PREP-05

TECHNICAL PROCEDURE Revision-02

UNCG Chemistry and Biochemistry
Effective Date:
Coulometric Determination of Vitamin C Page 1 of 8
10-05-2022

UNCG Department of Chemistry and Biochemistry

Version Remarks
Revision-01 Original reformatted into SOP.
Revision-02 Dr. Taylor Mabe

1. Scope
The goal of this experiment is help students gain proficiency in coulometric determinations.

2. Principle
Students will use Faradays Law to calculate the amount of ascorbic acid in solution. The solution will consist of
KI, sulfuric acid, and vitamin C pills.

3. Safety Precautions
 Mercuric iodide causes serious eye and skin irritation. May cause respiratory irritation. Fatal if
swallowed, in contact with skin, or inhaled. Suspected of damaging fertility and the unborn child. Wash
hands thoroughly after handling. Do not breathe dust/fume/gas/mist/vapors/spray. Use only in well-
ventilated areas.
 Potassium Iodide causes serious eye and skin irritation. Wash hands after handling and use only in well-
ventilated areas.
 Sulfuric acid causes severe skin burns and eye damage. Do not breathe dust/fume/gas/mist/vapors/spray.
Wash hands thoroughly after handling.
Wear the following PPE when handling: for skin, wear rubber gloves, apron, and/or clothing; for clothing, wear
appropriate protective clothing to prevent skin exposure; for eyes, wear appropriate eye protection (safety
goggles). See SDS for more information.

This document belongs to UNCG Department of Chemistry and Biochemistry. Copies are to be retained for reference only. Copies are not to be distributed.
 PREP-05
TECHNICAL PROCEDURE Revision-02
UNCG Chemistry and Biochemistry
Effective Date:
Coulometric Determination of Vitamin C Page 2 of 8
10-05-2022

4. Measurement of Uncertainty
The measurement of uncertainty for this method is to be determined.

5. Analytical Procedure
5.1. Apparatus
1. Mortar and pestle

5.2. Reagents
1. Vitamin C pills
2. Potassium iodide
3. Starch
4. Mercuric iodide

5.3. Vitamin C Preparation

Using a mortar and pestle, grind 20-25 pills into a powder and transfer into a bottle. Make sure there is a
separate container for the spatula next to the bottle at the balance.

5.4. Potassium Iodide Preparation

Transfer 750g potassium iodide to bottles for students to weigh out. Make sure there are separate containers for
the spatula next to the bottles at the balances.

5.5. Preparation of concentrated H2SO4

Place the concentrated sulfuric acid in the vent hood.

5.6. Preparation of Starch Indicator

1. Bring ~1000 mL DI water to boiling in a 1000 mL beaker.
2. Using a mortar and pestle, grind 1g starch and 10mg mercuric iodide into a powder then transfer to a
2000 mL beaker.
3. Add 100mL cold DI water into the beaker to make a paste.
4. Add 900mL boiling water and a magnetic stir bar to beaker.
5. Place beaker with boiling water, starch, and indicator on the hot/stir plate and allow the solution to boil
and stir.
6. Allow the solution to boil until it becomes cloudy.
7. Turn the heat off but continue stirring the solution until it becomes clear.
8. Allow the solution to come to room temperature, then transfer to an amber glass bottle.

OLDER COPIES OF SOP BELOW, MAY NOT BE NEEDED

This document belongs to UNCG Department of Chemistry and Biochemistry. Copies are to be retained for reference only. Copies are not to be distributed.
 PREP-05
TECHNICAL PROCEDURE Revision-02
UNCG Chemistry and Biochemistry
Effective Date:
Coulometric Determination of Vitamin C Page 3 of 8
10-05-2022

Coulometric Determination of Vitamin C

Starch Indicator Solution (3% Starch in Formamide):

 In a hood, heat formamide to 100º - 110 ºC. while stirring in a slurry of the required amount of “soluble” starch.
 A 5% solution is prepared by pouring a slurry of 5 grams of soluble starch and 30 mL of cold (room temperature)
formamide with stirring into 65 mL of hot (100º - 110 ºC) formamide.
 The starch dissolves within 1 minute after addition.
 The solution is ready for use as soon as it cools to room temperature.

Students Need to Make Up the Following:

 0.45 M Sulfuric acid: Make up about 150 mL of dilute sulfuric acid ( approx. 1 part acid to 40 parts water.) Add
the acid to the water.
 Vitamin C pill (previously ground up): Weigh precisely about 0.6 g of the crushed pill using weighing paper
and transfer to a 50 mL beaker. Add about 30 mL of the dilute sulfuric acid; mixing thoroughly with a stirring rod. A
small amount of fine filler may not go into solution, but this will not cause a significant error. Transfer quantitatively
to a 100 mL vol. Flask with the dilute sulfuric acid. Mix and dilute to the mark.
 5 % Potassium Iodide Solution: 10 g of KI in 200 mL of water.

Lab 5. Coulometric Determination of Vitamin C

a. Constant Current Sources
b. Crushed up Vitamin C pills
i. Crush about ~20-25 pills for the students
1. Crush pills with a mortar and pestle (There should be one in the stock room or quant
lab). Pills are extremely soft and should be grounded to a powder
ii. Need a separate beaker to hold spatula. Place next to the balance.
iii. Weight of 10 vitamin C pills: 13.78 g
iv. Weight of 1 vitamin C pill: 1.37 g
c. Potassium Iodide
i. In a bottle for the students to weigh out. Make sure there is a separate container for the spatula
next to the bottle at the balance.
d. Sulfuric Acid
e. Starch Indicator
i. 1g of soluble starch to 1000 mL DI H 2O with 10mg of mercuric iodide. Grind starch & iodide with
mortar & pestle (pictured below). Add to beaker with 100 mL of DI H 2O to make a paste. Add
900 mL boiling water. Boil until clear solution.

This document belongs to UNCG Department of Chemistry and Biochemistry. Copies are to be retained for reference only. Copies are not to be distributed.