PROCEDURE FOR PREPARATION OF OXALATE COMPOUND

Weight accurately about 125 mg of the airdried complex into a conical flask and add 25 ml of dilute
sulphuric acid to dissolve. Heat the solution to 60-70 0 C and titrate with approximately 0.02 M
potassium permanganate solution provided. Note that during the initial stages of the titration the
solution is cloudy due to undissolved complex. This clears during the titration. Ensure that the solution is
still hot as the endpoint (pale pink solution) is approached. Take care not overshoot the endpoint as the
presence of a large excess of permanganate makes the copper determination difficult. Record the
volume of potassium permanganate taken. Preserve the resulting liquid for the determination of copper
(section 3.3). The permanganate solution should be standardized against sodium oxalate in the following
manner. Weight accurately two portions of about 100 mg of sodium oxalate into conical flasks. Dissolve
each in 20-25 ml of distilled water, acidify the solutions with 10 ml of 3M sulphuric acid and titrate with
permanganate as above, at 60 0 C. Titrate to the end point as a pale pink solution (the titrate solution
discard at a waste container No. 4). Record the volume of KMnO4. Calculate the concentration of KMnO.

Please take note that potassium permanganate solution is a powerful oxidant and the dilute solution is a
disinfectant. Avoid skin contact, but if you do spill it on yourself, simply wash with cold water. Any
remaining brown stain will soon disappear.