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Experiment 3 PDF
Experiment 3 PDF
School of Chemistry
The University of Melbourne
Laboratory Report Cover Sheet
Student Name:
Student Number: Edie Nicolson
Subject Name & Code: Chemistry 1
Demonstrator:
Experiment Title: Experiment 3: Extracting Chemicals from Nature- Caffeine from Coffee Beans
By submitting work for assessment, I hereby declare that I understand the University’s policy
on academic integrity and I declare that:
• This laboratory report is my own original work and does not involve plagiarism or
unauthorised collusion, except where due credit is given to the work of others. The report is
based on results and spectra obtained by me during my laboratory session.
• This laboratory report has not previously been submitted for assessment in this or any other
subject.
For the purposes of assessment, I give the assessor of this assignment the permission to:
• Reproduce this laboratory report and provide a copy to another member of staff; and
• Take steps to authenticate the assignment/laboratory report, including communicating a copy
of this assignment to a checking service (which may retain a copy of the assignment on its
database for future plagiarism checking).
Feedback on Report: Feedback on your report and the mark you received will be available on the
Online Practical Assignments page on Canvas.
Plagiarism:
Plagiarism is the act of representing as one's own original work the creative works of another,
without appropriate acknowledgment of the author or source.
Collusion:
Collusion is the presentation by a student of an assignment as his or her own work, but which is in fact
the result in whole or in part of unauthorised collaboration with another person or persons. Collusion
involves the cooperation of two or more students in plagiarism or other forms of academic
misconduct.
Both collusion and plagiarism can even occur in group work. For examples of plagiarism, collusion and
academic misconduct in group work please see the University’s policy on Academic Honesty and
Plagiarism: https://academichonesty.unimelb.edu.au
Plagiarism and collusion constitute cheating. Disciplinary action will be taken against students who
engage in plagiarism and collusion as outlined in University policy. Proven involvement in plagiarism
or collusion may be recorded on your academic file in accordance with Statute 13.1.18.
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Experiment 3. Extracting Chemicals from Nature
– Caffeine from coffee beans.
Executive Summary (replaces Abstract, Introduction and Conclusion for this Experiment)
(see Guide notes at end of template – better completed after the rest of the report)
Aims (What are you trying to find out? Not in dot points)
This experiment aims to compare two methods of caffeine extraction from coffee beans to
determine which is more effective taking into account yield, cost, and environmental
impact.
Experimental:
(How did you perform your experiment? Refer to Student Notes using full name, year and
publisher)
Average mass(caffeine)
Show working
(0.002+0.002+0.003)/3 = 0.00233
g
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Solvent used to extract chemicals from ground coffee beans: acetone
Method B
Calculate the average mass of caffeine in 10mL portion of the total volume, using the three
sets of data provided.
Calculate the mass of caffeine in the total volume of extract from the coffee machine.
Calculate the %yield of caffeine by mass, showing all working.
Table 2. Method B Coffee Machine Extraction
Include units Run 1 Run 2 Run 3
Mass of coffee grounds g 15.16
Total volume (coffee extract) mL 44 mL
volume(coffee) per trial mL 10 mL
m (Beaker + Boiling Chips) g 33.577 34.675 35.453
m (Beaker + Boiling Chips + caffeine) g 33.587 34.684 35.462
m (caffeine) g 0.010 0.009 0.009
Average mass(caffeine) – use data
from Runs 1 to 3 (0.010+0.009+0.009)/3
Show working = 0.0093
= 0.009
Mobile Phase: 55%:10%:35% (v/v) Ethyl Acetate : Acetic Acid : Petroleum Ether
Sketch your tlc plate and calculate Rf values (show working) for all spots observed.
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Question 1 REMEMBER THAT ANSWERS NEED TO BE SUPPORTED BY EVIDENCE FROM
YOUR DATA OR THEORY
i. Suggest a compound that may be dissolved in the lower brown NaOH (aqueous) layer.
Tannic Acid/Melanoidins
ii. What type of intermolecular forces would be attracting this molecule into the aqueous
layer?
NaOH is polar due to its hydroxyl groups and hence is likely to attract and interact with
other polar molecules through hydrogen bonding. As melanoidins and tannic acid are polar,
they are attracted to the NaOH and form hydrogen bonds with it.
NaOH is also classified as a base, and hence attracts and interacts with acids such as tannic
acid.
Question 2
Why do you think the extract using Method B looks different (colour, clarity) to the
extract obtained by Method A (what was different about the conditions)?
Method A -
Method B – Extracted using water, DARKER due to higher amount of melanoidins
Method A, conversely, was a much less intense extraction method as the compounds
found in coffee beans were dissolved in acetone at a lower temperature and pressure
since caffeine should dissolve more easily in acetone than water, hence less intense
temperature and pressure was required. This process extracted a lesser amount of
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melanoidins and tannic acids as the extraction technique was more selective and gentler.
Therefore, the extract was lighter in colour.
Question 3 (make sure to refer to your TLC results and discuss relative polarity)
i. Analyse your TLC results: How many compounds have been extracted? What
compound(s) have been extracted? Have you extracted caffeine and how do you know?
Are there other compounds present? Name any possible compound that fits your polarity
assessment (see Introduction to Student Notes). Explain your answer.
From the TLC results, it can be determined that one compound has been extracted as all
three marks on the TLC are similar. As we can compare both spots A and B to spot C (pure
caffeine) which acts as a control, we find that spots A and B concur to spot C, and thus are
caffeine. As there aren’t any discrepancies between the spots, it is highly unlikely that any
other compounds are present, and aren’t present in high enough quantities to affect the
TLC.
ii. Using your TLC results, how pure is the product form your extraction? Explain your
answer.
As each method (spots A,B, and C) sits at the same spot on the TLC, and none have
branched into multiple spots, it can be determined that only one compound is present in
each sample. Hence the produce, previously determined to be caffeine, is highly pure.
iii. The caffeine obtained in Method B was discoloured, however this was not observed on
the TLC plate. Why not? What are the limitations of TLC?
The caffeine obtained in Method B was discoloured due to the presence of tannic acid and
melanoidins, which are highly polar and dissolve easily in water. As molecules only show up
on the TLC if they absorb UV light, and molecules such as water aren’t detected, the
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melanoidins were not absorbed on the TLC plate. Further limitations of TLC stem from the
polarity of the molecules tested, as a highly polar stationary phase will result in polar
molecules not moving with the non-polar mobile phase and vice versa, thus impacting the
results. As the molecules are suspended in a solution, high temperatures or long periods left
uncovered can result in the solution evaporating, leaving only precipitate that won’t travel
up the TLC plate and will lead to inaccurate results.
Conclusion:
(What have you found out?)
It was found that both Method A and Method B extracted caffeine from coffee
grounds, however Method B extracted 0.27% (w/w) caffeine compared to Method A
which extracted 0.24% (w/w) – hence it can be determined that Method B was more
effective. It was also found that Method B extracted a larger proportion of other
chemicals from the coffee, and thus lead to a darker extract. Possible limitations of
TLC were identified and outlined above, however, it is unlikely that these limitations
impacted the results of the experiment.
A. Executive Summary
An executive summary is essentially a short document produced for business purposes to
give a brief description of the purpose and scope of an investigation as well as conclusions
and recommendations. It is usually accompanied by a much longer scientific report giving
more details about the investigation and results.
As part of the executive summary in this experiment, you will use your findings to make
a recommendation to the pharmaceutical company as to which extraction technique is most
suitable for large scale extractions of caffeine (for typical production of a million 100 mg
caffeine tablets per day) from coffee beans. You should consider the yield by percentage
mass of ground coffee used, the cost of chemicals, operating costs, labour, environmental
impact and sustainability. A list of expenses has provided below in the table which you may
use for your consideration of the most appropriate extraction technique.
Your executive summary should be NO MORE THAN 200 words written in
paragraph/sentence form in past tense, passive voice and plain language that a person with
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little scientific understanding can understand. Although there is not one set format for an
executive summary, the following is a good guideline of what should be included in the
summary:
a) Subject Matter – what is being investigated (brief)
b) Methods of Analysis – what techniques were used (not in detail)
c) Results – brief description using data tables (here you would consider a cost analysis, yields
and waste management). As a footnote, show how you have calculated the cost for each
method.
d) Conclusions and Recommendations – which technique do you recommend and why?
e) Limitations – are there any items that the report does not include or assumptions made or
limitations to the results?
The methods used were UV-vis analysis (Method A) as well as chemical gravimetric analysis
by mass (Method B). The results are for three garden beds are shown in Table 1.
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i) Costing analysis does not include the labour costs of analysis or the ongoing laboratory
costs, and
ii) Phosphorus content results are for 1 sample from each bed so not tested for
reproducibility.
Are there ways to improve costs and sustainability i.e. recycling of solvents?
Any environmental costs associated with use of organic solvents?
Any environmental costs associated with use of large volumes of water?
Are there any limitations on your assessment – any factor not considered, reproducible data,
sample size representative (how many samples have you tested?)
You need to recommend one method (or neither method): think about the supporting
evidence and use it in your argument.
Make sure to complete Table 3.1 from last page of template, completing parts in red
(choose between options in red, include your yield)
An executive summary is brief – only the main points are included. Time is money!
Executive Summary
Two methods of caffeine extraction from coffee beans were examined in order to
determine which method was most effective in terms of amount of caffeine extracted,
environmental impact, and cost. Method A involved using a Soxhlet which yielded 0.24%
caffeine (w/w) whilst Method B used an espresso machine yielding 0.27% (w/w). Further
results from both methods is shown in Table 3.1 below.
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water
acetone
Solvent used in Primary Extraction Method $3/kL
$47.00/L
=$ 0.003/L
Workup – extraction/NaOH, ethyl acetate/evaporation same same
Operating Costs – electricity, water (recycled for
same same
condenser), high pressure
2 min/15g ground coffee
Time required/sample 15 min/1g ground coffee = 8 seconds/1g ground
coffee
i.organic solvents:
i. organic solvents:
acetone, ethyl acetate
ethyl acetate
ii.MgSO4/organic solvent
ii.MgSO4/organic solvent
Waste – type sludge
sludge
iii. organic solvent
iii. aqueous extracted
contaminated coffee
coffee grounds
grounds
Environmental Impact of wastes generated in method:
higher lower
greenhouse gases, landfill
Cost of waste disposal/ waste to energy conversion* higher lower
The cost of the solvent used in Method B is far lower than that of Method A, and resulted in
a lower environmental impact as only Method A produced acetone in addition to the other
waste products from Method B. Method B was also far more time effective, requiring 8
seconds per gram of ground coffee compared to Method A’s 15 minutes per gram.
It is recommended that Method B is used. It was found to be less expensive, has a higher
yield, and has less environmental cost as both methods produce organic solvents that can
contribute to air pollution (NetRegs.org) but the aqueous coffee grounds produced in
Method B are compostable whilst those from Method A are not. However it should be
noted that the water required for Method B will have a greater environmental cost if water
is restricted i.e. in a drought.
It is also recommended that this experiment be repeated to ensure that the results are both
precise and accurate.
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Waste Type Cost Method A Method B
Organic/Hydrocarbon contaminated sludge
(e.g. MgSO4 residues, organic solvent $500/tonne Yes Yes
contaminated coffee grounds)
Liquid hydrocarbons $100/tonne Yes Yes
Solid waste – not hydrocarbon/metal
containing $100/tonne No Yes
(e.g. coffee grounds from Method B)
Liquid waste requiring neutralisation
$100/tonne Yes Yes
treatment (e.g. highly acidic or highly basic)
Aqueous solvents not requiring
$15/tonne No Yes
neutralisation
** Based on Estimate of the cost of hazardous waste in Australia
Report to Dept of Environment Australia 2014 Marsden Jacob Associates
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