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Procedure:

Day One
Preparation of Crystals:
For this step on our experiment both of our groups did a pretty much identical procedure,
1. Using a 10.0ml graduated cylinder, we carefully measured out 8.00ml of 2.50M
FeCl3.6H2O, and transferred it into a 50ml beaker. (Then we set it aside)
2. We weighted out 12.0052g of K2C2O4.H2O, for this we used a 50ml beaker, a spatula and
the analytical balance found in the stock room. To get the an accurate reading we first
placed the beaker in the analytical balance and pressed the TARE button. After the
reading stabilized at zero, using our plastic spatula we slowly added the solid from the
container into our beaker. Then we took it to our workstation where we transferred our
solid into a 150ml beaker, then using our graduated cylinder twice, we measured out
about 20ml of distilled water and poured it into the 150ml beaker.
3. Then we set up the hot plate, we turned the dial to setting 3 and kept it there for the
entirety of the heating process. After the hot plate was hot enough, we placed the beaker
containing the potassium oxalate mixed in water on top of it. We stirred it using one of
our glass stir rods making sure not to boil the solution, until all the solid dissolved in
solution. It took about a total of 5 minutes for all the solid to dissolve, during the process
we added a little more water to aid in the dissolution of the solid, because some of it
evaporated during the heating. When a temperature reading was taken it was 57oC, Tara
and Destineys group found a temperature of 51.5oC when the solid dissolved, we found
the ideal temperature for the solid to dissolve to be around 50-55oC.
4. After the potassium oxalate was completely dissolved, we took our iron (III) solution and
placed it close to our hot plate, then using beaker tongs we removed our oxalate solution
from the hot plate and immediately poured it into our 50ml beaker containing our iron
(III) solution. The solution turned green immediately, which indicated we successfully
formed the green crystalline compound. We shook it slightly to aid in the mixing of the
compounds. During our experiment we found a white residue left in our oxalate
containing beaker as it cooled down, it is completely normal.
5. Setting the new solution aside, we prepared an ice bath to cool down the solution. For the
ice bath we took a small amount of ice into a 250ml beaker and added a little water. Gave
it a couple seconds to cool down and then we placed our beaker containing the green
solution into it, we let it sit there for a total of 30 minutes. During the cooling process, the
actual crystals started to form, and they started to appear after about 1 minute. While the
solution was cooling down, we switched the ice and water once, because most of our ice
had melted off already.
6. After the 30 minutes, we decanted the supernatant (liquid above the precipitate) into our
waste beaker and then into the waste container, we did it very slowly and carefully in
order to not lose any of our crystals. Then we moved on onto the recrystallization.
7. For the recrystallization, we used our 10.0ml graduated cylinder twice in order to add
20ml of distilled water into our crystals. Then keeping the hot plate on the setting 3, and

while stirring with a glass stir rod, we slowly heated our crystals solution, we continued
until all the crystals dissolved. The temperature reading when all crystals were dissolved
was 55oC.
8. The next step in the process was to create large crystals, and that required us to cover our
solution beaker with either a watch glass or parafilm with holes in it, and then place it
into our lockers, making sure to keep it in the dark.For about 1 day.
Because of time constraints, we skipped this step and opted to form small crystals.
In order to form our crystals, we prepared another ice bath, took water and ice into a
250ml beaker. Then we submerged our beaker with green crystal solution into the ice
bath. We then let it sit for about 30 minutes, during this time, crystals will form.
Comparing to our first crystal formation, this time it took longer for crystals to form.
9. While the crystals were forming we prepared another ice bath, then we filled two test
tubes with distilled water and placed them into the new ice bath. All of this was done in
preparation to vacuum filter the crystals.
In order to vacuum filter our crystals, we first had to set up a Buchner funnel and filter
flask. For this we took the funnel inserted in a rubber stopper and inserted it into the filter
flask, then we connected the rubber hose to the flask and lab faucet. After that we took a
filter paper and set it inside the funnel, once inside we wetted it with a little distilled
water. The setup is complete.
To do the actual vacuum filtration we opened the water in the faucet, this creates a
vacuum which helps dry the crystals, then we poured our solution into the funnel making
sure that the crystals also went into the funnel. Once all the crystals were inside the
funnel we rinsed them a couple times with about 5ml aliquots of the cold water we had
cooling in the test tubes. After the filtration was done we saved the filtrate in one 250ml
beaker. After that we rinsed the crystals twice with 5ml aliquots of acetone in order to
remove all the water. We discarded this new filtrate into the waste container. (The
aliquots were just estimated, not exactly 5ml were measured)
10. Once all filtrations were done, we carefully took our crystals from the Buchner funnel
and placed them into a watch glass, and discarded the filter paper in the trash can. Then
we took some parafilm, poked holes in it with a medicine dropper and covered our
crystals. Finally, we placed the watch glass with our crystals into our locker to let the
acetone and water slowly dry out.

Day Two
Determination of % Water: (This Procedure was completed by Destiney and Taras group)
1. We took two crucibles, cleaned them and dried them.
2. After they were cleaned, we placed them into 50ml Beakers. Then we labeled each
beaker 1 and 2, with pencil.
3. Simultaneously we took both beakers to the oven room, and placed them inside the oven
using beaker tongs, the oven was preset to 110-120oC. We left them there for about 5
minutes and we removed them from the oven using the beaker tongs because now the
beakers are really hot. We allowed them to cool off to room temperature and took them to

the analytical balance in order to take the mass of the crucibles. To take the
measurements we used the same analytical balance for all our readings. Once we were
ready, we took the crucibles from the beakers using clean crucible tongs to make sure that
we didnt changed the weight by touching them, and we placed them inside the analytical
balance and took our readings to 0.0001g. We repeated this process until we achieved a
constant weight, meaning that no moisture or water was present anymore in our crucibles.
First heat
Second heat
Third heat

Crucible 1
44.0897
44.0017
44.0015

Crucible 2
44.2562
44.2533
44.2529

4. Now that the crucibles have been brought to a constant mass we move on to weight our
samples. We took two duplicate samples, to weight our samples we took our crystals to
the weight room and using weighing paper and TARE function we took our
measurements. Our two samples were 1.0784g and 1.0086g, and placed each sample into
one of the crucibles.
5. Then, using the crucible tongs we placed the crucibles inside the 50ml beakers once
again. And repeated the process to obtain a constant weight. Place them inside the oven,
let them cool, remove from beaker and take the weight to 0.0001g in the analytical
balance.
First heat
Second heat
Third heat
Four heat

Sample 1 and crucible 1


45.0799
44.8960
44.8936
44.8921

Sample 2 and crucible 2


45.2615
45.1771
45.0871
45.0867

After we have recorded all the data, we kept the crystals in our drawer.

Determination of %K and %Fe: (This Procedure was completed by Susana and Jovanys Group)
For this step on our experiment Susana and Jovany followed an identical process.
1. We had to test two duplicate samples, for this we took a sample from our crystal batch
and one form the other group crystal batch.
2. To weight the samples, we took both crystal batches to the weighing room, there we
placed a 50ml beaker inside the analytical balance and pressed the TARE function. Once
the reading stabilized, we slowly started to add crystal into the beaker.
Sample 1: 0.1538g
Sample 2: 0.1570g
3. After we measured out 4ml of distilled water in our 10.0ml graduated cylinder, and added
it to the beaker. And dissolved the crystals. We covered the beaker with parafilm and
placed it aside.
4. Now we set up for the ion exchange column. We took a lab stand, secured a burette clamp
to it, and clamped our ion exchange column to it. Then we removed both covers from the

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ion exchange column, one at the top and one small one at the bottom. After this we set up
a waste beaker under the tip of the ion exchange column to collect the filtrates.
We then rinsed the ion exchange column with 10ml of 0.1M HCl, we measured this with
a 10.0ml graduated cylinder. (always make sure to not let the column run dry) collect this
rinse in your waste beaker and discard it into the waste container.
We measured 4ml of distilled water with our 10.0ml graduated cylinder and we rinsed the
column with it. After that we let the column run until the liquid almost touched the resin
and closed the ion exchange column. Then using pH paper we touched the tip of the ion
exchange column to take a pH reading. We repeated this process until we got a pH
reading which was identical to that of distilled water. It took 4 rinses.
1st Wash - Light Orange Distilled Water Dark Yellow Slightly Greenish
2nd Wash - Light Yellow
3rd Wash - Dark Yellow
4th Wash - Dark Yellow Slightly Greenish
-Based on these reading the pH of distilled water that day was about 6-7
Then we set up for the filtration of the crystal solution. We placed a clean and dry 150ml
beaker under the tip of our ion exchange column to collect the filtrate. Now we carefully
poured our crystal solution into our ion exchange column and let it run making sure to not
let it run dry. Then we measured 4ml of distilled water in our 10.0ml Graduated Cylinder
and poured it into our ion exchange column, and let it run. We repeated this process once
more, and collected both filtrates in the same 150ml beaker. We then covered the beaker
with parafilm and set it aside.
After the last rinse we placed our waste beaker under the ion exchange column and in
order to regenerate the column we rinsed it with 10ml of 1.0M HCl, we collected this
filtrate and discarded it into the waste container.
Due to time constraints we stopped our experiment here and continued on the next day.

Day Three:
Continuation of %K and %Fe Titrations:
Tara and Destineys group completed one titration and Jovany and Susanas Group Completed
another titration. We followed similar procedures.
1. We set up for a titration procedure. First we prepared our burette stand. We placed a lab
stand in our workstation, and secured a burette clamp to it. Then we prepared our burette.
2. First set up a waste beaker to capture all your rinses. To prepare our burette first we
rinsed twice with distilled water, letting it flow out from the tip and also rinsing the whole
burette. Then we rinsed the burette twice with 5ml samples of Standardized NaOH,
following the same procedure as with the water rinses. Then, we filled it with about 50ml
of Standardized NaOH and let it run for a little bit, until all the bubbles from the tip
disappeared. The molarity of NaOH that day was 0.10524M.Finally, we secured our
burette to our Burette Clamp and discarded the rinses into the waste container.
3. The next step was to set up the magnetic stirrer. First we took the hot plate and set it to
the stir setting, then took one small magnetic bar, cleaned it and placed it into our green

crystal solution. Then took our solution beaker and placed it on top the hot plate, making
sure that the magnetic bar was spinning and not getting hot.
4. Then we set the pH meter. First of all, we calibrated our pH meter using both 4.0 and 7.0
calibration solutions. A detailed procedure is found in the website. After that we took the
electrode and submerged it into our solution. We added distilled water into our solution to
make sure that the electrode was sufficiently submerged in water, and the magnetic stir
bar didnt hit the electrode. And we started our titration.
5. We started our titration by taking pH readings at every 0.1 pH change. And after the
inflection points we started adding bigger increment of NaOH.
6. Then we graphed our data, which showed two inflection points.
Crystalline Shape Investigation:
1. To investigate the shapes of our crystals, we first gathered samples of our crystals and
took them into the balance room.
2. Then using a microscope plastic slide, we placed samples of our crystals one by one
under the microscope. And using our phone cameras, we took pictured of all the crystals
in order to analyze the images.
3. Basic observation include that hydrated crystals, look shiny and the shapes are sharper.
Also the crystals look a little translucent. Semi-hydrated crystals are not as shiny and the
shapes start to look more uniform, the crystals are no longer translucent. The dry crystals
have lost all shine to them and the shapes are more uniform, almost rocklike.
Ultraviolet Light Investigations:
This part of the procedure was performed by Tara and Destineys Group
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We obtained a sample of 0.2034g in the analytical balance.


We added 10ml of distilled water to the sample.
We filled the cuvette with distilled water and we calibrated it at 500nm
We rinsed the cuvette with 1ml of solution twice. Then we filled it and measured it at
500nm and calculated its molar absorptivity at 500nm.
We calibrated %T to 100 and set nm to 500 before measuring blank.
Then we measured the blank with 500nm and %T being at 100.0
The we calculated molar absorptivity and found it to be 0.186ABS
Then we set it at 400nm, reset the %T to 100.0 and continued to measure solution at
every 20nm (400nm-580)
The wavelength of maximum absorbance we found to be 600nm and the absorbance was
1.46abs.

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