Chen Lab 2
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University of Waterloo *
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Course
121
Subject
Chemistry
Date
Dec 6, 2023
Type
Pages
4
Uploaded by DrFlyMaster964
Procedure:
Sign out from the storeroom:
50 mL round bottom flask
500 mL vacuum flask
Buchner funnel
powder funnel
thermometer
Pick up from the side bench or cabinets: (*if not already at your bench)
metal rod
utility clamp
2
2
filter paper
melting point tubes
hot plate and cord*
Mel Temp (melting point apparatus)*
As soon as you arrive in the laboratory, set up a water bath, on a hot plate, using ~250 mL of
deionized water in a 400 mL beaker. The reaction mixture will be heated in a water bath at
65-75
•C. monitor the temperature with a thermometer. Bring the water bath to the desired
temperature
quickly by heating @ 400 °C, then turn the temperature down. Try to find a setting on the hot
plate which will maintain the water bath within this temperature range. Note that it is easy to
cool down a water bath quickly by adding some cool DI water.
Part 1: Synthesis
On the top-loading balance, weigh ~3.0 g of p-aminophenol into a clean, dry 50 mL beaker.
Record the actual mass ed, with correct significant digits, on your data sheet. Using the powder
funnel (which has a wide neck, signed out from the storeroom), add the p-aminophenol to the 50
mL round bottom flask.
Measure 10 mL of deionized water using a 25 mL graduated cylinder, use this water to rinse the
beaker and funnel and add it to the round bottom flask
When the water bath has reached the desired temperature range, attach a utility clamp to the
neck
of the round bottom flask, and clamp it in place in the water bath.
Heat the mixture in the water bath for 5 minutes while stirring continuously with a glass rod.
Some p-aminophenol will dissolve at this time; the rest will dissolve upon the addition of acetic
anhydride.
In the fume hood, measure 4.0 mL of pure acetic anhydride with a dry 10 mL graduated
cylinder.
Back at your bench, quickly pour the acetic anhydride into the round bottom flask.
Continue heating and stirring the reaction mixture for 5 more minutes. All of the p-aminophenol
should dissolve during this step, and you should observe a clear solution when it does.
Remember that observations need to be recorded on your data sheet throughout the
experiment.
Be sure not note when you next see solid form in the flask.
Remove the round bottom flask from the heated water bath and continue to mix the reaction at
room temperature for 5-10 more minutes (stir with a glass rod, or simply swirl the flask gently).
Next, place the flask in an ice-water bath (mix ice and water in a 250 mL, or larger, beaker) to
cool: DO NOT STIR! The solid product should precipitate from solution. If no precipitate forms
after 10 minutes, scratch the bottom of the flask with a glass rod, to induce precipitation. Cool
for another ~5 minutes after scratching.
Collect the crude product using vacuum filtration. Use a small amount of cold deionized water
to assist in the transfer of the solid to the Buchner funnel. Keep the solid under vacuum for ~5
minutes to dry.
Load a small portion of this crude solid into a melting point tube and set aside for melting point
determination once both crude and purified products are isolated. (Your instructor will
demonstrate how during the pre-lab talk.) After filtration, keep the solid and discard the filtrate
(liquid) into the aqueous waste container.
Part 2: Recrystallization
The crude product will now be purified by recrystallization using DI water as the solvent.
Using a top-loading balance, weigh a clean and dry 125 mL Erlenmeyer flask. Record this mass
on your data sheet. Back at your lab bench, transfer the crude product to the weighed
Erlenmeyer
flask. (Do not transfer chemicals at the balances.) Return to the top-loading balance and
reweigh
the flask plus product. Record this mass on your data sheet. Calculate the mass of crude
product
and record this value on your data sheet.
Add 10.0 mL of deionized water per gram of crude product to the Erlenmeyer flask. Record the
volume of water added on your data sheet. Heat the mixture in the flask on a hot plate until all
the product dissolves, swirl the mixture frequently to ensure even heating. The solution
temperature will need to reach 85-90 °C for the crude product to dissolve.
Once the solid has dissolved, remove the flask from the hotplate and let the flask cool on the lab
bench, undisturbed, to room temperature (~5 minutes). Turn off and unplug the hotplate.
After 5 minutes, carefully move the flask to an ice-water bath for ~10 minutes, do not disturb the
flask while it cools. If after 10 minutes the product has not recrystallized out of solution scratch
the bottom of the flask with a glass rod to induce crystallization, cool for 5 more minutes.
Recover the pure product by vacuum filtration using a small amount of cold deionized water to
assist in the transfer of the solid to the Buchner funnel. Keep the solid under vacuum for 5
minutes to dry. Weigh the purified product using the top-loading balance. Record the mass of
purified product on your data sheet.
Load a sample of purified product into a melting point tube for melting point determination.
Using a MelTemp melting point apparatus from the side bench, take a melting point of both the
crude and purified products. The MelTemp will accommodate up to three melting point tubes, do
both melting points at the same time. Record the melting temperature (or temperature range) for
both the crude and purified products on your data sheet.
Conclusion:
Acid -base reactions (ex. this reaction) are exothermic, meaning they release heat, when water
is produced, the heat the reaction produces fe allows the water to turn into steam/ water vapour,
The water vapour can create a bubbling / fizzing affect
Identify one factor that could cause the percent recovery of copper to be less than 100%.
How could the experiment be modified to prevent this result?
- Copper may have been lost over the course of the experiments. if the final yield is less than
100%. In order to prevent this the person doing the experiment has to be careful to get all the
copper solids or precipitates ford while thransferring, specifically when decanting. Additionally
following the direction closely is important.
6. Was solid cod hen decan i le it oly hat He insteady is important
deviation from 100%?
Our % yield was greater than 100%. Specifically, it was: 267, 78% The reasons for our deviation
include the fact that we did not thoroughly clean our equipment before using it, and we also did
not have sufficient time to evaporate the remaining water, likely along mass to our final product.
One factor causing the yield to be greater than 100% is the presence of impurities in the final
product. To prevent this, one can make sure that all glasswore is clean before use, weigh
reagents as acuranely as possible, keeping temperatures accurate to instructiong stirring
thoroughly,
Throughout this laboratory experiment, the transformation of copper from its metallic form into
various compounds and ultimately back to metallic copper, was observed. The primary objective
was to understand the chemical changes that occur when copper undergoes a series of
reactions.
During this experiment, copper was successively converted into copper (Il) nitrate, copper)
hydroxide, copper(II) oxide, and copper (II) sulfate. Each transformation was accompanied by
specific changes in color, state, and chemical composition. The final step of the experiment saw
the successful return of copper to its metallic form. This reaction illustrated the reversibility of
certain chemical processes and the importance of redox reactions in chemical transformations.
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