Advanced Chemistry with Vernier 8 - 1

Computer
8
An Oxidation-Reduction Titration:
The Reaction of Fe
2+
and Ce
4+
A titration, as you recall, is a convenient method of learning more about a solution by reacting it
with a second solution of known molar concentration. There are a number of ways to measure
the progress of a titration. The method used in this experiment is called a potentiometric titration,
in which the electric potential of a reaction is monitored. All acid-base titrations that are
measured by a pH probe are potentiometric; thus, this method is not as unusual as it may seem.
ou will conduct an oxidation-reduction reaction in this experiment in order to determine the
amount of iron !""# ions in a solid sample of ferrous ammonium sulfate hexahydrate,
!$H%#&'e!()%#&*+H&). The oxidi,ing agent for the sample will be ammonium cerium !"-#
nitrate, !$H%#&.e!$)/#+. The net ionic e0uation for the reaction is shown below.
.e
%1
!a0# 1 'e
&1
!a0# .e
/1
!a0# 1 'e
/1
!a0#
This experiment illustrates the electrical nature of chemical reactions, and offers practice with a
process for observing and measuring an oxidation-reduction reaction.
OBJECT!E"
"n this experiment, you will
.onduct the potentiometric titration of the reaction between ferrous ammonium sulfate
hexahydrate and ammonium cerium !"-# nitrate.
2easure the potential change of the reaction.
3etermine the molar concentration of iron !""# ions in a sample of ferrous ammonium
sulfate hexahydrate.
Figure 1
8 - 2 Advanced Chemistry with Vernier
Computer 8
#ATERA$"
#ateria%&
-ernier computer interface magnetic stirrer
computer stirring bar or 2icrostirrer
-ernier )45 (ensor wash bottle
6.766 2 !$H%#&.e!$)/#+ in 7 2 H&()% distilled water
!$H%#&'e!()%#&*+H&) solution ring stand
86 m9 graduated cylinder utility clamp
#ateria%&
86 m9 buret buret clamp
76 or &8 m9 pipet and pump 786 m9 beaker
#ET'O( ): #ea&urin* !o%ume +&in* a Buret
7. )btain and wear goggles.
&. 2easure out precisely &8.66 m9 of a ferrous ammonium sulfate solution of unknown molar
concentration and transfer it to a 786 m9 beaker.
/. 5lace the beaker of ferrous ammonium sulfate solution on a magnetic stirrer and add a
stirring bar. "f no magnetic stirrer is available, stir the mixture with a stirring rod during the
titration.
%. .onnect an )45 (ensor to .hannel 7 of a -ernier computer interface. .onnect the interface
to the computer with the proper cable.
8. (tart the 9ogger Pro program on your computer. )pen the file :6;a 5otentiometric< from the
Advanced Chemistry with Vernier folder.
+. (et up a ring stand, buret clamp, and 86 m9 buret to conduct the titration !see 'igure 7#.
4inse and fill the buret with 6.766 2 .e
%1
solution. CAUTION: Handle the solution with
care; it contains 1.0 M sulfuric acid. t can cause !ainful "urns if it comes in contact with the
s#in.
=. 5lace a utility clamp on the ring stand to hold the )45 (ensor in place during the titration.
5osition the )45 (ensor so that its tip is immersed in the 'e
&1
solution but does not interfere
with the movement of the magnetic stirring bar. >ently stir the beaker of solution.
;. ou are now ready to begin the titration. The ob?ective of your first trial is to determine the
region of the titration curve near the e0uivalence point, and not to precisely determine the
e0uivalence point.
a. @efore adding .e
%1
titrant, click . )nce the displayed potential reading has
stabili,ed, click . "n the edit box, type :6< !for 6 m9 added#. 5ress the A$TA4 key to
store the first data pair.
b. Add 7 m9 of the .e
%1
titrant. (tir the solution gently at all times. Bhen the potential
stabili,es, again click . "n the edit box, type the current buret reading. 5ress A$TA4
to store the second data pair.
Advanced Chemistry with Vernier 8 - 3
An Oxidation-Reduction Titration: The Reaction of Fe
2
and Ce
!
c. Add .e
%1
solution in 7m9 increments and enter the buret reading after each increment.
.ontinue adding .e
%1
solution until the potential value remains constant.
d. .lick when you have finished collecting data.
e. Axamine the titration curve and estimate the volume of .e
%1
solution used to reach the
e0uivalence point of the titration. 4ecord this value in your data table for Trial 7.
C. Bhen you have completed the titration, dispose of the reaction mixture as directed. 4inse the
)45 (ensor with distilled water in preparation for the second trial.
76. 4epeat the necessary steps to conduct a second titration with a new sample of
!$H%#&'e!()%#&*+H&) solution.
77. Bhen you conduct the second trial, carefully add the .e
%1
solution drop by drop in the region
near the e0uivalence point so that you can precisely identify the e0uivalence point of the
reaction.
7&. 'ollow the steps below to find the e$uivalence !oint, which that is the largest increase in
potential upon the addition of a very small amount of .e
%1
solution. A good method of
determining the precise e0uivalence point of the titration is to take the second derivative of
the potential-volume data, a plot of
&
potentialDvol
&
.
a. -iew a plot of the second derivative on 5age / by clicking on the $ext 5age button, .
b. Analy,e the second derivative plot and record the volume of .e
%1
at the e0uivalence point.
7/. At the direction of your instructor, conduct a third trial. Ese your titration data from the
second !or third# trial to determine the e0uivalence point of the reaction.
7%. 5rint a copy of the trial and the data set that you intend to use in your data analysis.
DATA TABLE
Trial 1 Trial 2
Volume of Fe
2+
solution (mL)
Volume of Ce
4+
solution used to
reach equivalence point (mL)
8 - 4 Advanced Chemistry with Vernier
Computer 8
(ATA A,A$-""
7. .alculate the molar amount of .e
%1
used to reach the e0uivalence point of the reaction.
&. .alculate the molar amount of iron in the sample of ferrous ammonium sulfate solution.
/. .alculate the molar concentration of the ferrous ammonium sulfate solution.
%. The ferrous ammonium sulfate solution that you tested was prepared by dissolving %6.6 g of
solid !$H%#&'e!()%#&*+H&) in 7.66 liter of solution. This substance is often impure.
a. .alculate the theoretical percent 'e in a pure sample of !$H%#&'e!()%#&*+H&).
b. .alculate the percent 'e in the sample that you tested.
c. .ompare your experimental percent 'e to the theoretical percent 'e. How pure was your
sampleF Ese a calculation to support your assertion.