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Caffeine Extraction 1 PDF
Caffeine Extraction 1 PDF
Contents
Abstract ............................................................................................. 3
Objective ............................................................................................... 4
Spike test……………………………………………………………………………………………….7
Apparatus and Chemicals .................................................................... 8
Experimental Methods and Procedure .......................................... 9-13
Result ...........................................................................................14-18
Discussion .........................................................................................21
Conclusion ........................................................................................22
Reference ..........................................................................................24
Acknowledgement…………………………………………………………………………….25
Christian Alliance S C Chan Memorial College/2013-14 Chemistry Olympiad/Caffeine
3
Abstract
The following project will investigate the chemical test for caffeine.
At first, we extract caffeine from coffee. Then we need to prove that
the extraction contain caffeine. Finally we try to find out the amount of
caffeine in coffee.
Objective
Principles
(2) As the solution ( contains the solvent with the dissolved solutes )
moves along a stationary solid surface ( a solid surface ) , different
solutes adsorbed onto the solid surface in different extent as they
have different degree of adsorption characteristics ( due to the
different degrees of dissolve tendency).
Christian Alliance S C Chan Memorial College/2013-14 Chemistry Olympiad/Caffeine
6
(3) The “less soluble” solute will be retained first, and the “more
soluble” solutes will be retained afterwards.
( Note : No two substances have the same solubility and adsorption
characteristics. )
Pure caffeine and the extract are analyzed in the same TLC plate and
compare any differences of their Rf .
Spike Test
By adding known amount of standard caffeine in distilled water and raw
coffee solution , then carry out solvent extraction. By comparing the
extraction results, we can analyze the recovery percentage of the spiked
caffeine and efficiency of solvent extraction.
Chemicals
Solvent Extraction :
Chloroform (CHCl3)
TLC
Ethyl Acetate (C4H8O2)
Ethanoic acid
Apparatus
Separating funnel
TLC plate ( 0.25mm silica gel )
Burette
Pipette
Volumetric flask
Analytical balance
1. 4.58g of fine grinded raw coffee powder is weighted, add 100 cm3
of distilled water and 3.0g of sodium carbonate to increase
solubility of Caffeine (alkaloid) and boil it and brew it by following
the instruction on the Coffee package (one tablespoon of coffee
powder in 100 cm3 of hot water, about 4.58g /100 cm3).
Solvent Extraction
1. Rinse all apparatus with chloroform.
7. Put the beaker with filtrate into hot water bath to evaporate
chloroform (Boiling Point : 61.2 oC) (Figure d)
Figure a Figure c
Figure b Figure d
1. Dissolve the extract and pure caffeine into distilled water separately.
3. Use a pencil to draw a horizontal line 0.5 cm above the bottom of the
TLC plate.
5. Immerse the TLC plate into the solvent ( a mixture of 20:1 of ethyl
acetate : ethanoic acid ).
7. Visualize the result with a UV lamp, use a pencil to circle the spot
seen under UV light.
6. Add a few drops of starch solution when the titrand becomes pale
brown.
7. Slowly run Na2S2O3 until titrand become colorless from dark blue.
9. Repeat the above steps until two to three consistent results are
obtained.
Results
Picture 1
Standard Caffeine solution , Extract from coffee solution , Raw coffee solution
(red) (blue) (brown)
Volume of Mass of
Mass of the Mass of
standard caffeine
extract spiked Recovery
Trial caffeine spiked (mg)
obtained caffeine percentage
solution spiked
(mg) recovered (mg)
(cm3)
1 10 48.3080 95.63 37.83 78.31%
2 20 96.6160 105.87 48.07 49.75%
Volume of Mass of
Mass of
standard caffeine caffeine spiked Recovery
Trial spiked caffeine
solution spiked (mg) percentage
3 recovered (mg)
(cm )
1 10 48.3080 29.46 60.99 %
2 20 96.6160 60.95 63.08 %
100
Recovery Percentage (%)
80
60
40 Coffee
20 Water
0
10 20
Volume of Standard Caffeine Solution added
(cm3)
(2) To find the amount of caffeine in the extract ( from raw coffee
solution )
Discussion
For the TLC test, the possible reason that we can’t see other
impurities maybe impurities can’t be visualize under UV light or they
dissolved in the solvent used to develop the plate. The detail
constituent compounds and elements can be known by some advance
instrument, e.g. HPLC etc.
Conclusion
After the above tests, we confirmed that the about solvent extraction
method is a practical experimental procedure for extracting caffeine in
school laboratory. Due to the nature of the partition coefficients of
solvent-solvent extraction, the amount of loss of caffeine could be
reduced by increasing the number of portion of chloroform used in the
process. ( Refer to the step 3 of the section of Solvent Extraction).
However, chloroform is a CFCs and a carcinogenic substance, it is not
recommended to use.
The TLC results proved that caffeine was successfully extracted from
the raw coffee solution. It also showed that no obviously impurities in
the chromatogram under UV light.
Further Work
The above spike test can be further developed for checking the
extraction efficiency of the above extraction method. Spiking different
concentrations of standard caffeine into the coffee solutions to
consolidate the relationship of caffeine concentration and recovery
percentage by constructing a curve that shows the relationship between
the recovery percentage and the concentration of caffeine in the coffee
solution. So the titration results can be “adjusted” by the recovery
percentage ( dividing the titration result by the corresponding recovery
percentage ) to find a more reliable result.
However, for the Iodometric Back Titration, we can try to reduce the
limitations and find out if other constituent substances in the extract will
react with iodine, contributing to error.
Acknowledgement
Our Chemistry Teachers:
Mr. Kwok Yu
References
[1] Triradar.com:
http://www.triradar.com/training-advice/the-truth-about-caffeine/
[4] 醫學教育網:
http://www.med66.com/new/53a270aa2009/20091022qiji172334.shtm
l
[5] Yahoo 知識 :
https://tw.knowledge.yahoo.com/question/question?qid=1509061403
307
[7] 中山大學化學與化學工程學院:
http://ce.sysu.edu.cn/echemi/basechemlab/Item/956.aspx
Other reference:
Wikipedia: http://en.wikipedia.org/wiki/Caffeine
Chemical Book:
http://www.chemicalbook.com/ChemicalProductProperty_US_CB0202769.aspx
新竹市立香山高級中學第 50 屆中小學科學展覽會:
http://activity.ntsec.gov.tw/activity/race-1/50/pdf/040214.pdf