CHM 204: Quantitative Analysis

Report 1:

Title of the experiment: redox titration

Names: Hiba Kurdi, Aline Obeid, Zuheir Al-Kasti

Semester: Spring 2023

Experiment Date: 15/3/2023

 A. Purpose of the experiment I:
The purpose of this experiment is to determine the unknown weight of ammonium
oxalate through dissolving this mass and titrating it with a solution of KMnO4.
B. Theory I:

C. Procedure:
1- Standardize KMnO4 against oxalate (Fowler-Bright Method)
Prepare the primary oxalate standard:
A dilute solution of sulfuric acid (H2SO4) was prepared for you by adding 20 mL
of concentrated H2SO4 into 400 mL water. So, you use it without dilution. Weigh
50 g of ammonium oxalate [(NH4)2C2O4], transfer to a 100.0 mL volumetric
flask, dilute to 100 ml with the dilute solution of H2SO4 prepared. Fill the burette
with KMnO4 solution. Pipet 20.00 mL of oxalate using the 10.00 mL volumetric
pipet and 20.0 mL of water (to increase volume for better stirring) using the
graduated cylinder into an Erlenmeyer flask. Titrate at room temperature to within
a few mL of the equivalence point (~ 12mL). Heat the solution until the color
disappears. Don’t exceed 50-60 °C, use a thermometer. Continue the titration while
the solution is still warm with very slow additions until one drop imparts the
solution a faint pink color that persists for at least 30 seconds. (Do not exceed 60
°C) Repeat once. Avoid quick addition of KMnO4 above the solution of
ammonium oxalate to decrease the possibility of the side reaction.
2- Detection of unknown weight of ammonium oxalate:
This procedure is carried out only once by dissolving all the solid present in the
vial in 50 mL of the sulfuric acid solution to which 50 mL of water was added.
Take 20.00 mL out of the 100 mL solution and titrate according to the Fowler-
Bright method: 9 mL of KMnO4 is added slowly at room temperature, the solution
is heated to 50-60 °C, and the titration is continued with very slow additions until
one drop imparts the solution a faint pink color that persists for at least 30 seconds.
(Do not exceed 60 °C). Record the volume and find the mass of unknown
ammonium oxalate.
Purpose of the experiment II:
Determine the amount of Vitamin C in fruit juice.
 Theory II:
Vitamin C, also known as ascorbic acid, is not carboxylic acid but a cyclic ester
having acidic hydrogens. Only L- optical isomer has physiological activity.
Vitamin C is involved in several biochemical functions in humans including the
healing process of bone deposition and transport of Fe in the body. Green
vegetables and citrus fruits are good sources of vitamins, but some get destroyed in
cooking. Because it is water-soluble, vitamin C cannot be stored in the body.
However, the amount needed daily is not clear. The recommended daily allowance
(RDA) for an adult used to be 45mg. The Food and Drug Administration (FDA)
now recommends 60mg while the National Academy of Sciences suggests 80mg
for active females. Many nutritionists consider a daily intake of 50-150 mg per day
necessary for health maintenance. Finally, chemist Linus Pauling believed that
very large doses of up to 10 grams (10000 mg) are necessary to protect against the
common cold. The vitamin C content of various fruit juices may be determined by
oxidation with elemental iodine in an aqueous solution.
Procedure II:
Rinse your burette with a few ml of standard iodine solution (0.0100 M). Fill the
buret with the I2 solution and record the initial reading. Using a graduated cylinder
pour 25.00 ml of desired juice into a 125 ml Erlenmeyer flask add 25 ml of
distilled water and 4 drops of starch solution. Titrate the sample with the I2
solution (0.01 M), while swirling the flask add the I2 solution slowly so that you
do not “overshoot” the endpoint. Continue adding the I2 solution dropwise until a
purple-blue color is obtained. Record the reading. Repeat the titration another time
so that the volume of I2 solution in the two trials is within 0.1 ml. The reaction
between ascorbic acid and iodine occurs in a 1:1 ratio.

Sources of errors:
- Extremely diluted substances
- Incorrect volume of KMnO4 drained due to few extra drops.
- Impure apparatus
- Absorption of humidity and moisture from air