Revised 10/30/2013

Experiment 7
Quantitative Reactions and Titrations

Chemicals: 6 M NaOH, Potassium Hydrogen Phthalate (KHP), sulfuric acid solution of

unknown molarity, phenolphthalein
Materials: buret, Erlenmeyer flasks, volumetric pipet
Waste Disposal: Completed titration solutions should be disposed of in the red bucket
labeled Acid/Base Waste. Your instructor will neutralize the waste before disposal.

Titrations
In Experiment 4, we learned that the mole is used to determine the quantity of a substance by
one of two methods: gravimetric analysis or volumetric analysis. In this experiment, we will
use volumetric analysis to determine the concentration of an unknown acid solution using a
base solution with a known concentration. The reaction between an acid and a base is
termed neutralization and involves the combination of hydrogen ions (or hydronium ions, if
you prefer) with hydroxide ions to form water:
H+(aq) + OH-(aq) H2O(l)
In order to accurately determine the concentration of your solution, you will perform the
experiment in two parts, over two weeks (two lab sessions):
1) Standardization of NaOH: You will prepare a solution of sodium hydroxide with a
concentration of approximately 0.3 M by diluting a stock solution of NaOH. (See the
Examples for a sample dilution problem.) You will determine the exact concentration
of the dilute NaOH solution by reacting it with a known amount of the solid organic
acid potassium hydrogen phthalate, often abbreviated KHP. The structure, given
below, is not terribly important except to note that it is a monoprotic acid meaning that
there is one mole of H+ per mole of acid.
H

H
OH
OK
H

Figure 1: The structure of KHP, KHC8H4O4, Molar Mass = 204.2 g

CHM 151 Lab 6 Quantitative Reactions and Titrations

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The reaction between KHP and NaOH is given below. Notice that there is a one-toone mole ratio of KHP to NaOH required per the balanced reaction. One mole of KHP
will neutralize one mole of NaOH.
KHC8H4O4(aq) + NaOH(aq) H2O(l) + KNaC8H4O4(aq)
The point in the titration when the number of moles of each reactant are equal is
called the equivalence point. In other words, # moles NaOH = # moles KHP at the
equivalence point.
For a simple one-to-one mole ratio reaction, this point is also called the end point.
More precisely, the end point refers to the observed physical change associated with
the equivalence point, usually a color change in a chemical indicator. If done properly,
the end point and equivalence point should be very near one another. Therefore, at
the end point (as indicated by a color change in the indicator) you will assume an
equivalence point where # moles NaOH = # moles KHP.
Moles of KHP will be calculated from the mass of KHP used and the molar mass for
KHP provided above. Thus, if you measure the volume of base, NaOH, required to
neutralize a known amount of KHP, you will be able to calculate the molarity of the
NaOH solution.
M=

moles of NaOH
liters of NaOH

Today, you will use a chemical indicator called phenolphthalein which is colorless at
a pH < 8.2 and turns a faint fuscia or pink color at 8.3 and above. You will perform
this reaction in triplicate and calculate an average concentration in molarity of NaOH
solution. The triplicate determinations should agree to within 1%. If they do not,
repeat the standardization a fourth time and consult with your instructor.
To calculate the percent agreement:

Highest Conc. - Lowest Conc.

Lowest Conc.

100

2) Concentration of an unknown H2SO4 solution: As a repetition of the same concepts

from Part 1, you will calculate the number of moles of H2SO4 in a measured volume of
solution by titrating to the end point with the standardized NaOH solution.
H2SO4 (aq) + 2 NaOH(aq) 2 H2O(l) + Na2SO4(aq)
Notice that the mole to mole ration between H2SO4 and NaOH is not 1:1. You will
need to perform a stoichiometry calculation to find the moles of H2SO4 from the moles
of NaOH required to reach the endpoint of the titration. Once you have found moles of
H2SO4 you can then calculate the molarity of the acid solution by dividing the number
of moles of H2SO4 by the volume of H2SO4 in liters.

CHM 151 Lab 6 Quantitative Reactions and Titrations

Revised 10/30/2013
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You will perform this titration in triplicate and calculate an average concentration in
molarity of H2SO4 solution. Again, the triplicate determinations should agree to within
1%. If they do not, repeat the titration a fourth time and consult with your instructor.
Examples:
Dilution:
How will you prepare 500 mL of a 0.2 M solution of NaOH using a 6 M NaOH stock solution?
Solution:
When adding solvent to a solution (dilution) the number of moles of solute remain constant.
Moles of solute can be found by multiplying the concentration of the solution (Molarity) by the
volume in liters:
moles = M x V (L)
We show that the moles of solute stay the same during a dilution as:
M1V1 = M2V2
You are asked to prepare 500 mL of 0.2 M NaOH so V2 = 500 mL and M2 = 0.2 M. The stock
solution has a concentration of 6 M so M1 = 6 M:
(6 M)V1 = (0.2 M)(500 mL)
V1 = 16.7 mL (volume of 6 M stock solution)
To find the amount of distilled water to add to create 500 mL of the dilute solution:
500 mL total 16.7 mL stock 6 M NaOH = 483.3 mL of water

Titration Calculations:
What is the molarity of the NaOH solution considering 1.050 g of KHP was neutralized by
26.45 mL of the NaOH solution?
Solution:
Given the reaction: KHC8H4O4(aq) + NaOH(aq) H2O(l) + KNaC8H4O4(aq), you know
that # moles NaOH = # moles KHP.
moles KHP = 1.050 g KHP
M=

moles of NaOH
liters of NaOH

1 mole KHP
204.2 g KHP

0.0051240 mol NaOH

= 0.0051420 mol KHP = mol NaOH

= 0.02645 liters of NaOH = 0.1937 M NaOH

CHM 151 Lab 6 Quantitative Reactions and Titrations

Revised 10/30/2013
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Procedure
Preparation:
To prepare a buret for use, you should rinse the buret thoroughly with distilled water, then
add approximately 10-mL of the solution to be used in the buret. (Note: Do Not rinse the
buret with the stock NaOH solution! You must prepare your dilute NaOH solution before
preparing the buret.) Each rinse should flow freely through the stopcock, making sure it does
not leak at the stopcock and it turns freely. Collect each rinse for disposal. To fill the buret,
close the stopcock and add solution to above the top volume mark. Allow the buret to settle
for at least 30 seconds then open the stopcock to drain the solution to below the top volume
mark and to release any air bubbles. You should not try to stop the volume exactly on the
mark. Simply read and document whatever volume is contained.
Reading a buret:
Liquids contained in a buret will give a curved meniscus at the surface. As you previously
have done, make sure to read the graduations at the bottom of the meniscus. Keep your eye
level with the meniscus when measuring volumes and verify the buret is completely vertical. It
may be helpful to hold a piece of paper behind the buret when reading the scale. When
dispensing a solution from the buret, remove any hanging drops from the buret tip by gently
touching it against the side wall of the container. Question for thought: Considering the
graduations on the buret are given to the tenth of a mL (0.1 mL), to how many decimal places
should you report the volumes on a buret?
Week 1: Standardization of a NaOH solution
1. Prepare 500 mL of ~0.3 M NaOH solution using the stock solution provided.
Remember that for a dilution: M1V1 = M2V2.
2. Prepare a buret and fill with the NaOH solution to be standardized. Record an initial
volume of NaOH solution.
3. Weigh approximately 1.000 g of KHP and transfer into an Erlenmeyer flask, accurately
record the mass of KHP. Be sure to measure at least 1.000 g of KHP so that there are
4 significant figures in your mass.
4. Add approximately 50 mL of distilled water to the flask and swirl gently to completely
dissolve the KHP. Add two drops of the phenolphthalein indicator to the flask.
5. Slowly add the NaOH solution to a flask while stirring gently. As the NaOH is added,
you may see a pink color appear and disappear upon swirly. As the end point is
neared the pink color may remain longer. You should then add the NaOH solution
drop-by-drop until the faint pink color appears and remains after continued swirling for
at least 1 minute. This is the end point of the titration. Your goal is to have the faintest
pink color remain at this point. Adding too much NaOH will result in a darker pink color
and will skew your results.
6. Record the final volume of NaOH solution in the buret. Calculate the amount of NaOH
required to titrate the KHP sample to the end point. Using the volume of NaOH
solution and mass of KHP, calculate the molarity of the NaOH solution.
7. Repeat steps 2-6 for remaining two additional KHP samples. Calculate the average
molarity of the NaOH solution. If any of the results disagree by greater than 1%,
repeat the titration a fourth time and contact your instructor.

CHM 151 Lab 6 Quantitative Reactions and Titrations

Revised 10/30/2013
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Your report for Week 1 must include the average concentration of your NaOH solution and
the range of the trials used to calculate the average.
Week 2: Titration of H2SO4 with NaOH to determine the Molarity of an H2SO4 solution
1. Using a volumetric pipet, dispense exactly 10.00 mL of the H2SO4 solution of unknown
concentration into an Erlenmeyer flask. [Review the procedure for use of a volumetric
pipet from Experiment 1 if needed.] Add two drops of the phenolphthalein indicator to
each flask.
2. Following the procedure as in Part 1, slowly titrate the H2SO4 solutions with the
standardized NaOH solution to the end point. Make sure to record the initial volume
and final volume of NaOH for each titration.
3. Calculate the molarity of the H2SO4 solution using the volume of NaOH and its molarity
as determined in Part 1. Calculate the average molarity of the H2SO4 solution. If any
of the results disagree by greater than 1%, repeat the titration a fourth time and
contact your instructor.
Your report for Week 2 must include the average concentration of the unknown H2SO4
solution as well as the range of the trials used to calculate the average.
Discussion Questions:
1. Suppose your sample of KHP was inadvertently contaminated with a substance that is
neither an acid nor a base. Would this cause your concentration of NaOH to be falsely
high or falsely low? Justify your answer using the calculations from the experiment.
2. How would the contaminated KHP effect the calculated concentration of the unknown
H2SO4 solution, would it be too high or too low? Again, justify your answer using the
calculations from the experiment.

CHM 151 Lab 6 Quantitative Reactions and Titrations