Rogelio Tovar Medel - A01701398

Diego Campos Ramírez - A01701794

Eduardo González Melgoza - A01701446
Rafael Treviño (He is in the balloons) - A00570194
Final Practice: Volumetric Determination of Iron Through Redox Reactions
11 de Octubre del 2017
Chemistry Laboratory Group #5
Wednesday 10:30am Prof. Víctor Olvera
Objectives:
Prepare a ferrous solution with a predetermined molar concentration
2. Determine the concentration and percentage of iron in a ferrous solution by REDOX titration.
3. Understand the use of Sodium Oxalate as a primary standard for the titration of Permanganate
4. Understand the use and importance of Permanganate as a primary standard for REDOX titrations
Introduction:
Among the thousands of elements that make up the earth and that can be found in nature, iron stands out as
one of the most abundant, being in second place after aluminum with a proportion of 5% in the
Earth's crust (Acuña, 2008). It is also considered one of the most important elements, being useful
en múltiples ámbitos como el de la ingeniería civil, donde se aplica sobre todo para la creación de aleaciones
structural materials such as steel or coatings inside pipes in conjunction with other chemicals (Acuña, 2008). Therefore,
In general, this can be obtained directly from various mineral samples, found in an oxidized state.
(III) or in the form of an ionic compound such as ferrous sulfate, from which the maximum amount of iron possible is extracted.
(Acuña, 2008).

It is for this reason that the following practice is focused on determining the amount of iron in a solution.
ferrous through a REDOX (oxidation-reduction) valuation method, as it is of great importance to know the
iron concentration that may be present in a mineral sample or salty compound like this so that, at the moment of
obtain it, have an estimated amount from the beginning.

The titration itself is a quantitative method of volumetric analysis that is performed to determine the concentration.
unknown of a reagent, known as the analyte, from another reagent with a known concentration and
standardized referred to as standard solution or primary standard, which is a type of standard solution (Méndez,
2012). A process of this type generally requires the use of indicators to determine the endpoint of a
reaction, being that point at which the amount of valencing substance added is stoichiometrically equivalent
to the amount present of the analyte (Ángeles, 2012). These substances vary depending on the type of reaction that occurs
at the end, allowing to observe precisely the endpoint with a sudden change, particularly in the color of the solution.

There are different types of assessments that can be made:

- Acid-base evaluation: It is based on a neutralization reaction between the analyte and a solution of acid or
reference base. The endpoint or equivalence point is measured in this case with a pH meter or an indicator.
of pH. (Ayres, 1970, Chap.21, pg.284)
- REDOX valuation: It is one in which a REDOX reaction occurs between the analyte and the oxidizing solution or
reducer that serves as a reference. The endpoint is determined with a potentiometer or a REDOX indicator, the
what can be the same oxidizing or reducing solution in some cases. (Ayres, 1970, Ch.21, pg.284)
- Precipitation assessment: They are based on precipitation reactions, producing ionic compounds of limited
solubility. (Álvaro, 2011)
- Assessment of complex formation: It is based on the formation of complexes between the analyte and the standard solution.
the standard. It requires specialized indicators. (Ayres, 1970, Ch.21, pg.285)

As mentioned, the type of valuation for the determination of iron in ferrous sulfate in this case is oxidation-
reduction (REDOX), this through the use of potassium permanganate (KMnO4) which has the ability to
to function as a very powerful oxidizing agent (Ayres, 1970, Ch.28, p.417). This is one of the properties
key features that highlight permanganate as an ideal component for conducting oxidation titrations
reduction, besides the fact that it also functions as an indicator during a REDOX assessment, due to
color change that occurs in a solution due to the manganese ion when it goes through a process of
oxidation or reduction, varying between violet/pink and colorless (Ayres, 1970, Chap. 28, p. 417).
However, it should be mentioned that permanganate is not considered a primary standard due to its instability and
to its lack of purity, being requirements for all primary patterns (Barrozo, 2017). Therefore, any solution
The substance containing this reagent must initially be valued by REDOX method with some other component.
suitable, such as sodium oxalate (Na2C2O4), which indeed has the properties of a primary pattern. In this way,
the true concentration of potassium permanganate is adequately determined before using it for any
another valuation process.

To calculate the concentration of the analyte through titration, the following concentration formula is used.
balance
Where:
=
C1analyte concentration

V1Volume of the analyte

(Slideshare, 2010) C2concentration of standard solution

V2Volume of standard solution

Using this same method, after a volumetric analysis where the endpoint is determined, the...
missing concentration of the analyte being standardized. The concentration in this case refers to the amount of
solute that is dissolved in a certain amount of solvent (Arena S. 2010, Cap.14, p.346), and it can be established that
various forms: Molarity (M), Normality (N), Molality (m), mole fraction (X), etc. (Chemistry Libre Texts). However,
Generally, normality or molarity is used in titration processes.

The following are the reactions that take place throughout the execution of the experimental process:

Reaction #1:

+ + → + + + +
(Moreno, 2017)

The first reaction that takes place is between sodium oxalate and potassium permanganate in order to
standardize the same permanganate. A REDOX process is generated where the permanganate ion is reduced from 7+ to
2+, while the oxalate ion is oxidized forming different products by donating a total of 5 electrons.

Reaction #2:

+ + → + ( ) + +
(Chemical equations)

When determining iron with permanganate, a REDOX reaction occurs where permanganate is reduced from 7+ to 2+.
while the iron ion is oxidized from the 2+ state to the 3+. A total of 5 electrons are transferred.

It must be considered that each of the reagents used in this practice has different characteristics and risks.
to consider. This is shown below:

KMnO4: Potassium permanganate is a bright purple crystalline powder. It is non-combustible, but it can
accelerate the burning process of flammable materials. It is used for the production of other chemicals and as
disinfectant. Causes severe burns to the skin and eye damage upon contact. It is harmful if ingested and causes
damage to internal organs after continuous exposure to the chemical. Handle using appropriate equipment
security items such as gloves and laboratory coat. (PubChem)

H2SO4: Sulfuric acid is a colorless, transparent oily liquid that is corrosive to metal and organic tissue.
Causes severe burns to the skin and eyes upon contact with them. It also causes severe damage to the
airways if the gases it releases are inhaled. Handle inside the extraction hood and
using the appropriate safety equipment. (PubChem)

Na2C2O4: Sodium oxalate is a strong dicarboxylic acid that is naturally generated in plants and vegetables.
It is used as an analytical reagent and a general reducing agent. It is harmful upon contact with skin and if ingested.
due to its toxicity. It should be handled using appropriate laboratory safety equipment such as
gloves and gown. (PubChem)
FeSO4: Ferrous sulfate is a yellowish crystalline powder that is used, for example, in water treatment.
cloacal and as an ingredient in fertilizer. It causes irritation to both the skin and the eyes, it is also harmful.
upon ingestion. It should be handled using appropriate laboratory safety equipment such as gloves and a lab coat.
(PubChem)
Resultados:

Description: For the experimentation process, it was necessary to first prepare a primary standard and standardize it.
To prepare this, a solution of concentrated sulfuric acid diluted in water was made in a ratio of 1:8 (25 mL of acid.
200 mL of water); to this solution, 0.316 g of KMnO4 was then added. Next, a 0.5 M solution was prepared.
sodium oxalate. This was prepared by adding 0.67 g of oxalate and diluting to 100 mL with water. To standardize the
potassium permanganate, this solution was titrated with sodium oxalate while it was maintained at 60 ºC on the grill and
with constant agitation. In this way, the concentration of the potassium permanganate solution was determined.

Once the concentration of the permanganate solution was calculated, the 0.1M ferrous sulfate solution was prepared.
what is to which the amount of iron present will be determined. To prepare this solution, 2.77 g of sulfate were weighed.
ferrous heptahydrate and were dissolved in 50 mL of the previously prepared 1:8 acid solution to then be
up to 100 mL with water.

This 0.1M ferrous sulfate solution was then titrated using the solution of known concentration of
potassium permanganate.
Table #1:

Valuation of: Standard Solution: Volume of Solution Used: Average Volumes:

8 mL
Potassium permanganate Sodium oxalate 9.1 mL 8.76 mL
9.2 mL
Table #2

Valuation of: Standard Solution: Volume of Solution Used: Average Volumes:

9.5 mL
Iron Sulfate 9.4 mL
Potassium permanganate 9.43 mL
9.4 mL

Analysis of Results:
The first process that was carried out was the titration of the potassium permanganate solution with a solution of
sodium oxalate 0.05M diluted in sulfuric acid, allowing the following oxidation reaction to occur
reduction

+ + → + + + +
(Moreno, 2017)

This reaction, generated from the titration process, was made possible by the introduction of the acid.
sulfuric, since it provides the necessary acidic medium, which adds hydronium and water to the half-reactions for
balance the reaction. If the solution were too basic or too acidic, the reaction might not take place.
cabo (Easy Chemistry, 2017).

However, the reaction can be simplified in terms of ionic interaction, where the permanganate ion reacts.
with the oxalate ion in the following way:
−
+ +− +→ ++ +

Alone
The manganese ion is reduced fromMn7+ aMn2+ acting as an oxidizing agent, and generating the visible color change
at the endpoint, which could be observed by the presence of a pale pink color whose intensity was changing.
change, within the oxalate ion, the carbon was oxidized from a state of 3+ to 4+, acting as an agent
reducer. In total, 10 electrons were exchanged in the reaction considering the stoichiometric coefficients.
As can be seen, the valuation process was carried out in triplicate (see table #1), resulting in a
average volume of KMnO4 used is 8.76 ml. Using this average value, the true can be obtained
concentration of the potassium permanganate solution, this through the equilibrium concentration formula.

Where:

= C1analyte concentration

( . )( ) V1Volume of the analyte

=
( . ) C2standard solution concentration

= . V2= Volume of standard solution

Given that the standard solution used, which was sodium oxalate, had a molarity of 0.05 and a
Volume of 10ml, the concentration obtained for the permanganate solution was 0.0577M. Note how the value
obtained has a deviation of 65% compared to the pre-calculated theoretical value, which is 0.02M. Nevertheless, the
The real value of the solution can be considered as 0.0577M since the process was performed in triplicate and the amount of
Errors that could have occurred during the permanganate solution process are significant. This could have been...
reacted with some other component due to its low instability, and it may be that at the time of gauging it has not
done correctly.

Continuing with the experimental process, once the permanganate solution was standardized with the oxalate, it
proceeded to prepare the evaluation of the iron sulfate solution, which was prepared in such a way that its concentration
theoretical was 0.1M. Again, sulfuric acid was added in order to create the acidic medium.
necessary for the reaction to take place. The reaction that was generated during the titration process was the
next:

+ + → + ( ) + +
(Chemical equations)

As can be observed, a REDOX reaction is generated again, where the participating ions are the
permanganate and iron (II). This can be better visualized in the following simplification of the reaction:
− ++ +→ ++ ++
+
(Alonso)
In this case, the reducing agent is iron. + ), which oxidizes to enter the state +. Instead, the agent
the oxidizing agent is manganese again, reducing and transitioning from a state +a + The total number of electrons that
they exchanged was 5.

Once again, as can be observed in the results, the valuation of ferrous sulfate was done three times (note that
Table #2), and the average volume of KMnO4 used was this time 9.43 ml. In this case, to obtain the
concentration of the solution and subsequently obtain the percentage of iron in it, the process is more
complex, since it is necessary to take into account the interactions that occur between the main participating ions.

First, the amount of moles of potassium permanganate that interacted in the reaction was determined,
obtaining the molarity of this same solution initially obtained:
0.0577 4
0.0577 4= = 5.76 × 10−5 4/
1000ml
4
5.76 × 10−5 ∗ 9.43ml = 5.44× 10-4 4

Note that the total moles were obtained in one milliliter, and subsequently, the amount that was present in the
9.43ml spent on the assessment. Once the total moles are obtained, the stoichiometric calculation proceeds, where
It is observed in the previously proposed reaction that 2 moles of potassium permanganate react with 10 moles of
ferrous sulfate

10 mmol FeSO4
5.44× 10-4 4× | | = 2.72× 10−3 4
2 4
With this, the amount of moles of ferrous sulfate is obtained, and from this data with the total volume of solution.
(0.031lts), the concentration of iron in the solution is obtained, as this is the same as that of the sulfate due to
to the 1:1 relationship that exists between both.

2.72× 10−3 4
[ ]4= = .
0.031lt
[ 2+ ]
= .
The final concentration of iron obtained in the solution is 0.0877M. To calculate the percentage of iron, we
perform the following calculation:

2+ |
55.845g Fe2+
| 0.0877 ×| | = 40.898g Fe2+
1 mol Fe2+

2+ (
4.898g Fe2+
% )= × 100 = 0.49%
1000ml solution
In itself, the final percentage of iron determined in the ferrous solution is 0.49%, which is a relatively low value.

Note that there is an error from the result obtained for the concentration of ferrous sulfate and iron.
being 0.0877M when the true value is 0.1M. This difference represents an error of 12.3%, which was
propagated to the final result obtained, being considerably high.

0.1− 0.0877
% = ( 100 ) = . %
0.1
There are different reasons why the error may have occurred, including instability the
permanganate at the time of performing the titration and random errors generated at the time of making the solutions with
quantities not completely exact. Likewise, the results may have been affected by lack of
cleaning in some containers, affecting the reaction process by potassium permanganate.

Conclusions:

Questionnaire:

1. What is an indicator?
The color indicators are always weak acids or bases that have the property of changing their color.
depending on the pH of the medium in which they are found. And they are used to determine and characterize the
acids and bases. (Méndez, 2012).
2. Why is potassium permanganate indicator used?
In this practice, the KMnO indicator is used.4, because it is a very strong oxidizer and self-indicator.
(Barroso, 2017).
3. Why does it need to be valued?
KMnO4it cannot be used as a primary standard because the KMnO is still4for analysis always contains
small amounts of MnO2Additionally, when preparing the potassium permanganate solution, the water
 distilled may contain organic substances that can reduce KMnO4a MnO2and the same
Potassium permanganate4is capable of oxidizing water. (Barrozo, 2017).
4. What is a primary pattern? What is it for?
It is a substance used in chemistry as a reference to value another substance or standardize it.
The characteristics of this are:
a. It has a known composition.
b. It must have high purity.
c. It must be stable at room temperature.
d. It should be possible to dry it in an oven.
e. It should not absorb gases.
f. It must react chemically and stoichiometrically with the titrant.
It must have a large equivalent weight.
(Galano, Rojas, n.d.).
5. What does sulfuric acid provide in the reaction?
Provide enough acidic medium for the reaction to take place, as if the solution is too
too acidic or too basic the reaction may not occur. REFERENCE
6. What reaction does potassium permanganate have when exposed to light?
The same MnO2what is formed in the reaction of potassium permanganate and water serves as a catalyst for
this reaction and that together with heat, light, the presence of acids or bases and Mn salts, catalyze it with
greater intensity. (Barrozo, 2017).
7. If the sample to be used were a vitamin, what results would be obtained?
The assessment could not be carried out, as the turning point of this substance cannot be observed with the naked eye.
From this perspective, another type of assessment would need to be used to determine the concentration of iron in the vitamin.
8. Balance the redox reaction of Fe using the ion-electron method. 2+with MnO4-.

9. Calculate the % p/v of iron (II) in a problem sample of 50 ml, which was diluted to 100 ml in a flask.
volumetric, 25 ml of this solution was taken and titrated with a permanganate solution of
potassium 0.098 M, using 34.5 ml.
If only 34.5 ml were used, then the moles of KMnO4 used are;

According to our reaction, 2 moles of KMnO4 react with 10 moles of Fe2+.

To obtain the grams used of Fe2+, its molar mass is used:

 Then only the concentration in %p/v of iron present in the solution is calculated.

What is volumetric analysis?

It is the assessment where the volume of reagent consumed in the reaction to be addressed is measured.
to carry out a volumetric analysis that allows us to identify an analyte, certain conditions must be met
a series of conditions such as, for example, the existence of a chemical reaction between the analyte and another type of substance,
la cual puede ser o no un reactivo, que se encuentre bien desplazada hacia la derecha y de la cual conozcamos
good your stoichiometry. (Méndez, 2012).

Ethics in the Laboratory:

Generated waste How was the discarded Do you find the handling appropriate?
residue? Was it given? Justify your answer.

Sulfuric Acid (H2SO4) 1:8 Acids Yes, we found the management that was done appropriate.
gave it to the residue, since when measuring its pH,
this was less than 7, turning it into a
acid.

Potassium Permanganate Acids Yes, we found the handling to be appropriate.

(KMnO40.02M gave it to the residue, since when measuring its pH,
this was less than 7, turning it into a
acid.

Sodium Oxalate (Na2C2O4) Acids Yes, we found the handling to be appropriate.

0.05M it gave the residue, since when measuring its pH,
this was less than 7, turning it into a
acid.

Ferrous Sulfate (FeSO4) Acids Yes, we found the management that was done appropriate.
0.1M he gave it to the residue, since when measuring its pH,
this was less than 7, turning it into a
acid.

Reaction of Na2C2O40.05M Acids Yes, we found the handling that was done appropriate.
with KMnO40.02M he gave it to the residue, since when measuring its pH,
this was less than 7, turning it into a
acid.

FeSO reaction40.1M Acids Yes, we found the management to be appropriate.

with KMnO40.02M it gave the residue, since when measuring its pH,
this was less than 7, turning it into a
acid.
 Personal Reflections:

Rogelio Tovar Medel

The development of the practice was definitely a challenge, as initially there were no results due to the presence
from many experimental errors. However, in the end, it was possible to meet the objectives set and it was possible to carry out
the experimental process correctly. I found the practice interesting, and I could notice the importance that the
Volumetric processes can have in different fields such as civil engineering.

Diego Campos Ramírez:

During the development of this practice, we had many problems; we wanted to have something complete, but we couldn't.
Taking other factors into account, in the end we were able to obtain results that could serve us and that are close to reality.
He put our minds to work to figure out what we should do. Even with the change of experiment, we had
certain complications, for example, that we did not know exactly how the concentration would be determined, since
In the practices we took as reference, it didn’t say how to obtain it and, doing the calculations on our own,
correct stoichiometric ratios allowed us to determine the concentration. I am satisfied with the results, as if we
He worked hard to reach them and that they are the right ones is very satisfying.

Eduardo González Melgoza

Rafael Treviño Perales:

This practice was very laborious and took a long time to complete; the original idea also included the calculation of iron in a
Pharmaton brand vitamin, however, after several attempts it was not possible to determine this, so it was discarded.
Throughout this experiment, I applied my acquired knowledge about oxidation-reduction reactions and
volumetry. What I found most interesting is the approach we were able to take with the career that most of the
Team members study: Civil Engineering, which may help us in some future subject or in
our professional life.

References:

Méndez, A., (2012). Chemistry: Volumetric Analysis. The Guide. Retrieved on November 17, 2017 from:
[Link]
Galano, A., Rojas, A., (N.D.). Standard substances for the standardization of acids and bases. UNAM. Retrieved on the 17th
of November of 2017 de:
[Link]
Barrozo, M. (2017). Permanganimetría. Ciencia Básica Experimental Para Estudiantes de Ingeniería Química.
Retrieved on November 17, 2017 from: [Link]
S.A. (2017) Enter Compound Name or Formula. PubChem, The Open Chemistry Database. Accessed on the 22nd
November 2017. Available en: [Link]
Solá, Jaime. (S.F.). Reacción entre los iones de permanganato y oxalato. GRUPO HEUREMA. Recuperado de:
[Link]
Arena, Susan. Hein Morris. (2010). Fundamentos de Química. México: Cengage Learning.
Ayres. H. (1970). Análisis Químico. México: Harla.

Moreno, Mario Barroso. (2017). Permanganimetría. Ciencia Básica Experimental para Estudiantes de Ingeniería
Chemistry. Retrieved frome:[Link]

Acuña, Anthony Martin. (2008). El Fierro en la Ingeniería Civil. FIERRO. Recuperado de:
[Link]
Ramírez, Johann. (N.D.). What is ferrous sulfate used for? [Link]. Retrieved from:
[Link]
S.A. (S.F.). Chemical equations. Retrieved from: [Link]/homework-help/Thomas-Calculus-Multivariable-12th
edition-chapter-15.2-problem-11E-solution-9780321643698
Méndez, A., (2012). Química: Análisis volumétrico. La Guía. Recuperado el 12 de septiembre de 2017 de:
[Link]
Ángeles. (2012). Curvas de Valoración: El punto de equivalencia y el punto final. Química.
[Link]
Álvaro, L. (2011). Analysis Quantitative. Valuation by Precipitated. Recovered de:
[Link]
S.A. (2010). Concentration Balancey Chemist. Slideshare. Recovered de:
[Link]
S.A. (2017). Oxidation Reduction REDOX–Acidic Medium. Easy Chemistry. Retrieved from:
[Link]
Alonso, Carlos. (S.F.). Electrochemistry. Problems of Chemistry. Recovered de:
[Link]
S.A. (S.F.). DETERMINATION OF IRON (II) IN COMMERCIAL VITAMINS BY REDOX.
Recovered de:
[Link]
[Link]