Experimental Procedure

1. Prepare Standard Solution:

a) Weigh 0.8375g of sodium oxalate by differences using the analytical balance:

- (Use top-loading balance first to get an approximate amount, then use the analytical
balance).

Mass of Weigh Boat + Sodium Oxalate (record all d.p.) =

- Transfer sodium oxalate to beaker and then weigh the empty boat.

Mass of Empty Weigh Boat (record all d.p.) =

b) Add 100 ml deionized water to the sample and 25 ml of sulfuric acid. Place on hot-plate
at setting 2 and stir until all the sodium oxalate dissolves.

c) Rinse 250 ml volumetric flask and funnel with deionized water to ensure they are clean.

d) Transfer solution into the volumetric flask. Remember to rinse the beaker, stirring rod and
funnel with deionized water several times to ensure all washings are transferred.

e) Fill the volumetric flask with deionized water almost close to the 250 ml mark.

f ) Stopper the flask and invert it several times. (No shimmering waves should be seen in the
light).

g) Read the meniscus again and use a dropper to add water until the bottom of the
meniscus lines up with the mark. Mix slightly again.

2. Titration 1 - The McBride Titration

a) Prepare the Buret

Rinse buret with deionized water.

Roll buret horizontally.
Drain all the water through the tap.
Repeat this twice.

Rinse the buret with the potassium permanganate.

Roll buret horizontally.
Drain all the potassium permanganate through the tap.

Place funnel on buret and fill the buret with the potassium permanganate over the 0 mark.

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 Open the tap to ensure the buret tap is filled and that the meniscus lines up with the 0
mark.
Remove the funnel.

b) Prepare 25 ml of the Sodium Oxalate Solution

Transfer about 30 ml of the sodium oxalate into a 50 ml beaker.

Using a volumetric pipette, transfer 25.00 ml of sodium oxalate into an Erlenmeyer flask.

Add 50 ml of water and 15 ml of sulfuric acid.

Place thermometer into flask and heat the mixture gradually to 750c .

Remove from the hotplate and remove the thermometer. Rinse the thermometer with a
few drops of water into the solution.

c) Carry out the McBride Titration

Initial Buret Reading (to 4 s.f.) =

Add less than 5 drops of potassium permanganate into the solution. The solution will turn
slightly pink due to this and so wait for about a minute for this colour to disappear.

Continue adding the potassium permanganate until the first palest pink colour is observed.

Add a few drops of deionized water to the sides of the Erlenmeyer flask - If the endpoint
colour disappears, add one more drop to the flask and rinse with deionized water to reach
the endpoint.

Final Buret Reading (to 4 s.f.) =

d) Carry out the Fowler and Bright Titration

Pipet 25.00 ml of the sodium oxalate solution into an Erlenmeyer flask.

Add 50 ml of water and 15 ml of sulfuric acid.

Calculate 75% of the potassium permanganate required for the first titration and deliver it
into the Erlenmeyer flask using the burette.
75
Initial Burette Reading (to 4s.f.) = × ____________ =
100

Burette Reading after Adding 75% (to 4 s.f.) =

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 Heat the solution in the flask to 550c. Rinse the thermometer with a few drops of water.

Continue with the titration until the first pale pink is observed.

Record the final burette reading and calculate the volume of potassium permanganate
used.

Volume of Potassium Permanganate = _______________ — _______________ =

e) Repeat the Titration

Repeat the titration once again by filling the burette with potassium permanganate,
transferring 75%, heating and then continuing the titration.

Initial Burette Reading (to 4s.f.) =

Burette Reading after Adding 75% (to 4 s.f.) =

Final Burette Reading (to 4s.f.) =

Volume of Potassium Permanganate = _______________ — _______________ =

Check if the volumes are concordant within 0.15ml.

Calculation

1. Find the average volume of potassium permanganate used.

2. From the mass of sodium oxalate used, calculate the moles of sodium oxalate.

3. Find the concentration of the sodium oxalate solution using:

moles × 1000
concentration =
volume

4. Find the moles of sodium oxalate used from the 25.00 ml solution:
moles = concentration × 25.00
5. Use the mole ratio 5 moles of C2O42- to 2 moles of MnO4- to calculate the moles of MnO4-
in the unknown potassium permanganate solution.

6. Using the average volume of potassium permanganate calculated in (1), calculate the
concentration using:
moles × 1000
concentration =
volume (1)

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