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09/22/2020

Chem-343-06
TA: Sarah Metzger

Fermentation and Distillation of Ethanol

Objective: The goal of this experiment is to learn simple distillation and fractional distillation.

The outcome of this experiment will be the formation of ethanol in the fermentation process that

will be tested with both simple and fractional distillation.

Procedure:

1. 20 g of sucrose and 1.5 g of yeast was weighed out and placed into a 250 mL round-

bottom flask.

2. 100 mL of DI water was added to the round-bottom flask to dissolve all sugar.

3. Roughly 17-18mL of Pasteur’s salt solution was added to round-bottom flask and swirled

to mix.

4. The flask was then capped and with a greased glass vacuum adapter that had rubber

tubbing attached.

5. Round bottom flask was placed in a cushioned beaker

6. The rubber tubing was then inserted into a halfway filled test tube of limewater that sat in

a separate beaker

7. Fermentation setup was then complete and left undisturbed in a sunny corner of the lab

for a week.

8. After a week had passed the distillation solution was prepared

a. Roughly 1 tbs. of celite was added to a beaker and dissolved with 100mL of DI

water

b. The dissolved celite was stirred vigorously and poured onto filter paper in a

Büchner funnel while vacuum was on


09/22/2020
Chem-343-06
TA: Sarah Metzger

c. The water that was vacuumed was discarded and dried

d. Once only a thin layer of celite remained on the filter paper the ethanol solution in

round bottom flask was decanted into the funnel with the celite layer

Simple Distillation

1. 90 mL of the filtered ethanol solution was poured into a 250 mL round bottom flask with

2-3 boiling chips

2. The simple distillation was then set-up with greased joints and clamped at joints

a. The round-bottom flask is placed in a heating element. The round bottom flask

was then connected to the three-way adapter. The three-way adapter was then

connected to thermometer with adapter connected at top joint and a condensing

column was connected at the side joint. The other end of the condensing column

was then connected to a vacuum adapter which would drip into a graduated

cylinder below. The water inlet and outlet tubes were connected to the condensing

column.
09/22/2020
Chem-343-06
TA: Sarah Metzger

3. The ethanol solution was heated from room temperature until it began dripping at a rate

of 1-2 drops/sec.

4. Weigh 1mLof distillate in a clean tarred beaker to get density

5. The temperature was recorded every 0.5-1mL of distillate within for a total 20 mL or till

temperature has held from 96-100℃ range for 5 minutes.

Fractional Distillation

1. 90 mL of the filtered ethanol solution was poured into a 250 mL round bottom flask with

2-3 boiling chips

2. The simple distillation was then set-up with greased joints and clamped at joints

a. The round-bottom flask is placed in a heating mantle. The round bottom flask was

then connected to a fractioning column that was filled roughly halfway with glass

beads. The fractioning column was then connected to the three-way adapter. The

three-way adapter was then connected to thermometer with adapter connected at


09/22/2020
Chem-343-06
TA: Sarah Metzger

top joint and a condensing column was connected at the side joint. The other end

of the condensing column was then connected to a vacuum adapter which would

drip into a graduated cylinder below. The water inlet and outlet tubes were

connected to the condensing column.

3. Collect distillate from 77-80℃

4. Collect distillate from 80-96℃ in a new graduated column

5. Collect distillate from 96-100℃ in a new graduated cylinder for 2-3 mL

6. When collecting the fractions record the temperature at every 0.5-1mL

7. Determine density for each fraction collected by weighing 1 mL in a clean tarred beaker

for density measurements

Observations:
09/22/2020
Chem-343-06
TA: Sarah Metzger

During the fractional distillation condensation was seen in round-bottom flask before the

temperature on the thermometer rose. Condensation was noted in fractioning column after the rb

flask was continued heating and condensation was noted dripping back into flask from

fractioning column. Once liquid reached the condensing column there was liquid noted sticking

in a crook of the glass. Distillate was collected before the first theoretical stage but not included

in the determination of ethanol for the first fraction. Very little distillate was collected for the

second fraction as well as the third fraction. The limit of the distillate collected from the third

fraction was because time was cut short and it was known that most of the distillate collected

would be water.
09/22/2020
Chem-343-06
TA: Sarah Metzger
09/22/2020
Chem-343-06
TA: Sarah Metzger

Results:

Density from Simple Distillation: 0.9231 g/mL


09/22/2020
Chem-343-06
TA: Sarah Metzger

Density from Fraction 1: 0.8079 g/mL

Density from Fraction 2: 0.9153 g/mL

Density from Fraction 3: 0.9815 g/mL

Discussion:

From this lab it can be concluded that some ethanol was formed from the fermentation process

due to the density lower than water’s density. Ethanol was synthesized from the combination of

sucrose and water forming glucose and then undergoing the fermentation process to form

ethanol. The density and boiling temperature of ethanol are both lower than water, proving to

separate when being distilled. It is also observed that there is a difference in the accuracy of

simple distillation versus fractional distillation. Fractional distillation utilizes theoretical stages

to predict the density based on what should be evaporating based on the boiling points of each

component. Once density is acquired the percent ethanol by weight or by volume can be

identified.
09/22/2020
Chem-343-06
TA: Sarah Metzger

There is roughly a 44% difference by volume and a 50% difference by weight between the

simple distillation density and the first fraction in the theoretical ethanol boiling stage. This

difference in % ethanol by volume or by weight is because ethanol is lighter than water which

makes the % by weight lower than % by volume. If you compared 100g of ethanol to 100g of

water there would be less ethanol conversely, 100 mL of ethanol to 100mL of water would be

the same amount of liquid. The fractional density results collected are only 0.0189 difference

from known ethanol density. Due to time constraints to the last two distillations were rushed and

did not produce as thorough results. The variable box that the heating mantle was plugged into

was at a higher rate than desired, so the drop rate was higher than necessary. The higher than

necessary drop rate of distillate lead to discrepancies in the actual volume readings per fractional

distillation. When viewing lab partner’s simple distillation results it appear that some ethanol had

to of been formed but there is still a significant portion of distillate that is water.

Post-Lab Questions:

1. After we filter our fermentation mixture, we’re basically left with ethanol and water.

These 2 miscible liquids form an azeotropic mixture. What is an azeotrope? Specifically,

what is the boiling point and % composition of our ethanol-water azeotrope? Compare

this boiling point to the boiling points of pure ethanol and pure water.

a. An azeotrope is a mixture of two miscible liquids that boil at a constant

temperature. The boiling of the 95.6%:4.4% ethanol–water azeotrope is 78.2℃.

This constant temperature boiling point is lower than both ethanol (78.4℃) and

water (100℃)
09/22/2020
Chem-343-06
TA: Sarah Metzger

2. Explain the following statement: A pure liquid has a constant boiling point, but a constant

boiling point does not necessarily imply a pure liquid.

a. The constant boiling point could imply an azeotrope which is when you can not

separate part of the two liquids because of the non-ideal constant temperature

boiling.

3. In the fractional distillation procedure for this experiment, you are directed to collect 3

fractions: distillate collected from 77-80°C, distillate collected from 80-96°C, and

distillate collected above 96°C. Which fraction should contain the highest %volume of

ethanol? What is the probable composition of the fraction which boiled above 96°C?

a. The first fraction which is distilled from 77-80℃ should contain the highest

percent ethanol because it is furthest away from the boiling point of water and is

in the boiling range of ethanol. The fraction of distillate collected above 96℃

should be comprised of a composition of majority water. This majority water

composition is due to the proximity to the boiling point of water.

4. What is the difference between a minimum-boiling azeotrope and a maximum-boiling

azeotrope? The ethanol-water azeotrope falls under which classification?

a. A minimum-boiling azeotrope shows positive deviation from Raoult’s Law

however, a maximum-boiling point azeotrope shows negative deviation from

Raoult’s Law. If you have a minimum-boiling point azeotrope, then the azeotrope

boils off first leaving the component to distill if any remains. If you have a

maximum-boiling point azeotrope, then the azeotrope boils off after the

component first boils. The ethanol-water azeotrope is minimum boiling point.

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