F24 203 Lab 3 Final
F24 203 Lab 3 Final
You will work and discuss in pairs for this lab, Before your lab...
BUT you will individually submit a completed
report. 1. Read briefly through…
ü Lab 3 (this document)
Complete your lab Worksheet at home within
2. Complete…
one week after your lab session. Upload the
Worksheet file (as a PDF) to Gradescope by ü Pre-lab 3 (D2L quiz), with a score of
the starting time of your lab section. 50% or higher
ü Questions P1 and P2 in this
document – Page 12. You will need
What laboratory techniques and skills will you these ideas and values in the lab, so
practice? come prepared! The pre-lab quiz is
• Preparing solutions in volumetric closely related and will help.
glassware
• Calibration and use of a You will not be allowed to
enter the lab have not passed
spectrophotometer
the pre-lab quiz, which closes
What chemical concepts will you apply? 1-h before lab. Contact your
TA or lab coordinator if you
• Solution concentration and dilutions have issues
UCalgary Chemistry Textbook
Molarity; Solutions & Dilutions; If concepts are unclear or new, refer to the
course textbook to review them.
• Equilibrium constants
UCalgary Chemistry Textbook On your lab day...
Chapter 8.4 – Calculation of an • Wear clothes & footwear that covers
Equilibrium Constant any exposed skin below the hem of the
OpenStax 2e lab coat, including your ankles.
Example 13.7 • Bring your lab coat & safety glasses
• Bring printed copies of...
• Spectrophotometry and Beer’s Law ü Lab 3
Beer’s Law Lab (PhET simulation) ü Lab Manual Appendix C (graphs) and
Appendix I (Spectrophotometer use)
What communication and reporting skills will • Bring a pen (not pencil) and scientific
you use? calculator
Background
Ferric thiocyanate, Fe(SCN)2+, is a coloured species produced when the iron (III) cation, Fe3+, reacts with a
thiocyanate ion, SCN−, in aqueous solution as shown in equation [1].
The value of the equilibrium constant K for this reaction can be calculated if the concentration of each species
at equilibrium is known. The magnitude of the equilibrium constant K indicates to what extent a reaction
proceeds, or, phrased differently, the degree to which the products or reactants are favoured. In this
experiment, you will determine the equilibrium constant for this reaction.
By comparing the intensity of light before it hits the sample (I0) versus the intensity of light (I) after passing
through the sample, one can calculate the absorbance (A) or the percent transmittance (%T) of the sample.
Equations [2] and [3] show how this ratio of light intensities relates to the absorbance (A) and percent
transmittance (%T). Since absorbance and transmittance depend on the colour or wavelength of light used, A
and %T are often reported with a subscript (λ) indicating the wavelength of light for those measurements.
In this experiment, you will use a spectrophotometer to measure the absorbance (A) of light for a series of
solutions containing Fe(SCN)2+. Absorbance Beer’s law provides a relationship between the concentration of the
light absorbing species in solution (in this case, [Fe(SCN)2+]) and the measured absorbance values. This
relationship is summarized by equation [4]:
To use equation [4] to determine unknown values of [Fe(SCN)2+]E (and then determine K for the reaction), the
proportionality constant εℓ will be needed. Thus, investigation into the formation of Fe(SCN)2+ needs to be
conducted in two parts.
Part 1. Determination of εℓ
According to equation [4], there is a linear relationship between the absorbance value A and the equilibrium
concentration of the absorbing species [Fe(SCN)2+]E. Thus, graphing the absorbance A as a function of
[Fe(SCN)2+]E should yield a linear plot with a slope of εℓ. Measuring the absorbance (A) values for a series of
solutions with known [Fe(SCN)2+]E values will provide the data needed to determine this proportionality
constant.
But how can we determine the amount of [Fe(SCN)2+]E produced by our reaction if we do not yet know the
equilibrium constant K? Instead, we must choose reaction conditions in Part 1 which force the reaction
effectively to completion.
Once the εℓ value has been determined, you will carry out reaction [1] without pushing the equilibrium strongly
towards the products (i.e. neither reactant will be in great excess to the other as in Part 1). From your
experimentally obtained absorbance (A), you will be able to calculate the equilibrium concentration of
[Fe(SCN)2+]E using Beer’s law (equation [4]) and the value of εℓ from Part 1.
Since the change in the amount of each compound is related by the molar coefficients in the chemical equation,
you can use an ICE table to calculate the values of [Fe3+]E and [SCN] as shown in the example below. When all
equilibrium concentrations have been calculated, the value of K for reaction [1] can be determined. By
performing the reaction five times using different initial concentrations of reactants, you will investigate the
effects of this change on the equilibrium constant K.
The equilibrium constant, K, for the reaction is given by the expression where the subscript E indicates that the
concentration is measured at equilibrium:
['((*+,)!" ]#
𝐾= ['( $" ]# [*+, % ]#
[6]
Scenario: Suppose a student prepares a test tube in Part 2 such that the initial concentration of [Fe(NO3)3]0 is
0.00025 M and the initial concentration of [KSCN]0 is 0.00032 M. They determined from their absorbance
measurements that the equilibrium concentration of [Fe(SCN)2+]E was 1.1x10-5 M. What will be the
equilibrium concentrations of [Fe3+]E and [SCN]E?
As described above, the student used their experimental absorbance measurement for this solution to determine
that [Fe(SCN)2+]E was 1.1 × 10-5 M. Therefore, x = 1.1 × 10-5 M, and we can use this value to solve for the other
two equilibrium concentrations in the table.
Procedure
Take notes in the margins during the lab presentation, especially when your TA provides suggestions for
time management.
Part 0: Preparation
3. Rinse spectrophotometer cuvettes with RO water. These do not need to be dried, as they will be rinsed
with your solution before each use.
4. Label a 600 mL beaker as waste and use this to collect your aqueous waste and rinse solutions at your
benchtop during the experiment.
Part 1: Determination of εℓ
5. Mark the five clean and dry test tubes with identification numbers (1 through 5).
The order in which solutions are added to the labelled test tubes does not matter in Part 1, so you can
complete this part efficiently by dividing up the work between partners.
Partner A
A7. Pour some of your dilute Fe(NO3)3 solution from the volumetric flask into a small beaker that you can
pipette from. Label and rinse a 10.0 mL graduated pipet with the dilute Fe(NO3)3 solution. Discard
each of the rinsing solutions. Transfer aliquots of dilute Fe(NO3)3 solution to the five marked test tubes
in the amounts outlined in Procedure Table A.
The graduated pipets
Partner B used in CHEM 203
allow you to measure
by differences. Use
B6. Collect no more than 40 mL of 1.0 M KSCN solution in a
your finger to stop the
labelled 50 mL beaker. Cover this beaker with a clean flow of solution.
watch glass when not in use. Label and rinse a second
10.0 mL graduated pipet with this solution, then add Do not allow the liquid
5.0 mL of the 1.0 M KSCN solution to each test tube (as level to go below the
10.0 mL mark – the
outlined in Procedure Table A). Record the exact volume in the tip of the
concentration of this solution in Data Table 0. pipet is not measured.
Now that all five samples have been prepared, work together to make your measurements.
8. Stopper each test tube with a previously washed and dried rubber stopper then thoroughly mix the
contents of each test tube.
9. Using a spectrophotometer, measure the absorbance of each solution in order of increasing initial
concentrations of Fe3+ as follows (refer to Appendix I as needed):
Check that the wavelength is correctly set for the experiment (λ = 450nm) AND
that the reading mode of the spectrophotometer is set for Absorbance.
Your lab TA must check and initial your data from Part 1 before you continue.
If there are any problems with your values, these should be sorted out
before creating more serious difficulties in Part 2
10. After your TA has approved and initialed your data from Part 1, you can dispose of any remaining
1.0 M KSCN solution and any remaining dilute Fe(NO3)3 solution into your waste beaker. Neither of
these solutions is used in Part 2. Wash and dry the test tubes and stoppers used in Part 1. Re-number
the test tubes (6 through 10).
Here, the order in which solutions are added to the labelled test tubes can help you ensure that you get reliable
results (see margin notes).
B12. Refill your previously used HNO3 beaker so it contains at least 40 mL of solution. Using your already
labeled 10.0 mL graduated pipet (from Part 1, step B7), add the correct amount of 0.1 M HNO3 solution
as given in Procedure Table B to bring the total volume of solution in each test tube to 10.0 mL.
Now that all five samples have been prepared, work together to make your measurements.
13. Stopper each test tube with a previously washed and dried rubber stopper. Then thoroughly mix the
contents of each test tube.
15. Use the digital thermometer to measure the temperature of reaction mixture in Test Tube 6. Record
this value for reference in Data Table 2.
16. Rinse the spectrophotometer cuvettes, pipets, rubber stoppers and test tubes with copious amounts
of RO water.
17. Clean all labels from your beakers and test tubes using a Kimwipe dampened with a small amount of
methanol.
18. Have your lab TA check your cleaned Supplementary Equipment Tray.
Your lab TA must check and initial your data from Part 2 before you leave. Your TA will
also check that your equipment has been cleaned and returned before signing.
If you have time, we strongly advise staying in the lab to begin your calculations with TA support!
• Update or complete your calculations P1 and P2 (Page 12) using the actual stock
concentration of Fe(NO3)3. Repeat the process in calculation P2 to fill-in the remaining
concentrations in Data Table 1 (Page 13).
• Complete the sample calculation in Question 3 (Page 18) in the Worksheet. Repeat this
process to calculate all initial concentrations in Part 2, [Fe3+]0 and [SCN-]0, and fill these in
Analysis Table 1 (Page 15).
If you wish, you can also graph your data from Part 1 by hand using the graph paper provided on
Page 16. Rulers are provided in the lab for drawing your line-of-best fit. Guidance in Question 2
(Page 17) of the worksheet will help you.
DUE DATE: One week after your lab period, at the regular start time for your lab.
Grade deductions may apply if your submission for this report does not meet all these criteria.
Academic Integrity Note: Remember, even though you collected your data with a partner, your worksheet
should be completed individually. You should use your own data, and you may consult the lab manual, lab
appendices, lecture notes, course textbook, and your TA.
Pre-laboratory preparation
As part of your pre-lab quiz on D2L, you were asked questions about calculations you will use in the lab. Before
you arrive at the lab, use the feedback received on your quiz to layout the sample calculations below so you can
repeat them confidently during the lab period. Show all work for full credit.
P1. Diluted Fe(NO3)3 (aq) prepared for Part 1 RELATED TO PRE-LAB QUIZ QUESTION 7
3+
Calculate the concentration [Fe ] in the dilute solution that Partner A prepares in Step A6 of the
procedure. Show all your work and use the exact concentrations in your laboratory room.
P2. Part 1: Initial [Fe3+]0 concentration calculation (Pages 5-6) RELATED TO PRE-LAB QUIZ QUESTION 8
3+
Calculate the initial concentration of [Fe ]0 in Reaction 3 according to Procedure Table A.
Note that initial concentrations refer to the concentration after all solutions have been mixed in the test
tube, but before any reaction has taken place.
Show all your work and use the exact concentrations in your laboratory room.
NOTE: You will repeat a similar calculation to determine all concentrations in Data Table 1.
• Use the exact concentrations from your laboratory room, as recorded in Data Table 0 (not the
approximate concentrations from your procedure).
• Use the notes next to Data Table 1 and what you learned from PRE-LAB QUIZ QUESTION 9 to relate your
calculated [Fe3+]0 to the [Fe(SCN)2+]E in Part 1.
Part 1 Part 2
Data Table 1: Raw Data from Part 1 – Calibration curve for Determination of εℓ
7 1.00 2.00
8 1.00 3.00
N/A
9 2.00 2.00
10 2.00 3.00
TA initials here
Data Analysis
Complete your analysis for both Part 1 and Part 2 in the pages that follow – summarize your results below.
Initial concentrations
Equilibrium concentrations
in reaction mixtures Absorbance
KC
Rxn (450 nm)
[Fe3+]0 (M) [SCN-]0 (M) [Fe(SCN)2+]E (M) [Fe3+]E (M) [SCN-]E (M)
#
10
Hints: Work through the sample calculations Questions 2-6 which focus on just Reaction 10 – and then repeat the
process for your other rows. An ungraded D2L quiz is also available for feedback, to help you check that you
have the right process for calculating each column value.
Make sure that you are using the correct Part 2 stock concentrations from Data Table 0.
Detailed Graph Title (refer to Appendix C - Visualizing Experimental Data with Graphs for guidelines)
Hand-draw your Part 1 graph here or REPLACE this page in your PDF with a graph you
make in Excel or other graphing software.
Sample Calculations
Question 2: (a) Graph your data for absorbance vs. FeSCN2+ concentrations from Part 1 on the previous
page. You can use the provided graph paper OR use graphing software such as Microsoft Excel.
If graphing by computer, REPLACE the provided blank graph paper page with a page containing
your final graph.
Using either method, make sure that…
• Your graph is sized to fills a reasonable portion of the page.
• You follow the graphing format guidelines in Appendix C (Page A12). Note: Since only
one quantity is being graphed, a legend is not required.
• You include a straight line-of-best-fit (review your pre-lab quiz and procedure margin
questions for ensuring your line is appropriate).
(b) Calculate a value for eℓ from your graph.
If you graphed by hand, state the points used from your line of best fit AND show your
calculation below.
If you graphed by computer, display the computer’s equation for the line-of-best-fit on your
graph AND copy that equation into the space below.
The sample calculations in Questions 3-6 will help you fill-in Analysis Table 1 based on your data from Part 2
If you want to check that you have the right approach, an ungraded “post-lab” quiz is available on D2L that can
help you check your work using sample values.
Question 3: Calculate the initial reactant concentrations for both [Fe3+]0 and [SCN–]0 in Reaction 10.
Remember that initial concentrations refer to the concentration after all solutions have been
mixed in the test tube, but before any reaction has taken place.
Question 4: Use your absorbance measurements and calculated εℓ to calculate the equilibrium
concentration of ferric thiocyanate [Fe(SCN)2+]E for Reaction 10 in Analysis Table 1.
Question 5: Use an ICE table, initial reaction concentrations, and your calculated value of [Fe(SCN)2+]E to
calculate [Fe3+]E and [SCN-]E for Reaction 10 in Analysis Table 1.
A sample ICE table setup is shown in the Background on Page 4.
Question 6: Calculate a value for the equilibrium constant, K, for Reaction 10 in Analysis Table 1.
Statistical analysis
Question 7: Calculate the average value of the equilibrium constant, K, for the formation of Fe(SCN)2+ based
on your data from Reactions 6-10 in Part 2.
Question 9: Standard deviation is one way to measure or quantify the spread or variation in a pool of data.
Calculate the standard deviation for your equilibrium constant, K.
See Lab Manual Appendix C (linked in the materials in Lab 1 on D2L) for details on how to
calculate the standard deviation.
Question 11: In 1 sentence, comment on the precision of your experimentally determined value of K for this
reaction, using value(s) from your statistical analysis to support your claim.
Question 12: Experimental design. Why is spectrophotometry used in this experiment? Provide the evidence
(facts) and reasoning (why) that support the claim that spectrophotometry is an appropriate
technique to meet your experiment goals. Use 1-2 sentences.
Question 13: Experimental design. (a) Explain why we used an excess of KSCN in Part 1. State what we
assume about how this excess affects the reaction(s) and why this is needed to achieve the
experiment goal(s). Use 2 sentences.
(b) If this assumption was not true, would it affect the accuracy of your result? Would it affect
the precision? Use 1 sentence.