Electrochemistry

Lab: REDOX Titration

In this lab, a redox titration (analogous to an acid/base titration) is performed and concepts of redox chemistry are
studied. In this redox reaction, Fe
2+
is converted into Fe
3+
and MnO
4
-
(dark purple) is converted into Mn
2+
. The change in
the oxidation state of manganese in MnO
4
-
to Mn
2+
causes a change in color. When the reaction is complete and excess
MnO
4
-
is added to the reaction mixture, the solution turns pink and the titration is done. The unbalanced equation that
describes this REDOX reaction is described below:

Fe
2+
+ MnO
4
-
Fe
3+
+ Mn
2+


Materials:
Ring Stand
Buret Clamp
Buret
Erlenmeyer Flask
Stir Plate
Stir Bar
Magnetic Stir Bar Retriever

Chemicals:
0.01M potassium permanganate
iron (II) sulfate heptahydrate
1.0M sulfuric acid
distilled water

Safety Precautions

Always wear safety goggles and a lab apron to protect your eyes and clothing. If you get a chemical in
your eyes, immediately flush the chemical out at the eyewash station while calling to your teacher. Know the
location of the emergency lab shower and the eyewash station and the procedure for using them.

Do not touch any chemicals. If you get a chemical on your skin or clothing, wash the chemical off at the
sink while calling to your teacher. Make sure you carefully read the labels and follow the precautions on
all containers of chemicals that you use. If there are no precautions stated on the label, ask your teacher
what precautions you should follow. Do not taste any chemicals or items used in the laboratory. Never
return leftovers to their original containers; take only small amounts to avoid wasting supplies.

Call your teacher in the event of a spill. Spills should be cleaned up promptly, according to your
teachers directions.

Never put broken glass in a regular waste container. Broken glass should be disposed of properly
according to your teachers instructions.


Procedure:
1. Clean out burets as instructed.

2. Add enough 0.01 M KMnO
4
solution to fill the buret above the zero level. Open the stopper and allow a small amount
of the solution to drain into a waste beaker (enough to decrease the volume below the zero mark of the buret). Record
the initial volume of the KMnO
4
in Data Table 1.





Electrochemistry
Lab: REDOX Titration

3. Measure out 10.0 mL of distilled water in a 10 mL graduated cylinder. Mass 0.278 g of FeSO
4
into a weigh boat. Add
the 10.0 mL of distilled water to a 125 Erlenmeyer flask and add the FeSO
4
. Swirl the flask to dissolve the FeSO
4
.

4. Add 5 mL of 1M H
2
SO
4
to the flask. The acid helps to keep the Fe
2+
ions stable to allow time to titrate. Note the acidic
conditions indicated by the H
+
in the balanced redox reaction.

5. Add a stir bar.

6. Add the KMnO
4
from the buret approximately 1.00mL at a time to the flask. Use the stir plate while swirling
constantly. The purple color should disappear when the flask is swirled (the reaction is taking place). You can make the
additions fairly quickly in the initial part of the titration.

7. After 15 mL has been added, slow down the titration (make additions of 0.25-0.50mL). When it takes a few seconds to
get rid of the purplish color slow down even more (drop by drop). When the reaction is complete, the solution turns
pink and stays pink. Record the final volume of the KMnO
4
from the buret in Data Table 1.

8. Dump the contents of the waste beaker and the 125 Erlenmeyer flask into the class waste beaker. Clean out the buret
as instructed. Dump the waste in the waste container and clean the glassware used.

9. Complete Data Tables 1-4 and their corresponding calculations.

10. Complete the Google Form to compile class data and to get a look at the average of multiple runs. Use this class
average in the conclusions of your lab portfolio entry.

Data Table 1: MnO
4
-
Buret Readings (mL)
MnO
4
-

Initial (mL) Final (mL) Volume Used
mL L
Trial 1
Show the calculations for determining volumes used for one of your trials below.




Data Table 2: Calculating Moles of Solution with Known Concentration (MnO
4
-
)
Concentration (M) Volume Used (L) Moles of MnO
4
-

Trial 1
Show the calculations for determining number of moles of MnO
4
-
used for one of your trials below.











Electrochemistry
Lab: REDOX Titration

Data Table 3: Calculating Moles of Solution with Unknown Concentration (Fe
2+
)
Moles of Known Molar Ratio Moles of Unknown
Trial 1
Show the calculations for determining number of moles of Fe
2+
used for one of your trials below.






Data Table 4: Calculating Concentration of Unknown Solution (Fe
2+
)
Moles of Unknown Volume Used (L) Concentration
Trial 1
Show the calculations for determining [Fe
2+
] used for one of your trials below.





Analysis and Conclusion:
1. Rewrite the reaction (in bold at the top of the first page) and assign oxidation numbers to each species in the reaction.
Using this information, identify the following:
the element being oxidized, the element being reduced, the element that acts as the oxidizing agent, and the
element that acts as the reducing agent.







2. Using the steps from class notes, write the balanced redox equation. Remember that the reaction takes place in an
acidic solution. Show all work and box the final balanced equation.















3. Flesh out your conclusion with your group.

Sentence 1: Thesis Statement
tells the reader how you will interpret the significance of your results of the specific lab.
is a road map for your conclusion; in other words, it tells the reader what to expect from the
rest of the conclusion.

Sentence 2: What were your results?
Just tell the reader what your results were. The concentration of the Fe
2+
solution was
determined to be

Sentence 3: How did your results compare to the accepted value?
Just tell the reader what the expected result should have been. The actual concentration of the
Fe
2+
solution was

Sentence 4: What was your percent error?
Just use the percent error formula and tell your reader the error of your results. The accepted
value is determined from a reference or is provided by your instructor.

Sentence 5-?: Provide specific potential sources of error AND how this caused your experimental value to be
larger/smaller than the accepted value.
It is unacceptable to simply state, The results were off due to human error. You will receive a
zero for your entire lab grade if you use anything similar to this in your conclusion.
You need to be explicit. The experimental concentration value was higher than the accepted
concentration value because the measured volume of titrant added was too large. The larger
measured volume translated into a larger calculated number of moles of the titrant, and
therefore a higher concentration of the unknown than the accepted value of ___.
THINK ABOUT WHAT YOU ACTUALLY MEASURED IN THE LAB that would cause your
experimental value to be higher or lower than the accepted value.

Sentence ?: Conclusion Sentence
Neatly wrap it up. Show the reader you have completed your analysis and leave the reader with
a clear understanding of your results. Tie it back to your introductory sentence/thesis
statement.
Do not introduce additional analysis or data.