high-boiling component (residue).
- a condenser to condense the low-boiling
component (distillate).
Residue - one or more vessels in which to collect the
Distillate distillate

Distillation does not produce a complete separation


Fig. 4.2 Distillation, schematic of the initial mixture. It just divides the initial mixture
into two mixtures with different mixture ratios.
In simple distillation, all of the distillate is collected.
There is also the process in which the condensate
is collected in different vessels, known as
fractions, as distillation time passes.
This is known as fractional distillation.
To protect temperature-sensitive substances dur-
ing distillation, their mixtures are distilled in a vac-
uum where boiling points are lower. This method is
known as vacuum distillation.
Essentially vacuum distillation works exactly like
conventional distillation, except that a vacuum
pump downstream of the condenser maintains a
vacuum throughout the system.

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4.1.2 Rectification

The result of the separation obtained by distillation is


not sufficient in all cases.
y4

y3 To improve separation, the collected condensate


should be distilled again. This process should be
y2
repeated until the required material is satisfactorily
purified. Multiple-stage distillation of this type is ex-
y1
pensive and energy-intensive.
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Rectification is therefore used.


x1 x2 x3 x4 x5 In rectification, the released vapour is first passed
Fig. 4.3 Equilibrium diagram for through a vertical tube called the column before it
multiple-stage distillation reaches the condenser. Instead of all of the distillate
collected in the condenser being drawn off straight
away, part of it is returned to the column as the
so-called reflux.

The difference between rectification and distilla-


tion is that the rising vapour mixture and returning
Top condensate flow counter to one another. The pro-
Top product
cess is therefore also known as counterflow dis-
tillation.
Column

The returned condensate now runs down the col-


Reflux umn and is forced into contact with the rising va-
pours on suitable internals.

Bottom
The result is an exchange of material and heat be-
Bottom product
tween the rising vapours and the falling liquid.
The high-boiling component condenses first from
the rising vapours. The resulting condensation
heat causes more low-boiling component to evap-
Fig. 4.4 Rectification, schematic orate in turn. The result is that the liquid flowing
back to the bottom of the column is enriched with
high-boiling components. The vapours at the top

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of the column are correspondingly richer in


low-boiling components.

The exchange of materials that occurs in the col-


umn can be intensified by increasing the contact
area over which the exchange can take place.
Columns therefore contain suitable internalsW0
such as trays or packed beds which increase
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this contact area.

Packing pieces are small, regularly shaped pieces


of plastic, ceramics or metal. There is a very large
number of different packing pieces to suit a wide
variety of separation applications.
At the top of the column, the distillate is divided into
one part reflux and one part top product. The ratio

Condenser

Column head
Reflux

Reflux divider Aftercooler


Column
with internals

Top product
Evaporator (low-boiling)

Initial Column bottom


mixture

Bottom product
(high-boiling)

Aftercooler

Fig. 4.5 Rectification system, schematic representation

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of reflux to top product is called the reflux ratio. It


is an important parameter of the column.
Liquid mixtures can be almost totally separated by
rectification, especially mixtures whose equilib-
rium curves deviate only slightly from the diagram
diagonal.
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5 Experiments

5.1 Distillation Experiment

5.1.1 Preparation

· Prepare the apparatus as described in Chapter 2.3


· Prepare approx. 5 litres of test mixture:
Ethanol: approx. 20% (weight per cent),
Filler Water: approx. 80% (weight per cent)
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Determine the specific gravity of the solution


and note it
· Fill the evaporator with the test mixture
· Set the reflux ratio to zero in order to run pure
distillation
· Supply the condenser with cooling water and set
Fig. 5.1 Filling the Evaporator the flow rate to approx. 150 ... 200 l/h
· Switch on the heater at the controller
(manual mode) and select 100% power.
· Now set the valves on the reflux divider so
that collecting distillate flows off to the top
product vessel.
· Determine and note the specific gravity of the
distillate, and compare with the concentra-
tion of the initial product
· After the cooling-down time, take a sample of
the residue in the evaporator.
Determine and note the specific gravity of the
residue, and compare with the concentration
of the initial product and of the distillate.

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6 Appendix

6.1 Technical Data

Overall Unit: l x w x h: 1300 x 750 x 2100 mm


Weight: 180 kg
Power supply: 3 x 400 V / 50 Hz
Alternatives optional, see rating plate
Cooling water: 30 ... 400 ltr/h
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Sieve tray column: Ø x h: 50 x 765 mm


Material: Stainless steel
Borosilicate Glass
Number of trays 8

Packed column: Ø x h: 50 x 765 mm


Material Stainless steel
Column packing Raschig rings
Ø x h: 4 x 4 mm
Material Soda glass

Evaporator: Heating power max. 4.0 kW


Safety temperature limiter 110 °C
Capacity max. 12 ltr
Minimum fill min. 5 ltr
Cutoff volume ~ 3 ltr

Test mixture: Ethanol / Water ~ 20 : 80 %

Capacities: Top product vessel approx. 1.5 ltr


Reflux divider approx. 0.5 ltr

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6.2 Tables

Density and content of aqueous ethanol solutions


relative to water 15 °C = 1.000 (according to Windisch)
0,00

Density Weight % Vol. % g/


l
0,00 0,00 0,00 0,00
1 0 0 0
0,995 2,73 3,42 27,2
0,99 5,76 7,18 57
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0,985 9,2 11,41 90,6


0,98 13,08 16,14 128,1
0,975 17,23 21,16 167,9
0,97 21,32 26,03 206,6
0,965 25,09 30,49 241,9
0,96 28,52 34,47 273,6
0,955 31,66 38,06 302,1
0,95 34,56 41,33 328
0,945 37,28 44,35 352
0,94 39,86 47,18 374,4
0,935 42,34 49,85 395,6
0,93 44,75 52,39 415,8
0,925 47,09 54,84 435,2
0,92 49,39 57,21 454
0,915 51,65 59,5 472,2
0,91 53,88 61,73 489,9
0,905 56,09 63,91 507,1
0,9 58,27 66,03 524
0,895 60,45 68,12 540,5
0,89 62,61 70,16 556,7
0,885 64,75 72,15 572,6
0,88 66,89 74,11 588,1
0,875 69,01 76,02 603,3
0,87 71,12 77,9 618,2
0,865 73,21 79,73 632,7
0,86 75,29 81,52 646,9
0,855 77,35 83,27 660,8
0,85 79,4 84,97 674,3
0,845 81,43 86,63 687,5
0,84 83,43 88,23 700,2
0,835 85,41 89,79 712,6
0,83 87,35 91,29 724,4
0,825 89,26 92,72 735,8
0,82 91,13 94,09 746,6
0,815 92,96 95,38 756,9
0,81 94,73 96,61 766,7
0,805 96,46 97,76 775,8
0,8 98,13 98,84 784,4
0,795 99,76 99,86 792,4
0,79425 100 100 793,6

Fig. 6.1 Density of aqueous alcohol solutions

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Fig. 6.2 System Diagram

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6.3 Specimen Report Sheet

Experiment : Experiment No. :


Comments : Date :

Test mixture
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Sp. gr. of the mixture g/


ml

Concentration %

Heating power %

Top temperature T13 °C

Cooling water temp. at inlet T11 °C

Cooling water temp. at outlet T12 °C

Cooling water flow rate l/h

Reflux ratio %

Differential pressure over the column mbar

Test duration min

Amount of distillate obtained ml

Distillate density g/ml

Distillate concentration %

6 Appendix 26
DTP_4
07/2014

CE 602 DISCONTINUOUS RECTIFICATION

6.4 Items Supplied

1 System complete in steel trolley on castors


1 Sieve tray column
1 Packed column
1 Instruction manual
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 07/2014

6 Appendix 27