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: Rodney Pujada
Lab Partner: Armin Vossooghi
I. 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 Mn 2+ with an analyte of acidified FeSO 4 until all the
Fe2+ in the solution was oxidized to Fe 3+. The color of the MnO 4-/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 FeSO4.

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+ + e-

Balanced 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
KMnO4, 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 H 2SO4. Swirl gently for the crystals to
dissolve.
h. Add between 2 to 4 mL of 85% H 3PO4 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 KMnO 4 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 KMnO 4 in the flask.
j. Read and record the top buret’s 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 Run 1 Run 2 Run 3

Sample No 21

Mass Unknown Fe compound (g) 0.2029 0.2162 0.1941

Normality KMnO4 bottle (Equiv/L) 0.1070 0.1070 0.1070

Initial buret reading Vi KMnO4(mL) 24.6 30.0 35.2
Final buret reading Vf KMnO4 (mL) 30.0 35.2 40.0
volume of KMnO4 consumed (mL) 5.4 5.2 4.8
volume of KMnO4 consumed (L) 0.0054 0.0052 0.0048
 IV.1 Calculate the # Equivalents of KMnO4 reduced ()
Table No 2

Titration Data Run 1 Run 2 Run 3

# of Equiv-g KMnO4 0.0005778 0.0005564 0.0005136
# of Equiv-g Fe compound 0.0005778 0.0005564 0.0005136

By Formula:

# of Equiv-g compound = Normality (N) * Volume (L)

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:

# of Equiv-g KMnO4 = # of Equiv-g Fe compound

Titration Data Run 1 Run 2 Run 3 Table no 3

Normality KMnO4 bottle (Equiv/L) 0.1070 0.1070 0.1070
volume of KMnO4 consumed (L) 0.0054 0.0052 0.0048
# of Equiv-g KMnO4 0.0005778 0.0005564 0.0005136

For Run No 1: by Table No 3

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 / Ɵ

Oxidation : Fe2+ --------------------------> Fe3+ + e-
Ɵ= 1 which is transferred electrons.

Equivalent weight for Fe = 55.845 g/mol

Mass of Iron = # of equivalent of Fe * Equivalent weight of Fe

Table No 4

Calculate the weight of Fe Run 1 Run 2 Run 3

# of Equiv-g Fe 0.0005778 0.0005564 0.0005136

Molecular Weight of Fe 55.845 55.845 55.845
Mass of Fe (g) 0.03226724 0.031072158 0.02868199
Mass Unknown Fe compound (g) 0.2029 0.2162 0.1941
% of Fe 15.9 14.4 14.8
Average % of Fe in the compound 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 Mn 2+ with an analyte of acidified FeSO 4 until all the
Fe2+ in the solution was oxidized to Fe 3+. The color of the MnO 4-/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 FeSO4.

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 FeSO 4. 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 FeSO4 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:

H2SO4
Trial FeSO4 start FeSO4 stop KMnO4 start KMnO4 stop
added
1 5.0mL 14.76mL 24.60mL 9.18mL 26.20mL

2 5.1mL 24.60mL 34.59mL 26.20mL 43.65mL

3 4.9mL 34.59mL 44.61mL 27.93mL 45.17mL

CALCULATIONS:

Balancing:

Reduction: 8H+ + MnO4- + 5e- -> Mn2+ + 4H2O

Oxidation : Fe2+ -> Fe3+ + e-

8H+ + MnO4- + 5e- -> Mn2+ + 4H2O

5Fe2+ -> 5Fe3+ + 5e-

Balanced overall: 8H+(aq) +MnO4-(aq) + 5Fe2+(aq) -> 5Fe3+(aq) + Mn2+(aq) + 4H2O(l)

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 Fe 3+. 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 FeSO 4 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 skin-staining 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, MnO 4-, 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, Fe2+ was the reducing agent and got oxidized to form Fe 3+. 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 Fe2+ was oxidized to Fe3+ there was no more reducing

agent and thus the MnO4- 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 MnO 4- 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 Fe 2+ to oxidize,

but as excess permanganate was added, the solution turned purple with MnO 4- 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 Cr 3+. Likewise, CrO42- could have been used and would have also

changed color as it oxidized the Fe 3+. 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 Fe3+ + 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

FeSO4 solution. From the balanced chemical equation, the number of the electrons reacting with MnO 4-, 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 Fe2+ to Fe3+. Thus, there was a 5:1 stoichometric ratio between the two reagents. From the

normality of KMnO4- 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 Fe 2+ 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 FeSO4 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 Fe2+ in the FeSO4 analyte got oxidized to give Fe 3+. Because the newly formed Fe 3+ 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.