Experiment 1

Checking pH Electrode Functionality

Aim: Verification of glass electrode equation.

Outcomes: After completing this experiment, the student should be able to:
1. Explain the fundamental principal behind potentiometric analysis.
2. Construct titration curves for the titration process.
3. Prepare buffer solution.
4. Understand how glass electrode operates.

Requirements:
Materials and Equipment Chemicals
 Combination glass electrode  H3PO4
 pH-meter  CH3COOH
 Magnetic stirrer  H3BO3
 Stir bar  NaOH
 Glass or plastic bottles-50 mL (150
bottles)
 Erlenmeyer flasks and beakers

Theoretical background:
There are many different industries that rely on the use of a pH meter to make
decisions about a process. Calibration is an important function that must be done
routinely to standardize the electrode in face of its ever-changing characteristic. That is,
when the meter is calibrated, it is done to compensate for the changes that have taken
place to the electrode since the previous calibration.
There are many influences, including aging, temperature, coatings, and chemicals
used, that will affect the probe characteristic. So, the question becomes, what is typical
and how do you check it?
A pH meter is a very sensitive voltmeter. When a pH probe is placed into a
solution, an mV potential is generated in response to the hydrogen ion concentration
[H+]. The theoretical voltage generated can be determined by the Nernst-equation.
Theoretically, at 25oC, a pH 7.0 solution will generate 0 mV and there will be a 59.16 mV

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change for each pH unit. So, at pH 4.0, +177.48 mV will be generated while at pH 10.0,
with a lower H+ concentration relative to pH 7.0, a potential of -177.48 mV will be
generated. Again, this is theoretical and does not represent the real-world behavior. In
fact, a new pH electrode will generate between +/- 10 mV in pH 7.0 and will have a slope
percentage between 95 and 105%. The slope percentage is determined by dividing the
actual voltage generated by the theoretical and then multiplied by 100.

Procedure:
Preparation of stock solutions:
 2000 mL solution of approximately 0.04 M [H3PO4+ CH3COOH+ H3BO3]
 2000 mL 0.2 M NaOH

Part-I Preparation of buffer solutions:

 A mixture of 0.04 M [H3PO4+ CH3COOH+ H3BO3] is prepared.
 To obtain a buffer solution of the required pH value, the given amount of 0.2 M
NaOH solution is poured into 100 mL of the mixture above.

NaOH, 0.2 pH NaOH, 0.2 pH

M mL M mL
0 1.81 62.5 8.36
7.5 2.09 72.5 9.37
20 3.29 80.0 10.38
25 4.1
35 5.02
42.5 6.09
52.5 7.00

Standardization of pH meters:

1. Solutions containing standard pH 4.0 and pH 7.0 buffers will be supplied

in plastic bottles with magnetic stirrers.
2. Immerse the clean pH electrode in the pH 7.0 buffer, stir for about a
minute until the readings stabilize and adjust the calibration knob until the
meter reads 7.0.
1. Repeat the procedure with the 4.0 buffer and adjust the slope or temperature
compensation knob until the meter reads 4.0.
2. Re-measure the 7.0 buffer to ensure that it still reads 7.0.

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3. Repeat the procedure until both buffers read correctly or consult the instructor.

Verifying the glass electrode equation:

1. Transfer exactly 25 mL of each buffer prepared from the above into a 50-mL
beaker.
2. Place a stir bar into the beaker and immerse the glass electrode (note: make sure
that the reference is fully immersed, and the solution is well stirred).
3. Record the pH value on the meter once the pH is stabilized (check the value
measured with the readings in the table above).
4. Switch the knop to measure the corresponding mV value for each buffer.
5. Record the pH value on the axis versus the mV value on the y-axis for all buffer
solutions.
6. Calculate the slope and write down the equation of the glass electrode.

Pre-lab questions:
1- What is the main concept of galvanic cells?
2- What is the electrode potential?
3- How the glass electrode operates?
Post-lab questions:
4. What is the potential of a hydrogen electrode at pH = 10?
5. When a glass electrode was immersed in 0.1 mM HCl, a potential of
+177.48 mV mV (versus SCE) was recorded. What is the potential if the
electrode were immersed in a solution at pH 10.00?

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 Experiment 1

Laboratory Data Sheet

Name: Number: Mark:

Mistakes

PH MV

The calculated slope =……………………………

The Slope Percentage = Calculated slope / Theoretical slope x 100

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 Experiment 2
Potentiometric titrations using glass electrode

Aim: Verification of glass electrode equation.

Outcomes: After completing this experiment, the student should be able to:
1. To perform a potentiometric titration of an acidic solution of known molarity.
2. To graph the volume of base added vs the pH and to determine the equivalence
point.
3. To calculate the molarity of the basic
solution.

Requirements:

Materials and Equipment Chemicals

 Combination glass electrode  HCl (0.1 M) 4 Liter

 pH-meter  Na2CO3 (0.1 M) 1 Liter

 Magnetic stirrer  NaOH (0.1 M) 1 Liter

 Stir bar

 Glass burette

 Erlenmeyer flasks and beakers

Theoretical background:
In an acid-base titration, the important information to obtain is the equivalence
point. If there are a given number of moles of acid in the titration flask, the equivalence
point is reached when that same number of moles of base has been added from the
burette. The molarity of the base can then be calculated since the number of moles of
base added is the same as the number of moles of acid in the flask, and the volume of the
base added is also known. Similarly, if the number of moles of acid in the titration flask
is unknown, it can be calculated for the equivalence point if the molarity of the base and
the volume of base added are known.

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 Often the pH of the solution will change dramatically at the equivalence point.
An acid-base indicator works by changing color over a given pH range. If an indicator
which changes color near the equivalence point is chosen, there is also a dramatic change
in the color of the indicator at the equivalence point because the pH changes so rapidly.
In a potentiometric acid-base titration, an indicator is not necessary. A pH meter
is used to measure the pH as base is added in small increments (called aliquots) to an acid
solution. A graph is then made with pH along the vertical axis and volume of base added
along the horizontal axis. From this graph the equivalence point can be determined and
the molarity of the base calculated.

Procedure:
Part I- Standardization of HCl using Na2CO3
1. Transfer exactly 30 mL of Na2CO3 into 50 ml beaker.
2. Immerse the glass electrode into the solution and place a stir bar into the beaker>
3. Record the pH reading of the pH meter.
4. Titrate Na2CO3 solution with HCl and record the pH change after each addition
(also record the mV change). (Note: two inflection breaks will be observed in this
titration, and you need to add small increments around each end point).
5. Tabulate your data and plot a graph of the first derivative (plot ∆pH/∆volume
versus volume).
6. From the end point of the titration and the concentration of Na2CO3, calculate the
concentration of HCl.
Part II- Potentiometric titration of NaOH with HCl
1. Obtain about 100 mL of 0.1 M HCl in a clean, dry beaker. This beaker should be
labeled. Never pour any solution back into this beaker.
2. Rinse your burette with distilled water. Then use a small amount of the 0.l M HCl
solution to rinse the burette.
3. Fill the burette to some point higher than the markings with the HCl solution and
then carefully let the HCl solution out into a waste container until the bottom of
the meniscus is on the 0.00 line.
4. Place a 100 mL beaker under the burette containing 50 ml of 0.1 M NaOH.
5. Carefully drop a magnetic stirring bar into the beaker containing the NaOH
solution. Set the beaker on the magnetic stirring motor and position the burette
containing the HCl solution and the pH electrode.
6. Carefully turn on the stirring motor and make sure that the stirring bar does not hit
the electrode. Adjust the stirring speed as directed by your teacher.
7. Measure and record the pH of the solution before any HCl has been added.

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 8. Add 2.0 mL of HCl solution carefully from the burette. Record the pH when it has
stabilized. Add another 1.0 mL of HCl and record the pH. Continue adding HCl
in 2.0 mL increments until you have obtained a pH reading less than 2.
9. Remove the pH electrode from the solution, rinse it with distilled water, and store
it as directed by your teacher.
10. The solutions may be discarded down the sink. Rinse the burets with distilled
water and place it upside down in the burette holder to drain.

Pre-lab questions:
4- What is the main concept of galvanic cells?
5- What is the electrode potential?
6- How the glass electrode operates?

Post-lab questions:
a. What is the potential of a hydrogen electrode at pH = 10?
b. When a glass electrode was immersed in 0.1 mM HCl, a potential of +177.48
mV mV (versus SCE) was recorded. What is the potential if the electrode were
immersed in a solution at pH 10.00?

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 Experiment 2

Laboratory Data Sheet

Name: Number: Mark:

Part I
VOLUME PH
ADDED

The molarity of HCl =………………mol/L.

Part II
VOLUME PH
ADDED

The molarity of NaOH =………………mol/L.

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