CHEMISTRY 4: Frontiers of Chemistry - Elective Class

GROUP NO. 1 Date Performed: March 4, 2020

NAMES: Comuelo, J.Z.; Socrates, L.D.; Tionko, S.W. Date Submitted: March 13, 2020

LABORATORY REPORT NO. 1

REDOX TITRATION - Iodometry
I) Standardization of sodium thiosulphate
II) Estimation of copper

A. OBJECTIVES

1. To titrate a primary standard solution of potassium iodate against a standard

solution of sodium thiosulphate;
2. To titrate the copper(II) salt against a standard solution of sodium thiosulphate;
3. To calculate the normality of sodium thiosulphate; and
4. To calculate the percentage of copper in the given salt

B. PURPOSE/PRINCIPLE

Titration is the slow addition of one reagent of known concentration (titrant) to another of
unknown concentration (analyte). An indicator, which changes color when pH changes is added to
the solution of unknown concentration. Neutralization will be achieved when the color changes very
slightly from the indicator’s original color. A redox titration is defined as a type of titration that
involves a redox reaction between the analyte and titrant. Iodometry is the most common type of a
redox titration, where the appearance or disappearance of elementary iodine indicates the endpoint.
Iodometry involves the indirect titration of iodine liberated by reaction with the analyte. Sodium
thiosulphate (Na2S2O3) is usually the reducing agent used as it is used to specifically titrate iodine.
Iodometry is commonly used to determine the concentration of an oxidizing agent in solution, which
in this experiment, is copper(II) [1].

Iodometry is usually used due to the following reasons: Potassium iodide is readily available
in high purity; Starch is available as an indicator to signal the equivalence point in the reaction
between iodine and thiosulfate. Starch turns blue-black in the presence of iodine. Therefore, when
the blue-black color disappears, the iodine has been completely reduced to the iodide ion.
Iodometric reactions are rapid and quantitative, and; a precise and stable reducing agent is available
to react with the iodine [2].

In the experiment, the normality of Na2S2O3 was determined from the volume dispensed and
the percentage of copper in copper(II) nitrate trihydrate was also calculated from the volume of
Na2S2O3 dispensed.
C. MATERIALS/APPARATUS

Table 1. Materials and apparatus to be used.

Quantity Item Description

0.35g KIO Analytical grade

12g Na₂S₂O₃.H₂O Analytical Grade

2g KI 10%

30mL H₂SO₄ 1M

1g Cu(NO₃)₂.3H2O Analytical Grade

2L Distilled water N/A

1 pc Volumetric Flask 500-mL

2 pcs Beaker 250-mL

3 pcs Beaker 100-mL

2pc Volumetric Flask 100-mL

1 pc Volumetric Flask 250-mL

1pc Glass dropper N/A

1pc Glass Rod N/A

1pc Wash Bottle N/A

1pc Burette N/A

1pc Iron Stand N/A

1pc Burette clamp N/A

7 pcs Erlenmeyer flasks 250-mL

2 pcs Measuring pipette 10-mL

1 pc Empty Plastic Bottles 1-L

1 pc Analytical Balance N/A

1 pc Rubber Aspirator N/A

D. SCHEMATIC DIAGRAM OF METHODS

Standardisation of sodium thiosulfate (Na2S2O3)

Estimation of copper in copper(II) nitrate trihydrate

E. RAW DATA

Table 2 shows the weights of potassium iodate, sodium thiosulfate, and copper(II) nitrate
trihydrate used for the experiment.

Table 2. Weight (in grams) of chemicals.

Chemical Weight (in grams)

Potassium Iodate 0.36451

Sodium Thiosulfate 12.24201

Copper(II) Nitrate Trihydrate 1.99890

Potassium iodate solution was titrated against sodium thiosulfate solution with starch as an
indicator. Table 3 shows the volume of Na2S2O3 used in titrating 25.0 mL of KIO3 solution with starch
as an indicator. Color change was from blackish-red to colorless.

Table 3. Volume of Na2S2O3 used in titrating 25.0 mL of KIO3 solution with starch as an indicator.
Sample (KIO3) Initial burette Final burette Volume of Na2S2O3
reading (mL) reading (mL) used (mL)

Sample 1 0.00 29.95 29.95

Sample 2 0.00 28.00 28.00

Sample 3 12.85 42.40 29.55

25 mL distilled water (blank) 0.00 0.00 0.00

Copper(II) nitrate trihydrate was titrated against sodium thiosulfate solution with starch as an
indicator. Table 4 shows the volume of Na2S2O3 used in titrating 25.0 mL of CuN2O6*3H2O with starch
as an indicator. Color change was from blue to white.

Table 4. Volume of Na2S2O3 used in titrating 25.0 mL of CuN2O6*3H2O solution with starch as an indicator.

Sample (CuN2O6*3H2O) Initial burette Final burette Volume of Na2S2O3

reading (mL) reading (mL) used (mL)

Sample 1 6.85 23.80 16.95

Sample 2 28.00 45.40 17.40

Sample 3 0.00 16.35 16.35

25 mL distilled water (blank) 0.00 0.00 0.00

F. SAMPLE CALCULATIONS

Calculation for molarity

Molarity of KIO3 can be calculated by dividing the mass weighed by its molecular weight to
obtain the moles of KIO3 and dividing the moles of KIO3 by the volume of solution:

0.36451 𝑔𝑟𝑎𝑚𝑠
Molarity (KIO3) = 214. 001 𝑔/𝑚𝑜𝑙
0.1 𝐿 𝑠𝑜𝑙'𝑛

Molarity (KIO3) = 0.01703309798 M

Molarity (KIO3) = 0.017 M

Calculation for normality

Normality of Na2S2O3 can be calculated by the obtaining the molarity of Na2S2O3 and
multiplying it to its equivalent (mole of reacting species):

Normality (Na2S2O3*5H2O) = Molarity * n (equivalent)

12.24201 𝑔𝑟𝑎𝑚𝑠
Normality = 248.18 𝑔/𝑚𝑜𝑙 *2
0.5 𝐿 𝑠𝑜𝑙'𝑛

Normality = 0.1973085664 N

Normality = 0.2 N

Calculation for percentage of copper(II)

The two equations involved in the titration of copper(II) nitrate trihydrate with sodium
thiosulfate and starch as an indicator are as follows [3]:

2Cu²⁺ + 4I⁻ ⇌ 2CuI(s) + I₂

I₂ + 2S₂O₃²⁻ ⇌ 2I⁻ + S₄O₆²⁻

From the equations, the net stoichiometry of copper ions to sodium thiosulfate ions is 1:1
because 2 moles of copper requires 2 moles of sodium thiosulfate.

To calculate the percentage of copper(II), moles of the sodium thiosulfate must be determined
which is equal to moles of copper(II) ions. Then, the percentage of copper(II) can be calculated by
multiplying the moles of copper(II) ions to its molecular weight and dividing it by the mass of the
weighed copper(II) nitrate trihydrate.

1𝐿 0.0987 𝑀 𝑁𝑎2𝑆2𝑂3
No. of moles of Na2S2O3 = 16.95 mL * ( ) *( )
1000 𝑚𝐿 1000 𝑚𝐿
No. of moles of Na2S2O3 = 1.6721901 * 10-3 moles
 No. of moles of Na2S2O3 = No. of moles of Cu2+

2+
63.546 𝑔 𝐶𝑢
g Cu = 1.6721901 * 10 moles Cu *(
2+ -3 2+
2+ )
1 𝑚𝑜𝑙 𝐶𝑢

g Cu2+ = 0.1062609921 g

0.1062609921 𝑔
% Cu2+ = ( ) * 100
1.99890 𝑔

% Cu2+ = 5.32%

G. RESULTS

Table 5 shows the calculated and average percentage (with standard deviation) of copper(II)
in copper(II) nitrate trihydrate.

Table 5. Calculated and average percentage of copper(II) in copper(II) nitrate trihydrate.

Sample 1 Sample 2 Sample 3 Average

% Cu(II) 5.32 5.46 5.13 5.303 ± 0.13524

H. DISCUSSION

A redox titration is defined as a type of titration that involves a redox reaction between the
analyte and titrant. Iodometry is the most common type of a redox titration, where the
appearance or disappearance of elementary iodine indicates the endpoint. Iodometry involves
the indirect titration of iodine liberated by reaction with the analyte. Sodium thiosulphate is
usually the reducing agent used as it is used to specifically titrate iodine. Iodometry is commonly
used to determine the concentration of an oxidizing agent in solution, which in this experiment,
is copper(II) [1].

Iodometry is usually used due to the following reasons: Potassium Iodide is readily available
in high purity; Starch is available as an indicator to signal the equivalence point in the reaction
between iodine and thiosulfate. Starch turns blue-black in the presence of iodine. Therefore,
when the blue-black color disappears, the iodine has been completely reduced to the iodide ion.
Iodometric reactions are rapid and quantitative, and; A precise and stable reducing agent is
available to react with the iodine [2].

The amount of iodine liberated in the reaction between iodide ion and an oxidizing agent is a
measure of the quantity of oxidizing agent originally present in the solution. The amount of
standard sodium thiosulfate solution required to titrate the liberated iodine is then equivalent to
the amount of oxidizing agent. To a known volume of sample, an excess but a known amount of
iodide is added, which the oxidizing agent then oxidizes to iodine. Iodine dissolves in the
iodide-containing solution to give triiodide ions, which have a dark brown color. The triiodide ion
solution is then titrated against standard thiosulfate solution to give iodide again using starch
indicator:
I₃⁻ + 2e⁻ ⇌ 3 I⁻

The reaction between iodine and the thiosulfate ion is as follows:

I₂ + 2S₂O₃²⁻ ⇌ 2I⁻ + S₄O₆²⁻

Sulfuric acid was added in this experiment to control the pH and due to the nature of Copper
being a strong oxidizing agent. The titration of the liberated iodine must be completed quickly in
order to eliminate undue exposure to the atmosphere since an acid medium constitutes an
optimum condition for atmospheric oxidation of the excess iodide ion, which is why the
Erlenmeyer flasks were immediately covered using parafilm [1].

The reaction of copper in the iodometric method is determined by the equation:

2Cu²⁺ + 4I⁻ ⇌ 2CuI(s) + I₂

This is a rapid, quantitative reaction in slightly acidic solutions. The iodine that is liberated
was titrated in the usual manner with standard thiosulfate solution [2].

The sample had an average copper percentage of 5.303 % with a standard deviation of
0.13524.

Sources of error in the experiment would include loss of iodine by evaporation from the
solution and the atmospheric oxidation of iodide ion in acidic solution [1].

GUIDE QUESTIONS:

1. In solutions containing iodine and an iodide, the following equilibrium is obtained:

I2(aq) + I- + →I3-

Will this affect the accuracy of the above titrations? Explain.

No as the triiodide exists in equilibrium with both the iodine and iodide. The addition
of thiosulphate will reduce the aqueous iodine which will then cause the reaction to
proceed from right to left in order to achieve equilibrium.

2. Iodide is slowly oxidized by oxygen in presence of light. Write a balanced equation.

How will you minimize the error due to reaction in your work?

4 I- + 4 H+ + O2 ⇔2 I2 + 2 H2O

To minimize the error, the reaction vessel shall be immediately covered by a cling
wrap or parafilm so that no air (O2) will go in and react with the reactants.
 3. Iodine has appreciable volatility. How will you minimize the error due to this?

The error was minimized by immediately sealing the mouth of the container of the
solution after the iodine was added in order for air to be unable to escape the
container.

4. You have analysed a pure copper(II) salt. What complications may arise when you try
to apply this procedure to estimate the percentage of copper in an ore?

An ore may contain an excessive amount of impurities, some of which may be

oxidizing agents that will react with the iodide causing the estimation to be
inaccurate.

I. CONCLUSION

Iodometry, or Iodometric titration, was used in order to determine the percentage of copper
present in Copper (II) nitrate trihydrate. This is a type of redox titration where the disappearance
of the iodine indicates the endpoint. Potassium Iodide was used as the source iodine and starch
was used as the indicator during the titration. Results showed that the sample had an average Cu
percentage of 5.303% with a standard deviation of 0.13524.

J. SOURCES

[1] Libretexts. (2019, June 5). Iodometric Determination of Cu in Brass. Retrieved from
https://chem.libretexts.org/Bookshelves/Ancillary_Materials/Laboratory_Experiments/Wet_
Lab_Experiments/Analytical_Chemistry_Labs/Iodometric_Determination_of_Cu_in_Brass

[2] Shatter PA and Hartmann AF. (n.d.). The iodometric determination of copper and its use in sugar
analysis. Retrieved from https://www.jbc.org/content/45/2/349.full.pdf

[3] Jaramillo E, Dua S. (2019). Iodometric Determination of Copper. Retrieved from

https://www.studocu.com/en-us/document/new-jersey-city-university/analytical-chemistry-l
aboratory/other/iodometric-determination-of-copper/6010856/view

K. DIVISION OF TASKS

Comuelo, J.Z. – Objectives, Purpose and Principle, Materials/Apparatus, Appendices

Socrates, L.D. – Discussion, Conclusion, Guide Questions
Tionko, S.W. – Purpose and Principle, Schematic Diagram of Methods, Raw Data, Sample
Calculations, Results, Guide Questions
L. APPENDICES

Figure 1. KIO3 sample 1. Figure 2. KIO3 sample 2 . Figure 3. KIO3 sample 3.

Figure 4. Cu(II) salt sample 1. Figure 5. Cu(II) salt sample 2. Figure 6. Cu(II) salt sample 3.

Figure 7. Cu(II) salt sample 1. Figure 8. Untreated Cu(II) samples. Figure 9. Weighing
Na₂S₂O₃.H₂O