EXPERIMENT JOURNAL OF BASICS ANALYTICAL CHEMISTRY

Iodo-Iodimetric Titration

By :
Gus Fajar Arrasyid Insani
22030194102
PKI 2022

CHEMISTRY EDUCATION STUDY PROGRAM

CHEMISTRY MAJOR
FACULTY MATH AND SCIENCE
SURABAYA STATE UNIVERSITY
2023
 I. Title
Iodo-Iodimetric Titration

II. Purpose
1. Determine the standardization of Na2S2O3 solution with KIO3 solution

2. Determine sample levels of Betadine and Bleach

III. Day and Date of Experiment

Tuesday, May, 16th 2023 at 09.30 AM

IV. Theoretical Basis

Analytical chemistry is divided into two parts, qualitative analysis and

quantitative analysis. Qualitative analysis is a branch of analytical
chemistry that focuses on determining the presence or absence of specific
chemical components in a sample. It involves identifying the constituents
and understanding the composition of a substance without determining
their exact quantities or concentrations. Quantitative analysis is a branch
of analytical chemistry that focuses on determining the exact amount or
concentration of specific chemical components in a sample. It provides
numerical data about the composition of a substance. (Skoog, D. A, 2017).
Titration is an example of a method in quantitative analysis. Titration
is a common analytical technique used in chemistry to determine the
concentration of a substance in a sample by reacting it with a standardized
solution of another substance (known as the titrant). The process involves
gradually adding the titrant to the analyte until a specific reaction or
endpoint is reached, which indicates the completion of the reaction. By
measuring the volume of titrant required to reach the endpoint, the
concentration of the analyte can be calculated.(Harris, D. C., 2016).
The working principle of titration involves the gradual addition of a
standardized solution (titrant) to a solution containing the analyte until a
specific reaction or endpoint is reached. The endpoint indicates the
completion of the reaction between the analyte and the titrant. By
measuring the volume of titrant required to reach the endpoint, the
concentration of the analyte can be determined. (Skoog, D. A, 2017).
There are various kinds of titrations contained in quantitative analysis,
one of which is Iodo-Iodimetric Titration.

1. Iodo-Iodimetric Titration

Iodometric titration is a type of redox titration that involves the use

of iodine and iodide ions in the reaction. It is commonly used to
determine the concentration of oxidizing agents or compounds that can
be oxidized by iodine. During the titration, iodine is generated and
reacts with the analyte, resulting in the formation of iodide ions. The
endpoint is reached when all the analyte has reacted, and the excess
iodine imparts a characteristic color change. (Mendham, J,2000). . The
salt is usually in the form of the pentahydrate Na2S2O3.5H2O.
Solutions should not standardized by direct weighing, but must be
standardized with standard stock solutions. Sodium thiosulfate solution
is unstable for a long time. The color of the iodine solution is strong
enough for iodine to serve as an indicator on its own. However, the use
of starch solutions is more common because the dark blue color of the
starch-iodine complex is used for the iodine sensitivity test.
(Underwood, 2004).
The term "oxidation" refers to a chemical reaction in which a
substance loses electrons or increases its oxidation state. It is typically
associated with the transfer of oxygen atoms, removal of hydrogen
atoms, or loss of electrons from a chemical species. The term
"reduction" refers to a chemical reaction in which a substance gains
electrons or decreases its oxidation state. It involves the addition of
hydrogen atoms, the gain of electrons, or the transfer of oxygen atoms
from a chemical species. (Chang, R., 2017).
The term "oxidizing agent" refers to a substance that is capable of
accepting electrons from another substance, leading to the oxidation of
that substance. Conversely, a "reducing agent" is a substance that
 donates electrons to another substance, causing the reduction of that
substance. (Harris, D. C, 2016). This method is used more frequently in
analysis than other methods. This method was chosen because the
stoichiometric equation is easy to apply and practical, poses few
problems, and is simple.

2. Process in the Iodometic Titration Method

a. Direct lodometric processes

Very strong reducing agents such as thiosulfate,

arsenic(III), stibium(III), antimony(II), sulfide, sulfite, tin(I) and
ferracyanide are often used in direct iodometry. reducing power.
Some of these substances depend on the hydrogen ion
concentration, and the reaction with iodine cannot be analyzed
quantitatively without time-consuming pH adjustment. This direct
iodine determination method allows the reaction of iodine and
thiosulfate to go to completion. Excess iodide ions are added to the
specified oxidizing reagent to liberate iodine. This excess can be
titrated. with sodium thiosulfate. According to this method, for
example, when titrating Na2S2O3 with I2 , the reducing agent is
directly titrated with iodine.
2Na2S2O3 + I2 → 2Nal + Na2S4O6
The indicator used in this reaction is a starch solution.
Addition of the thiosulfate solution to the iodine solution
eventually changes the appearance from colorless to blue.
However, adding an iodine solution to a thiosulfate solution will
eventually change its appearance to blue.

b. Indirect or lodometric processes

Iodide ions are converted as reducing agents and the

resulting iodine is titrated with a standard solution of Na2S2O3.
The iodine assay is used to measure oxidants, such as when
measuring oxidants (H2O2). A solution of HCl and acid is added to
this oxidant to generate iodine, which is then titrated.
 Na2S2O3. H2O2 + 2HCl → I2 + 2KCl + 2H2O
many strong oxidizing agents can be analyzed by adding
excess potassium iodide and titrating the liberated iodine. Since
many oxidizing agents require an acidic solution to react with
iodine, sodium thiosulfate is usually used as the titrant, in a pH of
3-4. Titration with arsenic (III) (above) requires a slightly alkaline
solution. (Underwood, 2002).
In a solution, concentration indicates the content of
dissolved substances (solutes). This term means that the amount of
dissolved mass is calculated as unit volume (milliliters) or weight
(grams) per unit solution, so the unit of concentration is
grams/milliliter. This method is called the weight/volume method
or b/v method. In addition to this method, there is a method of
expressing the concentration of solute in grams per gram of solvent
or per gram of solution, called the weight/weight or w/w method.
Mathematically, the volume content of a compound can be
calculated using the following general formula:

3. Standardization

Standardization, in the context of analytical chemistry, refers to the

process of determining the exact concentration or quantity of a solution
or reagent. It involves comparing the unknown solution or reagent with
a known standard, which has a precisely known concentration or
quantity. (Skoog, D. A, 2017).
Primary standard substances are highly pure compounds that
possess certain characteristics, making them suitable for precise and
accurate standardization in analytical chemistry. Here are some
common requirements of a primary standard substance:

a. High Purity: Primary standard substances should have a high

level of purity, typically exceeding 99.9%. Impurities can
affect the accuracy of standardization, so primary standards
undergo extensive purification processes.
 b. Stability: Primary standard substances should be chemically
stable, meaning they do not readily undergo decomposition or
react with the environment. This stability ensures the long-term
reliability of the standard.
c. High Molar Mass: Primary standards often have high molar
masses to minimize errors associated with weighing and to
improve the precision of measurements.
d. Known Stoichiometry: Primary standards should have a well-
defined stoichiometry, meaning the reaction between the
substance and the analyte is well understood and can be
accurately quantified.

Non-hygroscopic: Primary standards should not absorb

moisture from the atmosphere, as this can lead to changes in
weight and concentration. (Harris, D. C., 2016)

V. Tools and Materials

 Tools
a. Burette 50 ml (1 pcs)
b. Erlenmeyer Flask 250 ml (3 pcs)
c. Measuring Cylinder 25 ml (1 pcs)
d. Drop Pipette - (1 pcs)
e. Goiter Sized - (1 pcs)
f. Funnel Clamps and Stands - (1 pcs)

 Materials
a. Potassium Iodide (KIO3) ± 0,1 N 30 ml
b. Na2S2O3 solution ± 0,1 N as needed
c. KI 20% solution - 18 ml
d. HCl solution 4N 9 ml
e. Aquadest - 60 ml
f. Starch (ammilum) indicator - 18 ml
 g. Betadine sample - 30 ml
h. Bleach Sample - 30 ml

VI. Experiment Procedure

A. Determining (Standardization) Na2S2O3 Solution ± 0,1 N with
KIO3 solution
1. Determining (standardization) Na2S2O3 Solution ± 0,1 N with
KIO3 solution

Na2S2O3 solution KIO3 solution

1. Rinsed the burette with Na2S2O3 5. Pipetted with a goiter pipette as

solution 3 times much as 10 ml

2. Added Na2S2O3 solution into the 6. Put it into 250 ml Erlenmeyer

flask
Burette until 2-3 cm above the 7. Added 2 ml of KI 20% solution

Zero point 8. Added 1 ml HCl 4 N solution

3. Opened the tap slowly so that all 9. Placed the Erlenmeyer flask under
parts of burette under the tap are the burette

filled

4. Adjusted the solution to zero point.

if the solution passing below zero

point no need to fill it again. Note

down the number

10. Performed the titration with while continuing to be shaken

11. Stopped when the color of solution turn into light yellow
 Light yellow solution

12. Added 2 ml of starch indicator

13. Titrated until the blue color disappears

Blue color disappears

14. Read and record the number, then calculate the volume of the Na2S2O3
solution is used

15. Repeated the titration 3 times (triplo) with the same volume of KIO3
solution

16. Calculated the average concentration of the Na2S2O3 solution

Average concentration of Na2S2O3 solution

Reaction : KIO3 + 5KI + 6HCl → 6KCl + 3I2 + 3H2O

Reduction : 2IO3- + 12H+ + 10e- → I2 + 6H2O

Oxidation : 2I- → I2 + 2e-

Redox reaction : 2IO3- + 10I- + 12H+ → 6I2 + 6H2O

3I2 + 6Na2S2O3 → 6NaI + 3Na2S4O6

Reduction : I2 + 2e- → 2I-

Oxidation : 2S2O32- → S2O62- + 2e-

Redox reaction : I2 + 2S2O32- → 2I- + S4O62-

A. Determining sample levels of Betadine and Bleach

1. Determining sample levels of Betadine

Na2S2O3 solution Betadine sample

1. Rinsed the burette with Na2S2O3 5. Pipetted 10 ml of Betadine sample

solution 3 times 6. Put it into 250 ml Erlenmeyer flask
2. Added Na2S2O3 solution into the 7. Added 10 ml of aquadest
Burette until 2-3 cm above the 8. Added 2 ml of KI 20% solution

Zero point 9. Added 1 ml HCl 4 N solution

3. Opened the tap slowly so that all 10. Placed the Erlenmeyer flask
under the burette
parts of burette under the tap are \

filled

4. Adjusted the solution to zero point.

if the solution passing below zero

point no need to fill it again. Note

down the number

11. Performed the titration with while continuing to be shaken

12. Stopped when the color of solution turn into light yellow
Light yellow solution

13. Added 2 ml of starch indicator

14. Titrated until the blue color disappears

Blue color disappears

15. Read and record the number, then calculate the volume of the Na2S2O3
solution is used

16. Repeated the titration 3 times (triplo) with the same volume of Betadine
sample

17. Calculated the average concentration of the Betadine sample

Average concentration of Betadine sample

Formula : 3I2 + 6Na2S2O3 → 6NaI + 3Na2S4O6

Reduction : I2 + 2e- → 2I-

Oxidation : 2S2O32- → S2O62- + 2e-

Redox reaction : I2 + 2S2O32- → 2I- + S4O62-

2. Determining sample levels of Bleach

Na2S2O3 solution Bleach sample

1. Rinsed the burette with Na2S2O3 5. Pipetted 10 ml of Bleach sample

solution 3 times 6. Put it into 250 ml Erlenmeyer

2. Added Na2S2O3 solution into the flask

Burette until 2-3 cm above the
Zero point
3. Opened the tap slowly so that all
under parts of burette under the
tap are filled
4. Adjusted the solution to zero point.
if the solution passing below zero
7. Added 10 ml of aquadest
8. Added 2 ml of KI 20% solution
9. Added 1 ml HCl 4 N solution
10. Placed the Erlenmeyer flask
the burette

point no need to fill it again. Note

down the number

11. Performed the titration with while continuing to be shaken

12. Stopped when the color of solution turn into light yellow
Light yellow solution

13. Added 2 ml of starch indicator

14. Titrated until the blue color disappears

Blue color disappears
 15. Read and record the number, then calculate the volume of the Na2S2O3
solution is used

16. Repeated the titration 3 times (triplo) with the same volume of Bleach
sample

17. Calculated the average concentration of the Bleach sample

Average concentration of Bleach sample

Reaction : NaOCl + 2KI + 2HCl → 2KCl + NaCl + I2 + H2O

Reduction : OCl- + 2H+ + 2e- → Cl- + H2O

Oxidation : 2I- → I2 + 2e-

Redox reaction : OCl- + 2H+ + 2I- → Cl- + I2 + H2O

3I2 + 6Na2S2O3 → 6NaI + 3Na2S4O6

Reduction : I2 + 2e- → 2I-

Oxidation : 2S2O32- → S2O62- + 2e-

Redox reaction : I2 + 2S2O32- → 2I- + S4O62-

Formula : e1 . M1 . V1 = e2 . M2 . V2

N1 . V1 = N2 . V2
VII. Bibliography

Chang, R. (2017). Chemistry (13th ed.). McGraw-Hill Education.

Harris, D. C. (2016). Quantitative Chemical Analysis. W. H. Freeman.

Mendham, J. D. (2000). Vogels's Quanitative Chemical Analysis (6th ed). Prentice

Hall.

Skoog, D. A. (2017). Fundamentals of Analytical Chemistry. Cengage Learning.

Underwood, A. L. (1993). Analisis Kimia Kualitatif, Edisi IV. Jakarta: Penerbit

Erlangga.

Underwood, A. L. (2002). Analisa Kimia Kuantitatif Edisi Keempat. Jakarta:

Erlangga.