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The Equivalent Weight of An Unknown Fe Compound

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.

Potassium permanganate, KMnO4, is widely used as an oxidizing agent in volumetric analysis. In


acidic solution, permanganate ion undergoes a 5-electron reduction to manganese(II) ion:
Balancing:
Reduction: 8H+ + MnO4- + 5e- -------> Mn2+ + 4H2O
Oxidation : Fe2+ --------------------------> Fe3+ + eBalanced overall: : 8H+(aq) +MnO4-(aq) + 5Fe2+(aq) -> 5Fe3+(aq) + Mn2+(aq) +
4H2O(l)

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.

Data and Calculation


Table No 1

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

Calculate the # Equivalents of KMnO4 reduced ()


Table No 2

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

Calculate the # Equivalents of Fe oxidized


Balancing:
Reduction: 8H+ + MnO4- + 5e- -------> Mn2+ + 4H2O
Oxidation : Fe2+ --------------------------> Fe3+ + e-

Balanced overall: : 8H+(aq) +MnO4-(aq) + 5Fe2+(aq) -> 5Fe3+(aq) + Mn2+(aq) +


4H2O(l)

Therefore by the following equation:

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 Equiv-g KMnO4 = 0.0005778


# of Equiv-g Fe compound = 0.0005778
IV.3

Calculate the mass of unknown Fe compound (g)


# of equivalent = mass of compound /
Equivalent weight
Equivalent
weight = Molecular Weigth /
Oxidation : Fe2+ --------------------------> Fe3+ + e= 1 which is transferred electrons.
Equivalent weight for Fe = 55.845 g/mol
Mass of Iron
weight of Fe

= # of equivalent of Fe * Equivalent
Table No 4

Calculate the weight of


Fe
# of Equiv-g Fe
Molecular Weight of Fe
Mass of Fe (g)
Mass Unknown Fe compound
(g)
% of Fe
Average % of Fe in the
compound

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

Calculate the percent of Iron in the compound.


For Run No 1:
Data:
Mass of Fe (g)
= 0.0326 g
Mass Unknown Fe compound (g) = 0.2029 g
% of Fe in the compound = Mass of Fe (g) *100 / Mass Unknown Fe
compound (g)
% of Fe in the compound = 0.0326 g *100 / 0.2029 g
% of Fe in the compound =
15.9 %

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

unknown solid sample dissolved in water. The permanganate oxidation of Fe 2+ to


Fe3+ is carried out in an acidic solution to prevent the air oxidation of Fe 2+.
Phosphoric acid is added to the titration mixture to form a colorless complex with
the normally yellow or orange Fe3+ ion, which markedly sharpens the appearance of
the endpoint.
The indicator in the titration is the Mn2+ ion which is nearly colorless, the
end point in titrations using KMnO4 can be taken as the first pink color
that persists in the solution in excess.

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

Lab: Quantitative Oxidation/Reduction


Titration
Alexander Kazberouk
Period 5/6 Chemistry AP

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:

FeSO4: 34.59mL - 24.60mL = 9.99mL


KMnO4: 43.65mL - 26.20mL = 17.45mL
Trial 3:
FeSO4: 44.61mL - 34.59mL = 10.02mL
KMnO4: 45.17mL - 27.93mL = 17.24mL
Average:
FeSO4: (9.84mL + 9.99mL + 10.02mL)/3 = 9.95mL
KMnO4: (17.02mL + 17.45mL + 17.24mL)/3 = 17.23mL

FeSO4 normality and molarity:


17.02mL mL KMnO4 * 0.100 equivalents/1000mL KMnO4 = 1.70 * 10-3 equivalents
KMnO4
1 equivalent FeSO4 = 1 equivalent KMnO4
1.70 * 10-3 equivalents KMnO4 = 1.70 * 10-3 equivalents FeSO4
1.70 * 10-3 equivalents FeSO4 / 9.84mL * 1000mL/1L = 0.173N
Number of electrons transferred = number of equivalents = 1, normality = molarity
Molarity FeSO4 = 0.173M

17.45mL KMnO4 * 0.100 equivalents/1000mL KMnO4 = 1.75 * 10-3 equivalents KMnO4


1 equivalent FeSO4 = 1 equivalent KMnO4
1.75 * 10-3 equivalents KMnO4 = 1.75 * 10-3 equivalents FeSO4
1.75 * 10-3 equivalents FeSO4 / 9.99mL * 1000mL/1L = 0.175N
Molarity FeSO4 = 0.175M

17.24mL KMnO4 * 0.100 equivalents/1000mL KMnO4 = 1.72 * 10-3 equivalents KMnO4


1 equivalent FeSO4 = 1 equivalent KMnO4
1.72 * 10-3 equivalents KMnO4 = 1.72 * 10-3 equivalents FeSO4

1.72 * 10-3 equivalents FeSO4 / 10.02mL * 1000mL/1L = 0.172N


Molarity FeSO4 = 0.172M

Average molarity: (0.173M + 0.175M + 0.172M)/3 = 0.173M

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

manganese and the ease of obtaining manganese-containing compounds made it the


simplest choice.
Having gotten the volumes necessary for the titration, the next step calculated
the molarity of the FeSO 4 solution. From the balanced chemical equation, the number
of the electrons reacting with MnO4-, and the molarity of the standardized KMnO 4
solution, the normality of the solution was calculated to be 1.00N. For every mole of
MnO4- reduced to Mn2+, 5 moles of electrons were required and thus the normality of
the solution, 1.00N, was 5 times its molarity, 0.020M. However, only a single mole of
electrons was gotten from the oxidation of Fe 2+ to Fe3+. Thus, there was a 5:1
stoichometric ratio between the two reagents. From the normality of KMnO 4- and the
volumes used in the titrations, the average normality of the FeSO 4 solution was gotten
to be 0.173N. That was also equal to the molarity of the solution as the oxidation of
Fe2+ to Fe3+ dealt with only a single electron.
Overall, it is unlikely that error played a major role in the experiment. The three
values for the molarity of the FeSO 4 were very close, 0.172M, 0.173M, and 0.175M and
the results were precise. To determine the accuracy of the results, the actual value
would be needed. Minor error can be attributed to going slightly past the equivalence
point for the second titration, thus producing a higher value of 0.175M than is the
actual value. A more likely source of error is the oxidation/reduction reaction between
the iron sulfate and oxygen in the air. Oxygen got reduced and reacted with H+ in the
analyte to form water while the Fe 2+ in the FeSO4 analyte got oxidized to give Fe 3+.
Because the newly formed Fe3+ did not react with the potassium permanganate, less
potassium permanganate was added than was needed to oxidize all the Fe 2+ originally
present in solution. Thus, the actual molarity of the FeSO 4 solution was probably higher

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.

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