Heating in The Laboratory
Heating in The Laboratory
Introduction
Heating is an essential requirement in laboratories for carrying out common
operations such as:
i. Purification of solvents by distillation
ii. Extractions using rotary evaporators
iii. Studies on kinetics of chemical reactions
iv. Determination of physical parameters such as boiling point, melting point,
flashpoint, etc
v. Sample digestions
vi. Drying of cleaned glassware for subsequent use
vii. Drying of precipitates or determinations of loss on drying
The selection of a device depends on the application in hand.
Heating exposes one to burns and boils resulting from contact with
hot surfaces, boiling liquids, vapours or flames.
Contact hazards generally affect the user only but fires and explosions
can cause injuries to others in addition to widespread damage.
LABORATORY HEATING DEVICES
• Most labs use at least one type of heating device, such as ovens, hot plates,
heating mantles and tapes, oil baths, salt baths, sand baths, air baths, hot-
tube furnaces, hot-air guns and microwave ovens.
• Steam-heated devices are generally preferred whenever temperatures of
100o C or less are required because they do not present shock or spark risks
and can be left unattended with assurance that their temperature will
never exceed 100o C.
• Ensure the supply of water for steam generation is sufficient prior to
leaving the reaction for any extended period of time.
General Precautions
The following precautions need to be considered while using heating devices in the
Laboratory:
• The actual heating element in any laboratory heating device should be enclosed in
such a way as to prevent a laboratory worker or any metallic conductor from
accidentally touching the wire carrying the electric current.
• Repair a worn out or damaged heating device before it is used again or discard of the
device.
• Use a variable autotransformer on a laboratory heating device to control the input
voltage by supplying some fraction of the total line voltage, typically 110 V.
• Locate the external cases of all variable autotransformers where water and other
chemicals cannot be spilled onto them and where they will not be exposed to
flammable liquids or vapors.
NOTE:
Fail-safe devices can prevent fires or explosions that may arise if the
temperature of a reaction increases significantly because of a change
in line voltage, the accidental loss of reaction solvent or loss of
cooling.
Some devices will turn off the electric power if the temperature of
the heating device exceeds some preset limit or if the flow of cooling
water through a condenser is stopped owing to the loss of water
pressure or loosening of the water supply hose to a condenser.
Examples of Laboratory heating devices
Drying ovens can be used in laboratory or industrial
1. Ovens settings for a variety of tasks such as evaporation,
drying of laboratory glassware, sterilization,
temperature testing, and for incubating temperature
sensitive experiments.
Drying is a delicate process as drying too fast, too
slow, or unevenly can ruin an otherwise perfect
process.
Types of ovens
A basic double wall utility drying oven is not
much different from the oven that is used in home
kitchens.
Gravity convection or forced air convection
drying ovens provide a greater degree of evenness,
control of temperature, rapid drying capabilities, and
most models are programmable.
Drying ovens with a maximum temperature of
250°°C, 300°C and 350°C are available.
Drying ovens are available in a wide range of sizes,
from a small bench top drying oven to a room-sized,
walk-in drying oven.
• Laboratory ovens are constructed such that their heating elements and
their temperature controls are physically separated from their interior
atmospheres.
• Laboratory ovens rarely have a provision for preventing the discharge of
the substances volatilized in them. Connecting the oven vent directly to
an exhaust system can reduce the possibility of substances escaping into
the lab or an explosive concentration developing within the oven.
• Do not use ovens to dry any chemical sample that might pose a hazard
because of acute or chronic toxicity unless special precautions have been
taken to ensure continuous venting of the atmosphere inside the oven.
• Always rinse glassware with distilled water after rinsing with organic
solvents before being dried in an oven to avoid explosion.
• Do not dry glassware containing organic compounds in an unvented oven.
2. Hot Plates
Hot plates and magnetic stirrers are critical components in almost any laboratory as
they assist in the basic heating and mixing of chemicals or samples. Hot plates are
used in a laboratory as a heat source that can uniformly heat solutions and materials.
They are considered much safer than traditional Bunsen burners because there is no
open flame involved, just a heated plate.
Advantages
• Hot plates are very cost effective
• They are extremely easy to use
• They support a variety of essential laboratory procedures
• Hot plates are easily portable
Disadvantages
• Safety is important when working with a hot plate, so they must be kept in a secure location
away from flammable materials
• Additional gloves or tongs must be purchased to remove heated materials from the hot plate
to avoid burns
• The appropriate plate material and temperature range must be purchased or the longevity of
the hot plate may be compromised
Magnetic Stirrers
• A magnetic stirrer is an essential piece of equipment for most
laboratories. Certain procedures require a solution to be agitated in order
for it to be effectively dissolved.
1. Stirring motors
2. Magnetic stirrers
3. Shakers
4. Small pumps for fluids
5. Rotary evaporators for solvent removal
ASSIGMENT:
1. Describe how the above laboratory stirring, and mixing devices work,
outline the advantages and disadvantages of each device.
2.
a) Define sample digestion.
b) Describe the applications of microwave assisted, and wet digestion
methods as used in Analytical Chemistry
c) Describe the following sample digestion techniques, siting the
advantages and disadvantages of each technique.
i. Microwave assisted digestion
ii. Open system digestion
iii. Closed system digestion
d) Describe the digestion technique that is applied while preparing
sample for determination of lead in soil samples using atomic
absorption spectroscopy (AAS).