Experiment No. 4: Standardization of Sodium Thiosulphate Solution With A Standard Potassium Dichromate Solution

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Experiment No.

Standardization of Sodium Thiosulphate Solution with a


Standard Potassium Dichromate Solution
Objectives

• Main objective of this experiment is to determine the


strength of sodium thiosulphate

•To know about redox titration

• To know about iodometric titration

• Importance of sodium thiosulphate in industries


Redox titration

•This titration based on a redox reaction between the


analyte and titrant
• It involves the use of starch indicator
Why Iodometric Method for Standardization
of Na2S2O3 ?

• Experiment is standardization of Na2S2O3 with standard


K2Cr2O7 but they can’t react directly.

• In that case iodometric method is used to make a connection


between them.

• First K2Cr2O7 reacts with KI to liberate I2 and then this liberated


I2 is titrated with Na2S2O3. This is iodometric method.

• That’s how iodometric method can be applied in redox titration.


Iodometric Titration

Ø Iodometric titration is based on the oxidation of iodide into


iodine
Ø The amount of liberated iodine is measured by the titration
of iodine with thiosulphate

Ø When an excess of iodide ion is present, the tri-iodide ion


is formed.
Half reactions with Reduction Potential

In I2 liberation
Reduction half reaction: Cr2O72- + 14H+ + 6e- 2Cr3+ + 7H2O
E° = 1.36 V

Oxidation half reaction: 2I- I2 + 2e-


E° = - 0.54 V

Titration of I2 with Na2S2O3


Reduction half reaction: I2 + 2e- 2I- E° = 0.54 V

Oxidation half reaction: 2S2O32- S4O62- + 2e-


E° = - 0.080 V
Iodimetric titration

Ø This method refers to titration with a standard solution of


iodine. Sn2+ + I2 Sn4+ + 2I-
Ø Titration is performed in neutral or mildly alkaline to
weakly acid solutions.
Ø If the pH is too alkaline, I2 will disproportionate to
hypoiodate iodine.
Ø Starch is used to detect the end point of such titration.
Visual detection of end point
Self Indication:
If the reducing or oxidizing is colored, end point can be
detected by the appearance or disappearance of color of the
reagent. e.g. KMnO4
Starch Detection:
Starch is used for titrations involving iodine. It forms dark blue
color with iodine.
Redox Indicator:
These are dye compounds that are weak reducing or oxidizing
agents that can be oxidized or reduced and color of both forms
are different. e.g. diphenylamine is redox indicator.
Starch as Indicator
Ø Starch reacts with iodine in the presence of iodide to form
an intensely blue-colored starch-triiodide complex.

Ø Starch has two components, amylose and amylopectin.


Amylose gives a blue color with iodine.
Starch as Indicator

Ø Starch can’t be used in a strongly acid medium


because hydrolysis of the starch occurs.
Ø Iodine concentration diminishes the color changes to blue,
which becomes intense just before the end point and end
point is very sharp.
Reactions involve in titration are:

Ø After adding KI(excess), HCl, K2Cr2O7

Ø Then this liberated iodine is titrated with thiosulphate

Ø Starch is added to the solution to detect end point


Ø It forms starch-triiodide complex and its color is deep blue
Ø By reacting this complex with thiosulphate yields light
Ø Blue/green color solution which is end point
Apparatus and Chemicals
• Conical flask
• Burette
• Pipette
• Volumetric flask
• Stand
• Funnel
• Watch glass

• KI
• NaHCO3
• HCl (concentrated)
• K2Cr2O7
• Na2S2O3
• Starch
Solution Preparation
Preparation of 100 mL 0.1N K2Cr2O7 solution

Transfer 0.49 g pure K2Cr2O7 into a 100 mL volumetric flask

Dissolved with distilled water upto the mark


Experimental Procedure

4 mL of 10% KI solution in a conical flask and dilute it to


about 50 mL

1 g of NaHCO3 and shake the flask until the salt


dissolves
Produces CO2

4 mL conc. HCl acid and add 10 mL standard K2Cr2O7


solution by means of a pipette in the same flask

Contd…….
Experimental Procedure

Shake the flask and cover it with watch glass, allow it for
five minutes in dark.
I2 liberated and keep soluble in solution

Rinse the watch glass and dilute solution about 100 mL

Titrate the liberated iodine with Na2S2O3 until the brown


color fades (light yellow due to tri-iodide ion)
Experimental Procedure
Add about 1 mL starch solution
Form starch-triiodide complex

Continue titration by adding Na2S2O3 from burette

One drop of Na2S2O3 changes the color of the solution


from deep blue to light green or light blue (end point)

https://www.youtube.com/watch?v=X2KrBfnKw24
Data Table
Table Name:

Obs. Volume Burette reading of Difference Average


No. of Na2S2O3 solution, of Burette volume
K2Cr2O mL reading, of
7 Initial Final mL Na2S2O3
solution reading reading (B-A) solution
, mL (A) (B) mL
(Y) (C)
1 10
2
3
Calculation
Calculate the concentration of Na2S2O3 solution
using the following equation:

Volume of K2Cr2O7, V1 = Y mL
V1 ´ N1 = V2 ´ N2
Concentration of K2Cr2O7, N1 =

or, Y ´ 0.1 = C ´ N2 0.1 N

or, N2 = Z Volume of Na2S2O3 , V2 = C mL


Concentration of Na2S2O3, N2 = ?
Result and Discussion

Result: Concentration of Na2S2O3 is Z N

Percentage of Error:
Calculate % of error by using the following formula:

Known value - Observe value


´100
Known Value

Discussion:
Questions

1. Differentiate between iodometric and iodimetric titration.


2. Why do you add NaHCO3?
3. Why it is necessary to keep your experimental solution
in the dark?
4. What is the function of starch ?

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