Department of Chemical

Engineering

Experiment Plan
(Form CHE 3107L-1)
Laboratory Course: CHE 3107L
Experiment Title: Determination of Transference Number of Ions and Thermodynamic Analysis
of Electrolytic Cells
Group Code: CHE3107L02 Gr. 5
Students’ Name & Signature: Leyson, Aaron
Nalo, Julia
Villanueva, Marcloupe
Yaranon, Patricia
Scheduled Date: 10/17/2023
Submission Number: 1
Teacher: Engr. May V. Tampus
Term & Academic Year: 1st Semester A.Y. 2023-2024

Teacher’s Approval

This is to attest that the students have passed the pre-lab interview and are deemed prepared to conduct the experiment.

Assessed and Evaluated

By:
Engr. May V. Tampus
(Signature over printed name)
Date and Time
 Objectives of the Experiment

1. To determine the transference number of nitrate and hydronium ions

2. To describe the electrochemical reactions in the electrolysis of nitric acid
3. To determine the Gibbs energy of the electrolysis of nitric acid

Information Flow Diagram

Objective 1: To determine the transference number of nitrate and hydronium ions
Objective 2: To describe the electrochemical reactions in the electrolysis of nitric acid

Objective 3: To determine the Gibbs energy of the electrolysis of nitric acid.

Symbols Used
𝑽𝑯𝑵𝑶𝟑 Volume of HNO3 solution (mL) 𝒁𝑹 Charge number of the reaction
Initial/Final concentration of solution in Fraction of the total current carried by
𝑴𝑨𝒊 𝒕−
the anode (mol/L) anions
Initial/Final concentration of solution in Fraction of the total current carried by
𝑴𝑪𝒊 𝒕+
the cathode (mol/L) cations
Initial/Final number of electrolytes in the
𝒏𝑨𝒊 𝒕𝒆 Experimental transference number
anode (mol)
Initial/Final number of electrolytes in the
𝒏𝑪𝒊 𝒕𝒕 Theoretical transference number
cathode (mol)
Initial number of electrolytes in the
𝒏𝑨𝟏 𝑰− Current carried by anions (A)
anode (mol)
Final number of electrolytes in the Current carried by cations (A)
𝒏𝑨𝟐 𝑰+
anode (mol)
Initial number of electrolytes in the
𝒏𝑪𝟏 𝑰𝑻 Total current in the Coulometer (A)
cathode (mol)
 Final number of electrolytes in the Molar concentration of HNO3 solution
𝒏𝑪𝟐 𝑴𝑯𝑵𝑶𝟑
cathode (mol) (mol/L)
Change in the number of electrolytes in
∆𝒏𝑨 𝑸 Reaction Quotient
the anode (mol)
Change in the number of electrolytes in
∆𝒏𝑪 𝑬𝟎 Standard reduction potential (V)
the cathode (mol)
Initial mass of copper sheets in the
𝒎𝑨𝟏 𝑬 Non-standard reduction potential (V)
anode (g)
Final mass of copper sheets in the
𝒎𝑨𝟐 𝒏 Moles of electrons transferred (mol)
anode (g)
Initial mass of copper sheets in the
𝒎𝑪𝟏 𝑭 Faraday’s constant (C/mol)
cathode (g)
Final mass of copper sheets in the
𝒎𝑪𝟐 𝑹 Universal gas constant (J-mol/K)
cathode (g)
Change in the mass of copper sheets in
∆𝒎𝑨 𝑻 Temperature (K)
the anode (g)
Change in the mass of copper sheets
∆𝒎𝑪 𝒒 Total amount of electricity used (C)
in the cathode (g)
Gibbs free eq. (J)
𝑴 Molar mass of copper (g/mol) ∆𝑮
Work Plan

Time Task Person Responsible

Part 1: Preparation of Standard Solutions
Prepare 150 mL 0.1 M HNO3 standard solution Leyson
Prepare 250 mL of Sulfuric Acid Solution (0.5 M) Nalo
Prepare 250 mL 0.1 M NaOH standard solution Yaranon
Check Initial concentration of nitric acid used in the transference
1:00 – 1:30 vessel by titrating 5 mL samples with 0.1 M NaOH solution using
methyl red as an indicator.
Villanueva
Note: color change from red to yellow (Perform twice)
Part 2: Setup of Transference Vessel
Immerse the transference tube in a water-filled beaker. Make sure
that the lateral connecting tubes are not submerged in the water.
1:30 – 1:45 Fix the U-tube to support the rod. Fill the tube with HNO3. Nalo and Yaranon
Adjust the level of the electrolyte such that all three compartments
of the U-tube have the same level of solution. Mark with a
waterproof pen.
Lower the transference vessel until the marking are submerged in
the water bath.
Part 3: Copper Coulometer
Weighing of the cathode and anode of the coulometer which has
two sheets of copper.

Note: make sure it is properly labelled with its respective masses Leyson and Villanueva
Fix the copper sheets onto the electrode holder.
1:45 – 2:00 Immerse them into a 250 mL beaker filled with 0.5 M solution.
(in sulfuric acid and in CuSO4).
 Connect the coulometer with the transference vessel and
multirange meter in series.
Connect to the universal power supply with connection cables.
Part 4: Electrolysis of HNO3
Perform Electrolysis at about 50 mA. Measure temperature of bath
during reaction. Observe what happens at the cathode and the
anode regions.
Measure the exact time of electrolysis
Nearing the end of electrolysis, take 5 mL samples in the anode
and in the cathode regions of the transference vessel while the
electric field is still being applied as quickly as possible
Titrate to determine the concentration

Immediately after, interrupt the electric circuit and record the exact
length of the electrolysis period.
Washing of copper electrodes of the coulometer with water. Air
2:00 – 3:50 drying (can be hastened using blow dryer). Weighing – to All Members
determine mass change
After drying

Determine the marked volume of the cathode and anode regions

by filling them with water.

Note: Use pipette to accurately determine the volume. Consider

the fluid displacement by the immersed electrodes.

Part 5: Concluding the Experiment

Record all observed data onto sheet. Cleaning and returning of
3:55 – 4:00 apparatus. All Members

Dangers and Risks

a. Material Dangers and Risks

Copper Sulfate

- A white or off-white solid. Melting point 200°C with decomposition. Non-combustible.

▪ If ingested, induce vomiting and administer gastric lavage; give a saline cathartic, fluid therapy, and transfusions
if required; calcium disodium EDTA has been found moderately effective.
▪ If made contact with skin and eyes, wash affected tissues with water.

Source: https://cameochemicals.noaa.gov/chemical/3025

Nitric Acid
 - A pale yellow to reddish brown liquid generating red-brown fumes and having a suffocating odor. Very toxic by
inhalation. Corrosive to metals or tissue. Prolonged exposure to low concentrations or short-term exposure to high
concentrations may result in adverse health effects.
▪ When in contact with skin, immediately flush the contaminated skin with water. If this chemical penetrates the
clothing, immediately remove the clothing and flush the skin with water.
▪ If large amounts of this chemical is enhaled, move the exposed person to fresh air at once. If breathing has
stopped, perform artificial respiration. Keep the affected person warm and at rest.
▪ If accidentally taken orally, get medical attention immediately.
▪ When in contact with eyes, immediately wash the eyes with large amounts of water, occasionally lifting the lower
and upper lids

Always get medical assistance immediately.

Source: https://cameochemicals.noaa.gov/chemical/4044

Sodium Hydroxide
- A colorless liquid. More dense than water. Contact may severely irritate skin, eyes, and mucous membranes. Toxic
by ingestion. Corrosive to metals and tissue.
▪ If made contact with eyes, flush with water at once for at least 15 min.
▪ If made contact with skin, flush with water, then rinse with dilute vinegar (acetic acid)
▪ If ingested, give water and milk. Do NOT induce vomiting. Call physician at
once, even when injury seems to be slight.

Sulfuric Acid
- a colorless oily liquid. It is soluble in water with release of heat. It is corrosive to metals and tissue. It will
char wood and most other organic matter on contact, but is unlikely to cause a fire. Long term exposure
to low concentrations or short-term exposure to high concentrations can result in adverse health effects
from inhalation.

• Reaction with water is negligible unless acid strength is above 80-90% then heat from hydrolysis
is extreme, may cause severe burns [Merck, 11th ed. 1989]
• highly reactive and capable of igniting finely-divided combustible materials on contact. When
heated, it emits highly toxic fumes
• Corrosive to all body tissues. Inhalation of vapor may cause serious lung damage. Contact with
eyes may result in total loss of vision. Skin contact may produce severe necrosis
 Source: https://cameochemicals.noaa.gov/chemical/5193

b. Procedure Dangers and Risks

1. Mixing HNO3 and NaOH solution during Titration

▪ Acid may come in contact with skin, causing irritation.
Remedy: immediately wash contaminated skin with water

2. Preparing the Electrolysis Set-up

▪ The components of the set-up are mostly fragile. This may lead to breakage and cuts.
Precaution: Handle the set-up with care.

c. Equipment Dangers and Risks

1. U-Tube
It is fragile and may cause cuts when not handled properly. It can also spill the HNO3.

2. Beaker
Contains the materials and solutions. This may spill when beaker placed on a flat surface, leading to material risks and
dangers. It can also cause cuts when broken.

3. Erlenmeyer flask
▪ May result in cuts and skin scratches.
It can cause the spillage of the electrolysis mixture, irritating the skin when in contact, especially without PPE.

4. Burette
▪ A fragile apparatus.
It can also spill the NaOH solution.

5. universal power supply

contact with live parts may cause shocks and burns.

6. blow dryer
may be hot when utilized.

7. Transference Vessel
It is fragile and may cause cuts when not handled properly. It can also spill the NaOH solution.

d. Personal Protective Equipment Required

1. Laboratory Gown – provides protection from spillage and prevents contamination.

2. Safety Glasses – protects eyes from vapors, splashes from substances and impact from equipment that may
cause irritation or injury
3. Closed Shoes – protects our feet from spillage and broken glasswares.
4. Mask – prevents direct inhalation of fumes, vapors, and particles that may irritate or block respiration
5. Gloves – protects hands from direct contact with substances that may irritate or injure skin

Raw Data Tables

Sample Data Table
Part 1: Preparation of standard solutions.
Table 1. Mass needed for the preparation of standard solutions.
Mass of HNO3 (g)
Mass of sulfuric acid (g)
Mass of CuSO4 (g)
Mass of NaOH (g)

Part 2: Initial concentration check for 0.1 M NaOH standard solution.

Table 2. Readings in the determination of initial concentration for HNO 3 solution using 0.1 M NaOH solution.
Indicator used
 Color change
Initial reading (mL) Final reading (mL) Volume of Analyte
Sample No. Trial No.
(mL)
Trial 1
Sample 1 Trial 2
Trial 1
Sample 2
Trial 2

Part 4: Copper Coulometer

Table 3. Measurement of mass of copper plates at the cathode and anode before and after electrolysis of
HNO3.
Before electrolysis After electrolysis
Cathode (m1C) Anode (m1A) Cathode (m2C) Anode (m2A)
Mass of copper plates (g)

Part 5: Electrolysis of HNO3.

Table 4. Readings from the electrolysis of HNO3
Exact time of electrolysis
Time (m) Temperature (oC) Observations
10 Cathode region Anode region
20
30
40
50
60
70
University of San Carlos – Department of Chemical Engineering
CHE 3107L FORM-1-Experiment Plan

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90

Table 5. Readings in the determination of final concentration of HNO3

Indicator used
Color change
Initial reading (mL) Final reading (mL) Volume of Analyte
Sample No. Trial No.
(mL)
Trial 1
Sample 1
Trial 2
Trial 1
Sample 2
Trial 2

Table 6. Readings of the volume change in the three compartments of the U-tube.
Compartment Initial volume (mL) Final volume (mL)
Cathode
Middle
Anode

Appendix

Figure 1. Brief run through of over-all experiment proper.

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University of San Carlos – Department of Chemical Engineering
CHE 3107L FORM-1-Experiment Plan

Figure 2. Discussion on edits and finalization of the Experiment Plan.

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