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Name: Amalawa Aiwekhoe Quiz Section: AG

Lab Partner: Shumaila Student ID #: 1866021

CHEM 162 Experiment #4


Part I. Fractional Crystallization of KNO3 with (NH4)2Fe(SO4)2·6H2O Impurity
Part II. Determining the Solubilty Curve of KNO3
Goals of this lab:
Demonstrate the purification of a solid sample using the process of fractional crystallization
Construct a solubility curve for potassium nitrate
Apply the mechanics of dimensional analysis and an understanding of solubility of solids to calculate %
composition by mass, % impurity, % recovery, solubility product constant, enthalpy of solution formation,
entropy of solution formation
Apply Beer's law to detect the amount of impurity in a solid sample
Assess the accuracy of experimental data (compared to a known value) and identify sources of error
Use Excel to graphically represent and interpret experimental data

Your lab report will be grade on the following criteria using a poor/good/excellent rating system:
Data and results are detailed, reasonable, and complete
Calculations are complete and correct, with proper use of significant figures and units
Conclusions are reasonable and logical
Error analysis is well-supported and valid
All graphs and tables are clearly and accurately labeled; entire report is typed

By signing below, you certify that you have not falsified data, that you have not plagiarized any part of t
lab report, and that all calculations and responses other than the reporting of raw data are your own
independent work. Failure to sign this declaration will result in 5 points being deducted from your lab s

Signature: __Amalawa Aiwekhoe______________________________________

This lab is worth 60 points: 10 points for notebook pages, 50 points for the lab report
(Do NOT include your notebook pages when you scan your report for upload into Gradescope.)

Laboratory Waste Evaluation


Laboratory waste is considered anything generated during an experiment that is disposed of down the sewer drain,
thrown in the garbage, collected in a container for disposal by the UW Environmental Health & Safety department,
released into the environment. Based on the written lab procedure and your actions during the lab, list the identity
approximate amount (mass or volume) of waste that you generated while performing this experiment.

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approximate amount (mass or volume) of waste that you generated while performing this experiment.

Note: All sections of this report must be typed


DATA, CALCULATIONS, AND GRAPHS
Part I. Fractional Crystallization of KNO 3 with (NH4)2Fe(SO4)2·6H2O Impurity
A. Starting Components (Fract. Crystallization #0)

Step 3: Mixture before first crystallization

mass KNO3 4.501


mass (NH4)2Fe(SO4)2.6H2O 0.503
Total mass of the sample mixture 5.004
% Impurity (i.e., % Fe compound in the mixture)* 10.05
*(This is your % impurity for Fract. Crystallization # 0)

Fract. Crystallization #1

Step 7: mass of dry filter paper + watch glass 46.048

Step 10: mass of KNO3 crystals + filter paper + watch glass 50.544
mass of KNO3 crystallized 4.064
% KNO3 recovered (% of KNO3 in Step A.3.) 90.291

Step 11: mass of KNO3 crystals to be analyzed for purity in Part I.C 0.121

B. Fract. Crystallization # 2 (Re-crystallization)

Step 5: mass of dry filter paper + watch glass 31.445

Step 7: mass of KNO3 crystals + filter paper + watch glass 32.179


mass of KNO3 crystallized 0.734
% KNO3 recovered (% of KNO3 in Step A.3.) 16.150

Step 8: mass of KNO3 crystals to be analyzed for purity in Part I.C 0.397

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C. Analysis to Determine % Impurity
First Crystallization
Step 3: Absorbance of the Fe(phen)32+ complex at 510 nm 1.735

Does the absorbance exceed the desired range (0 to 2.0 A)? ____________

If so, what dilution factor did you use in order to get the absorbance in the desired range? _____________
What is your absorbance after dilution? (if applicable)

Multiply your absorbance by the dilution factor (if applicable)

Molar Absorptivity of ferroin, e 1.25E+04


Calculate the molarity of Fe2+ from the absorbance (pathlength = 1 cm)

Type your calculation for molarity of Fe2+ (1 mol ferroin = 1 mol Fe2+)

A =εbc b=1 cm A=1.735 ε=1.25E+04

1.735/(1cm*12500M^-1cm^-1)=c= 1.388e^-4

Volume of ferroin complex solution prepared in Steps C.1. and C.2. 0.0100
Calculate the moles of Fe2+ (moles of Fe2+= moles of (NH4)2Fe(SO4)2·6H2O) 1.39E-06

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Type your calculation for moles of Fe2+

Molarity (M) = mol/L M= 1.388e^-4 L=0.01

1.388e^-4 M*0.01L=mol=1.388e^-6

Calculate the molar mass (NH4)2Fe(SO4)2·6H2O 392.21

Calculate grams of (NH4)2Fe(SO4)2·6H2O in the crystals 5.44387E-4

Type your calculation for grams of (NH4)2Fe(SO4)2·6H2O

molae mass = g/mol mol=1.388E-6

392.21 g/mol*1.388e^-6 mol = 5.44387E-4

Mass KNO3 crystals analyzed for purity (from Step A.11.) (this cell will autofill) 0.121
Calculate % mass of (NH4)2Fe(SO4)2·6H2O in the crystals 0.449907
(This is your % impurity for Fract. Crystallization # 1)
Type your calculation for % mass of (NH4)2Fe(SO4)2·6H2O in the crystals.

%mass = [(mass impurity)/(mass KNO3 crystals)]*100

mass impurity = 5.44387E^-4 mass KNO3 crystals = 0.121 g

(5.44387E^-4 g/0.121 g) = 0.449907

Second Crystallization
Step 3: Absorbance of the Fe(phen)32+ complex at 510 nm 0.195

Does the absorbance exceed the desired range (0 to 2.0 A)? ____________

If so, what dilution factor did you use in order to get the absorbance in the desired range?
What_____________
is your absorbance after dilution? (if applicable)

Multiply your absorbance by the dilution factor (if applicable)

Molar Absorptivity of ferroin, e 1.25E+04


Calculate the molarity of Fe from the absorbance (pathlength = 1 cm)
2+
0.000

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Volume of solution prepared in Steps C.1. and C.2. 0.0100
Calculate the moles of Fe2+ (moles of Fe2+= moles of (NH4)2Fe(SO4)2·6H2O) 1.56E-07

Calculate the molar mass (NH4)2Fe(SO4)2·6H2O) (this cell will autofill) 392.21
Calculate grams of (NH4)2Fe(SO4)2·6H2O in the crystals 6.12E-05

Mass KNO3 crystals analyzed for purity (from Step B.8.) (this cell will autofill) 0.397
Calculate % mass of (NH4)2Fe(SO4)2·6H2O in the crystals 0.0158069
(This is your % impurity for Fract. Crystallization # 2)

Summary: % Impurity as a Function of Cystallization Number


Crystallization
% Impurity
Number
0 10.052 Note: Data is being restated here for
ease in plotting. The cells for % impurity
1 0.450 will autofill from your entries above.
2 0.016

Plot a graph of percent of (NH4)2Fe(SO4)2.6H2O vs.number of crystallization steps (0,1,2) and place it here. Cover this
Function
instruction box so that your graph is an ofsize.
appropriate Crystillization Numbers
12.000
Be sure to include a title, axis labels, and use the following chart type: "XY (scatter) with straight lines and markers."

10.000

8.000
%impurity

6.000

4.000

2.000

0.000
0 0.5 1 1.5 2 2.5
Number of Crystallizations

Part I Results and Discussion


Q1.Do your results indicate that fractional crystallization works? Why or why not?

Yes, since the the %impurity decrease over the number of crystallization. The proccess has produced more pure samples the
more times we repeated steps. This works because KNO3 is saturated when at higher temperatues but not with impurities, so
when cooled the KNO3 crystals form with less impurities because they dissolved.

Summary: % Mass KNO3 Recovered in Crystallization Steps


Note: Data is being restated here for ease in plotting. For the
mass of KNO3 crystallized in crystallization #0, the starting mas
Page 5 of KNO
18 3 you weighed out in Step A.3. will be the mass crystallized
resulting in 100% recovery. The cells for the mass of KNO3
crystallized and % of original KNO3 will autofill from earlier in th
Crystallization Mass KNO3 % of Original KNO3 Note: Data is being restated here for ease in plotting. For the
Number Crystallized Mass mass of KNO3 crystallized in crystallization #0, the starting mas
KNO3 you weighed out in Step A.3. will be the mass crystallized
0 4.501 100.0
resulting in 100% recovery. The cells for the mass of KNO3
1 4.064 90.291
crystallized and % of original KNO3 will autofill from earlier in th
2 0.734 16.150
report.

Plot a graph of percent of KNO3 recovered vs. the number of crystallization steps and place it here. Cover this instruction
Loss
box so your graph is appropriately sized. ofgraph
Your KNO3 Through
should Crystalization
have three points with the first point being 100%.

Be sure120.0
to include a title, axis labels, and use the following chart type: "XY (scatter) with straight lines and markers."

100.0

80.0
%KNO3 recovered

60.0

40.0

20.0

0.0
0 0.5 1 1.5 2 2.5

Number of Crystalizations

Part I Results and Discussion


Q2. What is the disadvantage of fractional crystallization?

The disadvantage would be the loss of subtance we began with as we start to purify our solution through
crystallization. looking at our loss of KNO3 we only had about 19% which shows we lost nearly all of our KNO3 in
the process.

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101.11

Part II. Determining the Solubility Curve of KNO 3


Solubility (in g KNO3 Molality KNO3 Ksp
Grams KNO3 Cryst. Temp, oC 1/T (K)
per 100 g water) (mol/kg) (using molality)
2.004 20.6 40.08 3.964 15.71 293.75000
3.008 43.0 60.16 5.950 35.40 316.15000
4.014 55.7 80.28 7.940 63.04 328.85000
5.014 61.0 100.28 9.918 98.36 334.15000
7.000 65.0 140.00 13.846 191.72 338.15000
7.990 70.0 159.80 15.805 249.78 343.15000

Type your calculation for solubility (in grams KNO3/100 grams water) using the data for the ~2.0 gram sample.

Type your calculation for molality of KNO3 (in mol KNO3/kg water) using the data for the ~2.0 gram sample.

Type your calculation for Ksp (using the molality values) using the data for the ~2.0 gram sample.

Plot a graph of solubility of KNO3 (g KNO3 / 100 g H2O) vs. Temperature(oC) and place it here. Cover this instruction
box so that you graph is appropriately sized.

Be sure to include a title, axis labels, and use the following chart type: "XY (scatter) with straight lines and markers."

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Be sure to include a title, axis labels, and use the following chart type: "XY (scatter) with straight lines and markers."

(Data autofills here from the previous page for ease of plo
Plot a graph of ln Ksp vs 1/Temperature(K) and place it here. Cover this instruction box so that you 1/T (K)
graph is appropriately sized. 293.75000
Be sure to include a title, axis labels, a trendline for the data, and the equation for the trendline. 316.15000
328.85000
334.15000
338.15000
343.15000

slope K-1 y-intercept


DH o
Soln kJ/mol DSoSoln J·mol-1·K-1

Type your calculations for DHsoln and DSsoln.

Part II Results and Discussion


Q1. The literature value for the enthalpy of solution of KNO3 is 34.89 kJ/mol and the entropy of solution of KNO3 is
248 J·mol-1·K-1. How do your values compare? Calculate the % error for both the enthalpy and entropy.

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Part II Results and Discussion
Q1. The literature value for the enthalpy of solution of KNO3 is 34.89 kJ/mol and the entropy of solution of KNO3 is
248 J·mol-1·K-1. How do your values compare? Calculate the % error for both the enthalpy and entropy.

Q2. Discuss reasonable source of error for both the measured values of enthalpy and entropy.

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mpurity

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M-1cm-1
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g/mole

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L
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ln Ksp

2.7545
3.5668
4.1438
4.5887
5.2560
5.5206

am sample.

sample.

instruction

d markers."

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d markers."

e for ease of plotting)


ln Ksp
2.75450703
3.567
4.144
4.589
5.256
5.521

n of KNO3 is
py.

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n of KNO3 is
py.

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