Name: Block: Date:

Chemistry 11 Experiment 4: Lab

Titration with Oxalic Acid

Abstract:

Titration is a versatile analytical procedure that can be used for a wide variety of
chemical analyses. For example, when your town’s water supply is tested for purity, or pond
water is tested for dissolved oxygen and contaminants, chances are a titration is carried out.
Some tests that are essential for a medical diagnosis require a titration of various body fluids.
A titration makes use of a known reaction between two chemicals. A solution of
unknown concentration is reacted with a precisely measured amount of another chemical. An
appropriate indicator must be used to determine when chemically equivalent amounts of each
chemical are present, that is, when no excess of either reactant is present. This is known as the
equivalence point. To measure solution volumes accurately, finely calibrated pipets and burets
are used. Titrations are commonly used to determine the strength of acids or bases.
Acid-base titrations follow a relatively standard procedure for analysis of acid or base
strength. The concentration of either an acid or base solution can be determined. A measured
amount of acid is neutralized by reacting it with a basic solution titrated from a buret. Consider
the following example:
HCl + NaOH → NaCl + H2O
(known) (unknown)
The example shows that the reaction is a special case of a double replacement reaction,
where the products are water and a corresponding salt. At the equivalence point, all of the NaOH
has been reacted with the HCl and a pH of 7 (a neutral solution) would result. Some reactions
(ones with weak acids or weak bases) do not reach their equivalence point at a pH of 7 because
of equilibria occurring in the solution.
In this experiment, you will determine the concentration of a solution of NaOH by
reacting it with a known concentration of oxalic acid, H2C2O4 – a weak acid, which will have an
equivalence point at approximately pH 8. The indicator phenolphthalein will be used to find the
endpoint of the titration because it is colourless below pH 8, but turns pink just above pH 8.

Purpose: To determine the concentration of a sodium hydroxide solution using the process of
titration.

Materials:

safety goggles wash bottle

laboratory apron buret
2 Erlenmeyer flasks, 250mL buret clamp
balance ring stand
oxalic acid dihydrate (H2C2O4 · 2H2O) sodium hydroxide solution (NaOH)
distilled water 2 beakers, 100mL
phenolphthalein white paper
Safety Warnings:

Wear safety goggles at all times during the laboratory period.

Ensure the top of the buret is below eye level when filling to avoid splashing solution into
your face.
Acids are corrosive and bases are caustic, so wipe up all spills immediately with a wet
paper towel and then dry the area. Wash affected skin areas with cold water and notify
the teacher.
Burets are cumbersome and break easily – handle them with care.

Procedure:
Part A: Preparation
1. Put on your safety goggles (and lab apron if desired). While one partner prepares the
oxalic acid solution (steps 2 + 3), the other should prepare the buret for titration (steps
4 – 9). Each group member should do one titration!
2. In a 250 mL Erlenmeyer flask weigh out approximately 0.20g of oxalic acid (this will
be a very small amount!). Record the exact mass of oxalic acid used in the data table.
Repeat this step in another Erlenmeyer flask for trial 2.
3. Dissolve the oxalic acid in the flask with approximately 50mL of distilled water. Add
2-3 drops of phenolphthalein indicator to the flask.
4. Obtain a buret and buret funnel.
5. Rinse the buret thoroughly with tap water, then rinse it once with a small amount of
distilled water, draining the final rinses through the tip. Clamp the clean buret to the
ring stand.
6. Obtain 50-60 mL of NaOH solution in a 100 mL beaker. Position the buret so that the
top is below eye level and ensure it is closed!
7. Pour approximately 5 mL of the NaOH into the buret. Drain this solution through the
tip to remove water and coat the inside of the buret with base.
8. Fill the buret to slightly above the zero line with NaOH. With a waste beaker below
the buret, drain some of the base through the tip to clear the buret of air. Stop between
0.0 and 2.0 mL. Remove the hanging drop by touching the tip to the inside of the
waste beaker.
9. Read the initial volume of the buret and record it in the data table.
Part B: Titration:
10. Place the flask with acid and phenolphthalein under the buret. The buret tip should be
down about 1cm inside the mouth of the flask to avoid losing any of the base. Place a
sheet of white paper under the flask to help highlight the pink indicator colour.
11. Drip the base into the flask while swirling the flask to stir it. Add base quickly at first,
but as the pink colour starts to last longer, slow the drip rate. It is better to take longer
on this part than to need to start again! When the whole flask flashes pink before
turning clear again, add only one drop at a time and swirl the flask before adding
more. Occasionally rinse down the splashes on the side of the flask using a little
distilled water from a wash bottle (this water will not change your results).
12. When the faintest pink colour persists for 30 seconds, stop and record the final
volume in the buret.
13. Repeat the titration for trial 2.
14. Flush all chemicals down the sink and clean out the buret as described in step 5.
15. Have your instructor sign your data.
16. Clean up your work area and wash your hands.

Observations:

Mass of oxalic acid used: Trial 1: ____________g Trial 2: ____________g

Data Table: Titration of H2C2O4 oxalic acid with unknown concentration of NaOH
Volume of NaOH (mL): Trial 1 Trial 2
Initial

Final

Used

Questions and Calculations:

1. Why is it difficult to see whether you have added the phenolphthalein to the flask
solution before you have titrated it?

2. Why did you need to rinse the buret with base before you completely fill it with NaOH?

3. Write and balance the neutralization equation for the reaction performed in this
experiment.
 4. Does the amount of water in which you dissolved the oxalic acid affect the outcome of
the experiment? Explain.

5. Why is it important to wash down the sides of the reaction flask with water as you near
the equivalence point?

6. How many moles of base (sodium hydroxide) are needed to neutralize one mole of acid
(oxalic acid)?

7. Determine the molarity of the unknown NaOH. (Do all these calculations for each trial!)
a. Calculate the number of moles of oxalic acid used.
b. Determine the number of moles of base needed to neutralize the moles of oxalic
acid.
c. Knowing the volume of NaOH you used in each trial, calculate the molarity of the
NaOH.

Conclusions:
What is the [NaOH] that was used in this experiment?
What are some sources of error for this experiment? Why might your result not be
accurate? How could you improve your results?