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Experiment: Separation of Liquids by Fractional

Distillation and Analysis by Gas Chromatography
Date Performed: March 9, 2020 (Post Quarantine)
Date Submitted: April 26, 2020
Russybel Richiez Partner: Thiana Ruiz
CHEM 2223L
P. Spellane
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Abstract: Gas chromatography is used to separate a mixture of two volatile liquids. In this

experiment two compounds are mixed and then separated into components and then placed in a

gas chromatograph. The boiling point of Ethyl acetate (C4H8O2) is 77°C and the boiling point

of Butyl acetate (C6H12O2) is 126.3°C. The boiling points are important in this experiment

because the substance with the lowest boiling point is the most volatile, this being Ethyl acetate.

The substance with the highest boiling point is the least volatile this being Butyl acetate. The

substance that is most volatile in the vapor phase the substance that’s most volatile will boil

easily, meaning Ethyl acetate is the one that will boil easily and quickly. In this experiment there

is a long gas glass tube in which there is a fractionalization column. Here the mixture is

separated into component based on the differences in volatilities. Because Ethyl acetate is more

volatile than Butyl acetate it will be easier to separate into components. Once placed into the gas

chromatograph the components get adsorbed to the mobile phase and move through the column.

Those who have a high affinity or attraction to the stationary phase move slowly. Here the more

volatile substance Ethyl acetate will move faster. It was found that

Materials:

 Hot plate  Keck clips

 Syringes  Condenser
 Still head  Two balloons
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 Thermometer  Bend vacuum adapter

 100 mL still pot
 Two water rubber
 Graduated cylinder
 Thermometer adapter
 West condenser (thick column)
 Gas chromatography instrument
 Hempel column with raschig rings
 30 mL of 1:1 mixture of ethyl acetate
and butyl acetate

Results:
A1: Faction 1

Volume (mL) Temperature ºC

1 75
2 75
3 75
4 75.1
5 75.5
6 75.6
7 75.8
8 75.8
9 75.8
10 75.8
11 75.8
12 76.5
13 93
A2: Faction 2

Volume (mL) Temperature ºC

14 119
15 122
16 122

A3: Faction 3
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Volume (mL) Temperature ºC

17 122.1
18 122.1
19 122.1
20 122.1
21 120

Conclusion: For the first faction, the temperature for collection was 75-75.1°C with the outlier

being 93°C. The temperature for collection is close to the boiling point of ethyl acetate (77°C).

This means the first fraction had higher moles of ethyl acetate than butyl acetate. For the second

faction collection occurred at was collected at 93-122° C. This indicates that the sample

contained equal proportions of the Ethyl acetate and Butyl acetate. For the third faction the

collection temperature was 122-122.1°C. This is close to the boiling point of Butyl acetate

126.3°C. This data means the third fraction had larger portion of Butyl acetate than Ethyl acetate.

Based on the data, the third fraction was collected between 122-122.1ºC. This is not close to the

boiling point of Butyl acetate. This means there might be impurities in the distillation. The

overall experiment data concludes that Ethyl acetate is more volatile and has a lower boiling

point would meaning it would come out first and Butyl acetate which is less volatile and has a

higher boiling point came out last.