TITRATION: STANDARDIZATION OF A BASE

AND ANALYSIS OF POLYPROTIC ACIDS

2013, 2007, 1996 by David A. Katz. All rights reserved.
Reproduction permitted for education use provided original copyright is included.

OBJECTIVE:
The object of this experiment is to become familiar with making solutions and to titrate an acid with a base. Phosphoric
acid, H3PO4, a triprotic acid will be titrated, and the amount of citric acid, C3H4OH(COOH)3, in a soft drink will be
determined.

PART I: PREPARATION AND STANDARDIZATION OF A BASE SOLUTION

MATERIALS NEEDED:
sodium hydroxide, NaOH (pellets)
potassium acid phthalate, KHC8H4O4, oven dried
phenolphthalein solution (1% by mass in ethanol)
buffer solutions, pH 4 and pH 7
10 mL graduated cylinder
100 mL graduated cylinder
250 mL volumetric flask with cap or stopper
2 100-mL beakers
2 250-mL beakers
2 burets, 25-mL or 50-mL
2 small funnels to fit the burets
LabPro unit and computer with pH electrode
Drop counter
Magnetic stirrer with stir bar

SAFETY PRECAUTIONS:
Wear approved eye protection in the laboratory at all times.

Sodium hydroxide is caustic. Do not handle the solid with your hands. In the event of skin contact, wash well with
water. If the skin is irritated or broken, seek professional medical treatment. The dilute sodium hydroxide solution is
less caustic, but one should exercise similar precautions.

Dissolving of sodium hydroxide generates heat. Take care in handling the dilution container.

DISPOSAL:

All solutions in this experiment should be disposed of in the proper waste containers as provided in the laboratory.

PREPARING SOLUTIONS:

Prepare 250 mL (0.25 L) of 0.1 M sodium hydroxide solution starting with solid sodium hydroxide (See Solutions from
Solid Solutes, below). Use distilled or deionized water. The solution will be prepared in a 250-mL volumetric flask.

To prepare the sodium hydroxide solution:

Determine the mass of sodium hydroxide needed.
Fill the volumetric flask approximately 75% full with water. Use a funnel.
 Add the sodium hydroxide to the volumetric flask.
Stopper the volumetric flask and gently shake the solution.
After the sodium hydroxide has dissolved, fill the volumetric flask to the 250-mL mark. Stopper the flask and
gently shake the solution.
If necessary, adjust the volume of the solution to 250 mL using distilled water, and shake again.
Label the volumetric flask.

SOLUTIONS FROM SOLID SOLUTES

To prepare a Molar solution from a solid solute, the formula to use is:

M·V·W
g = —–—–––
1000

where g = mass of solute needed, in g

M = molarity of the desired solution
V = volume, in mL, of solution to be prepared
W = Molecular mass of the solute
NOTE: The 1000 is a conversion factor from mL to L

Example: To make 100 mL of a 1.5 M solution of sodium hydroxide.

(1.5 M) x (100 mL) x (40.0 g/mol)

g = —————–––––––——–––––––– = 6.00 g sodium hydroxide needed
1000 mL/L

To make the solution, 4.00 g of the solid sodium hydroxide is added to approximately 75 mL of water. After
the solid has dissolved, the volume of the solution is adjusted to 100 mL

PROCEDURE

A. Standardization of sodium hydroxide solution

Rinse a buret with 5 mL of 0.1 M sodium hydroxide solution. Discard the rinse solution. Repeat the rinsing two more
times. Fill the buret with 0.1 M NaOH solution. Adjust the volume to the zero mark. Use a piece of labeling tape to
identify this as the NaOH or base buret. This buret and solution will be used for this entire experiment.

Calibrate the drop counter using the buret with the sodium hydroxide solution. Read the starting volume of the buret.
Adjust the drop rate to 1 to 2 drops per second. Allow 10.0 mL of the sodium hydroxide solution to drip into a waste
beaker. Determine the exact volume of the NaOH solution used.

Weigh out 0.3 to 0.5 g of potassium acid phthalate into a clean 250-mL beaker. Add approximately 50 mL of distilled
water and gently swirl to dissolve the solid. Add 2 drops of phenolphthalein indicator solution.

Calibrate the pH electrode using approximately 25 mL of pH buffers of pH 4 and pH 7 in 50-mL or 100-mL beakers.
Save the buffer solutions in case the electrode has to be calibrated again during the lab period.

Titrate the potassium acid phthalate solution with 0.1 M NaOH. When the end point is reached, the indicator solution
will turn red. Allow the titration to continue for 10 seconds after a permanent red color is obtained. Determine the
volume of 0.1 M NaOH used.

Rinse the 250-mL beaker well with water. Give the beaker a final rinse with distilled or deionized water. The beaker
may be left wet for another titration.

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Repeat the titration procedure, above, 2 more times with fresh samples of potassium acid phthalate.

Calculate the molarity of the NaOH solution for each of the three titrations. If the values of the molarities do not agree,
try another titration.

PART II: TITRATION OF POLYPROTIC ACIDS

MATERIALS NEEDED:

sodium hydroxide, NaOH (previously prepared and standardized)

phosphoric acid, H3PO4, 0.1 M
soft drink such as 7Up, Sierria Mist, or similar, containing citric acid
phenolphthalein solution (1% by mass in ethanol)
10 mL graduated cylinder
2 100-mL beakers
2 burets, 25-mL or 50-mL
2 small funnels to fit the burets
LabPro unit and computer with pH electrode
Drop counter
Magnetic stirrer with stir bar

SAFETY PRECAUTIONS:

Wear approved eye protection in the laboratory at all times.

Phosphoric acid is corrosive. In the event of skin contact, wash well with water. If the skin is blistered or broken, seek
professional medical treatment. The dilute phosphoric acid, used in this experiment, is less reactive, but one should
exercise similar precautions.

There are no hazards associated with a soft drink.

Soft drinks, used in this experiment, have been stored under laboratory conditions and may be contaminated. Do not
taste any materials used in this experiment.

DISPOSAL:

All solutions in this experiment should be disposed in the proper containers provided in the laboratory. Solid waste can
be disposed of in the trash.

INTRODUCTION:

This experiment will determine the amount of citric acid in a soft drink. NOTE: Ascorbic acid, vitamin C, will
interfere with this titration. Except for any ascorbic acid added the the soft drink, the drink must be free of any
significant amount of vitamin C. Carbon dioxide, in the form of HCO3- or H2CO3 will interfere with this procedure.

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 The structure of citric acid, C3H4OH(COOH)3

PROCEDURE:

Measure 10.0 mL of 0.10 M phosphoric acid into a 100 mL beaker. Add 25 mL of distilled or deionized water.

Titrate the solution with your standardized NaOH. When the end point is reached, the pH should remain somewhat
constant (approximately pH 11).

Repeat this procedure a second time using a new sample of the phosphoric acid. If your results agree with your first
titration, a 3rd trial is not needed.

Place approximately 50 mL of the soft drink, you are working with, into a 250 mL flask. Stopper the flask and shake it
several times to release the carbon dioxide in the drink. Vent the flask. Repeat the shaking and venting of the flask
several times to remove as much of the carbon dioxide from the soft drink as possible.

Measure 10.0 mL of the soft drink into a 100 mL beaker. Add 25 mL of distilled or deionized water.

Repeat this procedure a second time using a new sample of the soft drink. If your results agree with your first titration,
a 3rd trial is not needed.

CLEAN-UP

At the conclusion of the experiment, empty the burets and rinse them three times with distilled or deionized water.

DATA ANALYSIS
1. Determine the quantitiy of sodium hydroxide needed to prepare 250 mL of a 0.10 M Solution of sodium
hydroxide. This calculation was done in the laboratory.

2. Using the titration data with KHP, calculate the concentration of the sodium hydroxide solution.

3. Using the titration data, determine the volume of the sodium hydroxide at each of the equivalence points of the
titration of the phosphoric acid and list the pH of the mixture at each equivalence point.

4. Using the titration data, determine the volume of the sodium hydroxide at each of the equivalence points of the
titration of the soft drink and list the pH of the mixture at each equivalence point.

5. Determine the amount of citric acid in the sample of the soft drink. Calculate the amount of citric acid in one
serving (355 mL or 12 oz.) of the soft drink.

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