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Autumn Semester (2023-2024) Food Engineering Lab:01 8/1/2023

Aim
To study Boiling point elevation of solvent and different solution using rotary evaporator

Objectives
1. To determine pressure-temperature relation for solvent and different solution.
2. To determine relationship between P v/s T, ln(P) v/s 1/T, ∆H v/s T and ln(P) v/s
∆H/T by graphical interpretation.

Agricultural and Food Engineering Department


Indian Institute of Technology, Kharagpur
8/1/2023
1. Introduction
• Evaporation, a widely used method for the concentration of aqueous solutions, involves the removal of
water from a solution by boiling the liquor in a suitable vessel.
• Evaporation is achieved by adding heat to the solution to vaporize the solvent. The heat is supplied
principally to provide the latent heat of vaporization.
• Removal of water from food augments its microbial stability with assistance in reduction of storage and
transportation cost.

Evaporation v/s Drying Evaporation v/s Distillation

Distillation is the removal of vapors and their


fractional product. Moreover distillation is a
Evaporation is the removal of solvent to separation process. Evaporation is the removal
obtain concentrated liquor, employed for of solvent to obtain concentrated liquor the
liquid product. Whereas, drying is removal of vapors removed are not of particular use.
water from solid/ semisolid food. Evaporation is not separation process.
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Agricultural and Food Engineering Department Indian Institute of Technology, Kharagpur
Use of evaporation in Food process engineering 8/1/2023

1. Used in dairy and fruit juice 2. Used in Sugar refineries 3. Used for concentration of bioactive/
processing industries for nutraceutical food solutions
concentration

2. Theory
• For heat sensitive products it is required to work at lower
temperatures, so the evaporation is supplemented with vacuum
application that results in increased heat flux.
• The removal of water from liquid results in its concentration, the
boiling point of the liquid increases resulting in smaller
difference between the heating medium and product, which
reduces the rate of heat transfer.
• Boiling Point Rise (BPR): It is defined as the increase in the
boiling point of the solution over that of pure water under a
given pressure.
Fig. 1: Boiling point of solutions of sodium chloride as a
• D¨uhring’s line is often used to estimate the boiling point of function of the boiling point of water. D¨uhring lines

solution with respect to pure water at particular pressure. Source: Coulson Richardson’s Chemical Engineering Design Vol-02. 3
Agricultural and Food Engineering Department Indian Institute of Technology, Kharagpur
Theory 8/1/2023

The equipment used in this experiment is a rotary


evaporator that works on the principle of Carnot cycle

WTotal
Temperature Thigh Temperature Tlow

(1-2) (2-3) (3-4) (4-1)


Fig. 3: Schematic diagram of Carnot process
Fig. 2: P-V diagram of Carnot cycle
Process (1-2): Reversible-isothermal expansion:- The ideal gas is placed in thermal contact with a heat
reservoir at a temperature Thigh. The gas absorbs heat qin from the heat reservoir and is allowed to expand
isothermally. Because the internal energy E of an ideal gas is a function of the temperature only, the change of
the internal energy is zero, i.e. ΔE=0 during this isothermal expansion.
So, qin = W1-2 2
V 
qh = W1− 2 =  P.dV = nRT2 ln  2  Eq.1
1  V1 
Agricultural and Food Engineering Department Indian Institute of Technology, Kharagpur
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Process (2-3): Reversible-adiabatic expansion:- The gas is thermally isolated and allowed to expand 8/1/2023

further. Because this expansion is adiabatic, the temperature of the gas falls—in this case, from T2 to T3.
Since the process is adiabatic q=0. Therefore, W2-3 = ΔE
PV  = C
nRT2 nR(T2 − T3 )
2 2 = nRT2  P2 =
PV W2−3 =
V2  −1
T2V2 −1 = T3V3 −1 Eq.2

Process (3-4): Reversible isothermal compression:- The gas is placed in thermal contact with a cold reservoir at
temperature Tlow and compressed isothermally. During this process, work (W3-4) is done on the gas and it gives up
heat qc to the cold reservoir. 4
V 
qc = W3− 4 = −  P.dV = nRT3 ln  3  Eq.3
3  V4 
Process (3-4): Reversible adiabatic compression:- The gas is thermally isolated and returned to its initial state by
compression. In this process, work W4-1 is done on the gas. Because the compression is adiabatic, the temperature
of the gas rises from T4 to T1 in this particular case. q=0.
PV  = C nR(T4 − T1 )
W4−1 =
T4V4 −1 = TV
1 1
 −1 Eq.4
 −1
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Agricultural and Food Engineering Department Indian Institute of Technology, Kharagpur
8/1/2023
We get,
Since, we know T1= T2=Thigh; T3= T4= Tlow
 V2  Thigh
qh = nRThigh ln   = qc
 −1  −1  V1  Tlow
(T V
So, from Eq.2 2 2 = T V
3 3 )

 −1  −1 WTotal = qh − qc
& Eq.4 (T4V4 = TV
1 1 )
qh Thigh
T2 T1 =
= qc Tlow
T3 T4
WTotal qh − qc qc

V3 V4
= carnot = = 1−
V2 V1 qh qh qh
V3 V2 Tlow dT dW
 =
V4 V1  = 1 − = =
Thigh T q Eq.5
Substituting these values in Eq.1 and Eq.3
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Agricultural and Food Engineering Department Indian Institute of Technology, Kharagpur
8/1/2023
From 1st Law of thermodynamics
q = W + E
or , q − W = E Eq.6

Tlow dT dW
From Eq.5, we get  = 1− = =
Thigh T q
dW
q = T
dT

So, the Eq.6 can be rewritten as, T dW − W = E


dT
dW
T = E + W
dT
H Latent heat of vaporization
dW
T = H Eq.7
dT
Gibbs–Helmholtz equation
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Agricultural and Food Engineering Department Indian Institute of Technology, Kharagpur
8/1/2023

Since, dP HM w dT
=  2
P R T
Integrating both sides,

dP HM w
P2 T2
dT

P1
P
=
R
 2
T1
T
For an ideal gas
 P2  HM w  1 1 
W = P.VV ln   =  − 
 P1  R  T1 T2 
dW dP
= .VV  P2 − P1  HM w  1 1 
dT dT ln 1 + =  − 
RT  P1  R  T1 T2 
From Eq.7 and putting value VV =
M wP
ln(1 + e)
dW H dP  RT 
= = . 
dT T dT  M w P 
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Agricultural and Food Engineering Department Indian Institute of Technology, Kharagpur
8/1/2023

From Taylor series expansion and neglecting higher


terms
 ln(1 + e) = e

P2 − P1 HM w 1 1 
=  −  Eq.7
P1 R  T1 T2 
Clausius–Clapeyron relation

P1 − P2 HM w 1 1
=  − 
P1 R  T2 T1 
For, dilute solution T2  T1 and T = T1 − T2

P1 − P2 dP HM w T Eq.8
= =
P1 P RT2 2
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Agricultural and Food Engineering Department Indian Institute of Technology, Kharagpur
8/1/2023
Raoult’s Law: A solution of volatile liquids, the partial vapor pressure of each component of the solution is
directly proportional to its mole fraction present in the solution.
ms
P1 = Pw0 Ms
xs =
P2 = xw .P 0
w
ms mw
+
xw + xs = 1 Ms Mw

 P2 = (1 − xs ) Pw0
 P1 − P2 = xs .Pw0 ms
Ms
P1 − P2 xs =
 0
= xs mw
Pw
Mw
P1 − P2
 = xs Eq.9 ms  M w P1 − P2 dP
P1  xs = = = Eq.10
mw  M s P1 P
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Agricultural and Food Engineering Department Indian Institute of Technology, Kharagpur
8/1/2023
From Eq.8 and Eq.10
ms  M w P1 − P2 HM w T
xs = = =
mw  M s P1 RT2 2 400

Absolute Pressure (kPa)


ms  M w HM w T
 = 300
mw  M s RT2 2
RT22 ms 1
 T =   Eq.11 200 Series1
Distilled water
H mw M s
Series2
Sugar solution
100
So, T = Boiling point rise (BPR) Series3
Salt solution
T1 T2 T3
1
BPR = T  0
323 338 348 358
Ms
Temperaure (K)
1
BPR  Fig.04: Absolute pressure and temperature curve for
various solutions
Molecular mass of solute

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Agricultural and Food Engineering Department Indian Institute of Technology, Kharagpur
7 8/1/2023
2400
6
5

∆H(kJ/kg)
2350
4
ln(P)
Distilled water
Series1
3 Sugar solution
Series2 2300
2
Series3
Salt solution
1
2250
0
320 330 340 350 360
0.0027 0.00285 0.003 0.00315
1/T(K-1) Tempetarure (K)
Fig.05: ln(P) and (1/temperature) curve for various solutions Fig.06: ∆H and temperature curve

7
6
5
4
ln(P)

Series1
Distilled water
3
water
Sugar solution
Series2
2
1 Series3
Salt solution
Fig.07: ln(P) and (∆H/temperature)
curve for various solutions 0
6 6.5 7 7.5
∆H/T(kJ/kg-K) 12
Agricultural and Food Engineering Department Indian Institute of Technology, Kharagpur
8/1/2023
3. Materials and methods
A. Equipment required
1. Rotary Evaporator (Make: Buchi; Model: R-215)
2. Vacuum pump
3. Water chiller
B. Instruments required
1. Manometer
2. Thermocouple
3. Temperature indicator
C. Solutions required
1. Distilled water
2. 10%(%w/w) Sugar solution
3. 10%(%w/w) Salt solution
D. Data analysis are representation
1.MS-Excel
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Agricultural and Food Engineering Department Indian Institute of Technology, Kharagpur
4. Experimental setup and experimentation Pressure gauge
8/1/2023

Cold water out

Vacuum pump

Cold water in
Round bottom flask

Condensate
flask Water bath
(Temperature controlled)
Temperature
measurement

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Agricultural and Food Engineering Department Indian Institute of Technology, Kharagpur
5.Results: Observation tables and graphs: 8/1/2023
1. Distilled water
Vacuum pressure Absolute Pressure
∆H(kJ/kg)
Temperature (°C) (mm Hg) (kPa) Temperature(K) 1/T(K-1) ∆H/T(kJ/kg-K) ln(P)
50 2382.7
65 2346.2
75 2321.4
85 2296
2. Sugar solution
Vacuum pressure Absolute Pressure
∆H(kJ/kg)
Temperature (°C) (mm Hg) (kPa) Temperature(K) 1/T(K-1) ∆H/T(kJ/kg-K) ln(P)
50 2382.7
65 2346.2
75 2321.4
85 2296
3. Salt solution
Vacuum pressure Absolute Pressure
∆H(kJ/kg)
Temperature (°C) (mm Hg) (kPa) Temperature(K) 1/T(K-1) ∆H/T(kJ/kg-K) ln(P)
50 2382.7
65 2346.2
75 2321.4
85 2296
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Agricultural and Food Engineering Department Indian Institute of Technology, Kharagpur
8/1/2023
7
1. 400 2.

Absolute Pressure (kPa)


6
300 5
4

ln(P)
200 Series1
Series1
3
100 Series2 Series2
Series3 2
Series3
0 1
323 338 348 358 0
Temperaure (K) 0.0027 0.00285 0.003 0.00315
3. 1/T(K-1)
2400
4. 8
∆H(kJ/kg)

2350 6

ln(P)
4 Series1
Distilled water
2300
2 water
Series2
Sugar
solution
Salt solution
Series3
2250 0
320 330 340 350 360 6 6.5 7 7.5
Tempetarure (K) ∆H/T(kJ/kg-K)
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Agricultural and Food Engineering Department Indian Institute of Technology, Kharagpur
8/1/2023

Things to be instituted in the lab record


1. Aim and objectives of the experiment
2. Materials required
3. Theoretical background
4. Schematic sketch of the rotary evaporator
5. Experimental procedure
6. Observation table
7. Results
• Graphs between P v/s T, ln(P) v/s 1/T, ∆H v/s T and ln(P) v/s ∆H/T with
distinct units and clear markings.
8. Discussion
9. Conclusion
Thank you
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Agricultural and Food Engineering Department Indian Institute of Technology, Kharagpur

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