EXPERIMENT NO.

16(a)
STEAM DISTILLATION SETUP

1. Aim
To study the characteristics of simple steam distillation using turpentine oil as a feed stock.

2. Objective
To determine the vaporization efficiency, thermal efficiency and percentage recovery of simple
steam distillation.

3. Theory
Steam Distillation is a term used to describe a distillation process with open steam. Steam
distillation is a method for distilling compounds which are heat-sensitive. It is specifically used
where it is desired to separate substances at a temperature lower than their normal boiling point.
The temperature of the steam is easier to control than the surface of a heating element, and allows
a high rate of heat transfer without heating at a very high temperature. The vapor mixture is cooled
and condensed, usually yielding a layer of oil and a layer of water.
Steam distillation is commonly used in the following situations:
1. To separate relatively small amounts of volatile impurity from a large amount of material
2. To separate appreciable quantities of higher-boiling materials
3. To recover high-boiling materials from small amounts of impurity that has a higher
boiling point.
4. Where the material to be distilled is thermally unstable or reacts with other components
associated with it at the boiling temperature
5. Where the material cannot be distilled by indirect heating even under low pressure
because of the high boiling temperature
6. Where direct-fired heaters cannot be used because of fire hazards
In a steam distillation process, the liquid is distilled by feeding open steam to the distillation still.
The steam carries with it vapors of volatile liquid and is then condensed to separate the liquid from
water. The essential requirement for carrying out steam distillation is:
1. Substance does not react with steam.
2. Substance is in-soluble in water (immiscible).
From the Hausbrand vapor pressure diagram for turpentine water system at 101.3 kN/m2 pressure,
obtain the distillation temperature, T D oC (≥ 95°C).
From the Hausbrand diagram, curves for turpentine and water at atmospheric pressure cross at
distillation temperature.
Distillation: Turpentine oil at 101.3 kN/m2 pressure, (1.03kg/cm²) .The intersection of the two
curves gives the distillation temperature.
 (101.3 - PB) PA

Vapour
Pressure

T Distillation Temp.

Figure 1: Plot of PA Vs T and (101.3 - PB) Vs T.

Figure 2: Hausbrand vapor-pressure diagram for turpentine oil-water system

4. Experimental Setup
4.1 Description
The apparatus consists of simple batch distillation using steam as a source of heat. The feed stock
used is turpentine oil. Distillate is collected in a separating funnel for the formation of organic
layer and an aqueous layer. Experimental Setup is shown in Fig 3.

Cooling Water In
Cooling Water Out
Condenser

Turpentine oil In

Live
Steam
Distillate
(Turpentine Oil + Water)
Residue Out
Jacket
Water In PG
Steam

Heater

Fig 3: Experimental Setup

4.2. Requirements
Steam supply, electricity, turpentine oil, demineralized water and separating funnel

5. Experimental Procedure
1. Charge the distillation still with 1L of turpentine oil.
2. Try to adjust the jacket steam pressure to 110 kN/m2 (Pg,)/1.10 kg/cm² and start the cooling
water supply to the condenser. Record the still temp. Collect the steam condensed in the
jacket.
3. When the temperature in the still reaches 2°C below the distillation temp. (T d), the jacket
steam is stopped and the flow of live steam is started through the steam sparger.

4. The live steam pressure is try to adjust around ≥75 kN/m2 (Ps) /0.75 kg/cm².
5. Weigh the steam condensed in the jacket (WS), kg.
6. Continue the distillation process for sufficient time so that about 50-70% turpentine
charged is distilled (around 30min).
7. Stop the steam supply and collect the distillate in the 1L separating funnel. Allow the
formation of organic layer and an aqueous layer. Separate the two phases and weigh them,
(WAD, WBD), kg.
8. Collect the residue, separate the two layers and weigh WAB, WBB (kg).
9. Stop the water supply to the condenser.
6. Observations and Calculation

Mol. Wt. of turpentine oil MA =136.22

Normal boiling point of turpentine oil = 160oC (@ 1 atm)
Sp. heat of turpentine oil at 20°C = CpA = 1.8 kJ/kg °C
Sp. heat of turpentine oil at 50°C = CpA =1.926 kJ/kg °C
Sp. heat of turpentine oil at 100°C = CpA = 2.093 kJ/kg °C
Latent heat of vaporization of turpentine oil, A = 74 kcal/kg = 309.84 kJ/kg
Mol. wt. of Water = MB = 18
Thermal volume expansion coefficient of turpentine = 0.001/K
System Pressure, P = 101.3 KN/m2 /1.03kg/cm²
Wt. of turpentine (feed) = 1L * density of turpentine oil.

Distillation temp., TD = …… °C
Wt. of Steam Condensed in jacket = WS, kg
Steam pressure in the jacket, Pg = 110 KN/m2
Pressure of live steam, PS = 75 KN/m2
Steam pressure in the jacket = 112 kg/m2 = Pg
Live pressure in the still = 76 kg/m2 = Ps

Mass of steam condensed during pre-heating (feed change from initial tem to ….oC) WS =
Distillation time = min
Initial temperature of feed charge, T R = °C
Observed distillation temp., = °C

Distillate readings (Turpentine oil + water):

Wt. of turpentine oil in distillate WAD =
Wt. of water in distillate WBD=

Residue collected (Turpentine oil + water):

Wt. of turpentine oil in residue WAB =
Wt. of water in residue WBB =
Ambient temperature Tr = …..
Distillation time = 25 min approximately
Observed distillation temperature =

Converting Weights to moles:

No. of moles of turpentine oil in feed

WAF
NAF = ---------- =
MA
No. of moles of turpentine oil in distillate
WAD
NAD = ---------- =
MA
No. of moles of turpentine oil in Residue
WAB
NAF = ----------- =
MA
No. of moles of water in distillate
WBD
NBD = ------------ =
MB
No. of moles of water in residue
WBB
NBB = ---------- =
MB

Applying Material balance for turpentine oil,

NAF = NAD + NAB + NL

Losses from the still turpentine oil, NL = ……………

Steam Distillation Temp, TD =…………..

PAO= Partial Pressure of turpentine oil during distillation = P (system pressure) [NAD/ (NAD + NBD)]
Where P =total pressure = 101.3 KN/m2

 Vaporization efficiency =

PAº
 = --------- =
PA

WBD (P -  PA) MB NBD × MB

And ---------- = ----------------x ---------- = ---------- =
WAD  PA MA NAD × MA

Where PA is the pressure of turpentine oil and water system at TD°C from Hausbrand diagram.

WBD / WAD in distillate = ……

% Recovery =

Calculation of Thermal efficiency:

 Total heat output (Qo)
T = --------------------------------- x 100
Total heat input (Qi)

Heat Output:
QO = WAF (TD – TR) CpA + A WAD = WS + A WAD = ……..
TR = Feed initial temperature
TD = distillation temp. =……oC

Heat Input: Qi
Qi = Heat given by condensing steam in the jacket + Heat given by the condensing live steam
during distillation.

Qi = WSJ + (WBD + WBB) [S + Cp (TS – TD)] = ………

Jacket steam pressure = PJ (KN/m2)

J =latent heat of vaporization of steam corresponding to pressure PJ, kJ/kg (using steam
table)
PS = Pressure of live steam, KN/m2
TS = saturation temp. of steam at PS, °C corresponding to PS, kJ/kg (using steam table)
Cp = Specific heat of steam, kJ/kg°C.
PJ = 110 KN/m2
J = 2216 kJ/kg (Please check this value using steam table if pressure change)
PS = 75.95 KN/m2
S = 2230 kJ/kg (Please check this value using steam table if pressure change)
Cp = Sp. heat of steam = 2.0 kJ/kgoK

NOMENCLATURE
WAF = Wt. of turpentine in feed (kg)
TD = Distillation temp. °C
TR = Reference temp. (Ambient temp) °C
Cp = Specific heat of turpentine oil (kJ/kgoC)
A = Latent heat of evaporation of turpentine (kJ/kg)
WAD = Wt. of turpentine in distillate, (kg)
WS = Wt. of Steam Condensed in the jacket during pre-heating or charge (kg)
 = Latent heat of steam corresponding to jacket steam pressure P (kN/m2)
WBD = Wt. of water in distillate (kg)
WBB = Wt. of water in residue, kg
S = Latent heat of steam at live steam pressure P S (kN/m2)
TS = saturation temperature of steam at PS
Cp = Specific heat of steam (kJ/kgoC)
7. Results

Vaporization efficiency=
Recovery=
Thermal efficiency=

8. Discussion:

9. Conclusion

References
1. McCabe, W.L., Smith, J.C., Harriott, P., “Unit Operations of Chemical Engineering”,
7th ed.McGraw Hill, NY, 2005.
2. Coulson, J.M., Richardson, J.F., “Coulson & Richardson’s Chemical Engineering Vol.
- 1”, 5th ed., Asian Books ltd., ND, 1996.
3. Treybal, R.E., “Mass Transfer Operations”, 3rd ed., McGraw Hill, NY, 1981.
4. “Principles of Mass Transfer and Separation Process” by B.K.Dutta, 3rd ed, 2009
(Pages – 350-353).