Revised 11/14/17

CHM 112 Determination of Equilibrium

Constant
The equilibrium state of a chemical reaction can be characterized by quantitatively defining its
equilibrium constant, Keq. In this experiment, you will determine the value of Keq for the reaction
between iron (III) ions and thiocyanate ions, SCN–.
Fe3+ (aq) + SCN– (aq) ↔ FeSCN2+ (aq)
When you mix amounts of Fe3+ and SCN–, a reaction occurs to produce FeSCN2+, but not all of
the reactants react. Thus, your beaker (or flask or cauldron) will contain some of each of these
three species, which is your equilibrium system. To learn more about the system, we need to
figure out a way to count the number of different ions in the reaction mixture. That is the major
objective of this experiment, and to achieve this objective you will take advantage of something
about FeSCN2+ – in aqueous solution it has a reddish color. The two reactants, Fe3+ and SCN–, are
essentially colorless in solution, thus the red color you will see when you conduct the reaction is
produced by the FeSCN2+ ions.
One of the more important numbers that help us understand an equilibrium system is called the
equilibrium constant, Keq. For the reaction between Fe3+ and SCN–, the Keq is defined by the
equation shown below.

[ FeSCN 2+ ]
K eq = 3+
[ Fe ][ SCN− ]
To find the value of Keq at a given temperature, it is necessary to determine the molar
concentration of each of the three species in solution at equilibrium. You will determine the
concentrations by using a Vernier Colorimeter to measure the amount of light of a specific
wavelength that passes through a sample of the equilibrium mixtures. The amount of light
absorbed by a colored solution is proportional to its concentration. The red FeSCN2+ solution
absorbs blue light, thus the Colorimeter users will be instructed to use the 470 nm (blue) LED.

In order to successfully evaluate this equilibrium system, it is necessary to conduct two separate
tests. In Part I of the experiment, you will prepare a series of standard solutions of FeSCN2+ from
solutions of varying concentrations of SCN– and constant concentrations of H+ and Fe3+ that are
in stoichiometric excess. The excess of H+ ions will ensure that Fe3+ engages in no side reactions
(to form FeOH2+, for example) which could interfere with your measurements. In an excess of
Fe3+ ions, the SCN– ions will be the limiting reagent, thus all of the SCN– will form FeSCN2+
ions. The FeSCN2+ complex forms slowly, taking at least one minute for the color to develop. It
is best to take absorbance readings after a specific length of time has passed, between two and
four minutes after preparing the equilibrium mixture. Do not wait much longer than five minutes
to take readings, however, because the mixture is light sensitive and the FeSCN2+ ions will
slowly decompose.

In Part II of the experiment, you will prepare a new series of solutions that have varied
concentrations of the SCN– ions and constant concentrations of H+ ions and Fe3+ ions. You will
use the results of this test to accurately evaluate the equilibrium concentrations of each species
and calculate the Keq of the reaction.

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OBJECTIVES
In this experiment, you will
 Prepare and test standard solutions of FeSCN2+ in equilibrium.
 Determine the molar concentrations of the ions present in an equilibrium system.
 Determine the value of the equilibrium constant, Keq, for the reaction.

MATERIALS
Work in groups of two only.
Obtain (for each group):
10 mL Mohr pipet 0.200 M Fe(NO3)3 – 60 mL/group
Eight 20 x 150 mm Test tubes 9.00 x 10−4 M KSCN – 20 mL/group
100 mL beaker 0.500 M HNO3 – 60 mL/group
Plastic cuvette 0.010 M Fe(NO3)3 – 20 mL/group
LabQuest 1.13 x 10−3 M KSCN – 20 mL/group
Temperature Probe Kimwipes
Sharpies Stirring rod
Two 50 mL beakers Several Disposable pipets
Colorimeter

PROCEDURE
Part I: Prepare and Test Standard Solutions
1. Obtain, wear goggles, apron, and gloves.
2. Preparing Solutions

Place the five 20 x 150 mm test tubes in a test tube rack and clearly label them 1 through
5. Obtain 60 mL of 0.200 Fe(NO3)3 solution in a 100 mL beaker, 20 mL of 9.00 x 10−4 M
KSCN in a 50 mL beaker and 40 mL of 0.500 M HNO3 in another 50 mL beaker.

Prepare solutions 1 through 5 as indicated in Table I. Extreme care should be exercised

to ensure that the exact amount of each reagent is added to each test tube. Use the
Mohr pipet to dispense the specific volumes. If necessary, practice dispensing with Mohr
pipet using distill water before mixing solutions. Mohr pipet should be thoroughly

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cleaned after using with each solution in order to avoid contamination of the reagents.
Carefully mix the solution in each test tube so that the color is uniform.

Important: the mixtures you will prepare are light sensitive. You need to measure the
absorbances of these mixtures within 2-5 minutes of preparing them (Recommendation: prepare
and measure one mixture at a time).
Table I
Test tube mL of 0.200 Fe(NO3)3 mL of 9.00 x 10−4 M KSCN mL of 0.500 M HNO3
1 10.00 5.00 5.00
2 10.00 4.00 6.00
3 10.00 3.00 7.00
4 10.00 2.00 8.00
5 (Blank) 10.00 0.00 10.00

3. Fill the cuvette ¾ full with Blank solution using disposable pipet.
 Wipe the outside of each cuvette with a lint-free tissue.
 Handle cuvettes only by the top edge of the ribbed sides.
 Dislodge any bubbles by gently tapping the cuvette on a hard surface.
 Always position the cuvette so the light passes through the clear sides.

4. Connect the Colorimeter to LabQuest and choose New from the File menu.

5. Calibrate the Colorimeter.

a. Place the blank in the cuvette slot of the Colorimeter and close the lid.
b. Press the < or > button on the Colorimeter to select the 470 nm wavelength.
c. Press the CAL button until the red LED begins to flash and then release the CAL button.
d. When the LED stops flashing, the calibration is complete.
Empty the blank from the blank cuvette. Using the solution in Test tube 1, rinse the
cuvette twice with ~1 mL amounts and then fill it 3/4 full using disposable pipet. Wipe
the outside with a tissue, place it in the Colorimeter, and close the lid.

6. Set up the data-collection mode.

a. On the Meter screen, tap Mode. Change the mode to Events with Entry.
b. Enter the Name (Concentration) and Units (mol/L). Select OK.

7. Collect absorbance-concentration data for the four standard equilibrium mixtures (1 – 4).

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a. Leave the cuvette, containing the Test tube 1 mixture, in the Colorimeter.
b. Start data collection. After the absorbance reading stabilizes, tap Keep and enter
the value for the concentration of FeSCN2+ from your Pre-Lab calculations. Select
OK. The absorbance and concentration values have now been saved for the first
solution.
c. Discard the cuvette contents as directed. Using the solution in Test tube 2, rinse
the cuvette twice with ~1 mL amounts, and then fill it 3/4 full. Place the cuvette in
the device, wait for the value displayed on the screen to stabilize, and tap Keep.
Enter the value for the concentration of FeSCN2+ in Test tube 2, then select OK.
d. Repeat Part c of this step to measure the absorbance of the solutions in Test tubes
3 and 4. Enter Absorbance and Concentration in Part I of the Report Sheet, then
graph your data.
8. Display a graph of absorbance vs. concentration with a linear regression curve.
a. Choose Graph Options from the Graph menu.
b. Select Autoscale from 0 and select OK
c. Choose Curve Fit from the Analyze menu
d. Select Linear as the Fit Equation.
e. Select OK. The graph should indicate a direct relationship between absorbance
and concentration, a relationship known as Beer’s law. Record the linear fit
equation in your data table.
IMPORTANT: Don’t change anything in the LabQuest App. You will use the best-fit line
equation in Part II. Record the equation in your data sheet.

Part II: Prepare and Test Equilibrium Systems

9. Label three new test tubes A through C. Do not throw away solution 5 (Blank) in Part I.
Fill each test tube with amounts of reagents as specified in Table II and carefully mix
each solution so that the color is uniform.
Table II
Test tube mL of 1.00 x 10−2 M mL of 1.13 x 10−3 M mL of 0.500 M
Fe(NO3)3 KSCN HNO3
A 5.00 5.00 10.00
B 5.00 10.00 5.00
C 10.00 5.00 5.00

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10. Collect absorbance-concentration data for the four test tubes of equilibrium mixtures.
a. Using the solution in Test tube A, rinse the cuvette twice with ~1 mL amounts and then
fill it 3/4 full. Wipe the outside with a tissue and place the cuvette in the Colorimeter.
b. Write down, in your data table, the absorbance of the sample in Test tube A.
c. Trace along the linear regression equation to find the FeSCN2+ concentration for the
sample in Test tube A. Write down the concentration in your data table.
d. Discard the cuvette contents as directed. Rinse and fill the cuvette with the solution in
Test tube B and place it in the device. After the reading stabilizes, write down the
absorbance in your data table and use the Interpolate function to determine the
concentration of the sample.
e. Repeat Step d for the mixtures in Test tubes C.

Make sure to remove the cuvette from the sample compartment after you have finished
the lab. Rinse out the cuvette, dry it and return to your station before leaving the lab.
The cuvette can be dried by blowing air through it using the air available at the lab
tables.

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