Experiment

Acid-Base Titration

Introduction

A titration is a laboratory procedure in which a substance in a solution of known concentration is

reacted with a substance (usually in solution) whose quantity is utünown. (The reaction between

the substances and their relative stoichiometries must also be known.) By determining how much
of the first substance is consumed and using its concentration, the amount of the other substance
present can be determined. The solution of known concentration of a substance is called the stan-
dard solution. Titrations are often performed utilizing acid-base reactions. In this case, as the acid
and base combine, they neutralize each other. The equivalence point of the titration corresponds to
the point of the titration when the number of moles of acid and base are stoichiomefrically equiv-
Determining when this occurs during the course of a titration is usually performed with a
alent.
compound called an indicator—a substance which is one color under one set of conditions and
another color under another set of conditions.* For an acid-base titration, the indicator is a weak
acid or weak base and intensely colored so that a color can be observed when an amount of the
indicator is used that is so small as to not significantly affect the results of the titration. Thus, an
acid-base indicator is one color in its acid form and another color when the base conjugate of its

acid (Equation 1 where In- represents the base form of the indicator).

Hln (aq) + H20 (1) (aq) + H30+ (aq)

Color 1 Color 2
(Eqn. 1)

When strong acids and bases are used in a titration, the indicator phenolphthalein is often utilized.
Phenolphthalein is an intense pink color in the presence of excess base and colorless in its acid
form.

Solutions of strong bases, such as NaOH and KOH, are usually made by dissolving the solid in
water to a certain total volume. However, these bases as solids absorb water and carbon dioxide
from air; consequently, the solids are not pure. Thus, the concentration of solutions prepared in this
manner are only approximate to the calculated values obtained using the measured masses. Conse-
quently, the actual concentration has to be determined experimentally, usually by a titration. A
titration of this type to determine the concentration of a solution, which is to be used in further

experiments, is called a standardization. To standardize a solution ofa base such as NaOH, an acid
whose amount can be determined to a high degree of accuracy (a primary standard) is needed.
Potassium hydrogen phthalate (KHP), is often used as a primary standard

for titration of bases. KHP can conveniently be dried in an oven to drive away traces of water,
allowed to cool, and weighed. The reaction of KHP with a strong base is given in Equation 2 where
P represents phthalate and is a metal cation. M
1<HP (aq) + MOH (aq) —MIQ (aq) + H20 (1) (Eqn. 2)

*The point in the titration where the indicator changes color is called the endpoint. If the indicator is chosen carefully,
the end point is very close or nearly identical to the equivalence point.

From Laboratory Manual to accompany Chemisfry: A Molecular Approach, First Edition, John B. Vincent, Erica Livingston.
Copyright 0 2009 by Pearson Education, Inc. Published by Prentice Hall. All rights reserved.
39
Note that each mole ofKHP reacts with one mole of base.
Solutions of strong acids are usually prepared by dilution of commercial concentrated solutions.
However, the commercial solutions are provided as approximate concentrations; the concentration
is supposed to be within a certain range. Thus, if you prepare a solution of 6 M I-ICI by diluting
concentrated HCI 1 1 with water, you are preparing a solution with only an approximate concen-
:

tration of 6 M. If an accurate concentration is required, the concentration is often determined by

titration with a standardized base.
In this experiment, you will standardize a solution ofNaOH using KI-IP as the primary standard.
You will then determine the concentration of a solution of HCI using the standardized NaOH solution.

SAFETY NOTES: Safety goggles are required for all experiments.

Hydrochloric acid is a strong acid, while NaOH is a strong base; they should be handled
carefully. Spills should be cleaned up immediately. If contact is made with your skin, rinse

thoroughly with water.

Experimental Procedures

Washing the Buret

Obtain a buret from your instructor. First you will need to make certain that the buret is clean. Water
in the buret should form a meniscus and should not form beads on the walls of the buret. Turn the
stopcock perpendicular to the buret. Use a wash bottle to run deionized or distilled water down the
sides of the buret. Pour all the water out of the buret, rotating the buret so that water runs along
the entirehmer surface. Be careful not to hit the buret on the sink or any other objects. Repeat this
process two more times. Fill the buret with water; if a meniscus forms and water does not bead up on
the sides, then the calibrated portion of the buret is clean. (If the buret is not clean, then repeat the
step above with a solution of soap and water; finally, wash with watefthree times. Be certain that any
residue of soap is removed.) The stopcock and tip need to be cleaned. Open the stopcock and let the
water flow through the stopcock and tip into the sink or into a container (discard the water in the

sink).

Standardizing the NaOH Solution

Next you will fill the buret with —0.1 M NaOH solution, the buret should have at least 40 mL of
solution. You be determining the actual concentration of the NaOH as part of this experiment.
will
Set up the buret with a buret clamp and ringstand as shown in Figure 1. Read the initial volume to
0.01 mL and record; be sure to read the bottom of the meniscus while looking straight across the

buret.
If not already done, remove the beaker of KHP from the oven and let cool so that it is not too hot
to handle; use an insulated glove remove the beaker. Using an analytical balance, weigh out
to
three NO.6 g portions of KHP into pre-labeled weigh boats. Record the masses.
Return the beaker to the desiccator, Add the first sample of KHP to a clean 100 to
250 mL Erlenmeyer flask. Rinse the last traces of KHP from the weigh boat with deionized

40
 Buret

Buret Clamp

Ring stand

Figure 1 : Setting up the buret.

or distilled water from a wash bottle. Add another 20 mL of deionized or distilled water to the
flask; you need only estimate this volume. Swirl the flask to dissolve the KHP. Finally add 2 or 3
drops of phenolphthalein solution. You are ready to start your titration.

Place the flask under the buret as shown in Figure 2. Figure 2 is drawn showing the procedure
for a right-handed person; if you are left-handed, the stopcock will be manipulated with your right
hand, while swirling the flask with the left hand. You will start adding the NaOH solution by turn-
ing the stopcock. When the NaOH solution reaches the liquid in the flask, the liquid in the vicinity
of the NaOH will turn pink, the color of the deprotonated form of the phenolphthalein indicator.
However, the color will disappear as the flask is swirled. As more NaOH is added, the pink color
will last for longer periods of time. Reduce the rate at which NaOH is added as the color lasts
longer. Eventually, you will need to add the NaOH one drop at a time. To be certain that the entire
drop is added, you can rinse the of the buret with water from the wash bottle. You are trying to
tip

carefully get to the point of the titration where the addition of a drop of NaOH solution leaves a
faint pink color after the flask is swirled. This is the endpoint, Record the final volume. To double
check, add one more drop ofNaOH solution and swirl. Ifthe endpoint was reached with the previ-
ous drop, the solution should now be distinctly pink, and the color should not fade with swirling.
(Overshooting the end point is not difficult, especially on your first attempt. If you added too
much NaOH solution so that your solution in the flask went from clear to dark pink, do not worry
as you will be repeating the titration two more times. Just note the volume of NaOH used in the
 Buret

White paper

Figure 2: Procedure for titration,

first attempt and be careful the next two times as you approach delivering this volume ofNaOH solu-
tion.) Clean the Erlenmeyer flask and refill the buret with the NaOH solution. Repeat the titration

two more times with the other samples of KHP, being certain to record the initial and final volumes
of NaOH solution. You can use this information to calculate the concentration of your NaOH solu-
tion. Now this solution is the known standard, and you will use it to titrate a solution of HCI.

Determining the Concentration of a Solution of HCI

Use a 5 or 10 mL graduated cylinder to measure out 5.0 mL of the HCI solution of unknown con-
centration; record the volume. Add the solution to the cleaned Erlenmeyer flask and add an addi-
tional 20 mL of deionized or distilled water. Add two or three drops of phenolphthalein indicator,
Fill the buret with the NaOH solution and record the volume. Proceed as described above and
titrate the HCI solution with the standardized NaOH solution to the faint pink phenolphthalein
endpoint. Record the final volume. Clean the flask and refill the buret. Repeat the procedure two
more times.
Name: Date: Section:

Pre-Laboratory Questions

Show all calculations.

1. Find the structure of KI--IP and draw its structure. Calculate the formula weight of KHP. How
many moles are in 0.6000 g of KHP?

39.098 + 1.008 + 30.974 = 204.138 g/mol

0.6g / 204.138g/mol = 0.0029 mols

2. If 0.6000 g of KHP require 24.86 mL ofNaOH solution to just consume the KHP, what is the
concentration of the NaOH?

0.0029 mol / 0.02486L = 0.117 M

3. If 5.00 mL
of HCI require 4.96 mL of 0.9581 M NaOH to just consume the HCI, what is the
concentration of the HCI?

0.9581 M * (4.96 / 1000) = 0.00475 M

0.00475 M = 0.005 * x
0.00475/0.005 = x

x = 0.95 M
Name: Date: Section:

Report Sheet

KHP masses
0.601 0.603
2)

3)

Moles KHP
0.00294 0.00295
1) 2)

3)

Titration ofKHP
P
Original Volume
7.60 10.60
Run 1) Run 2) mL
Run 3)
Ycl
Final Volume
39 42.2
Run 1) Run 2) mL
Run 3)

Volume Utilized (Final — Initial)

31.4 31.6
Run 1) Run 2)
Run 3)
Concentration NaOH

Run 0.0936 0.0934

1) Run 2)
Run 3)

Average Concentration 0.0939

0.00294 mol / (31.4/1000)L = 0.0936 M NaOH 0.00295 mol / (31.6/1000)L = 0.0934 M NaOH

(Based on this chart)

 Titration ofHC1

Original Volume
13.1 21.8
Run 1) Run 2) mL
Run 3)

Final Volume
21.8 31.4
Run 1) mL Run 2) mL
Run 3)

Volume Utilized (Final Initial)

8.7
Run 1) Run 2) 9.6 mL
Run 3)

Concentration HCI
0.163 0.179
Run 1) Run 2)
Run 3)

0.171
Average Concentration (0.163 + 0.179) / 2 = 0.171

0.0936 M * (8.7/1000)L = 0.000814 mols 0.0934 M * (9.6/1000)L = 0.000896 mols

0.000814 mols / (5/1000)L HCl = 0.163 M HCl 0.000896 mols / (5/1000)L HCl = 0.179 M HCl
 Name: Date: Section:

Questions

1. What was the concentration of the NaOH solution? Show your calculations. If you did not use

all of your data, explain why.

*Calculations shown above*

The concentration of NaOH for the first run was 0.0936 M and the NaOH concentration for the second run was
0.0934 M.

Averaging the results from the 4 groups resulted in an average NaOH concentration of 0.0939 M.

2. What was the concentration of the HCI solution? Show your calculations. If you did not use all

of your data, explain why.

*Calculations Shown Above*

The HCl concentration for run 1 was calculated to be 0.163 M and the HCl concentration for run 2 was calculated to
be 0.179M.

46