Lab 1_ Separation of Liquids by Distillation Procedure (1)
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Feb 20, 2024
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Experiment #1 – Distillation – Report Form
Chem 2221L Fall 2021
Due: 11:59 PM one week after completing Exp 1
Please type your answers in this document and upload your answers to Brightspace.
Write up an introduction for this experiment in the space below.
Separation of Liquids by Distillation
The purpose of this experiment was to analyze the compositions of the distillate fractions
and the remaining solution in the flask to determine the effectiveness of separation of both
toluene and cyclohexane. Distillation is a “process involving the conversion of a liquid into
vapor that is subsequently condensed back to liquid form... Distillation is used to separate liquids
from nonvolatile solids, as in the separation of alcoholic liquors from fermented materials, or in
the separation of two or more liquids having different boiling points.” There are two types of
distillation that are primarily used to separate compounds: simple distillation and fractional
distillation. Simple distillation is a technique used to separate and purify liquids based on their
boiling points. It is used to remove one volatile liquid from another less volatile liquid and
typically required when a liquid compound needs to be removed from a solvent, or as a
purification process. Lastly, it is more effective and will get better results when there is a larger
difference between the boiling points of the two compounds (normally a 50 degree celsius
difference). Fractional distillation uses a fractionating column that allows the vapor to condense
and then re-vaporize at multiple points within the column. While the vapor is condensing, each
“condensation and vaporization produces a vapor that contains a larger percentage of the lowest
boiling point liquid.” Fractional distillation is used when simple distillation has been run and
fails to separate a mixture of liquids. Overall, distillation is typically used when comparing
liquids that have distinct boiling points like toluene (boiling point of 111.0 degrees celsius) and
cyclohexane (boiling point of 80.7 degrees celsius). Both toluene and cyclohexane are flammable
compounds and can cause minor irritants to the skin if contact is made. When setting up
distillation the jack stand and heating mantle need to be carefully assembled so the round bottom
flask (with boiling chip) rests inside the heating mantle with sand filled around it so the heat does
not escape. For fractional distillation only, a fractional column is connected to the round bottom
flask where the condensation and vapor process takes place. Both forms of distillation will have
a short-path distillation head and thermometer to measure the temperature. The short-path
distillation is used in place of the three-way adapter because there is no clamping involved and
when distilling small amounts, very little is lost in the apparatus. Attached to the short-path
distillation are the tubes for water (top one is for water flowing out while the bottom portion is
water flowing into the apparatus) and the angled receiver that receives the distilled liquid. Lastly,
you have keck clamps and 3 pronged clamps, attached to the apparatus for stability. When
running the fractionalized column (rings placed within the fractional column), with the 15 ml
40/60 mixture of toluene and cyclohexane, the resulting Index of Refraction of F, S, and R are: F
= 1.4443, S = 1.4805, R = 1.4952.
Questions to answer.
1)
Attach a graph of your data (temperature vs. volume of distillate collected). If your
goal was to maximize the purity of the cyclohexane collected would you change
when the switch from collecting F to S occurred? If your goal was to maximize the
purity of the toluene collected would you change when the switch from F to S
occurred?
-
During the distillation process, the liquid with the lower boiling point tends to come out
first (cyclohexane at 80.7). When the temperature reaches the boiling point and is able to
vaporize and condense in the fractionalization column, it is best to switch from the first
fraction (F) to the second fraction (S) well before the second boiling point is reached
(toluene 111.0). If too much of toluene is vaporized/distilled into the first fraction (F),
then it would lead to contamination of the cyclohexane in the first fraction. If my goal
was to maximize the purity of both cyclohexane and toluene collected, I would have
switched my receiver tubes earlier (around when the temperature reached 85 or 88
degrees celsius, referring back to my table). This would keep the purity of both
cyclohexane and toluene as pure as possible with little to no contamination.
2)
What volume of liquids (F, S and R) did you recover in the distillation? Where is the
missing material (if there is any missing material)?
-
My angled receiver was placed towards the back, where the numbers were facing away
from me, for this reason, my numbers are not exact. If I was to turn it around and get the
exact volume of distillate recovered, I predict that the total number of distillate recovered
would be less than the amount of the starting liquid mixture (15ml). I predict this because
some of the volume can be vaporized or left in the fractional column due to the high
temperature and the rings I had in the column. Since my total estimation volume is more
than the starting, I also predict that the condensation from the short path distillation tube
went to the receiver tube and resulted in a higher volume count.
-
Estimated volumes: F = 7ml, S = 2.5 ml, R = 5.9 ml = 15.4 ml
3)
Calculate and report the mole fractions of toluene and cyclohexane in the original
mixture and the mole fractions of F, S and R from this experiment. You need only
show one sample calculation.
Ri = (Xt * Rt) + (Xc * Rc)
Xt = (1 - Xc)
1.4952 = (1-Xc)(1.4696) + (Xc * 1.4262)
1.4952 = 1.4969 - 1.4969Xc + (1.4262Xc)
-0.0017 = -0.0707Xc
Xc = 0.024
Xt = 0.976
F) 1.4443s = (0.976)(1.4969) + (0.024)(1.4262)
1.443s = 1.46097 + 0.0342
1.443s = 1.4952
Fs = 1.036
S = 1.009
R = 1.00
4)
Obtain your section’s distillation data (your TA will distribute this to you) and
compare and comment on the compositions of F, S and R in the different distillation
setups.[calculating averages and standard deviations for each style of distillation is
helpful] Can you draw any conclusions from the data?
-
The distillation data of the simple distillation and the different fractional distillation
(empty, steel wool, beads, rings) were consistent throughout the experiment. The original
index of refraction of cyclohexane is: 1.4262 and for toluene: 1.4969. The composition of
the F composition was higher (average of 1.4432) and I predict that most people during
the experiment did not switch the first distillate tube early enough and had some residue
of toluene enter the first receiving tube. The average index of refraction for the second
distillate was 1.4703 which is lower when compared to the original index of refraction of
toluene. The liquid remaining in the flask index of refraction average was 1.4902 which
is closer to the index of refraction for toluene. Since cyclohexane has a lower boiling
point, it should leave the flask first, and the only thing that is left is toluene. I conclude
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that the timing of switching from F to S has to be earlier in the experiment run. The R
index of refraction was closest to the original toluene’s index of refraction.
5)
Which of the following will improve the separation of the mixture during a
distillation? Explain. (MULTIPLE CHOICES)
a)
Decrease the temperature of the heating mantle (but keep it hot enough to still
distill solution).
b) Increase the width of the column
.
c)
Increase the length of the column.
d)
Increase the drop rate at which distillate is collected.
-
Increasing the length and width of the column would improve the separation of the
mixture during distillation. It allows for more cycles of vaporization and condensation in
the fractionalization column which then leads to a better purifying process. In theory, it
provides a longer pathway for the liquid vapor to travel, furthering multiple cycles of the
vaporization and condensation process.
References:
https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9643092/
https://www.britannica.com/science/distillation
https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6781486/
https://www.nature.com/articles/161858a0
https://www.mdpi.com/2227-9717/9/11/2047
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1. what is the concentration in the original bottle (ppm)
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You obtain an Unknown Sample from the Stockroom. You begin testing the solution through the steps outlined in the flowchart of the experiment’s PDF file. You first add HCl and centrifuge your mixture. You observe the formation of a white precipitate in the bottom of the test tube. After pouring off the supernatant liquid, you add hot water to the white precipitate. Addition of the hot water dissolves some of the precipitate, but some white precipitate still remains on the bottom of the test tube.
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Hg22+ is definitely present.
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You obtain an Unknown Sample from the Stockroom. You begin testing the solution through the steps outlined in the flowchart of the experiment’s PDF file. You first add HCl and centrifuge your mixture. You observe the formation of a white precipitate in the bottom of the test tube. After pouring off the supernatant liquid, you add hot water to the white precipitate. Addition of the hot water dissolves some of the precipitate, but some white precipitate still remains on the bottom of the test tube. You pour off the supernatant liquid, and add ammonia (NH3) to the remaining precipitate. You now observe the formation of a gray-black precipitate.
Which of the following is a valid conclusion to draw at this point?
Select one:
Hg22+ is definitely present.
Pb2+ is definitely present.
Ag+ could be present, or Hg22+ could be present, or BOTH could be present.
Ag+ is definitely present
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Data Sheet
4
ble gives the recommended mass of salt to dissolve in each of the four test tubes. Show a
sample calculation for the solubility of KNO, using your actual mass from tube #1. Complete
your graph on the back of this sheet.
Solution #
Recommended
mass KNO3
Actual mass of KNO,
(g per 5 mL H₂O)
Solubility
& KNO,
100 g H₂O
Saturation
temperature
(°C)
(g)
1
2.0
51.3
2.1971
2
62.5
4.0
11.1568
3
72.7
6.0
6.0112
83.6
4
8.0
806
Sample Solubility Calculation:
Questions
1. According to your data, how does the solubility of KNO, change with increasing
temperature? Does this indicate an endothermic or exothermic dissolving process? Explain.
2. Using your graph, indicate if each of these solutions would be saturated or unsaturated:
a) 110 g of KNO3 in 100 g of water at 40 °C
b) 60 g of KNO3 in 100 g of water at 70 °C
c) 140 g of KNO3 in 100 g of water at 60 °C
3. According to your graph, what mass of KNO3 will dissolve in 100 g of water at 30 °C?
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Consider the following scenario:
You obtain an Unknown Sample from the Stockroom. You begin testing the solution through the steps outlined in the flowchart of the experiment’s PDF file. You first add HCl and centrifuge your mixture. You observe the formation of a white precipitate in the bottom of the test tube. After pouring off the supernatant liquid, you add hot water to the white precipitate. Addition of the hot water dissolves some of the precipitate, but some white precipitate still remains on the bottom of the test tube. You pour off the supernatant liquid, and add ammonia (NH3) to the remaining precipitate. You now observe the formation of a gray-black precipitate.
Which of the following is a valid conclusion to draw at this point?
Select one:
1. Hg22+ is definitely present.
2. Pb2+ is definitely present.
3. Ag+ could be present, or Hg22+ could be present, or BOTH could be present.
4. Ag+ is definitely present
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Solution 1 Solution 2
Solution 3
Solution 4
Solution 5
Concentration iron(III) nitrate
0.00200
0.00200
0.00200
0.00200
0.00200
[Fe(NO3)3] (M)
Concentration potassium thiocyanate
0.00200
0.00200
0.00200
0.00200
0.00200
[KSCN] (M)
Volume Fe(NO3)3 (mL)
5.00
5.00
5.00
5.00
5.00
Volume KSCN (mL)
5.00
4.00
3.00
2.00
1.00
Volume DI water (mL)
0.00
1.00
2.00
3.00
4.00
Initial concentration [Fe3+] (M)
0.00100
0.00100
0.00100
0.00100
0.00100
Initial concentration [SCN] (M)
0.00100
0.000800
0.000600
0.000400
0.000200
Absorbance
0.269
0.192
0.154
0.104
0.052
Equilibrium [FeSCN2+] (M)
0.000198
0.000141
0.000113
0.0000765
0.000038
Equilibrium constant Kc
Average Kc
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12:03 AM
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3NO(g) = N20(g) + NO2(g)
Construct the expression for Kc for
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2 X
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Construct the expression for Kc for
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3
CH4(g) + 2H2S(g) = CS2(g) + 4H2(g)
Construct the expression for Kc for
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4 X
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Which of the following is a valid conclusion to draw at this point? (Choose one.)
Select one:
1. Hg22+ is definitely present.
2. Pb2+ is NOT present.
3. Ag+ is definitely present.
4. Pb2+ is definitely present.
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Temperature (°C)
Stirring
small
59
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small
38
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60
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What should the student do?
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water and then stirred the mixture with a stirring rod. When the student carefully
touched the outside of the evaporating dish, do you expect the student to feel hot of
cold? Is the rehydration an exothermic or endothermic process?
4. A student had a sample of CaCl2 • nH2O. He heated the sample until the mass did not
change. From this data, calculate (a). the percentage of CaCl2 in the original sample
and (b). the formula of the hydrate
NOT ROUND
Mass of crucible + cover = 28.39 g T
Mass of crucible + cover + sample = 30.41g
Mass of crucible + cover + residue = 29.75
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