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Experiment 5: Titration of a Strong Acid with a Strong Base

PURPOSE
A titration is a process used to quantitate a solution by determining the volume of a solution with a known
concentration that is needed to react with a given amount of another substance.

In this experiment, your goal is to determine the molar concentration of an unknown acid solution by
conducting titrations with a base of known concentration. You will be testing a strong acid, HCl, solution
by two methods, 1) using the indicator phenolphthalein and 2) by using a pH meter. Both testing methods
will be combined during the titration process and you will compare the results obtained by the indicator
with the results obtained from a titration curve and a Second Derivative plot. You will use a standardized
sodium hydroxide, NaOH, solution as your strong base of known concentration for the titrations. The
reaction equation is shown below in net ionic form.

H+ (aq) + OH– (aq) → H2O(l)

The stoichiometry of the reaction is one mole of hydrogen ion reacts with one mole of hydroxide ion to
produce one mole of water. Therefore, your calculations will be straightforward. You will determine the
concentration of an unknown strong acid by both methods. The volume of NaOH titrant used at the end
point as determined by the indicator and the equivalence point as determined by the titration curves and the
Second Derivative plot will be used to determine the molarity of an unknown concentration of HCl
solution.

OBJECTIVES
In this experiment, you will
1) Prepare an aqueous solution of sodium hydroxide to a target molar concentration.
2) Determine the concentration of your secondary standard NaOH solution by titrating it with a
solution of a primary standard, potassium hydrogen phthalate, abbreviated KHP. (Two trials)
3) In LoggerPro, graph a Second Derivative plot.
4) Determine the precise concentration of the secondary standard, the sodium hydroxide, and the
solution from the results of using the indicator or from the results of the Second Derivative plot.
5) Conduct two acid-base titrations.
6) Determine the end point of a strong acid-strong base titration by measurement with an indicator
and the equivalence point by measurement with a pH meter.
7) Complete a titration curve for the neutralization reaction and a Second Derivative Plot.
8) Calculate and compare the molar concentrations of an unknown acid solution obtained by the
results of the titration curve, the Second Derivative Plot and the indicator.

PRINCIPLES
Acid-base reactions are among the most important kinds of reactions that occur in aqueous solutions
because of their significance in the metabolism of plants and animals and their plentiful use in
industrialized societies.

A neutralization reaction is the commonly used expression used to describe the reaction of an acid with a
metal hydroxide base that produces a salt and water. The term is derived from the observation that the

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standard properties of the acids and the bases are neutralized when reacted with each other. The driving
force of nearly all neutralization reactions is the combination of the H+ (aq) from an aqueous acid solution
with the OH− (aq) from an aqueous base solution to form water molecules.

All strong acids and strong bases completely or nearly completely ionize in dilute solution. Strong acid and
strong base solutions contain predominately ions rather than acid or base molecules; the equilibrium falls
almost entirely to the right in dilute solution. There are only seven strong acids and eight strong soluble
bases and you should commit all of them to memory. They are listed below.

Strong acids:
a) Three binary acids derived from Group VIIA halogens
1) Hydrochloric acid – HCl
2) Hydrobromic acid – HBr
3) Hydroiodic acid – HI
b) Four ternary acids (oxyacids) derived from polyatomic ions
4) Sulfuric acid – H2SO4
5) Nitric acid – HNO3
6) Chloric acid – HClO3
7) Perchloric acid – HClO4
Strong bases:
a) Group IA metal hydroxides
1) Lithium hydroxide – LiOH
2) Sodium hydroxide – NaOH
3) Potassium hydroxide – KOH
4) Rubidium hydroxide – RbOH
5) Cesium hydroxide – CsOH
b) Heavier Group IIA metal hydroxides
6) Calcium hydroxide – Ca(OH)2 (soluble in concentrations ≲ 0.0125M)
7) Strontium hydroxide – Sr(OH)2
8) Barium hydroxide – Ba(OH)2

Similarly, the three chemical equations used to describe precipitation reactions can be applied to acid-base
neutralization reactions. For example, write the formula unit, total ionic, and net ionic equation for the
reaction of aqueous sulfuric acid with aqueous potassium hydroxide to produce aqueous potassium sulfate
and water.

Formula Unit Equation


2 KOH (aq) + H2SO4 (aq) → K2SO4 (aq) + 2 H2O (l)

• The symbol (aq) indicates that the acid and base are ionized and hydrated in dilute aqueous
solution.
• The symbol (l) indicates that the water is a liquid water molecule.

Total Ionic Equation


2 K+ (aq) + 2 OH− (aq) + 2 H+ (aq) + SO42− (aq) → 2 K+ (aq) + SO42− (aq) + 2 H2O(l)

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Net Ionic Equation


2 H+ (aq) + 2 OH− (aq) → 2 H2O(l) – Reduce the equation by dividing by 2 to determine net ionic
equation.

H+ (aq) + OH− (aq) → H2O(l) (This is the net ionic equation for all strong acid and strong base
reactions that produce a soluble salt.)

Strong acid and strong base neutralization involves the reaction of an aqueous solution of an acid with a
base to form a solution that is driven by the formation of liquid water and usually a soluble salt, a notable
exception is the result of reacting aqueous barium hydroxide with sulfuric acid, which produces water and
an insoluble barium sulfate salt.

Acid-Base Solutions
Acids are substances that generate H+ in aqueous solutions. Strong acids ionize ≈100% in water. That is,
the strong acids completely ionize (or almost completely ionize) to produce H+ when in dilute aqueous
solution. The H+ ions produced in aqueous solutions produce acidic solutions. Acidic solutions have a pH
lower than 7.

An acid cannot be an acid unless it is in solution.


• It must be able to produce H+ and that can happen only in solution.
• Often, and correctly so, acids are named with the symbol (aq) because acids are more commonly
dissolved in water.

The protons (hydrogen ions) that are generated in acid solutions are not present in the solution by
themselves. Protons are surrounded by several water molecules.
• How many varies from solution to solution.
• H+(aq) is really H(H2O)n+
• Where n is a small integer.

Chemists normally write the hydrated hydrogen ion as H3O+ and call it the hydronium ion.

H+ = H3O+

The Brønsted-Lowry Theory


J.N. Brønsted and T.M. Lowry developed a general acid-base theory in 1923 that defines:
• An acid is a proton (H+) donor.
• A base is a proton acceptor.

Two examples to illustrate this concept:

→ H 3O + (aq) + Br - (aq)
HBr (aq) + H 2O (l) 

NaOH (aq) + H 3O + (aq) 


→ 2H 2O (l) + Na + (aq)

An important part of Brønsted-Lowry acid-base theory is the idea of conjugate acid-base pairs.

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The two species that differ by a proton are called acid-base conjugate pairs.

HNO3 + H 2O → H 3O + + NO3–

Acid Base conjugate acid conjugate base

The Autoionization of Water


Water can be either an acid or base according to the Bronsted-Lowry theory. Consequently, water can react
with itself. This reaction is called autoionization. Pure water ionizes very slightly. The concentration of the
ionized water is less than one-millionth molar at room temperature.

During the autoionization of water, one water molecule acts as a base and the other as an acid.


→ H 3O+ (aq) + OH − (aq)
H 2O (l ) + H 2O (l ) ←

Because the activity of pure water is 1, the equilibrium constant for this reaction is:

K w =  H 3O+  OH − 

This particular equilibrium constant is called the ion-product for water and given the symbol Kw.
Experimental measurements have determined that the concentration of each ion is 1.0 × 10-7 M at 25oC.
(Note that this is at 25oC, not every temperature!) We can determine the value of Kw from this information.

K w =  H 3O +  OH − 
= (1.0 x 10-7 )(1.0 x 10-7 )
= 1.0 x10−14

When a strong acid or a strong base is added to water at room temperature, the concentration of the
hydronium and the concentration of hydroxide ions can be calculated using the ion-product, Kw.

Example: Calculate the concentrations of H3O+ and OH- in 0.050 M HCl.

HCl + H 2O → H 3O + + Cl −
0.050 M 0.050 M 0.050 M
Thus the  H 3 O  = 0.050 M .
+

The  H 3 O +  and K w will allow us to calculate [OH - ].

 H 3O +   OH −  = 1.0 ×10−14
1.0 × 10 −14 1.0 ×10 −14
 OH −  = =
 H 3O +  5.0 × 10−2
OH −  = 2.0 × 10 −13 M

The pH and pOH scales


A convenient way to express the acidity and basicity of a solution is the pH and pOH scales.

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When [H3O+] = [OH−] in solution, the solution is considered neutral and has a pH = 7.
[H3O+] > [OH−] in solution, the solution is considered acidic and has a pH < 7
[H3O+] < [OH−] in solution, the solution is considered basic and has a pH > 7

The pH of an aqueous solution is defined as:

pH = − log  H 3O + 

If either the [H3O+] or [OH-] is known, the pH and pOH can be calculated.

Example 1: Calculate the pH of a solution in which the [H3O+] =0.030 M.

pH = ー log H 3O 
+

(
pH = − log 3.0 × 10
−2
)
pH = 1.52

Note: The number of significant figures in a log term is the number of figures after the decimal point. The
number before the decimal point is a result of the exponent and is not counted as a significant figure.

Example 2: Calculate the pOH of a solution in which the [OH-] =0.000615 M.

pOH = − log[OH − ]
= − log (6.15 ×10 − 4 )
= 3.211

If either the pH or pOH is known, the [H3O+] or [OH-] can be calculated:

Example 3: The pH of a solution is 4.597. What is the concentration of H3O+?

pH = − log[H 3O + ]
4.597 = − log[H 3O + ]
− 4.597 = log[ H 3O + ]
10− 4.597 = [ H 3O + ]
2.53×10− 5 = [ H 3O + ]

Example 4: The pOH of a solution is 9.403. What is the concentration of OH−?

pOH = − log[OH − ]
9.403 = − log[OH − ]
− 9.403 = log[OH − ]
log[OH − ] = 10 −9.403
[OH − ] = 3.95 ×10 −10

A convenient relationship between pH and pOH may be derived for all dilute aqueous solutions at 250C.
Taking the logarithm of both sides of this equation gives:

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[H 3O + ][OH − ] = 1.0 × 10−14


log  H 3O +  + log  OH −  = − 14.00

Multiplying both sides of this equation by -1 gives:

( )
−log  H 3O +  + −log OH −  = 14.00

This can be rearranged to this form:

pH + pOH = 14.00

Example 5: Calculate the [H3O+], pH, [OH-], and pOH for a 0.020 M HNO3 solution.

≈100%
HNO3 + H 2O  → H 3O + + NO3− pOH = 14.00 − 1.70
0.020 M 0.020M 0.020M = 12.30
 H 3O  = 2.0 × 10 M
+ −2
[OH − ] = 10 − pOH
pH = − log ( 2.0 × 10−2 M ) = 10 −12.30

pH = 1.70 = 5.01× 10 −13

To help develop familiarity with the pH and pOH scale we can look at a series of solutions in which [H3O+]
varies between 1.0 M and 1.0 x 10-14 M.

[H3O+] [OH-] pH pOH


1.0 M 1.0 x 10-14 M 0.00 14.00

1.0 x 10-3 M 1.0 x 10-11 M 3.00 11.00

1.0 x 10-7 M 1.0 x 10-7 M 7.00 7.00

2.0 x 10-12 M 5.0 x 10-3 M 11.70 2.30

1.0 x 10-14 M 1.0 M 14.00 0.00

An Introduction to Titration
A titration is used to quantitate solutions. It is a procedure that will allow us to go into the laboratory and
collect the data that is necessary in order to determine the concentration of a solution. Titrations can be
applied to many types of reactions in solutions, e.g. neutralization, precipitation and oxidation reactions. In
our lab, we will perform a titration of a strong acid of an unknown concentration with a strong base of a
known concentration. The volume of the strong base needed to completely neutralize a measured volume
of the strong acid will be used to determine the concentration of the acid.

Before you begin the titration lab, there are certain conditions that need to be satisfied. In order to perform
an acid-base neutralization titration, we need the following:
• An accurate method of measuring the amount of acid or base that is used during the neutralization
process.

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• A known volume of an acid or a base that will be used to neutralize an unknown concentration of
acid or base.
• A method of determining the exact amount (moles) of unknown acid or base that was neutralized
during the procedure.

1) The first criterion for titration is provided by using a burette.

2) The second criterion for titration is provided by using a standardized acid or base to neutralize the
unknown concentration of acid or base.
• Standardized means that we have used a very accurate method of determining the molarity of the
acid or base that we will use to neutralize the unknown concentration of an acid or a base.

3) Finally, a pH meter and an indicator will be added to our standard acid or base as our methods of
determining the moles of unknown acid or base that was neutralized.
• The pH meter is an instrument that contains a probe with two electrodes. One of the electrodes is a
glass electrode that is sensitive to [H3O+] and the other probe is a reference electrode. The glass
electrode has a silver-based electrical wire suspended in a solution of HCl (usually 1.0 M),
contained inside a thin glass membrane made from a very special glass coated with silica and
metal salts. The other electrode is called the reference electrode, which completes the circuit.
When you immerse the probe into your solution with H3O+ ions, a potential develops across the
thin glass membrane as a result of the concentration gradient between the solution of ions and the
1.0M HCl. This creates a tiny voltage across the glass that the silver electrode picks up and passes
to the voltmeter. The voltmeter measures the voltage generated by the solution and displays it as a
pH measurement. When a solution is acidic, there is an increase in hydronium ions that causes the
voltage to increase and the meter displays a decrease in pH. Alternatively, a basic solution has
fewer hydronium ions, more hydroxide ions, which results in a decrease in voltage, and the meter
displays an increase in pH.

• An acid-base indicator is an organic dye that is able to change color depending on the [H3O+] in
solution. The first indicators used were vegetable dyes, such as litmus. Most of the indicators used
in laboratories today are synthetic compounds; compounds made by chemists. Phenolphthalein is
the most common acid-base indicator and it is the indicator that we will use in our acid-base
titration. It is an organic compound (C20H14O4) that is colorless in acidic solution and pinkish in
basic solution (with the transition occurring around pH 9).

Standard solutions are solutions of accurately known concentrations. In the laboratory, we will use
sodium hydroxide as our standard to determine the concentration of an acid of an unknown concentration.
However, solutions of sodium hydroxide are virtually impossible to prepare to a precise molar
concentration because the substance is hygroscopic – absorbs moisture from the air. In fact, solid NaOH
absorbs so much moisture from the air that a measured sample of the compound is never 100% NaOH. In
order to obtain an accurate concentration of our standard, we will perform a process known as
standardization on our NaOH solution. Standardization is a process by which the accuracy of a secondary
standard (NaOH) is determined by measuring the volume of the secondary standard required to react with a
highly pure primary standard.

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To determine the concentration of the NaOH solution, the secondary standard, we will use a solution of an
acidic salt, potassium hydrogen phthalate (KHP), as a primary standard. The KHP compound is a weak
acid (see figure 2 below) that has an acidic hydrogen (see underlined –OH group in figure 1) that reacts
with NaOH in a simple 1:1 stoichiometric ratio. Potassium hydrogen phthalate, KHC8H4O4, (primary
standard) can be measured out in precise mass amounts; it is easily obtained in a high state of purity and is
soluble in water, thus making it an ideal substance to use to standardize a solution of NaOH. The results of
a KHP titration with NaOH is shown in figure 2 below.

Expt. 5 KHP Titration Curve (Part 1, Run1)


pH vs.[NaOH]

The equivalence point is


greater than 7.

Figure 2. The titration curve of KHP titrated with NaOH. The KHP in this titration is a weak acid.
The equivalence point in a titration of a weak acid with a strong base is greater than pH=7 as a
result of the hydrolysis of the strong conjugate base that is produced from the soluble salt. We will
cover this concept in greater detail in experiment 7.

The Method of Titration


Example: We will perform a strong acid – strong base titration with an indicator.

Standardizing Sodium Hydroxide


Before we begin to determine the unknown concentration of our acid, we need to standardize the NaOH
solution. (A very thorough description of titration is given for the determination of the unknown
concentration of sulfuric acid below.)
The reaction stoichiometry is: HP– (aq) + OH– (aq) → H2O(l) + P2– (aq)

We have:
1. A burette that holds a volume of 50.0 mL and is graduated in 0.01 mL increments.

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2. Phenolphthalein, an indicator that is colorless in acidic solutions but is pink in basic solutions.
3. A sodium hydroxide solution.
4. A measured weight of 2.0102 g of KHP, which is dissolved in 80.0 mL of distilled water.

Results: It took 8.95 mL of NaOH sol’n to reach the endpoint in the titration.

 2.0102 g KHP   1 mol KHP   1 mol NaOH  1.0997 mol NaOH


      = = 1.10 M NaOH
 0 . 00895 L NaOH sol' n   204.23 g KHP   1 mol KHP  L NaOH sol' n

We want to determine the concentration of a sulfuric acid solution using a standardized sodium hydroxide
solution and an indicator as our method of determining the amount (moles) of unknown acid or base that
was neutralized during the procedure.

The reaction stoichiometry is: H2SO4 (aq) + 2NaOH (aq) → 2H2O (l) + Na2SO4 (aq)

We have:
5. A burette that holds a volume of 50.0 mL and is graduated in 0.01 mL increments.
6. Phenolphthalein, an indicator that is colorless in acidic solutions but is pink in basic solutions.
7. A standardized solution of 1.10 M sodium hydroxide solution.
8. A 50.0 mL sample of sulfuric acid of an unknown concentration.

The procedure:
1. We fill the graduated cylinder to the 5.2 mL mark with our 1.10 M sodium hydroxide standard
solution.
2. We will use a few drops of phenolphthalein as our indicator. Phenolphthalein is colorless in acidic
solutions but will turn very light pink after the acid has been neutralized.
3. We will take a15.0 mL of our original unknown sulfuric acid (the 50.0 mL sample) and add it to
75.0 mL of water in a beaker and then place it under the tip of the burette.
4. We begin adding the basic secondary standard, NaOH, until our acid sample solution turns very
light pink, the end point. The point at which the indicator changes color and the titration is
stopped.
• Theoretically, the sample volume of the sulfuric acid will still be colorless at exactly to the
point in which the numbers of moles H+ have been completely neutralized by the OH− ions of
our standard, the equivalence point. The equivalence point occurs when all the excess H+ ions
from the acid have been neutralized by the OH− ions from the base. As a result, the solution is
neutral; the pH = 7. Note: The equivalence point and the end point do not necessarily
coincide. Therefore, the equivalence point and the end point are separate terms with different
meanings.
• If we add more OH− ions than are needed to exactly neutralize the H+ ions in the sample acid,
then the solution becomes basic and the color changes to pink. We want to add the sodium
hydroxide until the solution is very slightly pink (the end point). Ideally, the end point will
equal the equivalence point. However, when the color change of the indicator becomes
visible, the [OH-] is in excess. Therefore, the end point will not be exactly equal to the
equivalence point, but because the pH changes very abruptly at the equivalence point, the end
point will be very close.

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Data collected.
After a few minutes of adding the sodium hydroxide, the sulfuric acid solution turns very slightly pink,
indicating that the end point has been reached. The titration is stopped and the value on the burette is 22.42
mL.

Determination of concentration of sulfuric acid:


How many mL of sodium hydroxide was used?

Finished: 22.4 mL 1.10 M NaOH solution


Started: -5.2 mL 1.10 M NaOH solution
Used: 17.2 mL 1.10 M NaOH
Results
What is the concentration of the sulfuric acid?

H2SO4 (aq)+ 2 NaOH (aq) → 2 H2O (l) + Na2SO4 (aq)

 1.10 mol NaOH  1mol H 2SO 4 


0.0172 L NaOH    = 0.00946 mol H 2SO 4
 1.00 L NaOH  2 mol NaOH 

We know that the numbers of moles of H2SO4, determined from the titration, were in a15.0 mL sample:
Remember; you are only interested in the concentration of the sulfuric acid in the original sample, not the
concentration of the sulfuric acid after it has been diluted.

mol H 2 SO 4
M =
Volume H 2 SO 4 sol' n
0.00946 mol H 2 SO 4
= = 0.631 M H 2 SO 4
0.0150 mL H 2 SO 4 sol' n

If the titration had included a pH probe, we would record the volume used at certain intervals and continue
the titration beyond the end point of the color change of the indicator. We would graph the titration curve
(pH on y-axis and volume of NaOH on x-axis) and create a 2nd derivative graphs. The volume used to reach
the equivalence point can be determined from both graphs. (See figure 3 below)

Strong Acid/Strong Base Titration

endpoint

Figure 3. The pH vs. volume of strong base (Vbase) in mL. Note: to reach the endpoint
and attain the equivalence point, the volume of base required is the same.

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PART 1: STANDARDIZING A SOLUTION OF SODIUM HYDROXIDE (working in teams of two)


MATERIALS
computer solid sodium hydroxide
LabQuest solid potassium hydrogen phthalate, KHP
pH Sensor distilled water
ring stand Analytical balance (± 0.01 g)
250 mL beaker utility clamp
600 mL beaker burette and burette clamp
250 mL Erlenmeyer flask 500 mL screw top plastic bottle
50 mL and 100 mL graduated cylinders 100 mL graduated cylinder
magnetic stirrer and stirring bar phenolphthalein indicator

PROCEDURE
PRE-LAB PREPARATION (Show all calculations with the proper units and the correct significant
figures.)

1) Calculate the mass of sodium hydroxide needed to prepare 500.0 mL of a 0.500 M NaOH solution.
(Molar mass of NaOH = 40.0 g/mol)

2) Calculate the volume of 0.500 M NaOH solution in mL needed to react with 2.000 g of KHP
Consider the reaction equation to be as shown below. (Molar mass of KHP = 204.233 g/mol)
HP– (aq) + OH– (aq) → H2O(l) + P2– (aq)

PART 1: NaOH STANDARDIZATION PROCEDURE


1. Measure out the mass of NaOH that is needed to prepare a 500.0 mL of 0.500 M solution to the
nearest 0.0001 g. Record the mass of the NaOH and transfer the pellets to a 600 mL beaker. Add
400.0 mL of deionized water to the flask and stir to dissolve the solid – using stir bar and magnetic
stirrer. CAUTION: Sodium hydroxide solution is very exothermic and the beaker will become very
hot. Be careful and avoid spilling it on your skin or clothing.

2. Transfer the dissolved pellets solution to a 500 mL plastic bottle. Add enough deionized water to
bring the total volume to 500.0 mL (up to the mark on the bottle) and gently invert the bottle several
times to thoroughly mix the solution. (You will label the container with a drawer number of one of
the team member’s name and the concentration once the standardization process is complete.)
Keep the lid on plastic bottle when not in use to prevent the reaction of NaOH in the solution with
atmospheric carbon dioxide.

3. Measure and record 2.000 g of KHP to the nearest 0.001 g and dissolve in 80.0 mL of distilled
water in a 250 mL beaker and add 2-3 drops of phenolphthalein indicator.

pH SENSOR PROCEDURE (Although you are working in teams, you must write your own lab report.)

Set up the data collection system.

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1. Connect the pH Sensor to LabQuest and choose New from the File menu. DO NOT pull pH
sensor from storage bottle, loosen cap before removing pH Sensor from storage bottle.

2. On the Meter screen, tap “Mode”. Change the data-collection mode to “Events with Entry”. Enter
the Name (Volume) and Unit (mL) and select OK.

3. Clean the 50.0 mL burette with distilled water and rinse well with deionized water. Rinse the
burette with two small volumes of NaOH then fill it with the NaOH solution; slowly pour the
NaOH solution into a funnel that has been placed on the top of the burette. Record the initial
volume of the NaOH solution in the burette. CAUTION: Sodium hydroxide solution is caustic.
Avoid spilling it on your skin or clothing.

4. Place a magnetic stirring bar in the beaker and place the beaker of KHP solution on a magnetic
stirrer under the burette. Connect the pH Sensor to the utility clamp so that the tip of the sensor is
immersed in the KHP solution but does not interfere with the movement of the magnetic stirring
bar.

Start data collection.


5. Before you have added any NaOH solution, tap “Keep” and enter 0 representing the burette
volume in mL. Select OK to store the first data pair.

6. To calibrate the pH meter, add enough of the NaOH titrant to raise the pH about 0.15 units. When
the pH stabilizes, tap “Keep”, and enter the volume of NaOH dispensed as precisely as possible,
to two places after the decimal. Select OK to save the second data pair. (You may revise volume
entry mistakes by tapping the 4-square icon on the upper right of your LabQuest.)

7. Conduct the titration carefully. Add NaOH to your KHP solution, recording volume of NaOH at
5.00 mL intervals (tap “Keep” and OK after each interval) until you are about 3.00 mL below the
volume you calculated in the pre-lab. As the NaOH solution is added the KHP solution will briefly
turn pink and then disappear. As the endpoint of the titration is approached, the pink color remains
longer.

8. Add two 1.00-mL aliquots (volumes) of NaOH. The final 1.00 mL of NaOH should be added in
5fivedrop increments until the solution turns pink and remains pink for ten seconds; at this point
you halt the titration and record (tap “Keep”and OK) the volume of NaOH added. Write in your
lab notebook that this is the volume used to reach the end point using the indicator. If less than
five drops are needed, take the volume at the point that the titration is stopped (be sure to count the
number of drops). Twenty drops is approximately 1.00 mL. (See example procedure below.)

E.g. Let’s say you calculated a volume of 33.5 mL of approximately 0.250 M NaOH would be
needed to neutralize 8.375 × 10−3 moles of KHP. You would begin the titration, after the
calibration step, by adding 5.00 mL increments of NaOH (recording the volume after each
addition) until you have added 30.0 mL. You will continue the titration by adding 1.00 mL of
NaOH and then another 1.00 mL of NaOH (recording the volume after each addition). At this
point you will have added 32.0 mL of NaOH. Now you will begin adding five drops of NaOH
until the solution turns pink and remains pink for about 10 seconds. The pH at this point will

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CH204 Experiment 5: Strong Acid/Strong Base Titration spring 2015

rise sharply. Record the volume of NaOH needed to reach the endpoint. Continue the titration
until an additional 5 or 6 mL have been added in order to produce a useful second derivative
curve.

9. Once the endpoint has been reached, add five or six mL of NaOH, one mL at a time, to the
KHP solution (recording the volume after each addition). Note: you need at least five data
points before reaching the equivalence point pH and five data points after the equivalence point
has been reached in order to plot a useful second derivative graph. Stop the titration and record
the final volume of NaOH added (tap “Keep”and “Save”). Save the data from the first run by
tapping the File Cabinet icon. Save the data on the LabQuest and on your USB drive.

10. When you have completed the titration, dispose of the reaction mixture as directed.

11. Use the LoggerPro and the second derivative analysis to find the volume of NaOH used at the
equivalence point, this analysis is described in detail on the last page of this experiment. Since
KHP is a weak acid, the pH at its equivalence point will be greater than 7 (see figure 2); therefore,
the volume of NaOH used in the titration can only be determined from the second derivative plot.

12. E ach member should print copies of each graph; include the names of each team member and the
data sets on the graph printouts. You should two second derivative plots, one for each of the two
titrations.

13. Change roles with your partner and repeat the titration with a second KHP solution, Run 2. (No
more than three total runs will be allowed.) Analyze the titration results and record the equivalence
point. Record the results of the second titration.

Data Table 1: Part 1 Volume of NaOH used in titrations.


Volume of NaOH Volume of NaOH
NaOH
Trial Indicator End Point 2nd Derivative (mL)
(mL) Equivalence Point

average

DATA ANALYSIS (Show your work.)

1. Calculate the average moles of KHP neutralized by the NaOH. Calculate the average from the
masses recorded for two best titration runs
2. Calculate the molarity of the NaOH solution that you prepared by using the average volume
obtained from the indicator endpoint, the average volume from Second Derivative equivalence
point (Data Table 1).

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CH204 Experiment 5: Strong Acid/Strong Base Titration spring 2015

PART 2: STRONG ACID – STRONG BASE TITRATION (working in teams of two)

MATERIALS
pH Sensor Standardized 0.500 M sodium hydroxide, NaOH, solution
LabQuest hydrochloric acid, HCl, solution, unknown concentration
ring stand distilled water
250 mL beaker 50 mL burette and burette clamp
magnetic stirrer and stirring bar utility clamp
25 mL graduated cylinder 5.0 mL volumetric pipette
50 mL graduated cylinder phenolphthalein indicator

PROCEDURE: Titration: Unknown Strong Acid/ Strong Base Titration

1. Obtain and wear goggles.

Conduct the titration carefully.

2. Obtain a sample of hydrochloric acid solution of an unknown concentration from your TA.

3. Add 75.0 mL of distilled water to a 250 mL beaker. Use a 5.00 mL volumetric pipette to transfer
5.00 mL of the HCl solution into the beaker. Add 2-3 drops of phenolphthalein indicator to the
beaker. CAUTION: Handle the hydrochloric acid with care. It can cause painful burns if it
comes in contact with the skin.

4. Place the beaker on a magnetic stirrer and add a stirring bar.

5. Fill the burette with your standardized NaOH solution. CAUTION: Sodium hydroxide solution is
caustic. Avoid spilling it on your skin or clothing.

6. Position the pH Sensor so that its tip is immersed in the HCl solution but is not struck by the
stirring bar. Gently stir the beaker of acid solution. Run 3.

Start data collection. (Save the data on the LabQuest and USB drive after each run.)
7. Before you have added any standardized NaOH solution, tap “Keep” and enter 0 representing the
volume of NaOH dispensed in mL. Select OK to store the first data pair.

8. Add NaOH in 2.00 mL increments until the pH of the mixture is about pH 2.0, record the volume
after every 2.00 mL addition (tap “Keep” and OK after each interval). As the NaOH solution is
added the acid solution will briefly turn pink and then disappear. As the endpoint of the titration is
approached, the pink color remains longer.

9. At about pH 2.0, add the NaOH drop wise until the solution turns slightly pink and remains pink
for ten seconds; at this point you halt the titration and record the volume of NaOH used. (Record
the volume of NaOH used after every five drops until you reach the endpoint.) Write in your lab
notebook that this is the volume used to reach the end point using the indicator.

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CH204 Experiment 5: Strong Acid/Strong Base Titration spring 2015

10. Once the endpoint has been reached, add five or six mL of NaOH, one mL at a time. (Note: you
need at least five data points before reaching the equivalence point pH and five data points after
the equivalence point has been reached in order to plot a useful second derivative graph.) Stop the
titration.

11. When you have finished the titration, dispose of the reaction mixture as directed. Rinse the pH
Sensor with distilled water in preparation for a second titration. Change roles and repeat the
titration.

12. After the second titration is complete, divide the remaining standardized NaOH between the two
or three team members; use your 500mL or 1 L bottles with the screw caps to store the NaOH. We
will use this standard NaOH solution in a later experiment.

13. Use your titration data to graph a titration curve in LoggerPro (instructions on last page). The
titration curve is pH (y-axis) vs. volume of NaOH in mL (x-axis). Also use your pH vs. volume
data to graph a second derivative plot. Analyze your information and record the equivalence point.
You should have two titration curve graphs and two second derivative plots, one for each of the
two titrations.

14. Each member should print copies of each graph; include the names of each team member and the
data sets on the graph printouts. Use the LoggerPro software on the lab computers to copy data to
your lab partner’s USB. Do not leave the lab until your partner has the data copied; students who
do not have data because they did not copy their partner’s data before they left the lab will not be
given extended time to in which to complete the assignment.
DATA TABLES

Table 2: Part 2 Volume of NaOH used in titrations. Indicate the volume (5.00 mL) of HCl used in the
trials and the total volumes of NaOH used to reach the end point with the indicator and the equivalent
points as determined from the graphs.

Volume of
Volume of NaOH Volume of NaOH
Volume NaOH
HCl Equivalence Equivalence
HCl sample End Point
Trial Point Titration Curve Point 2nd Derivative
(mL) Indicator
(mL) (mL)
(mL)
1

average

DATA ANALYSIS (SHOW YOUR WORK). (Remember to use the molarity of the standardized NaOH
that you determined in part 1 for the following calculations.)

1. Calculate the molarity of the unknown HCl solution using the averaged results with the
phenolphthalein.

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CH204 Experiment 5: Strong Acid/Strong Base Titration spring 2015

2. Calculate the molarity of the unknown HCl solution using the averaged results of the titration
curve.
3. Calculate the molarity of the unknown HCl solution using the averaged results of the 2nd
Derivative Plot.

Select the molar concentration of your unknown from one of your results and record below. This should be
an individual selection.

RESULTS Unknown HCl concentration

DISCUSSION (Attach written discussion to end of lab report.)


Part I
1. What were the objectives of the experiment?
2. What were your primary standard and your secondary standards in part I, what is the difference
between the two types of standards? Why was it necessary to standardize the NaOH solution?
3. Briefly describe the processes used to determine the molar concentration of your NaOH. What is
the difference between an end point and an equivalence point?
4. Were the calculated molarities of your NaOH solutions from the indicator method and Second
Derivative plot method within a reasonable range (about 15%) of each other? If not, suggest
reasons for the inaccuracy.
5. Compare the actual molarity of your determined NaOH solution with your goal of 0.500M. Which
method did you use to determine your actual molar concentration of the NaOH solution? Why?

Part II
6. What were the objectives of the experiment?
7. Briefly describe the processes used to determine the unknown molarity of your acid.
8. Were the calculated molarities of your HCl solutions from the indicator method, titration curve
and Second Derivative plot method within a reasonable range (about 15%) of each other?
9. What was the concentration of your unknown acid? Which of the methods that you used to
calculate the molarity of your unknown acid concentration did you determine to have the most
accurate results; that is, which method do you believe provided you with the true value of your
unknown acid? Why?
10. Using the indicator phenolphthalein in an acid-base titration is a common method of determining
unknown concentrations of acids in general chemistry laboratories. Based on the observations you
made during the titration with phenolphthalein and considering the results you obtained from the
indicator and the results you obtained with the pH meter, either support or oppose the use of the
indicator as an effective method of determining the concentrations of acid solutions.
11. What were some of the possible sources of error in this experiment?

Be sure to upload a copy of your discussion into SafeAssign before your next lab period.

References:
Zumdahl, S. S. Chemical Principles, 5th Edition, Houghton Miffin Company, 2005, pp. 110-115, 293-297.
Atkins, P.W.; Jones, L. L. Chemical Principles: The Quest for Insight, 3rd Edition, W. H. Freeman and
Company, 2005, pp. F71-F72, F83-F85, 415-417.

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CH204 Experiment 5: Strong Acid/Strong Base Titration spring 2015

GRAPHICAL ANALYSIS OF EQUIVALENCE POINT: TITRATION CURVE AND SECOND


DERIVATIVE. (Do not copy any of the LoggerPro analysis instructions, or graphs, into lab
notebook.)
A way of determining the precise equivalence point of the titration is to take the second derivative of the
pH-volume data. The complete instructions of how to use LoggerPro to create titration curves and second
derivative plots are given below.

Using LoggerPro to Analyze Titration Data:


Below are examples of the graphs that you will use to analyze your titration data.

Titration Curve
Open the titration data from your USB on LoggerPro. Double click on the X column and open “column
definition”. Type NaOH Volume in the “Name” field, type volume in the “short name” field and type mL
in the “unit” field. Select the column “options” button at the top and change the number of decimal places
with the “drop down menu” to two decimal places (be sure the decimal places radial button is selected,
which is located just below the drop down menu).

Repeat the same procedure for Y-column except you will type pH in the “Name” field and pH in the “short
name” field and leave the “unit” field blank.

Create Graph A in LoggerPro (Select “insert” then “graph”).

There are two methods that can be used to analyze the titration curve for part 2 in experiment 5.
1. Print the graph and hand draw a horizontal line from pH=7 to the other side of the graph. Draw a vertical
line from the top of the graph through the horizontal line and through the x-axis. The volume of NaOH
used to reach the equivalence point is at the point where the vertical line crosses the x-axis. The example
for this method is in the experimental procedure.

2. Activate the interpolate function under analysis on the tool bar. Move the vertical line in the space
between the last pH point before the large jump in pH and the first pH point after the large jump in pH
(space between the two red arrows in Graph A below). Toggle the interpolate line left or right until the
circle is at pH = 7 (or as close to pH 7 as possible). Once the circle is placed correctly, you can read the
NaOH volume used to reach the equivalence point in the stat box. The stat box in Graph A indicates that
12.682 mL were required to reach the equivalence point at pH 7.003.

Unknown [HCl] Titration with NaOH, Trial 1 (Dr. Lyon)


pH vs. volume NaOH

interpolate line

Graph A: Strong acid/strong base titration curve.

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CH204 Experiment 5: Strong Acid/Strong Base Titration spring 2015

Second Derivative Plot – One run saved.


To obtain a more precise volume of the NaOH that was used to obtain pH 7 in the strong acid/strong base
titration, we will create a second derivative graph (Graph B) in LoggerPro. After you have created the
titration curve, create the second derivative graph as instructed below.

Create a third column next to your pH and volume columns for the second derivative data as follows:
1. Select “data menu” on the tool bar at the top of the page.
2. Choose “New calculated column”.
3. Enter Second Derivative in the “Name Field”.
4. Enter 2nd derivative in the “Short Name Field”.
5. Leave blank, there are no units in the “Unit Field”.
6. Click the mouse in the “Equation Field” at the bottom
7. Click “Functions” button
8. Click “Calculus” then “secondDerivative”.
9. Click “variables” and select pH.
10. Click “Done”.
11. A third column of data will appear in the data columns.

To analyze the second derivative data, we will create the second derivative graph (Select “insert” then
“graph”). Two graphs should now be visible in your LoggerPro data page, one similar to Graph A and one
similar to Graph B.

For Graph B, select analyze then interpolate. Move line until circle is at point that crosses zero (left or right
toggle keys can be used), see red arrow below. Read printout of volume used to reach pH7, as shown below
with green arrow. The stat box in Graph B below indicates that 12.716 mL of NaOH were dispensed at the
equivalence point.

Second Derivative of Unknown [HCl] Titration Curve, Trial 1 (Dr. Lyon)


ΔpH vs. Δvol NaoH

Point where line passes


through zero on the graph
indicates the volume
dispensed to reach pH = 7.

Graph B: Second derivative of titration curve in graph A.

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CH204 Experiment 5: Strong Acid/Strong Base Titration spring 2015

Second Derivative Plot – More than one run saved.


If you have more than one run saved under a title then multiple runs (Run 1, Run 2, etc.) will appear in the
analysis columns. To analyze the different runs:
1. After creating a titration curve and the second derivative graph for Run 1, click on the graph (the
titration curve or second derivative graph for Run 1). Select “Graph Options”.
2. Select the “Axis Options” tab at the top. There will be a box labeled “Y-axis columns”.
a. Note that Run 1 is open in the Y-axis columns box. Remove the check from the Y-box and the
second Derivative box. Open Run 2 below and check the Y-box to graph the titration curve
for Run 2 and select “done”. The titration curve on the screen for Run 1 will change to the
titration curve for Run 2.
3. To graph the second derivative for Run 2, right click on the graph (either titration or second derivative
graphs on the screen) and follow steps 2 and 3 above. Check the y-box and the second derivative box
under Run 2 and the second derivative graph on the screen for Run 1 will change to Run 2.
4. You can go back and forth between Runs by right clicking in the graph area (either the titration or
second derivative graph) and removing the checks from the boxes (the y-axis and second derivative
boxes) under the Run you want to leave and checking the boxes under the Run you want to analyze.
Only check the y-box if you want to change the titration curve on the screen to the curve for the new
run. Check both the y-box and second derivative boxes if you want the change the second derivative
graph on the screen to the 2nd derivative graph for the new run.

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