4.Thiết bị cô đặc màng
4.Thiết bị cô đặc màng
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Didacta Italia
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I TA114D
I Thin Layer Evaporator/Concentrator
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I' User's Manual 'j
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I TAl14D
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User's Manual
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and Exercise Guide
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I This manual illustrates the technical characteristics and operating instructions of
the system Didacta TA114D Thin Layer Evaporator/Concentrator, giving the
I instructor or the student a specific knowledge of the unit and its applications.
Besides the manual contains a choice of exercises ready to be performed in the
laboratory.
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I Didacta Italia Sri - Strada del Cascinotto, 139/30 - 10156 Torino
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The information contained in this manual has been selected and verified with the I
greatest care. However, no responsibilitystemming from its use can be ascribed to the
Authors or to Didacta Italia or any person or company involved in its preparation.
The information contained in this manual can be modified at any time and without
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warning on account of technical or educational needs.
table of contents
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I Table of Contents
I 1. General ································
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I 3.1 Preliminarychecks
3.2 Pre-settingthe system
· ·· ··15
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I 3.3 Start-up
3.4 Configuring the operating scheme
· 15
· 16
I 4. Exercises 21
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O!lO~1OPOPIO IA
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I s.J.U9~UOO ~O 9IQO-l-
I Chapter 1.
I 1. General
I The evaporation system has been conceived to perform the concentration of cosmetic
(IC16D) and alimentary products (TA1l4D), such as milk and fruit juice, as well as the
production of sugary solutions or purees in general (e.g. tomato puree).
I Such products are concentrated through the evaporation of the solvent (water) and
hence, in order to preserve the organoleptic and/or nutritional value of the products, the
The experiments that can be performed with the system concern both discontinuous
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I TAl14/IC16D - User's Manual
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I 2. Theoretical background
Since the volume of the container is limited, the molecules at the gaseous state exert
I a pressure on the space available to them, which will change some of the gas molecules
back into a liquid. This results in a sort of dynamic balance (which varies with
I temperature) in which the number of molecules leaving the liquid and changing into a
gas is the same as the number of molecules changing back from gas to liquid.
I The vapour tension of a liquid is the value taken on by the pressure when the
dynamic balance has been reached (this balance is achieved very quickly).
I The vapour tension increases with temperature at a higher than proportional rate.
p Vapour tension
I of the solvant
Vapour tension
of the solution
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Fig. 2.1 - Curves reflecting vapour tensions in a p-t diagram
I If you place a liquid in a container in which an inert gas, insoluble in the liquid,
applies a pressure Pg' the passage of some of the molecules of the liquid to the gaseous
I stage would take place all the same until vapour reached the same partial pressure p as it
would reach in an empty container. In this case, the dynamic balance is achieved more
slowly because the average velocity of the vapour molecules is reduced due to the
I collisions with the molecules of the inert gas, and the final pressure P g + q will be
reached only when the vapour is evenly distributed in the inert gas.
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Theoretical background
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When the vapour tension of the liquid exceeds the atmospheric pressure P a, the
vapour needs not spread in the air to move away: it pushes off the layer of air and the
evaporation becomes fast and tumultuous (boiling).
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Dalton's law
Two or more gases in a mixture exert a combined pressure that corresponds to the
sum of the pressures that each gas would exert if it occupied the same volume by itself.
Denoting with PI, P2, P3....... Pn (partial pressures) the pressures that the individual
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Amagat's law
In a mixture of two or more gasses, the volume (total volume) taken up by the gases
at a pressure p corresponds to the sum of the volumes (partial volumes) that each of
them would occupy by itself at the same pressure p, that is:
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Note
The number of alcohol moles will be 92 =2 , while the number of benzene moles
46
will be 90S = 11,64.
7S
4 Didacta Italia I
I Chapter 2.
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I The molar fraction of the solvent is:
= 0.849
I 11,64
2+11,64
I PI = XI p?;
P2 = X2 p~ = (1- XI ) p~
I P = PI + P2
I Since in the solutions of practical interest, the vapour tension of the solute (generally
a salt or some other solid substance) is negligible compared to the vapour tension of the
"In a solution in which the solute has a negligible vapour tension, total vapour
I tension p corresponds to the vapour tension of the pure solvent p~ multiplied by its
molar fraction.
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where IIp is referred to as relative reduction in vapour tension, and Xl is the solute's
I P2
molar fraction. "It may therefore be stated that the relative reduction in the vapour
tension of a solution (containing a non volatile solute) corresponds to the molar fraction
I of the solute".
A major practical consequence of Raoult's law is the fact that solutions containing a
I mole of any solute in the same amount by weight as a given solvent, having the same
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Theoretical background
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molar fractions and causing the same decrease in vapour tension, will undergo the same
increase in boiling point.
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2.2 Raise in the boiling point
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The increase in the boiling point caused by a mole of any solvent in 1000 gr. of a
given solvent is referred to as the molal ebullioscopic constant keb of that particular
solvent (and it is a specific characteristic of that solvent).
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DC
Substance
Water
Formula
H2O
keb
0,515
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Acetic acid CH3COOH 3,07 1
2,57
Benzol
Nitrobenzol C6HSN02
C6~
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Bromoform CHBr3 - 1
Acetone
Ethyl alcohol
CH3-CO-CH3
C2HsOH
1,73
1,20
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The boiling temperature is the temperature at which the vapour tension of a liquid
reaches the atmospheric pressure. Accordingly, it is higher in the solution than in the
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pure solvent, and the difference depends on the concentration of the solute.
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The relationship between the molar fraction and the variation in boiling point can be
used to obtain the MW of the solute.
/).t : k eb = C :1
where M = increase in the boiling point, i.e., difference between the boiling point of
the solution and that of the pure solvent at the same pressure;
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keb = molal ebullioscopic constant;
c = molality;
6 Didacta Italia 1
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I Chapter 2.
I c=----
a 1000
I M b
so that
I !1t _ a 1000'1
I keb - M -b-'
I M = keb . a ·1000
!1T ·b
I Molecular weight corresponds to the theoretical value only if the substances being
considered do not undergo association or dissociation processes in the solution,
I "If the substances in a solution undergo an association process, the increase in the
boiling point will be smaller; if they undergo a dissociation process, the increase in the
DUhring's diagram
I It should be noted that, for most solutions, the raise in the boiling point is a function
of their constituents and concentration, while it is virtually unaffected by pressure
I (though the boiling point of a solution does depend on pressure). Duhring identified this
property in 1878. It makes it possible to represent in a simple manner the relationship
between the concentration and the boiling point of a solution, on the basis of a limited
I number of test results.
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I TA114jlC16D - User's Manual 7
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Theoretical background
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In this diagram, the zero concentration line is a straight line at a 45° slant passing
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through the origin, and the lines relating to the other concentrations are straight lines
running parallel to the latter. This applies to ideal systems; if a system is not an ideal one
(i.e., the solution is not diluted and the solute undergoes a process of ionisation or
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complex formation), Duhring's lines are no longer parallel.
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8 Didacta Italia
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I Chapter 2.
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Theoretical background
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a) diaphragm type dry mixture condenser;
A product distribution ring placed around the rotor, at the level of the product inlet, 1
spreads the material evenly onto the inner surface, so as to create a film on the heat
exchange surface.
By gravity, the product moves down along a spiral path, and the film is maintained in
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conditions of great turbulence by the movement of the blades fitted to the rotor.
Furthermore, the cool surfaces of the blades in the proximity of the heat exchange
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wall protect the products against local heat peaks. The vapour passes through a
separation surface, mounted above the inlet, which stops any drops as may form and
returns them to the Thermal Treatment zone. The vapour leaves the machine through a
large-sized tube located in the upper part of the concentrator, whilst the liquid that has
undergone the treatment is discharged via a cone shaped nozzle located in the bottom
part of the machine.
The reason why film concentrators are able to treat highly viscous liquids, liquids
containing suspended particles or highly volatile liquids (entailing the risk of an
insufficient feed rate) is the presence of the mechanical stirrer which maintains the film
of material uniform. This determines the formation of a liquid-gas surface much more
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complex than in traditional evaporators.
On the opposite side of the blades, a zone of great turbulence is formed, where the
liquid takes on the shape of a vortex. Internal friction neutralises the turbulence in the
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10 Didacta Italia 1
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I Chapter 2.
vortices and a zone of calm is formed between the vortex and the wave created by the
I next blade. In addition to ensuring a good heat exchange coefficient, the turbulence
fosters the phenomenon of mass transfer, of special significance when the diffusion of
the liquid to be treated represents a limiting factor.
I In many applications it is more important to obtain low temperatures at the wall
(thanks to high heat exchange rates) rather than high heat exchange coefficients. With
I temperature differences of 80° to 100°C between the liquid and the heating fluid, the
temperature of the product on the wall generally is 10° to 20°C higher than the boiling
temperature of the liquid.
I Time through the reactor is also a key factor. Since the product flows along the
heating surface uninterruptedly, this time is determined by product viscosity and feed
I rate, and the rate of evaporation will be determined by the transfer of heat to the product
during the time it takes the film to reach the discharge outlet.
I Equipment
A Evaporator
I 1 Displacement pump
I 4-5-6 Tanks: for their intended use, see the Operating diagrams
7 Condenser
I 8-9-3 Measuring systems
I Steam line
11 By-pass valve
I 10 ON-OFF control solenoid valve
I 13 Condensate discharge
12 Discharge valve
I 31 Control valve
I 45 Condensate refrigerator
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Theoretical background
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43 Condensed vapour measuring valves
14 ON-OFF valve
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21 ON-OFF valve I
15 Return to tank 4 valve
27 By-pass valve
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25 Condenser ON-OFF valve I
29 Cooling circuit ON-OFF valve
28 Flow window
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30 Overflow ON-OFF valve
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I Chapter 2.
Vacuum line
I 36 Vacuum breaking valves
I 35 ON-OFF valve
I Lubricant line
Temperatures
I TI H20 at condenser inlet
I T4 Vapour inlet
I T5 Condensate outlet
I p2 Evaporated portion
I Levels
I LI Feed tank
L2 Concentrate tank
I L3 Condensate tank
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I Chapter 3.
I 3. 1 Preliminary checks
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Close all valves.
I • Check the connections and the availability of the distribution networks (water,
electric energy, steam).
I • Fill up the feed tank with the solution to be concentrated (e.g. a mixture of milk
(5-20%) and water).
I • Fill up the bush lubricant tank with the solution to be concentrated or with the
principal solvent (according to the foregoing example: water).
I • Pre-set the liquid line (solution feed line and concentrate discharge line)
according to the desired scheme (see 3.4).
I • Adjust the feed and extraction pumps according to the desired flowrate (e.g.
50% of maximum flowrate).
I • Close the main switch of the electric panel by means of the relative key.
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Open valve 38 and start the rotor inside the evaporator.
Adjust rotation speed at the desired value (for instance 1000 rpm).
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Starting the system
• Open the heating steam feed line (by turning on the boiler, when fitted).
• Wait a few minutes until the system reaches its operating temperature.
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• Start the heating and cooling fluid flowrate control systems.
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Start the vacuum pump.
Adjust system pressure by means of valve 32 at the desired value (e.g. 0.2 bar
vacuum).
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• Wait a few minutes until the system reaches its operating conditions.
The tables that follow show the uses of the different tanks and the positions of the
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valves during the various stages. A legend explaining the meaning of the tables is
provided before the tables.
The figures show the paths of the liquids (feed and concentrate) for the different
operating schemes.
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I Fig. 3.2 - Pre-setting the circuit for recirculation.
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I Fig. 3.3 - Pre-setting the circuit for product concentration in several stages.
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I TAl14/IC16D - User's Manual 17
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Starting the system
Fig. 3.4 - Pre-setting the circuit to transfer the product from the collection tank to the feed
tank (when you wish to the use the same product for several exercises).
Feed
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• Open valve 23.
• Measure the time it takes for the graduated cylinder to be emptied from an initial
reference notch to a final notch; the distance between these notches must be
sufficient to ensure that it takes at least 30 seconds.
Extraction
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• Measure the time it takes for graduated cylinder 8 to be filled partly from an
initial reference notch to a final notch; the distance between these notches must
be sufficient to ensure that it takes at least 30 seconds.
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notches corresponds to 0.05 It.
18 Didacta Italia
I Chapter 3.
Condensate
I Open valve 33.
I Measure the time it takes for the barrel to fill partly from the initial reference
notch to a final notch; the distance between the notches must be sufficient to
ensure that it takes at least 2 minutes (new barrel: 30 seconds).
I Evaluate flowrate keeping in mind that a distance of one centimetre between the
Example
I Difference between the notches: 10 em.
I Time: 36.18 s
I Thermostats TIC1 and TIC2 can be adjusted by means of the keys situated to the side
of the display.
I The key on the bottom left makes it possible to start the setting stage of the reference
value (set-point). Having pressed the key, wait a few seconds.
I With the left keys you can increase (upper key) or reduce (lower key) the set-points.
At the end of this operation, having reached the desired value, the upper right key
I makes it possible to transmit the value to the controller.
The value set is transmitted anyway if it is not changed for ca 15-20 seconds.
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3.7 Maintenance
I At the end of the tests, it is necessary to wash the equipment through the following
procedure:
I • Open the 3-way valves, 47 and 48
I • Wash the system with H20 entering through valve 48 and leaving the system via
valve 4 (back current - with H20 and specific products).
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starting the system
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• Empty out tanks 4 and 5;
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• To improve the efficiency of the washing process, start the motor and introduce
steam so as to raise the temperature of the wash liquid (e.g. 65°C);
Work with the valves so that all the pipes and tanks are reached by the wash
liquid.
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For long periods of inactivity, empty out the system and wash it thoroughly.
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I Chapter 4.
I 4. Exercises
I Introduction
This paragraph describes a number of basic exercises; all examples use a solution of
I milk and water (at 5%): these are low-cost substances that can be easily found and make
it possible to perform valuable learning experiences.
I However, it is possible to work with other solutions, whether containing fats, proteins
or sugars: for instance, you can use undiluted milk, fruit juice (not too pasty, as this
would make the cleaning process too time consuming). For each solution you must
I assess the ideal pressure for the concentration tests (the value of pressure depends on the
purposes for which a test is conducted).
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I TA 114/IC16D - User's Manual 21
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Exercises
• Adjust the extraction rate at the same percentage of the maximum flowrate
permitted by the feed pump;
The table below gives a set of values obtained from a test; these values depend on
many parameters and therefore must not be rated as binding.
time [min] 0 15 30 45 60
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I Chapter 4.
5 25 45 65 average
I time [min]
[I/h] 10 9 12 11 10.3
I Qcon
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R = Qeon • ~ = 10.0·~ = 0.444 leone
v, 60 Isol
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Determination of evaporation efficiency from the global balance of integral values:
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I TAl14/IC16D - User's Manual 23
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Exercises
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4.2 Exercise 2 -Inverse continuous concentration at constant
operating conditions 1
Prepare 60 It. of a 5% solution of milk in tap water;
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11 6 OI 8 [lIII] U030 I
=o
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Adjust vacuum at 0.75 bar;
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Didacta Italia
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I Chapter 4.
I • Adjust the extraction rate at the same percentage of the maximum flowrate
permitted by the feed pump;
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Exercises
Adjust the extraction rate at the same percentage of the maximum flowrate
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I permitted by the feed pump;
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Exercises
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• Turn off the feed and extraction pumps;
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Exercises
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• Tum off the feed and extraction pumps;
• Adjust the extraction rate at the same percentage of the maximum flowrate
I permitted by the feed pump;
I • Change the operating mode from direct continuous to inverse continuous mode;
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I TA 114/IC16D - User's Manual 33
Exercises
The table below gives a set of values obtained from a test; these figures depend on
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many parameters and hence should not be rated as binding.
T4 [DC] 127.1 111.6 116.7 120.5 114.0 132.8 112.2 112.8 120.2 111.2 113.4
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T5 [DC] 73.8 96.4 97.6 98.2 97.7 97.5 97.7 97.7 97.5 97.6 97.2
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T6 [DC] 68.6 66.7 66.9 66.0 66.3 60.6 66.2 65.7 67.2 65.4 65.2
TIC2 [DC] 40.9 35.5 32.4 29.5 30.4 28.3 31.2 31.2 32.0 33.4 32.0 I
time [min] 5 25 45 65 85 105 125 160 average
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<lin [IIh] 61 63 62 60 63 61 60 62 61.5 I
[IIh] 46 52 50 51 53 54 52 51 51.1
Qout
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34 Didacta Italia
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I Chapter 4.
I •
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Prepare 60 It. of the solution whose pressure curve has to be determined;
I The temperature values determined at each stationary stage must be entered in a table
which gives, in each line: a value of pressure, a value of temperature T5 and a value of
temperature T2.
I Temperature T2 represents the value of the boiling temperature of the liquid going
out (at a higher degree of concentration of the liquid coming in). Temperature T5
I represents the temperature of the vapour in conditions of dynamic balance with the
liquid leaving the equipment. The difference between these two temperatures represents
the raising of the boiling point of the solution. The values of the temperatures and their
I difference can also be presented in a chart providing a good description of the state
diagram for the solution in question.
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