Detection of Ions in Solutions Using Acid/Base Chemistry: A Quality Control Test

Objective: In this experiment you will standardize a NaOH solution to know the exact concentration. In
follow up experiments, you will used the standardized NaOH to determine the unknown concentrations
of HCl and HC2H3O2 solutions. You will learn to detect endpoints using different indicators.

What is a Titration?

A titration is an analytical procedure used to determine the concentration of a sample by reacting it with
a standard solution. One type of titration uses a neutralization reaction, in which an acid and a base
react to produce a salt and water.

In equation 1, the acid is HCl (called hydrochloric acid) and the base is NaOH (called sodium
hydroxide). When the acid and base react, they form NaCl (sodium chloride), which is also known as
table salt. The titration proceeds until the equivalence point is reached, where the number of moles of
acid is equal to the number of moles of base. This point is usually marked by observing a color change
in an added indicator.

In a titration, the standard solution goes in a buret, which is a piece of glassware used to measure the
volume of solvent to approximately 0.1 mL of accuracy. The solution that you are titrating goes in an
Erlenmeyer flask, which should be large enough to accommodate both your sample and the standard
solution you are adding.

What is an Indicator and What is it Used For?

An indicator is any substance in solution that changes its color as it reacts with either an acid or a base.
Selecting the proper indicator is important because each indicator changes its color over a particular
range of pH values. Indicators are either weak acids or weak bases. For example, phenolphthalein is a
weak acid (which we will represent as HIn). In aqueous solution, the phenolphthalein dissociates
slightly, forming an equilibrium.
An equilibrium occurs when the amount of reactants and the amount of products are constant. This
means the rate of the forward reaction is the same as the rate of the reverse reaction. When a system is
in equilibrium, it will stay there until something changes the conditions. A famous French chemist,
named LeChatelier, developed a way to predict how changes in equilibrium affect the system.
LeChatelier’s principle states that when an equilibrium is disturbed by applying stress, the equilibrium
will shift to relieve the stress. In an acidic solution, there is an excess of H3O+ ions so the equilibrium
will shift to the left and favor the formation of HIn, thus we observe a clear solution. In basic
solution, there is an excess of OH- ions that react with the H3O+ ions to form water. This shifts the
equilibrium to the right because water is being formed and H3O+ ions are being removed, thus we
observe a pink solution. We can use this color change to determine when the end of the titration has
been achieved.

Table 1 lists common indicators and the pH range over which they change colors.
The acid-base indicator indicates the endpoint of the titration by changing color. The color change in the
solution lets you know you have reached the pH that you need to have at the equivalence point. The
endpoint and the equivalence point are not exactly the same because the equivalence point is determined
by the stoichiometry of the reaction while the endpoint is just the color change from the indicator.
To be clear, the equivalence point is when the [H+] and the [OH-] that have been added to the solution
are the same. This is the answer that MATH gives you.
The endpoint of a titration is when the indicator used in the titration changes colors. This may or may not
be exactly at the equivalence point, but should be close to not create a large amount of error.

If you look at the titration graph, you should see that an indicator that changes in the range of pH of about
3 to 11 would have been good to determine the equivalence point in this titration. So, the indicator which
signals the endpoint of the titration at a pH of 6.8 would be a good choice. On the other hand, there is an
indicator option that signals the endpoint of the titration at a pH of 11.6. You can tell from the graph that
the volume of NaOH necessary to reach this endpoint is NOT the same as the actual equivalence point
volume. Choosing this indicator would have resulted in an error in your determination of the unknown
molarity of acid.

Sodium Hydroxide is strongly corrosive to ALL bodily tissue, especially SKIN and
EYES. Handle with care and clean up all spills IMMEDIATELY.
Wear goggles and aprons.
Wash your hands with soap and water before leaving.
 Standardizing a Sodium Hydroxide (NaOH) Solution

In a titration, it is critical to know the exact concentration of the titrant (the solution in the buret which
will be added to the unknown) in order to determine the concentration of the solution being tested. We
will standardize the ~0.1 M NaOH solution (the titrant) with potassium hydrogen phthalate (KHP,
KC8H4O4H) using phenolphthalein as the indicator. KHP is a weak acid and reacts with base in the
following way:

Dry primary standard potassium hydrogen phthalate, KHP, for two hours at 100 oC. This has been done
for you. You will not need to dry the KHP before you do the experiment. The technique information
remains for your learning pleasure. You should understand the necessity to dry the salt first.

Weigh ~0.75 g of dried KHP (MW = 204.23 g/mol) into an Erlenmeyer flask. Determine the exact mass
by weighing by difference.

Dissolve your sample in 50-75 mL of distilled water. Determine the amount of water added by weighing
by difference.

Record the amount of KHP and water used.

Add 4 drops of indicator into the flask.

Obtain approximately 100 mL of NaOH solution in a clean, dry beaker. Prepare the buret for titration by
rinsing with 2 aliquots of solution. Fill the buret and record the initial volume to 0.1 mL.

Titrate to the first permanent appearance of pink. Near the endpoint, add the NaOH dropwise to
determine the total volume most accurately. Record the final buret reading.

If time allows, repeat the titration.

Calculations and Questions

1. Calculate the number of moles of KHP used in the titration.
2. Calculate the molarity of the KHP solution after your addition of water.
3. Determine the number of moles of NaOH required to reach the endpoint of the titration.
4. Calculate the molarity of the NaOH standard solution.
5. How would the amount of NaOH required to neutralize the KHP have changed if you added twice
the volume of water to the KHP before the titration? Justify your answer.
6. During the titration, splatter from the drops of NaOH splashed some of the KHP solution onto the
sides of the Erlenmeyer flask. If the student did not rinse these droplets back down into the solution
with distilled water, how would that have affected the calculation of concentration of NaOH?