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Caffeine Isolation

The document outlines a procedure for extracting caffeine from tea or coffee using sodium carbonate and dichloromethane (DCM). It includes steps for filtering, separating, and evaporating the solvent to obtain pure caffeine, as well as methods for confirming its presence through TLC and a chemical test. The melting point of caffeine is noted to be between 234 – 237 °C.

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Pratik Khanal
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5 views1 page

Caffeine Isolation

The document outlines a procedure for extracting caffeine from tea or coffee using sodium carbonate and dichloromethane (DCM). It includes steps for filtering, separating, and evaporating the solvent to obtain pure caffeine, as well as methods for confirming its presence through TLC and a chemical test. The melting point of caffeine is noted to be between 234 – 237 °C.

Uploaded by

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

Extraction of caffeine

7 grams, of tea (or) coffee were taken in 150 ml of distilled water and 5g of sodium carbonate is added. The solution
was then heated and was kept at 100 °C for 15 min.

Then, the solution was cooled and filtered using Whatman filter paper.

This sample was placed into a separating funnel and 6 ml of dichloromethane (DCM) was added. The caffeine was
extracted by inverting the funnel at least three times, venting the funnel after each inversion.

Vigorous shaking will produce an intractable emulsion, while extremely gentle mixing will fail to extract the caffeine.

The bottom layer containing dichloromethane (DCM) was removed to a clean flask, leaving behind the layer of water
and the extraction procedure was repeated twice more and the solvent layers combined.

To the combined DCM fraction add anhydrous Sodium Sulphate to adsorb water.

Filter DCM layer again.

The dichloromethane was evaporated from the extract by heating the flask on water bath. The residue obtained was
whitish powder which was considered to be pure caffeine. The mass of flask with residue was measured on
electronic scale.

Calculate % crude caffeine extracted.

Perform TLC of caffeine in

1) mobile phase (Methanol: DCM 1:9) or 10% methanol in DCM and


2) 1% methanol in DCM with authentic if available

Confirmation of Caffeine in TLC:

Procedure:

1. Place the TLC plate in a closed chamber containing a few iodine crystals.
2. Allow it to sit for a few minutes.

Observation:
Caffeine spot appears as a brownish spot that fades upon exposure to air (temporary visualization).

Chemical test of caffeine (Murexide test):

Procedure:

1. Place a small amount of caffeine (or extract) in a porcelain dish.


2. Add a few drops of concentrated nitric acid (HNO₃).
3. Evaporate to dryness by gentle heating.
4. Add a drop of dilute ammonia solution (NH₃).

Observation:
A purple or violet color appears — confirms presence of caffeine.

Melting point of caffeine is 234 – 237 °C.

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