CHE501-V1

GROUP 2

Cebu Institute of Technology – University

Laboratory Experiment Report #7

Experiment #1
DISTILLATION

______________________________________________________________________________

Author: Jureen Flores Belicario

Fractional distillation is performed to separate a solution with boiling points close to each other
by subjecting the mixture to heating, which forces the components in the mixture to vaporize. This
experiment was done to determine the reflux ratio required to recover the ethanol of the desired
specification from the ethanol-water mixture. After performing the procedures given, the reflux
ratios were calculated. Distillation done at a steam pressure of 20 psig produced a reflux ratio of
0.11 while operating at 30 psig resulted with a higher reflux ratio of 1.06. This increase in the
reflux ratio implies that an efficient separation occurred suggesting a higher purity of the product
obtained.
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Objectives
The objective of this experiment was to determine the reflux ratio required to recover the
ethanol of the desired specification from the ethanol-water mixture.

Materials/Apparatus/ Equipment List

 Steam generation thermometer

 Pycnometer

 Ethanol

 Water

Relevant Theory/ Background Information

Distillation is a widely used method for separating mixtures based on differences in the

conditions required to change the phase of components of the mixture. To separate a mixture of

liquids, the liquid can be heated to force components, which have different boiling points, into the

gas phase. The gas is then condensed back into liquid form and collected.

Fractional distillation is used when the boiling points of the components of a mixture are

close to each other, as determined using Raoult's law. A fractionating column is used to separate

the components used a series of distillations called rectification. In fractional distillation, a mixture

is heated so vapor rises and enters the fractionating column. As the vapor cools, it condenses on

the packing material of the column. The heat of rising vapor causes this liquid to vaporize again,

moving it along the column and eventually yielding a higher purity sample of the more volatile

component of the mixture. The reflux ratio is the ratio between the boil up rate and the take-off

rate. In other words, it is the ratio between the amount of reflux that goes back down the distillation

column and the amount of reflux that is collected in the receiver (distillate).
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Procedures

Initially, all vent lines were opened. Overhead condenser cooling water supply was turned

on. The spherical vessel must be charged with 30% by weight ethanol – water up to the equator.

The by-pass around the steam trap was opened and the main steam supply was carefully but

positively turned on, as soon as the initial surge of condensate has been cleared, the steam trap by-

pass valve was closed and the steam pressure was set to a suitable figure between 20 and 50 psig.

The reflux divider for total reflux was set by closing the product off-take valve. The reboiler steam

pressure was adjusted to a value which gave adequate loading on the packed column. It should not

be less than 20 psig. The unit time to settle down after each change in the reboiler steam pressure

was given. Steam pressure for the duration of the experiment was maintained. Once the column

has settled down to uniform operation under total reflux, the drain valve on the lower product

receiver and the valve between the product receivers were closed. The vent valves on the product

receivers were re-checked and the overflow lines to the still were opened. The product line valve

by the reflux adapter was fully opened and the liquid in the adapter to drain to the still was allowed.

The recycle valve to the still was also closed and the time to half fill the upper product receiver

was measured accurately. The product line valve was closed and the level of the liquid collected

on the side of the receiver was marked. With the valve between the product receivers closed and

the product recycle valve open three-quarters, the product line valve was opened so as to give a

positive reflux ratio. The column was allowed to settle down for at least 15 minutes. The product

recycle valve was closed and the time required to half fill the upper product receiver was measured.

The product through the lower receiver was obtained as sample. The temperature and specific

gravity of the sample was measured accurately. The product recycle valve was re-opened and the

procedure along the valve between product receivers and product recycle valve was repeated with

a higher reflux ratio that was achieved by slightly closing the product line value.
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Experimental Data Analysis and Discussion

R
Steam Pressure Trial t1 t2
(reflux ratio)
1 30.1667 33.61667 0.1143635
20 psig
2 23.317 42.45 0.8205601
1 14.33 10.93 -0.2372645
30 psig
2 23.02 47.57 1.0664639
Table 1. Tabulated Results

The tabulated data above shows that at steam pressure setting of 20 psig the time it took to

fill half the product receiver at total make is about, t1, 30.17 seconds while the time it took to fill

half of the product receiver at position reflux ratio is about 33.62 seconds. The reflux ratio is

calculated using Equation 1 in Appendix A and was found to have a value of s 0.114. For the steam

pressure setting of 30 psig, the t1 is 23.02 secs. while t2 is 23.02 secs with a calculated reflux ratio

of 1.06.

Comparing the data of the two different steam pressure setting, the first run which has a

lower pressure setting (20 psig) had longer time to fill half the product receiver and also its reflux

ratio is lower than the pressure setting with a higher pressure setting (30 psig).

There was an error for the reflux ratio calculated for trial 1 operating at 30 psig since it

produced a negative value, which is physically meaningless. The method in computing for the

reflux ratio could have had limitations as they were derived from specific conditions which could

have varied with the condition during the experiment.

receiver when the product line valve was slightly closed implying a higher reflux ratio. Operating

at a steam pressure of 20 psig produced a reflux ratio of 0.82 while for operating at steam pressure

of 30 psig resulted in the reflux ratio of 1.06 which is relatively higher. The increase in the

temperature while keeping the other operating conditions constant ultimately resulted in a higher

reflux ratio. A higher value for reflux ratio reflects a higher purity for the product obtained in the

distillate, thus a more efficient operation.

References

[1] “Distillation Principle”. Retrieved from http://www.thermopedia.com/content/703/. (October

2, 2019)

[2] “Distillation”. Retrieved from https://www.thoughtco.com/what-is-distillation-601964.

(October 2, 2019).

[3] McCabe W.L. Smith J.C. and Harriott P. (1993), “Unit Operations in Chemical Engineering”,

McGraw-Hill, 5th Ed., pp. 463-494

𝟏 𝟏
−
𝑹 = 𝒕𝟏 𝒕𝟐
𝟏
𝒕𝟐

Equation 1.
R = reflux ratio
t1 = time to half fill product receiver on total make
t2 = time to half fill product receiver on position reflux ratio