METHODOLOGY

A. Materials and Reagents

Iron stand

Potassium Permanganate
Solution

Sodium Oxalate
Buret clamps
Erlenmeyer flask

Buret
0.75 M Sulfuric Acid

Distilled Water

B. Procedure

1. Preparation of a 0.02M Potassium Permanganate Solution

a) Approximately 1.6 g of a good grade of potassium permanganate was weighed and placed in
a clean 250 mL beaker.
b) The salt was then dissolved by adding 50 mL of water (and stirring). The solution was
decanted into a large beaker and 50 mL of additional water was added to dissolve any
crystals remaining in the first beaker.
c) The procedure was repeated until all the crystals are dissolved. The solution was then diluted
to about 500mL, then transferred to a glass-stoppered bottle and was labeled properly. (Note
1)

2. Standardization of Potassium Permanganate Solution

a) Three samples of about 0.20 to 0.25 g each of dried sodium oxalate was weighed accurately
into clean 250-mL Erlenmeyer flasks.
b) Each sample was dissolved in about 75 mL of 0.75 M sulfuric acid (20 mL of concentrated
sulfuric acid to 400 mL of water).
c) The first solution was then heated almost to boiling (80 OC-90OC) and titrated slowly with the
permanganate with constant swirling. (The end point was marked by the appearance of a
faint pink color that stays at least for 30 seconds. the temperature should not drop below
60OC during the titration.) The other two solutions were titrated in the same manner.
d) In about 100 mL of the 0.75M sulfuric acid, permanganate solution was added dropwise
until the color matched that of the titrated solution. This volume must be subtracted from the
volume used in the titration.
e) The normality of the permanganate solution should be calculated. The average deviation
should be as small as about 2ppt. (see results)

3. Determination of Oxalate in the Sample

a. Three portions of the dried material of appropriate size were weighed accurately (Note 2).
b. Each sample was dissolved in 75 mL of 0.75 M sulfuric acid (20 mL concentrated acid to 400
mL of water) in a 250-mL Erlenmeyer flask. The solution was heated almost to boiling and
was titrated as directed in the standardization of potassium permanganate solution.

Notes:

1) Since potassium permanganate solutions are susceptible to decomposition, special

precautions are recommended for preparing the solution if it is to be used over a period of
several weeks. If the instructor recommends removal of manganese dioxide, proceed as
follows: before transferring the solution to the bottle, heat it just to boiling and keep it
slightly below the boiling point for one hour. Then allow the solution to cool, and filter it
through the sintered-glass crucible using suction. Transfer the solution to a glass-stoppered
bottle and label properly. If the solution is to be prepared, standardized and used the same
day, the special precautions are not necessary.
2) Consult the instructor regarding the weight of the sample. The equivalent weight of sodium
oxalate is 67.00 for material containing about 25% sodium oxalate, a 1-g sample is a
convenient amount.