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ACID-BASE TITRATION

REFERENCE: Nelson, J., Chemistry: The Central Science, 3rd edition, Prentice-Hall,
1985

This experiment will demonstrate the techniques of volumetric analysis or titration. Here,
a quantitative determination of the amount of acid in an unknown sample will be made.

Apparatus and Chemicals

500 mL Erlenmeyer flask 1-pt bottles with caps (3) Unknown acid
Wash bottle 19 M NaOH Weighing bottle
250 mL Erlenmeyer flasks Potassium acid phthalate 50 mL Class A buret
(3) (primary standard)
600 mL beaker Ring stand
Buret clamp
Phenolphthalein solution

Discussion

One of the most common and familiar reactions in chemistry is the reaction of an acid
with a base. This reaction is termed neutralization, and the essential feature of this
process in aqueous solution is the combination of hydronium ions with hydroxide ions to
form water:
H3O+(aq) + OH−(aq) → 2 H2O(l)

In this experiment you will use the above reaction to accurately determine the
concentration of a sodium hydroxide solution that you have prepared. The process of
determining the concentration of a solution is called standardization. Next you will
measure the amount of acid present in an unknown. To do this, you will accurately
measure with a buret the volume of your standard base that is required to exactly
neutralize the acid present in the unknown. The technique of accurately measuring the
volume of a solution required to react with another reagent is termed titration.

An indicator solution is used to determine when an acid has exactly neutralized a base, or
vice versa. A suitable indicator changes colors at well-defined pH values; if this pH value
corresponds to the pH region in which equivalent amounts of acid and base are present
during a titration experiment, we can use the color change to determine the stoichiometric
point. The color change is termed the end point of the titration. Different indicators
change colors at different pH values. Phenolphthalein, for example, changes color from
colorless to pink at a pH of about 9; in slightly more acidic solutions it is colorless, while
in slightly more alkaline solutions it is pink.

In this experiment your solution of NaOH will be standardized by titrating it aginst a very
pure sample of potassium acid phthalate, (KHC8H4O4) of known mass. Potassium acid
phthalate (henceforth abbreviated as KHP) has only one replaceable acid hydrogen
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(indicated in BOLD). Its structure is shown below. It is a monoprotic acid with the acidic
hydrogen bonded to oxygen and has a molecular weight of 204.2 g/mole.

COOH

COO− K+

In the titration of a base against KHP, an equal number of moles of base and acid are
present at the end point (moles NaOH = moles KHP) or

COOH COO− Na+

+ Na+ + OH− + HOH

COOK COOK

Once the endpoint has been reached then the exact molarity can be calculated by dividing
the volume of base that was titrated (in liters) into the moles of NaOH present.

Moles NaOH / volume of base titrated (L) = M of NaOH in stock bottle

Now that the exact concentration of NaOH is known, a sample containing an unknown
amount of KHP (or any other acid, for that matter) can be determined.

Example of Standardization

0.3043 g of pure KHP was weighed out and titrated to an end point with 15.12 mL of a
NaOH solution that was approximately 0.1 M. What is the exactly concentration of the
NaOH titrant?

0.3043 gKHP
= 1.490 x10 −3 moleKHP
204.2 g / mole
At the end point:
1.490 x 10-3 mole KHP = 1.490 x 10-3 mole NaOH titrated

therefore,
1.490 x10 −3 moleNaOH
= 0.09854MNaOH (0.09856 M using all digits from first calc)
0.01512 LNaOHtitrated

Once the exact molarity of NaOH solution is known, the base can be used to determine
the amount of KHP, or any other acid, present in a known mass of an impure sample.
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Example: The percentage determination of an acid in an unknown sample.

0.5366 g of an KHP sample of unknown purity was massed. The sample was dissolved in
approximately 100 mL of distilled, degassed water and indicator was added. The end
point was reached after 21.35 mL of 0.09854 M NaOH solution was titrated into the
solution. What is the percentage of KHP in the original sample?

At the end point:

0.09854molesNaOH
× 0.02135L = 0.002104molesNaOH
L
0.002104 moles NaOH = 0.002104 moles KHP = 0.4296 g KHP
therefore,
0.4296 gKHP
× 100 = 80.06% KHP in the unknown sample
0.5366 gsample

Procedure

Preparation of approximately 0.1 M Sodium hydroxide

Wash the 1-pint bottles with caps. Heat a total of 1500 mL of distilled water to boiling
using no larger than 600 mL beakers or 500 mL flasks, and after cooling under the water
tap, transfer to three 1-pint bottles fitted with caps. Add 3 mL of stock solution of
carbonate-free sodium hydroxide (approximately 19 M) to only one of the pint bottles
and shake vigorously for at least 1 minute. The other two pint bottles containing the CO2-
free water will be used for the remainder of the experiment.

Preparation of a buret for use

Clean a 50 mL class A buret with soap solution and a buret brush and thoroughly rinse
with tap water. Then rinse with at least five 10 mL portions of distilled water. The water
must run freely from the buret without leaving any drops adhering to the sides. Make sure
that the buret does not leak and that the stopcock turns freely.

Reading a buret

All liquids, when placed in a buret, form a curved meniscus at their upper surfaces. In the
case of water or water solutions, this meniscus is concave (∪), and the most accurate
buret readings are obtained by observing the position of the lowest point on the meniscus
on the graduated scales.

To avoid parallax errors when taking reading, the eye must be on a level with the
meniscus. Obtain a 3 × 5 card. Color a 2 × 1 box in solid black ink in the center of the
card. When taking a volume reading involving the meniscus, hold the card so that the
lowest part of the meniscus is even with the “top” of the black colored box.
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STANDARDIZATION OF SODIUM HYDROXIDE SOLUTION

Mass from a weighing bottle (your instructor will show you how to use a weighing bottle
if you do not already know) triplicate samples of between 0.4 and 0.6 grams each of pure
KHP into 250 mL Erlenmeyer flasks; accurately weigh to four significant figures. Do not
weigh the flasks. Record the masses and label the three flasks in order to distinguish
them from one another. Add to each sample about 100 mL of CO2-free distilled water and
warm gently with swirling until the salt is completely dissolved. Add to each flask two
drops of phenolphthalein indicator solution.

Rinse the previously cleaned buret with at least four 5 mL portions of the approximately
0.1 M sodium hydroxide solution that you have prepared. Discard each portion. Do not
return any of the washings to the bottle. Completely fill the buret with the solution and
remove the air from the tip by running out some of the liquid into an empty beaker. Make
sure that the lower part of the meniscus is at the zero mark or slightly lower. Allow the
buret to stand for at least 30 seconds before reading the exact position of the meniscus.
Remove any hanging drop from the buret tip by touching it to the side of the beaker used
for the washings. Record the initial buret reading.

Slowly add the sodium hydroxide solution to one of your flasks of KHP solution while
gently swirling the contents of the flask as illustrated in Figure 1. As the sodium
hydroxide solution is added, a pink color appears where the drops of the base come in
contact with the solution. This coloration disappears with swirling. As the end point is
approached, the color disappears more slowly, at which time the sodium hydroxide
should be added drop by drop. It is most important that the flask be swirled constantly
throughout the entire titration. The end point is reached when one drop of the sodium
hydroxide solution turns the entire solution in the flask from colorless to pink. This
solution should remain pink when it is swirled. Allow the titrated solution to stand for at
least 1 minute so the buret will drain properly. Remove any hanging drop from the buret
tip by touching it to the side of the flask and wash down the sides of the flask with a
stream of water from the wash bottle. Record the buret reading. Repeat this procedure
with the other two samples.

Figure 1

Level of meniscus

Swirl the flask continuously until

one drop of titrant causes a color
change throughout the entire
solution.

A sheet of white paper below

the flask will help you to see
the color change.
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From the data you obtain in the three titrations, calculate the molarity of the sodium
hydroxide solution to four significant figures.

The three determinations should agree within 1.0 percent. If they do not, the standization
should be repeated until agreement is reached. The average of the three acceptable
determinations is taken as the molarity of the sodium hydroxide. Now, label your stock
bottle of NaOH solution with this average value.

ANALYSIS OF AN UNKNOWN ACID

Calculate the approximate mass of unknown that should be taken to require about 30 mL
of your standardized sodium hydroxide assuming that your unknown sample is 75%
KHP.

Example of Sample Size

How much mass of unknown that is approximately 75% by mass KHP will be required if
30. mL of 0.09854 M NaOH should be used?

(0.03000 L)(0.09854 M NaOH) = 0.002956 moles NaOH = 0.002956 moles KHP

(0.002956molesKHP)(204.223g / mol )
= 0.80 g approximately
0.75

Weigh by difference (from the unknown bottle) one portion of the sample to four
significant figures and place it in one clean 250 mL flasks. The sample size should be
about the amount determined by the above computation. Dissolve the sample in 100 mL
CO2-free distilled water and add two drops of phenolphthalein indicator solution. Titrate
with your standard sodium hydroxide solution to the faintest visible shade of pink as
described above in the standardization procedure. If the first trial requires less than 20
mL of NaOH to reach the end point, calculate how much sample should be used for trials
2 and 3. Weigh by difference the unknown for trials 2 and 3 and place in clean, labeled
250 mL Erlenmeyer flasks. Add 100 mL CO2-free water and two drops phenolphthalein
indicator to each flask. Dissolve the samples thoroughly and titrate. Record the initial and
final buret readings for each trial. Calculate the percentage of potassium acid phthalate
(KHP) in the samples. For best results the three determinations should agree within 1.0%.
Compute the standard deviation of your results.

Test your results by computing the average deviation from the mean. If one result is
noticeably different from the others, perform an additional titration. If any result is more
than two standard deviations away from the mean, and has a history of problems and/or
possible error in preparation discard it and titrate another sample.
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Acid-Base Titration Report Sheet

Name_____________________________________

Standarization of NaOH Solution

Trial 1 Trial 2 Trial 3

Mass of bottle + KHP
before removing trial mass
Mass of bottle + KHP after
removing trial mass
Final buret reading

Initial buret reading

mL of NaOH used for trial

Molarity of NaOH for trial

(show work below)

Sample calculation for calculation of NaOH molarity for one trial.

Calculate average NaOH Molarity:

Calculate standard deviation:

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Analysis of Unknown Acid Name_____________________________________

Unknown No:__________

Trial 1 Trial 2 Trial 3

Mass of bottle + Unk.
before removing mass
Mass of bottle + Unk.
after removing mass
Mass of unknown for
each trial
Final buret reading

Initial buret reading

ML of NaOH used for

each trial
Molarity of NaOH

Moles of NaOH used for

each trial (show calc)
Calculation for moles of NaOH used for one trial

Trial 1 Trial 2 Trial 3

Mass of KHP in
Unknown for each trial
Calculation for mass of KHP in Unknown for one trial

Trial 1 Trial 2 Trial 3

Percent KHP in
Unknown for each trial
Calculation of percent KHP for one trial

Calculation of Average Percent KHP

________________________________________________________________________
Calculation of standard deviation