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.

Types of Laboratory hot plates

a. Aluminum
 Aluminum is a great conductor of heat which makes this kind of hot plate heat
quickly and evenly.
 It is very easy to clean after cooling. However, an aluminum plate is not
recommended if any of the materials to be heated are corrosive.
 Aluminum is susceptible to corrosive materials and will degrade and rust in their
presence.
b. Ceramic
 Ceramic is very resistant to corrosion and can handle high temperatures.
 The light coloration of its surface makes viewing samples and solutions much easier
for reaction changes.
 The ceramic hot plate should be used with lots of caution as it can crack if handled
roughly or incorrectly.
c. Glass
Glass is another easy plate to observe your sample through.
It is easy to clean, resistant to corrosion, and heats effectively.
There is less heat transferred beyond the glass which may reduce the
occurrence of accidental burns if other portions of the hot plate are
touched.

Rules to observe when using a hot plate

• Do not store volatile flammable materials near a hot plate 
• Limit use of older hot plates for flammable materials. 
• Check for corrosion of thermostats. Corroded bimetallic thermostats
can be repaired or reconfigured to avoid spark hazards.
 advantages and disadvantages of using hot plates

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.

Uses of a magnetic stirrer

• Ensuring a homogenous mixing of sample prior to analysis
• Combining a variety of chemicals into a solution
• Getting solid materials to dissolve in a liquid solution
• Meeting a variable rotating speed required in a preparatory method

Types of Magnetic Stirrers

1.Multi position stirrers
2. Individual stirrers.
i. Multi Position Magnetic Stirrers
• These are used when a process requires simultaneous mixing of a large number of
solutions or reagents at once .
• The advantages of a multi position magnetic stirrer are:
• Saves space
• supports pH and temperature probes, making it perfect for buffer preparation
• It’s quiet and powerful
ii. Individual Magnetic Stirrers
• These are applied in processes that require solutions to be mixed individually.
• This could be due to limited space in a fume hood, the need to eliminate cross
contamination risks, or general safety.
• Appropriate choice should be done to ensure that a magnetic stirrer sized that is
adequate for the beaker container is chosen while mixing.
• Some models can support hugely different volumes, even from 200-10,000ml
• They are strong enough to maintain their rotation speed even when additional
reagents are needed.
Hot Plate Magnetic Stirrer
• This is a hot plate with an added bonus, it has a magnetic stirrer inside of it. The magnet can be
rotated at varying speeds which will create a magnetic field around the hot plate.
• Paired with a magnetic stir bar, the solution can be heated and mixed at the same time.
Advantages of hot plate magnetic stirrer
• It is able to simultaneously heat and mix chemicals hence the solutions can be developed quickly
and easily.
• They have easy rotational speed and temperature adjustments
• There are timer functions making it easy to track the length of time a solution is agitated
• They eliminate the need for externally stirring the solution, which saves employee time in prep
work
• It saves valuable bench space since two pieces of equipment are available in one

Disadvantages of hot plate magnetic stirrer

• They usually have a maximum capacity of around 4 Liters, hence cannot be used in mixing large
amount of solutions.
• They are more expensive to acquire as compared to the standalone hot plate or magnetic stirrer
 3. Heating mantles
 
 3. Heating mantles
• These refer to Laboratory heating devices that are commonly used for heating
round-bottomed flasks, reaction kettles and related reaction vessels.
• These mantles enclose a heating element in a series of layers of fiberglass cloth. As
long as the fiberglass coating is not worn or broken, and as long as no water or
other chemicals are spilled into the mantle, heating mantles pose no shock hazard.
• Be careful not to exceed the input voltage recommended by the mantle
manufacturer. Higher voltages will cause it to overheat, melt the fiberglass
insulation and expose the bare heating element. 
• If the heating mantle has an outer metal case that provides physical protection
against damage to the fiberglass, it is good practice to ground the outer metal case
to protect against an electric shock if the heating element inside the mantle shorts
against the metal case. 
 4. water, sand, and oil baths
Water baths
 Water heated on a hotplate, are most commonly used to heat solutions to 100°C. They may also be used to
heat to lower temperatures, although it can be difficult to maintain a constant temperature.
 Water baths can be covered with aluminum foil to prevent excessive evaporation, or to prevent excess
moisture from entering open vessels. Cold water baths can also be used to cool apparatuses in a quick
manner

Water bath Sand bath oil bath

 Sand baths
Sand baths, also heated on a hotplate, can be used to heat solutions
to a wide variety of temperatures, including very high temperatures (>
250°C ).
Sand can be placed inside Pyrex crystallizing dishes, although Pyrex
may crack if heated at too fast a rate.
Sand can also be heated to moderate temperatures inside thin
aluminum foil pie dishes, but should not be used at high temperatures
as aluminum will then oxidize, causing the thin foil to disintegrate.
Thick metal pie tins are indestructible alternatives when high
temperatures are required (but may interfere with the stirring
mechanism if used).
A vessel should be buried in a sand bath as much as possible as the
surface is often much cooler than the sand below.
 Sand baths
A vessel should be buried in a sand bath as much as possible as the surface
is often much cooler than the sand below.
A metal spatula can be used to pile the sand up to at least the height of
liquid inside the flask.
Sand takes a long time to heat up, and a long time to cool down. To save
time, a sand bath may be preheated away from the volatile organic liquids
while apparatus are being assembled.
The flask can be partially lifted out of the sand, or the sand moved with a
metal spatula away from contact with the liquid if the sand overheats and
causes a liquid to boil uncontrollably.
Sand will remain warm even after turning off the hotplate, and therefore
flasks have to be lifted out of the sand bath in order to cool.
Oil baths
Oil baths are much like water baths, but use silicone or mineral oils in order
to enable temperatures become hotter than the boiling point of water (>
100°C ). Silicone oil baths can be heated to 250°C , while mineral oil baths
can be heated to 300°C .
Mineral oil is composed of mixtures of long-chain alkanes, and so is
combustible. Direct contact with open flames should therefore be avoided.
Oil baths can be heated in a Pyrex crystallizing dish on top of a hotplate. It is
also quite common for the oil to be electrically heated, through immersion
of a coiled wire connected to a "Variac" (light blue piece of equipment).
A Variac connects to the outlet and can deliver variable voltage through the
wire.
A paper clip can also be used in an oil bath and stirred with a stirring plate in
order to dissipate heat. This allows for the temperature of an oil bath to
quickly respond to adjustments up or down.
 5. Muffle furnaces
• Muffle furnaces are capable of reaching temperatures upto 1800°C,
and should be housed in separate rooms away from inflammable or
combustible materials.
• Ordinary glassware should never be put inside and heat resistant
crucibles should be removed with suitable tongs and handled wearing
heatproof mittens
Laboratory stirring, mixing and apparatus

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).