Laboratory Experiment No.

Witness Caffe in extraction: Isolation of Caffeine from Coffee

Name: John Timothy B. Barrera

Chem 31.1 Section 6

Abstract

Different extraction techniques are employed to isolate a desired substance. Caffeine in

coffee is a well-known compound which acts as a stimulant. Thus, the experiment aimed to
extract caffeine from coffee using solid-liquid and liquid-liquid extraction methods and to
determine the percent caffeine in the coffee sample. The method used was a series of extraction
methods which started from solid-liquid extraction, then liquid-liquid extraction, and
eventually washing techniques to purify the crude caffeine. The result of the experiment
showed that crude caffeine was extracted, having 0.08g. Out of the 10.06g sample coffee, the
percent caffeine was calculated as 0.80%. The use of several reagents and the repeated liquid-
liquid extraction method enabled maximum caffeine yield.
Introduction

The common products such as food and beverages that we intake are usually a mixture
of several compounds or substances. Coffee is a common drink which actually consists of
proteins, carbohydrates, tannins, oil, and caffeine (Sharma, 2020). Wherein, Caffeine is a
known stimulant compound in coffee that increases energy levels by affecting
neurotransmitters in the brain (Link, 2022). In order to isolate the single desired substance or
component either for analysis or other particular laboratory use, various extraction methods are
applied. Solid-liquid extraction involves separation of the soluble components, with a specific
solvent, from insoluble components of a solid sample (Donau Lab Ukraine, 2022). On the other
hand, liquid-liquid extraction is used to extract a substance by moving it from its original
solvent to another solvent which is immiscible with the former (Finchsigmate, 2022). In line
with these, the objectives of this experiment are to extract caffeine from coffee using solid-
liquid and liquid-liquid extraction methods and to determine the percent caffeine in the coffee
sample.
Methodology

Preparation of Sample Coffee, Reagents and Laboratory equipment

Weigh 10.06 grams of Coffee and add to 250 mL Beaker

Add 100 mL of water into the Beaker, mix for 7-10 minutes

Filtration of the mixture using cheesecloth

Add 20g NaCl and 1g Ca(OH)2 into filtrate, then heat and stir for 15 minutes

Vacuum filter the mixture through Büchner funnel, then cool to room temperature

Perform liquid-liquid extraction three times using 20mL DCM solvent and 125
mL separatory funnel

Add total extract to another 125 mL separatory funnel and wash with 20mL 10%
NaOH

Dry extract using anhydrous Disodium Sulfate

Separate Caffeine from Organic Solvent using Distillation Method

Rinse crude caffeine with acetone and air dry using evaporating dish

Determination of Crude Caffeine Mass and Calculation of its percentage in sample

Results and Discussion

Table 1. Mass of Residue(M)

Mass of Empty Evaporating Dish 45.70 g
(E)
Mass of Evaporating dish with 45.78 g
residue(ER)
M= ER-E 0.08g

Table 2. % caffeine in the sample

Mass of Residue 0.08g
Mass of Sample 10.06g
%caffeine in sample= (mass of 0.80%
residue/mass of sample)*100

Table 1 shows that the mass of the final residue or the crude caffeine obtained was
0.08g. This existence of this residue mass is attributed to the series of extraction processes
done. The primary process was the solid-extraction method which filtered out water-insoluble
materials from the sample. Subsequently, prior to the liquid-liquid extraction, the resulting
filtrate was treated with NaCl and Ca(OH)2. The role of the salt (NaCl) was to fill up the amount
of solute that the water solvent can hold which made the solution ionic while Ca(OH)2 enabled
a neutralization reaction with the acidic tannins thus producing more salt and making the
solution neutral. As a result, since Dichloromethane ( DCM) was the organic solvent used,
caffeine was more attracted to the organic solvent than its original aqueous solvent. Although,
based from the study of Chaugule,et. Al in 2019, the solubility of caffeine in DCM (at
140mg/ml) is significantly higher than in water (at 22mg/ml), the addition of NaCl and
Ca(OH)2 only ensured that more caffeine would go into DCM for higher extraction rate.
Moreover, further ensure greater caffeine yield, the liquid-liquid extraction method was
done three times. Calculations actually prove that repeated extractions using portions of DCM
resulted to better yield compared to one extraction with a combined DCM amount. For
example, extraction in 3 portions of 20mL Dichloromethane is 9% more efficient than in one
60 mL DCM extraction.
 On the other hand, table 2 shows a 0.80% by mass percentage of Caffeine in the 10.06
g coffee sample. This percentage by mass is lower but close to the 1.1-2.2% caffeine in coffee
composition as presented by Wartenberg in 2019. The possible reason for the differences in
percentage of caffeine in the sample is the variations to the species of coffee beans used. Also,
deviations among the extraction methods used is another possible reason.

Conclusion
The reagents used ensured the maximized attraction of caffeine to the organic solvent
Dichloromethane (DCM). Further, the replication of the liquid-liquid extraction with DCM
ensured that more caffeine would be extracted.
Thus, the experiment was successful at extracting caffeine, with a mass of 0.08g, from
10.06g coffee sample using solid-liquid and liquid-liquid extraction methods. Consequently, it
led to the determination of the percent caffeine in the sample coffee which is found out to be
having 0.80% by mass Caffeine.
References

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