Chem&121 1

Acid – Base Titration

Over the quarter, we have looked at many topics: ionic and covalent compounds, chemical reactions and
balanced equations, stoichiometric ratios, and concentrations. Now we will put all of these topics
together: Using a balanced equation, a known concentration of base, and measured volumes of reactants,
we will calculate the unknown concentration of a sample of an acid.

Acid/Base reactions are very similar to double replacement reactions for ionic compounds. A double
replacement reaction can be symbolized as

AB + CD → AD + CB

An acid is a covalent compound that can donate hydrogen ions (H+) in a reaction. Not all hydrogen
atoms will become acidic hydrogens, only those in special cases. For this reason, the acidic hydrogens
are generally written first in a chemical formula. Some examples of acids are;

HCl = hydrochloric acid H2SO4 = sulfuric acid

HBr = hydrobromic acid HNO3 = nitric acid
HC2H3O2 = acetic acid H3C6H5O7 = citric acid

Notice acetic and citric acids have several H’s, but they are separated in the formula. Acetic acid could
be abbreviated as HOAc, and citric acid as H3CA. This would show how many acidic H’s each has and
only show the acidic H’s. This is also a useful way to think about the more complex acids when
balancing chemical reactions.

A Base is a compound that can accept hydrogen ions. The most notable ones are compounds that contain
hydroxide ion (OH-1). Others include ammonia and carbonate compounds. For hydroxide, we might
write

HA + BOH → BA + HOH
(where HOH is water and the B represents a general base – this is also a useful way to balance an
equation.)

We could also write a general equation with our abbreviation for citric acid.

H3CA + 3 BOH → B3CA + 3 HOH (This assumes that B is +1.)

A description of these reactions is to say an Acid and a Base react to form a “salt” (meaning an ionic
compound) and water.

Some examples of real acids and bases:

HBr + NaOH → NaBr + HOH

3 H2SO4 + 2 Al(OH)3 → Al2(SO4)3 + 6 HOH

The balanced equation shows us the ratio of molecules to molecules, or moles to moles of the substances
involved. Reactions occur best when the molecules are free to move and collide with each other, as in

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the case of compounds dissolved in water. Therefore, the most useful way to measure out these
substances in lab is to use volumes like mL where the concentrations are known very precisely in units
of molarity, or moles/liter.

In the experiment today, we will react an acid with a base in a process called titration. Titration means
that we will do the reaction in a quantitative way, for which we will use special glassware. We will use a
special “standardized” acid solution, which was prepared at a commercial laboratory with a
concentration known to 4 places after the decimal. By using the known concentration of acid, and the
measured volumes of acid and base, we can calculate the unknown concentration of the base and know it
very precisely. Once we know the concentration of the base, we can then react it with our acid by
titration to determine the concentration of the acid. This technique could then be applied to any
acid/base system, within reason. (Chemistry is filled with exceptions.)

The reactants need to be measured precisely. As you may have noticed with the glassware so far this
quarter, beakers are good for holding substances, but are not very precise when it comes to measuring.
We will use a graduated cylinder to pre-measure one of the reactants and new piece of glassware called
a buret to add variable volumes of the other. (In even higher precision work, we would replace the
graduated cylinder with a volumetric pipet.)

A buret is like a graduated cylinder with openings at both ends.

On the bottom, there is a valve called a stop-cock which can be
opened or closed. The shape of the buret is also very regular,
like the graduated cylinder, and it has many graduation lines to help you
read the precise volume. Just like weighing by difference on
a balance, we will measure the volume used by recording the
initial volume of liquid, then the final volume of liquid, and
subtracting them to find the actual volume of liquid used. Below
the stop-cock is the “tip” of the buret, which also holds some liquid.
Because the volume is found by difference, it is very important that
the tip not contain any air bubbles. If the bubble escapes or gets
smaller, our precisely measured volume will not be very accurate.

The “reaction flask” for this experiment will be an Erlenmeyer flask. The sloped sides and small
opening prevent liquid and reactant molecules from escaping while the reaction is vigorously swirled.

As we are making every effort to be quantitative in this lab, we want to make sure that contamination is
minimized, and only the single reaction we are looking at is happening. It is also vitally important that
we know the precise concentrations we are working with, in essence, knowing exactly how many
molecules we are working with. Water, even DI water will dilute our solutions, giving us fewer
molecules than we would expect in a certain volume. Any glassware that we use to measure volumes of
reactants needs to be rinsed with the solution we are going to measure so that it contains nothing but the
solution we are working with. (Instructions on how to do this for the graduated cylinder and the buret
are given to you in the Procedures section). If you need to change solutions, which you will do with the
graduated cylinder, you will need to rinse again with the new solution.

Glassware that is not used for volume measurements (such as the Erlenmeyer flask) must be clean, but
not necessarily dry, and should be rinsed with deionized water.

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The reaction we will be using in this experiment is

HCl (aq) + NaOH (aq) NaCl (aq) + HOH (l)

Check to see if this reaction is balanced as written. If you look carefully at these substances in solution,
and think back on our experiences with them over the quarter, you may realize that all of these solutions
look essentially like water. At least in the precipitation reactions, we could see a solid to know that our
reaction was done. How can we know that here?

There are some substances called indicators that are sensitive to the pH of a system. (We saw an
example of this in “Chemical Changes” with the dye extracted from red cabbage juice.) When all the
acid is used up in the reaction, the solution becomes neutral. When the first drop of base enters the
solution, the solution becomes basic and the indicator will change color. By observing the color change,
as evidence of a chemical change, we will know when the reaction is “complete”, stop adding base from
the buret, and record the volumes. In this experiment, we will be using thymol blue as the indicator,
which has the additional property of giving a warning color before the final color is reached. Thymol
blue is pink in strongly acidic solutions, yellow in mildly acidic conditions, and blue in basic solutions.
When you see the warning (yellow) color, slow down to one drop at a time, and stir well. This can be
done using quick turns of the stop-cock on the buret or by controlling the drop rate to one drop every 2
or 3 seconds. Your instructor will demonstrate. If you are not sure if you have reached the end-point,
stop adding, record the volume on the buret and then add one more drop. If, upon stirring, you see no
difference, keep your first number. If you see a definite difference, then draw a single line through your
first number and record the better value. Your goal is to make the final volumes reproducible to within
0.2 mL. You will repeat the experiment twice, and if the values are more than 0.2 mL apart, you will
perform it a third trial.

An example of the calculations with some sample data is on the next page.

Sample Calculation:

In Part B you will use a known volume and molarity of HCl to standardize (determine the molarity of) the NaOH.
Example: You used a 10.00 mL sample of 0.1000 M HCl and it reacted with 7.53 mL of NaOH. What is the
concentration, or molarity, of the NaOH?

Our Balanced Equation: HCl(aq) + NaOH(aq) NaCl(aq) + HOH(l)

AT the equivalence point: moles of acid = moles of base

Our strategy: Use unit analysis to solve for the molarity of the unknown base. For the example above;

(0.1000 M HCl x 10.00 mL x 1 mole NaOH/1 mol HCl)/7.53 mL = 0.133 M NaOH

Notice that we do not covert the mL volumes to L, as the mLs cancel in the statement. The unit analysis statement
also contains an equivalency (1 mol NaOH/1mol HCl) that comes from the balanced reaction equation. This
equivalency is necessary since we often encounter polyprotic acids (like H 2SO4) or polybasic bases (like Ca(OH)2)
where the molar ratio of acid to base are not 1:1.

In Part C, the unknown is the HCl concentration: you will know the M of NaOH, you will measure both volumes
of NaOH and HCl. Set up a unit analysis statement, as above, to determine the molarity of the unknown HCl.

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Procedures
Notes: Only Base (NaOH) goes in the Buret. Use your graduated cylinder for the acid
solutions.
Take care of your buret! The easiest place to break it is at the tip!
As all these liquids look alike, be sure to label them appropriately!

Part A: Experimental Set Up

1. Obtain about 35 mL of NaOH solution in a small, labeled beaker.
2. Condition the buret. Rinse and fill your buret with NaOH:
a. Use a double-sided buret clamp to attach the 10 mL buret to a ring stand. Make sure the stopcock
is closed. Using a disposable plastic dropper pipet, add 2-3 mL of BASE (NaOH) to the buret.
Save the disposable pipet in a small clean beaker for all buret filling.
b. Remove the buret from the clamp, tilt it at an angle, and position the open top over a waste beaker.
Slowly roll the buret with your fingers so the NaOH solution contacts and rinses all the interior
walls, but don’t spill it out of the top. Re-clamp it when you are done and position it over a labeled
waste beaker.
c. Open the stopcock and let the rinse solution go through the tip of the buret, and stop the flow when
the level is just above the stopcock. Rinse the buret a second time using the same procedure. When
draining it, inspect the stopcock tip and make sure it is free of bubbles. If there is a persistent
bubble, check with your instructor.
d. When ready, fill the buret to the 0.00 mark or slightly below. Do not waste time getting exactly to
0.00 mL, as you will record the initial volume and subtract it from the final volume to find the total
volume.
3. Rinse your graduated cylinder with “standardized” HCl:
a. Obtain about 35 mL of the commercially-standardized HCl solution in a small, labeled beaker.
Record the molarity from the label as precisely as possible. (The Molarity may also be listed as
Normality or N, but for HCl, the value is the same.) This is your known concentration.
b. Pour about 2 mL of the acid solution in your 10 mL graduated cylinder. Tilt and roll it around like
you did with the buret to rinse the inside. Discard the rinse to the waste beaker.
c. Rinse a second time and check for cleanliness, and proceed immediately to part B.

Part B: Determining the concentration of the NaOH solution.

4. When ready, pour acid into the graduated cylinder to the 10.00 mL line according to the bottom of
the curve or “meniscus”. Then pour the acid sample into the Erlenmeyer reaction flask. (The
cylinder is designed “to deliver” the correct volume without rinsing.)
5. Add two to three drops of thymol blue indicator to the reaction flask.
6. Check the buret tip for air bubbles or droplets on the end. Record the initial volume in the buret at
the bottom of the meniscus. Be sure to read the volume with your eye level to the sample. Read and
record the volume to 2 places after the decimal. You will need to count the divisions between the
numbered marks so you are sure what volume one mark represents!
7. Adjust the buret height so that the tip is just inside the lip of the flask. Do not let any liquid escape to
the outside of the flask or it will be unaccounted for!

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8. Begin adding the base while stirring the reaction flask constantly. This may require two people. The
recommended swirling technique is to tip the flask up on a side and swirl gently while pressing
against the bench top. Your instructor will demonstrate. Try not to splash the contents against the
sides or some of the molecules may not react. Add it in a steady flow but watch for a hint of color
change.
9. As you get closer to the endpoint of the titration, the color will change to yellow. Begin adding base
dropwise, with thorough swirling, until the final color change to blue. When the final color change
arrives, it will happen very quickly, often with one drop. The color must last at least 30 seconds. If it
fades back to yellow, you need to add another drop. Continue to swirl until you are sure you are
done. If you think you are done, record the volume, then add one more drop to see if there is a
difference. Record the final buret volume (which produced the final color change) to 2 places after
the decimal.
10. Discard the waste from the reaction flask into a waste beaker and wash the flask out well with tap
water. Rinse with several small samples of DI water and leave it wet.
11. Repeat the titration with another 10.00 mL sample of standardized acid. If the total volumes of the
base are not within 0.20 mL, repeat a third time.
12. Refill the buret with base. Discard the factory standardized HCl solution into the waste beaker.

Part C: Determining the unknown concentration of a new acid solution.

13. From the instructor’s bench, obtain a sample of acid of unknown concentration. Record the letter of
the unknown on the data sheet. (The acid is also HCl, but of unknown concentration.)
14. Rinse the graduated cylinder twice with the new acid solution and discard in the waste beaker.
Transfer 10.00 mL of the new acid solution to the reaction flask. Add two or three drops of the
indicator thymol blue and repeat the titration as before. Record the initial and final volumes of base.
15. Perform the titration twice. If the total volumes of base from the titrations of the unknown acid are
not within 0.20 mL, repeat a third time.
16. Discard all the wastes into the class waste container in the hood. Wash all glassware with tap water
and rinse with DI water at least twice before returning to the back bench or the lab drawer. Empty
and rinse the buret twice with small portions of deionized water, clamp the burets upside-down and
leave the stopcocks open to allow them to dry.
17. If this is the final lab, check over the contents list in your lab drawer to make sure everything is
accounted for. If anything is missing, check the instructor’s bench for a spare. If anything is extra,
please turn it in to the instructor’s bench for another. If you can’t find it there, ask the instructor for a
replacement. Wipe down your bench area and turn off the light before you go. Don’t forget to take
your goggles with you!

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Titration Name ____________________________

Chemistry 121

Pre-Lab Assignment

1. Before using a buret, the buret is “conditioned”. Briefly describe the conditioning procedure.

2. An example of finding the concentration of a sample of NaOH is given in the introduction

section. Now use the concentration of the sodium hydroxide (0.113 M), and show how you
would find the unknown concentration of an acid solution where 10.00 mL of the acid was
titrated with 11.35 mL of the base. (Set up a unit analysis statement to calculate the concentration
of the HCl.)

3. Re-evaluate significant figures in your answer to #2: How many significant figures are in
a) the M of the NaOH in the “sample calculation”? _____
b) the volume of the HCl in #2? _____
c) the volume of NaOH in #2? _____
d) your answer to #2 (correct it if necessary!)? _____

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Report Sheet Name ____________________________

Titration
Lab Partner _____________________________

Observations and Data

Part A: Experimental Set Up

Concentration of standardized HCl solution:

Volume of HCl from graduated cylinder used in each titration (be precise)

Part B: Determining the actual concentration of the NaOH solution.

Titration 1 Titration 2 Titration 3

Final buret reading

Initial buret reading

Total volume NaOH

(other calculations below)

Part C: Determining the concentration of the unknown acid solution.

Unknown Number/letter

Volume of HCl from graduated cylinder used in each titration:

Titration 4 Titration 5 Titration 6

Final buret reading

Initial buret reading

Total volume NaOH

(other calculations below)

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Calculations and Results

Write the balanced equation for the acid reacting with the base for these reactions:

Part B: Determine the actual concentration of the NaOH solution.

From your data above, calculate the concentration (molarity) of the NaOH solution from each titration
using unit analysis statements. Calculate the average concentration.

Concentration NaOH – T1

Concentration NaOH – T2

Concentration NaOH – T3

Average Concentration NaOH

Part C: Determine the unknown concentration of your chosen acid solution.

Using the average concentration of the NaOH solution above, calculate the concentration of the
unknown HCl solution separately for each titration in Part C using unit analysis statements. Calculate
the average concentration.

New Acid Conc. – T4

New Acid Conc. – T5

New Acid Conc. – T6

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