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Sublimation of Crude Caffeine

The document describes an experiment to purify caffeine through sublimation. Crude caffeine extracted from tea was placed in a petri dish on a hot plate, with an ice bath covering the lid. Low heat caused the pure caffeine to sublime and collect as crystals on the lid above the ice bath. The purified caffeine crystals were collected, weighed, and found to have a recovery percentage of 23.91% compared to the original crude caffeine. Sublimation successfully separated the pure caffeine through differences in vapor pressure under heating and cooling conditions.

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2K views2 pages

Sublimation of Crude Caffeine

The document describes an experiment to purify caffeine through sublimation. Crude caffeine extracted from tea was placed in a petri dish on a hot plate, with an ice bath covering the lid. Low heat caused the pure caffeine to sublime and collect as crystals on the lid above the ice bath. The purified caffeine crystals were collected, weighed, and found to have a recovery percentage of 23.91% compared to the original crude caffeine. Sublimation successfully separated the pure caffeine through differences in vapor pressure under heating and cooling conditions.

Uploaded by

Flora Mae
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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FLORA MAE GESULGA BS-CHEM 2

Date Performed: Jan. 26, 2021 Date Submitted: Feb. 2, 2021

SUBLIMATION OF CRUDE CAFFEINE


Experiment No. : 3
Objectives:
1. Use sublimation method to purify an organic compound (caffeine extract)
2. Determine the percent recovery of the purified caffeine from tea.

Results and Discussion


In this experiment, sublimation was the technique use in purifying the caffeine.
The crude caffeine collected from the extraction from tea was used in the sublimation. To
sublimate the crude caffeine, the crude extract was then put in the dry and clean petri dish and
put in the hot plate and cover. An ice bath was then put on top of the lid, the ice provides the
cooling and to allow the pure caffeine to form in the bottom of the ice bath. The cold
environment slows down the molecules of the gaseous product of the crude extract in heating
allowing them to stick to cold surface. The low medium heating of the crude extract was done to
bring the pure caffeine to the desired vapor pressure for sublimation. Overheating will destroy
the sample that was reason why caffeine was heated a low medium setting. Heating at high
temperature sublimates the entire crude sample and prevents the pure caffeine from separation.
After heating, crystals start to form at the cover of petri dish where the ice bath was put. In the
extraction of crude caffeine from tea, the color observed was brownish white while in the
sublimation to purify the crude caffeine, the crystals solid observe was amorphous white. After
cooling down the sublimated caffeine, scrapping of the crystals that form in the cover were
collected. With the data collected, percent recovery of sublimation was successfully calculated.

Table1. Mass of the Crude and Pure Caffeine


Mass of Crude Caffeine Mass of Pure Caffeine % Recovery of Sublimation

0. 046 g 0.011 g 23.91 %

% Recovery of Pure Caffeine


= 0.011 g/ 0.046 x 100
= 23.91 %

Conclusion
The sublimation method was used to purify the crude caffeine that was extracted
from tea in the last experiment. After cooling down the sublimated caffeine, the crystals
FLORA MAE GESULGA BS-CHEM 2

collected from the cover of petri dish were collected. With the collected purified caffeine from
tea, the percent recovery was successfully calculated. Thus the calculated percent recovery of
the purified caffeine was 23.91%.

ANSWER TO QUESTIONS
1. What do you think will happen if the caffeine is heated at high temperature?

 If the caffeine is heated at high temperature or if it’s overheated the material might be
destroyed. The excess heat would sublimate the entire crude sample, preventing the
pure caffeine from separation.

2. Which of the following three compounds would most likely be amenable to purification by
sublimation; polyethylene, menthol, or benzoic acid?

 The sublimation process is the purification of solid substances at low vapor pressure so
solid compound with a high melting point and low vapor pressure are the one that can be
purified easily by sublimation process unlike liquids. The benzoic acid is liquid room
temperature so it can be purify by recrystallization, menthol and polyethylene are solid
state at room temperature so they both have high melting point at room temp. The
purification of polymers is most amenable so purification of polyethylene by sublimation
is the most amenable.
3. Hexachloroethane has a vapor pressure of 780 mmHg at its melting point of 186 C. Describe
how solid would behave while carrying out melting point determination at atmospheric pressure
(760 mmHg) in a capillary tube at the top.

 The solid will sublime before it melted because the given atmospheric pressure is 760
mmHg not 780.

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