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Prepared by:
Rodney Pujada
Department of Chemistry
Los Angeles Trade Technical College
400 Washington Blvd, Los Angeles CA
March 21th, 2011
Rodney Pujada
Chemistry 102/ Section 4076
Prof: Manuel Acosta M.S.
Days of class: Monday and Wednesday
Time of class: 6.00 9:10 pm
Date Due :
March 21 th,2011
Experiment No 4:
The Equivalent Weight of an
Unknown Fe Compound
Name:
Lab Partner:
I.
Rodney Pujada
Armin Vossooghi
Introduction
The purpose of the experiment was to use the permanganate ion, a strong oxidizing
agent, in a titration in order to determine the concentration of a FeSO 4 solution. Purple
MnO4- ion from a standardized potassium permanganate solution was titrated thrice to
give clear Mn2+ with an analyte of acidified FeSO4 until all the Fe2+ in the solution was
oxidized to Fe3+. The color of the MnO4-/Mn2+ was used as the indicator for the titration.
A balanced oxidation-reduction, the molarity/normality of the standards potassium
permanganate, and the volume of potassium permanganate used allowed the
determination of the concentration of the FeSO 4.
Equivalent weight
Equivalent weight has the dimensions and units of mass, unlike atomic weight, which
is dimensionless. Equivalent weights were originally determined by experiment, but
(insofar as they are still used) are now derived from molar masses. Additionally, the
equivalent weight of a compound can be calculated by dividing the molecular weight
by the number of positive or negative electrical charges that result from the
dissolution of the compound.
II.
Material
50 mL Buret, 250 mL Erlenmeyer flask, buret clamp, wash
bottle, funnel, 50 mL and 300 mL beaker, 10 mL volumetric
cylinder, stirring rod, and 0.1070 N KMnO 4, and unknown Fe
compound.
III.
Procedure
a. Clean and rinse the buret with distilled water.
b. Precondition the buret by rinsing it with the KMnO 4 solution two or three
times, and fill the buret with a funnel.
c. Fill the buret with 0.1070 N KMnO4 to exact measurement.
d. Remove all gas bubbles in the liquid column of the buret.
e. Read the initial volume of KMnO4 by recording the position of mark that
line up with the meniscus of the liquid column.
f. Weigh 0.2 grams of the unknown Fe compound
g. Transfer the solid into 250 mL Erlenmeyer flask. Add
around 50 mL of distilled water plus about 20 mL of 3M
H2SO4. Swirl gently for the crystals to dissolve.
h. Add between 2 to 4 mL of 85% H3PO4 into the solution,
and then swirl gently to mix the solution.
i. Take 250 mL Erlenmeyer flask with the solution to the setup
buret.
i. Read the initial volume of the buret containing KMnO 4, Vi
KMnO4.
ii. Open the stopcock of the buret to deliver first 5 mL
KMnO4 solution.
iii. Close the stopcock when the liquid level drops to near
the position of (Vf KMnO4 + 5) mL.
iv. Read the final volume of the buret, Vf KMnO 4. The
difference between initial and final volumes is the
amount of KMnO4 in the flask.
j. Read and record the top burets meniscus reading, which gives
the final volume of KMnO4 solution, Vf KMnO4 .
k. Place the Erlenmeyer flask under the buret; open the stopcock
slowly to add the KMnO4 into the solution.
l. Add drop by drop and wait until the color slowly fades away.
m. Record the final volume Vf KMnO4 .when the solution turn to pink.
IV.
Titration Data
Sample No 21
Mass Unknown Fe compound
(g)
Normality
KMnO4
bottle
(Equiv/L)
Initial
buret
reading
Vi
KMnO4(mL)
Final buret reading Vf KMnO4
(mL)
volume of KMnO4 consumed
(mL)
volume of KMnO4 consumed
(L)
Run 1
Run 2
Run 3
0.1070
0.216
2
0.107
0
0.194
1
0.107
0
24.6
30.0
35.2
30.0
35.2
40.0
5.4
5.2
0.005
2
4.8
0.004
8
0.2029
0.0054
IV.1
By Formula:
# of Equiv-g compound
Volume (L)
= Normality (N) *
For Run No 1:
# of Equiv-g KMnO4 = Normality (N) * Volume (L)
# of Equiv-g KMnO4 = 0.1070 N * 0.0054 L
# of Equiv-g KMnO4 = 0.005778
# of Equiv-g KMnO4
0.005778
IV.2
Data
Run 1 Fe compound
Run 2
Run 3
# ofTitration
Equiv-g KMnO4
= # of Equiv-g
Normality KMnO4 bottle
(Equiv/L)
0.1070
0.1070
0.1070
volume of KMnO4 consumed
(L)
0.0054
0.0052
0.0048
0.00057
0.00055 0.00051
# of Equiv-g KMnO4
78
64
36
Table no
Titration Data
For
by
3
# of Equiv-g KMnO4
# of Equiv-g Fe compound
Run 1
0.00057
78
0.00057
78
Run 2
0.00055
64
0.00055
64
Run 3
0.00051
36
0.00051
36
Run No 1:
Table No
Data:
= # of equivalent of Fe * Equivalent
Table No 4
Run 1
Run 2
Run 3
0.000577
8
55.845
0.032267
24
0.000556
4
55.845
0.031072
158
0.000513
6
55.845
0.028681
99
0.2029
0.2162
0.1941
15.9
14.4
14.8
15.0
IV.4
V.
Conclusions:
The percentage of 15 % of Iron in the compound sample No 22 by table
No 4.
In this experiment, KMnO4 will be used to determine the percentage of Fe 2+ in an
References:
http://web.centre.edu/shiba/che132L/redox.pdf
http://web.centre.edu/shiba/che132L/redox.pdf
http://faculty.ccri.edu/eterezakis/1100%20Exp%205,%20Iron%20Analysis%20by
%20Redox%20Titration%20_egt_.pdf
TITLE:
Quantitative Oxidation/Reduction Titration
PURPOSE:
The purpose of the experiment was to use the permanganate ion, a strong oxidizing
agent, in a titration in order to determine the concentration of a FeSO 4 solution. Purple
MnO4- ion from a standardized potassium permanganate solution was titrated thrice to
give clear Mn2+ with an analyte of acidified FeSO4 until all the Fe2+ in the solution was
oxidized to Fe3+. The color of the MnO4-/Mn2+ was used as the indicator for the titration.
A balanced oxidation-reduction, the molarity/normality of the standards potassium
permanganate, and the volume of potassium permanganate used allowed the
determination of the concentration of the FeSO 4.
PROCEDURE:
1. Obtain about 100mL of potassium permanganate solution (.020M) from the
stock bottle
2. Obtain about 50mL of FeSO4 solution
3. Obtain 2 burets. Rinse one with 5mL of FeSO 4, discard rinsings, and fill it with
FeSO4. Repeat procedure for potassium permanganate and second buret
4. Place 50mL of distilled water and add 1 drop of potassium permanganate.
Observe, this will be the color standard for titration
5. Measure 10.0mL of FeSO 4 into flask from buret. Add 5.00mL of 3.0M sulfuric acid
to increase H+ concentration. Now titrate with potassium permanganate as
titrant, reach the endpoint, read the buret, and discard the contents of the flask
6. Rinse flask and repeat titration two more times using the same volume of FeSO 4
DATA & OBSERVATIONS:
1. Potassium permanganate solution = deep purple color, stains
o 99.2 mL of standardized .020M taken total
o no crystals visible, completely dissolved
o color standard for reaction = pink/purple, not as strong as permanganate
solution
2. FeSO4 solution = yellow/dirty grey murky color
o 50.0 mL of FeSO4 solution of unknown concentration taken
3. Titrations = solution turns pink/purple where drop of titrant lands, but later goes
back to murky yellow/grey color
o After endpoint, solution is pink/purple
4. Data Table 1: Titration volumes:
Trial
H2SO4
added
FeSO4 start
FeSO4 stop
KMnO4 start
KMnO4 stop
5.0mL
14.76mL
24.60mL
9.18mL
26.20mL
5.1mL
24.60mL
34.59mL
26.20mL
43.65mL
4.9mL
34.59mL
44.61mL
27.93mL
45.17mL
CALCULATIONS:
Balancing:
Reduction: 8H+ + MnO4- + 5e- -> Mn2+ + 4H2O
Oxidation : Fe2+ -> Fe3+ + e8H+ + MnO4- + 5e- -> Mn2+ + 4H2O
5Fe2+ -> 5Fe3+ + 5eBalanced overall: 8H+(aq) +MnO4-(aq) + 5Fe2+(aq) -> 5Fe3+(aq)
4H2O(l)
Mn2+(aq) +
Normality:
Number of electrons transferred = number of equivalents = 5
Equivalent weight: (39.10g/mol + 54.94g/mol + 4*16.00g/mol)/5 = 31.61g/mol
Normality = 5M = 5 * .020M = .100N
Volumes:
Trial 1:
FeSO4: 24.60mL - 14.76mL = 9.84mL
KMnO4: 26.20mL - 9.18mL = 17.02mL
Trial 2:
CONCLUSION:
The purpose of the laboratory exercise was to perform an oxidation/reducation
titration between a standardized solution of potassium permanganate and an unknown
iron (II) sulfate solution in order to determine the concentration of the latter. The
permanganate ion in the titrant was reduced to Mn2 + and the Fe2+ in the analyte was
oxidized to Fe3+. Everything was done in a solution acidified by sulfuric acid so that the
MnO4- would get reduced to Mn2+ and the extra oxygen atoms could form water. From
the titration data and the balanced oxidation/reduction equation the normality and
molarity of the FeSO4 solution were gotten.
The oxidation/reduction titration was the major part of the experiment and was
performed in order to determine the molarity of the FeSO 4. A deep purple and skinstaining 0.020M standardized solution of potassium permanganate was taken and
used as the titrant in the titration. The analyte was prepared from a murky grey/yellow
solution of unknown concentration of FeSO 4 and from 3.0M sulfuric acid. The sulfuric
acid was required so that an acidic environment was present with H + ions to take on
the oxygen atoms left over from the reduction of MnO 4- to Mn2+. In such an acidic
medium, the reaction 8H+(aq) +MnO4-(aq) + 5Fe2+(aq) -> 5Fe3+(aq) -> Mn2+(aq) +
4H2O(l) took place. The titrant, MnO4-, was the oxidizing agent and itself gained 5
electrons to get reduced to Mn2 +. The extra oxygen atoms formed water with the H +
ions from the sulfuric acid. The analyte, Fe 2+ was the reducing agent and got oxidized
to form Fe3+. Initially in the titration, the titrant was a deep purple and the analyte was
a pale murky yellow/grey color. As the MnO 4- was added to the analyte, the area
around the drop turned became a pink/purple color. The titration proceeded until the
entire solution stayed purple pink. Initially, the purple MnO 4- added to the analyte was
quickly reduced to clear Mn2+ and lost its color. However, after all the Fe 2+ was oxidized
to Fe3+ there was no more reducing agent and thus the MnO 4- stayed as MnO4- in the
analyte solution. The addition of extra MnO 4- after all the Fe2+ has been oxidized made
the color of the solution a light purple/pink color as there was no longer anything to
convert the MnO4- to the mostly colorless (slightly pink) Mn 2+. Thus, the potassium
permanganate was the indicator in the reaction. It turned clear to Mn 2+ while there still
was Fe2+ to oxidize, but as excess permanganate was added, the solution turned
purple with MnO4- having a distinctly different color. The color standard for the reaction
was simulated by the addition of a drop of potassium permanganate to water to show
what the potassium permanganate would look like after being added at the
equivalence point of the titration. Other oxidizing agents could have been used in the
titration as well. For instance, Cr2O72- would have likewise oxidized the Fe 2+ and could
have also acted as a self-indicator because of how it also changes color as it goes to
Cr3+. Likewise, CrO42- could have been used and would have also changed color as it
oxidized the Fe3+. Oxygen gas noticeably reacted with the FeSO 4 solutions to oxidize
the Fe2+ions. With a proper set-up that controlled exactly how much oxygen was put
in, it would be possible to use oxygen gas as an oxidizing agent. Finally, H 2O2 in an
acidic solution could have been used as an oxidizing agent and given water. By doing
the entire reaction in hydrogen peroxide and seeing how much water was made,
another experiment could have been possible. Anything with a reduction potential
greater than that of Fe 3+ + e- -> Fe2+ could have been used as an oxidizing agent.
However, the colorful changes that accompany the changes of oxidation numbers of
but the spontaneous reaction of the solution with air made it appear lower than it
really was. This can be avoided by performing the reaction in a vacuum.