Scribd
Upload
193 views4 pages

Caffeine Extraction from Coffee and Tea

This document describes the process of extracting caffeine from coffee and tea using solvent extraction. Solvent extraction involves using two immiscible solvents, such as water and an organic solvent like dichloromethane, to separate compounds based on their differential solubility. The process involves adding the solvents to a separatory funnel, shaking to mix them, and collecting the organic layer containing the extracted compound. Specifically, caffeine is more soluble in dichloromethane than water, so multiple extractions with DCM are used to remove caffeine from tea or coffee filtrate. The extracted solution is then dried and evaporated to obtain crude caffeine.

Uploaded by

Đoàn Ngọc
Copyright
© All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
193 views4 pages

Caffeine Extraction from Coffee and Tea

This document describes the process of extracting caffeine from coffee and tea using solvent extraction. Solvent extraction involves using two immiscible solvents, such as water and an organic solvent like dichloromethane, to separate compounds based on their differential solubility. The process involves adding the solvents to a separatory funnel, shaking to mix them, and collecting the organic layer containing the extracted compound. Specifically, caffeine is more soluble in dichloromethane than water, so multiple extractions with DCM are used to remove caffeine from tea or coffee filtrate. The extracted solution is then dried and evaporated to obtain crude caffeine.

Uploaded by

Đoàn Ngọc
Copyright
© All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd

Extraction of Caffeine from Coffee and Tea

Introduction:
- Caffeine is a natural product found in the fruit and bark of certain plants.
- It is well known that caffeine is a stimulant, a diuretic and is addictive. The
stimulant action is why a lot of us drink so much tea, coffee and certain soft
drinks, but it is also used in some medications to reverse drowsiness.
- Caffeine has been described as the "most abused drug in the US": a
single serving of coffee may contain 125mg, tea 75mg, Cocoa 40mg,
Coca-Cola 46mg. A regular 4-cups-a-day coffee drinker on withdrawal can
experience headaches, insomnia, even nausea!

Extraction Theory:

Solvent extraction is a process of purification involving the use of two


solvents or solutions that are immiscible with one another.

- The main use is to employ extraction as a means of isolating chemicals


that are present in plant or animal tissue (natural products).

- It is extensively used in organic chemistry as a way purifying reaction


mixtures after a laboratory experiment. It is based on the differential
solubility of compounds in water and an immiscible organic solvent
(typically diethyl ether, chloroform, dichloromethane, ethyl acetate). This
allows the desired

Organized by Lecturers: Sharifa A. Al-Ghamdi& Maha Baljoon 1


organic product to be separated from inorganic or very other polar by-products. This is the basis of
an older industrial method for "decaffeinating" coffee.

- A conically shaped piece of glassware called the separatory funnel is the laboratory tool used for
most types of extraction. Be careful when using them, they are not cheap!!! The general process
involves adding the two immiscible solutions to the separatory and shaking with occasional
opening of the stopcock.

(1) The Basic Process of Extraction:

(a) First make sure that the stopcock is secured and CLOSED.

(b) Place a collection flask underneath the funnel.

(c) Use an iron ring to support the separatory funnel.

(d) Two heterogeneous liquids/solutions are added to the separatory


funnel.

(e) The mixture of solutions is shaken with occasional venting to


relieve any pressure buildup.

(f) The lower layer is drawn off through the stopcock.

(2) The Difference between Extraction and Washing:


- Extraction is the removal of a desired compound from one phase (usually the aqueous phase)
into another (usually the organic phase).

- Washing involves the removal of impurities by shaking the solution with an aqueous solvent that
will dissolve only the impurities and leave the desired compound behind in the organic phase.

(3) Identifying the Aqueous Phase and the Organic Phase:


Keeping track of which layer is the organic layer and which is the aqueous layer can be frustrating.
However, if you remember one simple rule, then you troubles will be few. The rule here is that the
more dense liquid will be on the bottom. If you are in doubt, there are two things you should do:

1. Remove a drop of one layer and place it in a small test tube. Add a drop of water. If it dissolves,
the layer is aqueous. If it doesn't, then the layer is organic.
Organized by Lecturers: Sharifa A. Al-Ghamdi& Maha Baljoon 2
2. Save ALL of your discarded layers until the end of the experiment.

(4) How much solvent/ how many extractions?


The general rule is to perform multiple extractions with smaller amounts of extracting solvent rather
than one extraction with a large amount of solvent. Remember, we are dealing with the partitioning
of a solute equally between two phases. By performing the extraction a number of times, we can
effectively pull out more material than if doing it once with a large amount.

Aim of the Experiment:

-In this experiment you will extract caffeine from tea leaves with dichloromethane (caffeine is about
9 times more soluble in dichloromethane than in water) using a separatory funnel. Be careful not to
shake too vigorously or you will get an emulsion that is difficult to separate. You will also earn how
to dry an organic solution (removing trace quantities of water) using a chemical drying agent.

Materials:

1- Tea, coffee.
2- Dichloromethane (DCM).
3- 6M NaOH
4- Anhydrous MgSo4
5- DW, Ice

NOTE: Wear gloves when handling DCM. It also has harmful vapours. Avoid skin contact and
avoid breathing the vapor. Keep in the fume-hood whenever possible.

Procedure:

1- Weigh tea from 20 tea bags, 3 spoons Arabic coffee.


2- Add 100ml boiling DW and stir for 7 min.
3- Filter by filter paper- cool the filtrate in an ice bath.

Extraction:

1- Pour the cold tea filtrate into a separatory funnel.


2- Slowly add 20ml DCM and gently stir the 2 layers for about 5 min.
3- Replace the SF into the stand, remove the stopper and allow separating for about 5min.

Organized by Lecturers: Sharifa A. Al-Ghamdi& Maha Baljoon 3


4- Collect the organic phase into conical flask (Don’t allow any of the darker material to
escape through the stopcock).
5- Repeat the extraction twice more with fresh 20ml of DCM.
6- Add these 2 DCM layers to the first (If an emulsion remains in the DCM, filter through a
Buchner funnel).
7- Return the organic phase to the SF and extract with 20ml 6M NaOH (twice) and once with
20ml DW.
8- Collect the DCM layer into conical flask.
9- Dry the solution by adding 1 teaspoonful of anhydrous MgSO 4, and then allow standing
5min.
10- Filter
11- Weigh empty flask.
12- Transfer the filtrate into flask and evaporate DCM on the water bath.
13- Weigh the flask containing the crude product.

Calculation:

Determine the weight of pure caffeine in each of your sample


and calculate the weight % of caffeine.

Wt (g) of caffeine →→→→→→→Wt (g) of sample

Microscopic examination:

- Caffeine + drops of mercuric chloride HgCl2 ----------- examine under microscope------ needle-shape

References:

L. F. Fieser and K. L. Williamson, Organic Experiments, 6/e, D. C. Heath and Co.,


Lexington, MA, 1987.
2. D. L. Pavia, G. M. Lampman, G. S. Kriz, R. G. Engel, Introduction to Organic
Laboratory Techniques, A Microscale Approach, Saunders College Publications, San
Francisco, 1990.

Organized by Lecturers: Sharifa A. Al-Ghamdi& Maha Baljoon 4

Common questions

Powered by AI

Dichloromethane (DCM) presents various safety concerns, including harmful vapors that are hazardous if inhaled, and potential skin irritation upon contact. It is advised to use DCM in a fume hood to minimize inhalation risk, and to wear gloves to protect skin from exposure . Proper handling precautions are necessary to ensure safety in the laboratory environment.

Correct identification of the aqueous and organic phases is critical to ensure the accurate separation and recovery of the target compound. A simple method to determine each phase is to remove a drop of one layer; if it dissolves in water, it is the aqueous phase. If not, it is the organic phase . Accurate phase identification minimizes errors in compound isolation and ensures process efficiency.

The separatory funnel is the essential laboratory tool for most types of solvent extractions. It allows immiscible liquids to be separated based on density differences. The operation involves adding liquid mixtures into the funnel, shaking gently, and allowing the layers to separate. The denser layer is drawn off through the stopcock at the bottom . Its proper use facilitates efficient phase separation and compound isolation.

The relative densities of the two immiscible liquid phases determine which will be on the bottom; the more dense liquid naturally settles below the less dense one. This distinction is crucial for correctly identifying and separating the desired organic compound from impurities. Misidentification can lead to incorrect phase handling and loss of product . Understanding density hierarchy is key for effective extraction.

Shaking the separatory funnel too vigorously can lead to the formation of an emulsion, which is a stable mixture of the organic and aqueous phases that is difficult to separate. This can significantly hinder the extraction process, reducing the efficiency of phase separation and complicating the recovery of the desired compound . Careful handling is essential to avoid such issues and ensure smooth operation.

Anhydrous magnesium sulfate (MgSO4) acts as a drying agent in the caffeine extraction process. It is used to remove trace amounts of water from the organic phase. The organic solution is treated with MgSO4, allowed to stand for 5 minutes, and then filtered to remove the drying agent along with any absorbed water . This step ensures the purity of the extracted compound by eliminating moisture.

'Extraction' involves transferring a desired compound from one phase, usually aqueous, to another, typically organic. In contrast, 'washing' is used to purify a solution by dissolving impurities into an aqueous solvent, leaving the desired compound in the organic phase . These techniques leverage the selective solubility of compounds across different solvent phases.

The microscopic examination of caffeine involves adding drops of mercuric chloride (HgCl2) to caffeine and then examining the sample under a microscope. The specific feature to observe is the presence of needle-shaped crystals, which confirm the identity of caffeine .

The weight percentage of caffeine in a sample is calculated by determining the weight of the isolated caffeine and comparing it to the initial weight of the sample. This is done using the formula: (Weight of caffeine / Weight of sample) * 100 . This calculation provides insight into the efficiency of the extraction process and the purity of the final product.

Performing multiple extractions with smaller amounts of extracting solvent is favored because it enhances the efficiency of the solute's partitioning between the two phases, thereby extracting a greater amount of the desired compound compared to a single extraction with a large volume. This approach takes advantage of the principles of partitioning to pull out more caffeine from the solution .

You might also like