Titration Page 1 of 5

ACID AND BASE TITRATION

REFERENCES: 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
50 mL Class A buret
Buret clamp
Ring stand
19 M NaOH
Balance
Wash bottle

3 1pint bottles with caps

Phenolphthalein solution
Potassium acid phthalate (primary standard)
3 250 mL Erlenmeyer flasks
Weighing bottle
Unknown acid
600 mL beaker

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) 2H2O(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
trtration 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.

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In this experiment your solution of NaOH will be standardized by titrating it against 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 (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.

H
H

C
C

C
H

O
C
C

COOH
Or

O-K+

COOK

(in shortha nd notation)

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
COOK

COOK

Once the end point 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 then 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 exact concentration of the NaOH titrant?
0.3043 g KHP 204.2 g/mole = 1.490 x 103 mole KHP
At the end point:
1.490 x 103 mole KHP = 1.490 x 103 mole NaOH titrated
therefore,
1.490 x 103 mole NaOH 0.01512 L of NaOH titrated = 0.09854 M NaOH exactly

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Once the exact molarity of the 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.
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:
0.09854 moles/L NaOH x 0.02135 L = 0.002104 moles NaOH
0.002104 moles NaOH = 0.002104 moles JHP = 0.4296 g KHP
therefore,
(0.4296 g KHP 0.5366 g sample) * 100% = 80.06% KHP in the unknown sample
Procedure
Preparation of approximately 0.1000 M Sodium hydroxide.
Heat a total of 1500 mL of distilled water to boiling using no larger than 600 mL beakers, 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 2 pint bottles containing the CO2free 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 readings, 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.

STANDARDIZATION OF SODIUM HYDROXIDE SOLUTION

Titration Page 4 of 5

Mass from a weighing bottle (your lab 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 0.1000
M sodium hydroxide solution that you have prepared. Discard each portion. Do not return any
of the wash.ings 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 near the zero mark. 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.
Level of meniscus
Pull the stopcock in
against the taper
each time you turn it

Swirl the flask continuosly until one

drop of titrant causes a color change
thruout the entire solution
A sheet of white paper
below the flask will help
you to see the color change.

From the data you obtain in the three titrations, calculate the molarity of the sodium hydroxide
solution to four significant figures.

Titration Page 5 of 5
The three determinations should agree within 1.0 percent. If they do not, the standardization
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 percent KHP.
Weigh by difference (from a weighing bottle) triplicate portions of the sample to four significant
figures and place them in three separate clean 250 mL flasks. The sample size should be about
the amount determined by the above computation. Dissolve the sample in 100 mL Of 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. Calculate the percentage of potassium acid phthalate (KHP) in the
samples. For best results the three determination should agree with 1.0 percent. 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.

Name:____________________________

Titration Experiment Report Sheet

Standardization of NaOH Solution
Trial 1

Trial 2

Mass of bottle + KHP

Mass of bottle
Mass of KHP used
Final buret reading
Initial buret reading
mL of NaOH used
Molarity of NaOH

Average Molarity:

Standard deviation:

Show calculations for Molarity and standard deviation

Trial 3

Name:____________________________

Analysis of Unknown Acid

Unknown Number:_______
Trial 1

Trial 2

Mass of bottle +
Unknown
Mass of bottle
Mass of Unknown
used
Final buret reading
Initial buret reading
mL of NaOH used
Molarity of NaOH
used
Moles of NaOH used
Mass of KHP in
Unknown
Percent KHP in
Unknown
Average Percent KHP:

Standard deviation:

Show calculations of percent KHP and standard deviation.

Trial 3