Chemical Engineering Lab

Pre-Lab
The Kinetics of the Saponification of Ethyl Acetate in Sodium Hydroxide
Aubrey Luttrell
Dolce Lawless
Godson Adejumo

Description: The main objective of this experiment is to investigate the kinetics of the
reaction between Sodium Hydroxide and Ethyl Acetate at different temperatures.

For each temperature, the progress of the reaction will be tracked by specific conductivity
measurements that yield reaction rate constants. The calculation of reaction rate constants
will in turn allow calculations of activations energies and entropies of activation.
Important Information:
Compound

Molecular Weight
Molarity to be
(grams/mole)
Used (mole/liter)

Density at Room
Temperature
(grams/milliliter)

Boiling
Point (C)

Ethyl
Acetate

88.106

0.1

0.897

77.1C

Sodium
Hydroxide

39.997

0.1

2.13

1,388C

Equipment Needed:
Materials: Ethyl Acetate and Sodium Hydroxide are the materials to be used to
investigate the rate law of a chemical saponification reaction.
Laboratory: Volume measuring and holding will be needed to quantify and contain the
Ethyl Acetate and Sodium Hydroxide solutions. Laboratory coats, goggles, and gloves
will be needed for safety precautions.
Armfield CEM-MKII CSTR: The information to follow is provided by the manufacturers
of the Armfield CEM-MKII CSTR. The reactor vessel is set on a baseplate which is
designed to be located on the four studs of the CEX service unit and then secured by
thumb-nuts. The reactor is supported by three pillars; position the reactor on the CEX
service unit such that a single pillar is to the front.

A stainless steel coil inside the reactor provides the heat transfer surface for either
heating or coiling the chemical reactants. The coil is connected either to the hot water
circulator or the CW-16 chiller. The coil inlet is at the front of the reactor and the coil
return is at the rear of the reactor.
A turbine agitator works in conjunction with a baffle arrangement to provide efficient
mixing and heat transfer. The agitator is driven by an electric motor mounted on the lid of
the reactor. The motor is driven by a variable speed unit mounted in the front of the
service unit. The socket for the motor electrical plug is sited at the rear of the service
unit.
Glands in the reactor lid house the conductivity and temperature sensors provided with
the service unit. The larger of the two glands is for the conductivity probe. The glands are
unscrewed by hand, the probes inserted completely into the reactor until they rest on the
reactor base and then the glands re-tightened by hand. Sockets in the side of the console
on the service unit are provided to connect each probe. These are of different size so that
the probes cannot be wrongly connected.
Chemical reagents are pumped from the two feed tanks into the reactor separately
through connectors in the base of the reactor. The two feed pumps of the service unit are
connected to these. As reagents are pumped into the reactor, the level increases until it
finally overflows the stand pipe and flows to drain. The stand pipe may be adjusted in
height by loosening the hexagonal backing nut. A mark is etched onto the stand pipe. For
maximum operating volume of the reactor, this mark should be aligned with the backing
nut. A stop prevents the stand pipe from being completely removed, and this also defines
the minimum working volume which is half the maximum volume.
When the reactor is not being used, it can be drained using the valve sited on the
underside of the reactor.

Procedure: The laboratory experiment will begin with the calibration of the feed pump.
In order to calibrate the feed pump, Feed Tank A MK11 Reactor will be filled with water
to about 90% of its volume, the peristaltic pump will be turned on, and the discharge tube
of the tank will be detached from the reactor. The speed dial for pump A will be set to the
11-mark, which is the maximum speed, and the water will be allowed to flow into the
MK11 reactor tank. After the water is allowed to equilibrate, the times to collect about 20
mL will be noted and the average discharge rate and dial setting will be determined. As
soon as everything above is repeated at different dial settings, the entire process will be
repeated for tank B and feed pump B. After the calibration is completed, the calibration
curve for the pumps will be plotted. The second part of the experiment consists of the
actual steady state reaction in the CSTR reactor. In preparation, about 4 L of 0.1 M
NaOH and 0.1 M Ethyl Acetate solutions will be created. After this preparation, tank A
will be filled with the NaOH solution and tank B will be filled the Ethyl Acetate solution
to a level approximately 50 mL from the top and the lids will be refit. After determining
the discharge rate for pump B, the calibration curve will be used to set the discharge rate
for pump A equal to that of pump B. Then, the set point of the temperature controlled
will be adjusted to 20C and the temperature will be manually monitored to avoid the
waters overheating. The conductivity of the NaOH, ethyl acetate, and water will be
determined and this collection of conductivity data will be until a steady state condition is
reached in the reactor. This reaching of a steady state condition will take approximately
30 minutes but data will be collected for a period of 45 minutes. Then, the agitator speed
controlled will be set to 50%, based on minimum and maximum agitator speed values.
The calibrated speed pumps and stirrer will be switched on and when the reaction mixture
reaches the temperature and conductivity probes, the hot water circulation will be started.
The temperature and conductivity readings will be recorded at least once every minute
until the reaction reaches equilibrium and the flow reaches steady state (mixture reaches

the overflow tube). The conductivity of the reaction mixture will be determined and
recorded 24-hrs after the reaction. This procedure will be repeated for temperatures of
30C, 40C, and 50C and the results will be recorded. Steps 1-7 will be repeated with
pump Bs discharge rate set to 3 times that of pump A.
Data Needed: The calibration requires the recording of dial settings and discharge rates
for each tank or pump. The CSTR reaction requires the recording of the conductivity of
the content of the reactor over the period of the reaction at different temperatures.
Analysis: The conductivities of the sodium hydroxide and the sodium acetate over the
period of the reaction can be translated into concentrations and into degrees of
conversion. An overall mass balance at steady state and constant volume for each
temperature will allow the calculation of the specific rate constants for each temperature.
The relationship between temperature, reaction rate, and conversion will be noted. The
Arrhenius equation can be used to calculate the frequency factor and the activation
energies. The data will also be used to determine the rate law for the reaction.
Safety: The following information concerning the chemical safety of ethyl acetate and
sodium hydroxide is provided by their respective Material Safety Data Sheets.
Chemical Safety: is hazardous in the case of ingestion and inhalation. Ethyl Acetate is
slightly hazardous in the case of skin contact (irritant, permeator) and of eye contact
(irritant). Sodium hydroxide is very hazardous in case of skin contact (corrosive, irritant,
permeator), of eye contact (irritant, corrosive), of ingestion, of inhalation. The amount of
tissue damage depends on length of contact. Eye contact can result in corneal damage or
blindness. Skin contact can produce inflammation and blistering. Inhalation of dust will
produce irritation to gastro-intestinal or respiratory tract, characterized by burning,
sneezing and coughing. Severe over-exposure can produce lung damage, choking,
unconsciousness or death. Inflammation of the eye is characterized by redness, watering,
and itching. Skin inflammation is characterized by itching, scaling, reddening, or,
occasionally, blistering.
In case of eye contact, check for and remove any contact lenses. Immediately flush eyes
with plenty of water for at least 15 minutes. Cold water may be used. Get medical
attention immediately. In case of skin contact, immediately flush skin with plenty of
water for at least 15 minutes while removing contaminated clothing and shoes. Cover the
irritated skin with an emollient. Cold water may be used. Wash clothing before reuse.
Thoroughly clean shoes before reuse. Get medical attention immediately. In case of
serious skin contact, wash with a disinfectant soap and cover the contaminated skin with
an anti-bacterial cream. Seek medical attention. If inhaled, remove to fresh air. If not
breathing, give artificial respiration. If breathing is difficult, give oxygen. Get medical
attention immediately. In case of serious inhalation, evacuate the victim to a safe area as
soon as possible. Loosen tight clothing such as a collar, tie, belt or waistband. If
breathing is difficult, administer oxygen. If the victim is not breathing, perform mouth-tomouth resuscitation. It may be hazardous to the person providing aid to give mouth-tomouth resuscitation when the inhaled material is toxic, infectious or corrosive. Seek
immediate medical attention. If ingested, do NOT induce vomiting unless directed to do

so by medical personnel. Never give anything by mouth to an unconscious person. If

large quantities of this material are swallowed, call a physician immediately. Loosen tight
clothing such as a collar, tie, belt or waistband.
Protective Equipment
Lab coat
Gloves
goggles
long pants
long shirt
closed-toed shoes
The following information concerning waterborne hazards, electrical safety, and hot
surfaces and liquids is provided by the creators of the Armfield CEM-MKII CSTR online
user manual.
Waterborne Hazards: Armfield CEM-MKII CSTR involves the use of water which
under certain conditions can create a health hazard due to infection by harmful microorganisms. Any water contained within the product must not be allowed to stagnate, ie.
the water must be changed regularly. Any rust, sludge, scale or algae on which microorganisms can feed must be removed regularly, i.e. the equipment must be cleaned
regularly. Where practicable the water should be maintained at a temperature below
20C or above 45C. If this is not practicable then the water should be disinfected if it is
safe and appropriate to do so. Note that other hazards may exist in the handling of
biocides used to disinfect the water.
Electrical Safety: Armfield CEM-MKII CSTR operates from a mains voltage electrical
supply. It must be connected to a supply of the same frequency and voltage as marked on
the equipment or the mains lead. If in doubt, consult a qualified electrician or contact
Armfield. The equipment must not be operated with any of the panels removed.
Hot Surfaces and Liquids: Armfield CEM-MKII CSTR incorporates a pumped electric
water heater, and is capable of producing temperatures that could cause skin burns.
Before disconnecting any of the pipes or tubing:
- Stop all the pumps.
- Leave time for the water to cool
- Check that the temperature is at a safe level
Do not touch any surfaces close to Hot Surfaces warning labels, or any of the
interconnecting tubing, whilst the equipment is in use.
Group Assignments:
Aubrey: Data collection
Dolce: Creating Solutions
Godson: Analyzing Data