University of San Carlos – Department of Chemical Engineering

CHE 3107L FORM-1-Experiment Plan

Department of Chemical
Engineering

Laboratory Course
Experiment Title
Group Code
Students’ Name & Signature :
Scheduled Date
Submission Number
Teacher
Term & Academic Year
Experiment Plan
(Form CHE 3107L-1)
: CHE 3107L
: Determination of Transference Number of Ions and Thermodynamic Analysis
of Electrolytic Cells
: CHE3107L02 Gr. 4
Festejo, John Fritz
Mayormita, Jun Paul
Traya, Kristian Joseph
: September 27, 2022
: 1
: Engr. May V. Tampus
: 1st Semester A.Y. 2022-2023

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 Month/Day/Year Time

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

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

Figure 1. Electrolysis of nitric acid flow diagram and determination of transference number

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CHE 3107L FORM-1-Experiment Plan

Objective 2. To describe the electrochemical reactions in the electrolysis of nitric acid

Figure 2. Electrochemical reactions in the electrolysis of nitric acid

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

Figure 3. Determination of the Gibbs energy of the electrolysis of nitric acid

Symbols Used
Initial mass of copper sheet in the
VNaOH Amount of drops of NaOH (ml) miA/C
Anode or Cathode
xNaOH Concentration of NaOH Sol’n (0.1M) Final mass of copper sheet in the
mfA/C
VHNO3 Volume of HNO3 sample sol’n (5 ml) Anode or Cathode
Change in mass of copper sheet in the
xHNO3 Concentration of HNO3 Sol’n (M) mA/C
Anode or Cathode
Concentration of HNO3 in Anode
xHNO3A M Molar mass of Cu (63.546 g/mol)
Compartment (M)
Concentration of HNO3 in Cathode
xHNO3C Zr Reaction charge number (2)
Compartment (M)

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CHE 3107L FORM-1-Experiment Plan

initial moles of HNO3 sol’n in Anode or

niA/C
Cathode compartment (mol)
t_ Transference number of anion
A/C final moles of HNO3 sol’n in Anode or
n f
Cathode compartment (mol)
Change in moles of HNO3 sol’n in
nA/C t+ Transference number of cation
Anode or Cathode compartment (mol)
Eocell Standard cell potential (V) n Charge number (2)
Standard half cell potential of reduction
Eored F Faraday's Constant (96,485 J/V*mol*e-
reaction (V)
Standard half cell potential of oxidation
Eoox ΔGo Gibbs Energy of reaction
reaction (V)

Work Plan

Time Task Person Responsible

Part 1: Preparation of Solution
Clean and prepare the needed materials for the experimentation
Prepare 150 mL 0.1 M HNO3 standard solution Everyone
Prepare 250 mL of sulfuric acid/ CuSO4 solution (0.5M with
respect to each species)
1:00 - 1:30
Prepare 250 mL 0.1 M NaOH standard solution.
Titrate 5 mL samples with 0.1 M NaOH standard solution using
methyl red as an indicator to be able to check the initial
concentration of the nitric acid used in the transference vessel.
Part 2: Preparation of Transference Vessel
Immerse the transference tube (double U-tube with frits and cock)
in a water-filled beaker or container. Make sure that the lateral
connecting tubes are not submerged in the water. The water bath
serves as a temperature-controlling bath.
Fix the U-tube to the support rod. Fill the tube with HNO3.
1:30 - 1:45 Everyone
After hanging the carbon electrodes, adjust the level of the
electrolyte such that all three compartments of the U-tube have the
same level of solution.
Lower the transference vessel until the markings are submerged in
the water bath.
Part 3: Preparation of Copper Coulometer
Weigh the cathode and anode of the coulometer which consists of
two sheets of copper. Make sure they are properly labeled for easy
identification later and also Record their masses.
Fix the copper sheets onto the electrode holder and immerse them
1:45 - 2:00 Everyone
into a 250 mL beaker filled with 0.5 M solution (in sulfuric acid and
in CuSO4).
Connect this coulometer with the transference vessel and multi
range meter in series

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CHE 3107L FORM-1-Experiment Plan

Connect the coulometer to the universal power supply with the

connection cables
Part 4: Electrolysis of HNO3
Perform the electrolysis for 90 minutes at about 50mA ensuring
that the current intensity is nearly constant during the reaction.
Measure the temperature of this bath during reaction.
Measure the exact time of electrolysis using a stopwatch while
observing what happens at the cathode and the anode regions.
2:00 - 3:30 Near the end of the electrolysis period, take 5 mL samples in the Everyone
anode and in the cathode regions of the transference vessel while
the electric field is still being applied as quickly as possible.
Titrate the samples taken to obtain their concentrations.
After the taking of the samples, interrupt the electric circuit and
record the exact length of the electrolysis period.
Part 5: Post-Experimentation
Carefully wash the copper electrodes of the coulometer with water,
dry them in air and weigh them to determine the mass change.
Determine the marked volume of the cathode and anode regions
3:30 - 4:00 Everyone
by filling them with water.
Use a pipette to accurately determine the volume. While doing this,
consider the fluid displacement by the immersed electrodes.

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

Dangers and Risks

a. Materials Dangers and Risks

i. Copper (II) Sulfate
- Causes skin and eye irritation
- Harmful if swallowed and causes indigestion, nausea and
vomiting.
- May cause liver and kidney damage
- Rinse immediately with water. If it gets worse, seek medical help.
ii. Sodium Hydroxide
- Causes skin and eye irritation
- Can cause severe damage to digestive tract
- Irritation may lead to pneumonitis and respiratory disease
- Rinse with water immediately and consult a doctor right away.

iii. Sulfuric Acid

- Causes skin and eye irritation
- Can cause burning in the nose and throat
- Rinse immediately with soap and water and if gets worse, consult
medical help

iv. Phenolphthalein
- Causes eye and skin irritation
- May cause kidney injury
- Can cause nausea and vomiting
- Handle with care and rinse water immediately

v. Potassium Hydrogen Phthalate (KHP)

- Causes eye and skin irritation
- Can cause vomiting and respiratory tract irritation
- Rinse with water immediately
vi. Nitric Acid
- Cause severe eye and skin irritation
- Must be extremely handle with care
- Causes severe permanent damage in the digestive tract
- Handle with care and read the instructions properly
- Wash with water, avoid touching if exposed
vii. Methyl Red Indicator
- Causes skin and eye irritation
- Can cause vomiting and nausea
- Handle with care and rinse water immediately

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

viii. Copper Strip

- causes skin and eye irritation
- Can damage the throat, causes headache, cough and nausea
- may cause metallic fume fever
- rinse with water and must seek medical help when in contact

b. Equipment Dangers and Risks

i. Copper Coulometer
- This is a fragile sort of glassware that should be handled
with utmost attention since it contains copper, which is
an inflammatory and poisonous substance. It might be
hazardous if the glass breaks and the copper is not
carefully cleaned up.
- Carefully place power cords so they don’t come in contact with
water or chemicals. Contact with water is a shock hazard.
Corrosives and solvents can degrade the cord insulation.
ii. Multi-range Meter
- Voltage transients or voltage spikes are a common risk in handling
this equipment. Occasionally the voltage on a 480-volt system can
find itself all the way up to 8000-10,000 volts. Lighting strikes on
outdoor transmission lines is also a highly probable cause for a
voltage transient. It is important to make sure you have purchased
a digital multimeter with the proper category rating for the work
you are performing.
- A common error made during voltage measurements is leaving
the meter on the ohms setting. Some older style meters cannot
handle the voltage when set to ohms. This can lead to the meter
sparking or worst case blowing up.
- While taking readings the user is most likely going to need the use
of both hands to complete the task. As a result it is necessary to
be sure the meter is set securely in a safe place where it can be
read without having to change the user’s position.
- If no suitable spot is available, a second person to hold the meter
and/or record the readings may be necessary. Some meters also
can be equipped with magnetic straps or tethers to aid in their use
by a single technician.
iii. Beaker and Pipette
- Breakable if not handled properly
- Handle with care
iv. Connecting Tubes
- This is a long, thin wire that, if not handled properly, may
be harmful. To avoid mishaps such as tripping, make

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

sure it is set and maintained in the laboratory table

without flying cables that reach down to the table. To
avoid mishaps, inspect the cable before usage.

c. Procedure Dangers and Risks

i. Preparation of 0.5M H2SO4 / CuSO4 solution
- Causes severe eye burns. May be harmful if inhaled. Material is
extremely destructive to the tissue of the mucous membranes and
upper respiratory tract. May be harmful if absorbed through the
skin and it causes skin burns. May also be harmful if swallowed.
- Wear chemical safety glasses or goggles, and a face shield.
Provide local exhaust, preferably mechanical. If exposure levels
are excessive, use an approved respirator. Wear nitrile or rubber
gloves, and a full body suit.

ii. Preparation of 0.1M NaOH standard solution

- Contact with water causes violent frothing and spattering. Reacts
with metals to produce highly flammable hydrogen gas. Closed
containers may rupture violently when heated, releasing contents.
Toxic sodium oxide fumes can be generated at high temperatures.
- Before handling, it is important that all engineering controls are
operating and that protective equipment requirements and
personal hygiene measures are being followed.
- Avoid generating vapours or mists. Avoid generating dust. Use
corrosion-resistant tools and equipment.
- Never add water to a corrosive. Always add corrosives slowly to
cold water.
- Never reuse empty containers, even if they appear to be clean.
Keep containers tightly closed when not in use or empty.
iii. Preparation of 0.1M HNO3 standard solution
- It produces exothermic reactions, as well as toxic, corrosive, and
flammable vapors. Nitric acid can be extremely hazardous in cases of
inhalation (lung corrosive), skin contact (corrosive, irritant, permeator), eye
contact (corrosive), or ingestion.
- Nitric acid reacts violently with alcohols, alkalis, reducing agents,
combustible materials, organic materials, metals, acids, cyanides,
terpenes, charcoal, and acetone.
- Proper waste segregation can help avoid laboratory accidents and
explosions. Do not mix nitric acid waste with any other waste streams,
including other inorganic acids.
- Avoid contact with metals. Nitric acid is extremely corrosive in the
presence of aluminum, copper, and oxides and attacks all base metals.

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

Raw Data Tables

Table 1. Mass of Anode and Cathode Copper Sheets

Before Electrolysis After Electrolysis

Anode Cathode Anode Cathode

Mass of Copper
sheets

Table 2. HNO3 Titration

Color of solution
Volume sample Volume of 0.1 M NaOH Added
before after

Trial 1
HNO3
Trial 2

Table 3. HNO3 Concentration

Initial Concentration Final Concentration
(Before Electrolysis) (Near the end of Electrolysis)

Anode Cathode Anode Cathode

HNO3
Concentration
(mol/L)

Table 4. Other recorded values

Electrolysis Duration (mins) Temperature During Reaction Current Intensity (mA)
(oC)

Table 5. General Observations

Electrolysis Duration (mins) Transference Vessel Copper Coulometer

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

Appendix

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

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