CHM 229

(EXPERIMENTAL ANALYTICAL CHEMISTRY)

Lecturer: Mrs M.O. Oloyede
Email: mary.oloyede@covenantuniversity.edu.ng
Outline
• Introduction to Redox Titration
• Aim of Experiment
• Apparatus
• Procedure
• Conclusion
Introduction (1/2)
• Titration is a common laboratory method of quantitative chemical
analysis to determine the concentration of an identified analyte.
• There are different types (Acid-base, Complexometric, redox,
precipitation, etc.)
• A redox titration is a form of titration established on a redox reaction
between the titrant and analyte.
• In Redox titration, reduction-oxidation reaction takes place between
the analyte and the titrant. The titrant either reduces or oxidizes the
analyte.
A simple titration set-up
Introduction(2/2)
• Vitamin C (ascorbic acid) is a six carbon chain, closely related
chemically to glucose.
• It was first isolated in 1928 by the Hungarian-born scientist Szent-
Gyorgi and structurally characterized by Haworth in 1933.
• In 1934, Rechstein worked out a simple, inexpensive, four-step
process for synthesizing ascorbic acid from glucose. This method has
been used for commercial synthesis of Vitamin C.
• However, Vitamin C occurs naturally primarily in fresh fruits and
vegetables
Aim of Experiment
• To determine the vitamin C (ascorbic acid) concentration in a solution
using redox titration with iodine as the titrant

Learning Goal is to:

• Be familiar with the chemistry of vitamin C.
• Understand the technique of titration to determine the unknown
concentration of a known reactant.
Apparatus

• Burette and stand

• 100 mL or 200 mL
• volumetric flasks
• 20 mL pipette
• 10 mL and 100 mL measuring cylinders
• 250 mL conical flasks
Procedure(1/2)
• Preparation of 0.005 mol /L iodine solution:
• Weigh 2 g of potassium iodide into a 100 mL beaker. Weigh 1.3 g of iodine and
add it into the same beaker. Add a few mL of distilled water and swirl for a
few minutes until iodine is dissolved. Transfer iodine solution to a 1 L
volumetric flask, making sure to rinse all traces of solution into the volumetric
flask using distilled water. Make the solution up to the 1 L mark with distilled
water.
• Preparation of 0.5% starch indicator solution:
• Add soluble starch (0.25g) to a 100 mL conical flask or beaker and 50 mL of
distilled water. Heat the solution with stirring at 790oC for 5 minutes, care
must be taken not to exceed the stated temperature. Allow solution to cool to
room temperature.
 Procedure(2/2)
• Preparation of Sample:
• For analysis of vitamin C powders dissolved 1 gm in 100mL of
distilled water (in a volumetric flask).
• For analysis of vitamin C tablets dissolved a single tablet in 200 mL of
distilled water (in a volumetric flask).
• Transfer aliquot of the sample (20 mL) solution prepared above into a
250 mL conical flask, add about 150 mL of distilled water and 1 mL of
starch indicator solution.
• Titrate sample with 0.005 mol/L iodine solution.
• The endpoint of the titration is identified as the first distinct trace of a
dark blue-black colour due to the starch-iodine complex.
• Repeat the titrations with further aliquots of sample solution until
concordant results (titres agreeing within 0.1 mL) are obtained.
 Conclusion

As the iodine is added to the solution during the titration, the ascorbic acid is
oxidized to dehydroascorbic acid, while the iodine is reduced to iodide ions.
Ascorbic acid + I2 → 2I- + Dehydroascorbic acid
The endpoint of the titration is identified as the first distinct trace of a dark blue-
black colour due to formation of a starch-iodine complex
Notes
• Iodine stains both skin and clothing so proper care is advised.
• Ascorbic acid is susceptible to oxidation by atmospheric oxygen over
time. For this reason, the samples should be prepared immediately
before the titrations
• However, if the samples have to be prepared several hours earlier,
oxidation can be minimised by the addition of a small amount of
oxalic acid (e.g. 1 g oxalic acid per 100 mL of sample solution).
• Identification of the endpoint in this titration is significantly affected
by the colouration of the sample solution used
• Remember to do your ‘rough’ titration
Demo
• https://www.youtube.com/watch?v=djRv4TyJsC0
THANK YOU FOR LISTENING