ANALYTICAL CHEMISTRY

(Storage and handling of

Chemicals)
Dr.S.SURESH
Assistant Professor
Email:avitsureshindia@gm
ail.com

Storage and handling of chemicals

The following rules should be strictly observed
in storing and handling of chemicals.
After using a chemical, the container should be
tightly closed and returned to its original place.
Care should be taken to see if all the containers
have the appropriate labels stuck to them. No
bottle should be left unlabelled.
Corrosive chemicals should be stored in
corrosion-resistant chambers.
Some chemicals especially concentrated acids,
produce lot of fumes on exposing to the
atmosphere and therefore it is advisable to
handle these inside a fume-hood.

Storage and handling of chemicals

Flammable solvents like benzene, alcohol,
ether and carbon disulphide should never
be handled without turning off burners,
heaters, etc.
Some of the organic solvents like ether,
because of their high volatility, build-up a
pressure in the containers. Such containers
should be cooled in ice and then opened.
Flammable liquids should not be heated in
an open vessel over a free flame. They
should be heated in a flask fitted with a
reflux condenser

Handling of acids
Store strong acids separately and away from
volatile organic chemicals.
Wear acid resistant chemical gloves and aprons,
when working with acids. Emergency flood
showers or eye wash foundation must be
available.
Dilute acids by stirring the concentrated acid
slowly into the water. Do not pour water in to
acid.
When using acids, make available suitable
neutralizing agents for use in the event of spills.
Acids should be neutralized with weak bases
such as sodium carbonate or bicarbonate.

Handling of Ethers
When ethers are exposed to air for long
periods, peroxides are formed. Accidentally
detonation of peroxides will lead to
explosions. This danger is more, when
ether is distilled. When there is a doubt
about the presence of peroxides in ethers,
these should not be handled without check .

Toxic chemicals
The various chemical classes of toxic
compounds
S.No

Class

Examples

Aromatic hydrocarbons

Benzene, toluene, xylene,

naphthalene, Anthracene

Amines

Aliphatic amines, anilines,

Napthyl amine

Chlorinated aliphatic hydrocarbons

CHCl3, CCl4, CHCl2, CH2Cl

Inorganic Compounds

Compounds of the elements

Be, Cd, Co, Cr, Ni, Pb, Ti, V
etc.

Safe limits of vapour

concentrations
The safe limits of concentrations of
chemical vapours in the air we breathe are
much smaller than what we normally
assume. For example, the threshold
concentration limit for mercury vapour is
0.1g/cubic metre, which can be easily
attained from mercury spills on warm
laboratory floors. Therefore stringent
safety rules and careful handling of
chemicals are essential for keeping the
laboratory atmospheric concentrations of
chemicals below the threshold limits.

Threshold limit values for some

toxic vapours
S.No

Substance

Threshold limit
(g/cubic metre )

Acetone

2400

Ammonia

70

Carbon monoxide

110

Ethyl amine

45

Hydrogen sulphide

30

Mercury

0.1

Nitric acid

25

Formaldehyde

Antidotes
An antidote is a substance which can
counteract a form of poisoning. It is
prudent to assume that every chemical
used in the laboratory is a poison and
hence handle it with care.

Treatment of specific poisons

If a chemical is swallowed, immediate
treatment should be given to the patient.
Acetone: Induce vomiting and administer
universal antidote. Keep the patient awake.
Universal antidote: This is prepared by
mixing 2 parts of pulverised charcoal, 1
parts of magnesium oxide and 1 part of
tannic acid. A few grams of this can be
added to a cup of warm water and then
administered. This universal antidote is
administered when a specific antidote is
not known.

 Acids:
Do
not
induce
vomiting,
administer
magnesium
oxide,
or
lime
water
immediately. Repeat the dose every fifteen
or twenty minutes. Administer milk or white
egg in cold water. Carbonates should not be
given to the patient. Administer a few
millilitres of mineral oil four or five times
every fifteen minutes.
Alkalis:
Do not induce vomiting, administer 5%
acetic acid or vinegar. Then administer, milk
or white of egg.
Methyl alcohol:

First aid Technique

Organic substances on the skin:
Wash liberally with rectified spirit, then
with soap and warm water.
Acid on clothing:
Apply dilute ammonium hydroxide to the
affected area of the dress and then wash
thoroughly with water.
Alkali on clothing:
Apply dilute acetic acid on the affected
portion and then wash with plenty of
water

Heating methods
A variety of methods for heating chemicals can be used in the
laboratory. Some of the method includes, the use of Bunsen
burner, hot plate, and heating mantle.
Heating with a Bunsen burner:
The Bunsen burner is used routinely in the general chemistry
laboratory. Many organic chemicals are flammable, and an open
flame is an invitation to starting a laboratory fire or an explosion
of combustible vapours. Never use a Bunsen burner in the
presence of highly flammable solvents. In the organic chemistry
laboratory, the Bunsen burner provides a high-temperature heat
source (1000C) for heating.

Heating with a Hot Plate

The variable-temperature hot plate is a
very versatile heating unit. The main
advantage of using a hot plate is that it
provides
a
flameless
variabletemperature heat from a flat surface,
so no additional support is normally
required when using a flat- bottomed
flask.

Heating with a Heating Mantle

A heating mantle is a specialized kind
of heating device designed to be used
only with round-bottomed flasks
when liquids are being heated under
reflux or are being distilled. There are
different heating mantles for each
size of flask.

Stirring
A mixture can be agitated with a magnetic
stirrer and with a mechanical stirrer.
Magnetic Stirrers:
Magnetic stirring is the method of choice if
an extended period of continuous agitation
is required, since it is easy to set up the
apparatus; particularly for small scale setups or closed systems.

Mechanical Stirrers
Larger scale reactions or viscous
mixtures require the greater power of
an external motor unit turning a
stirrer
blade.
It
is
highly
advantageous for the motor to
possess a variable speed control and
a typical model is shown in the
diagram

Filtration
There are few experiments in
organic chemistry that do not
involve atleast one filtration
step. Filtration is done by
allowing the liquid to pass
through a porous barrier, such as
filter paper or sintered glass,
whereby the solid remains on
the barrier.

Gravity Filtration
Gravity
filtration
is
a
simple
technique only requiring a filter
funnel, a piece of filter paper and a
vessel, called the filter flask, usually
an Erlenmeyer flask, for collecting the
filtrate. Glass funnels are available in
several sizes

Vacuum Filtration
Carrying out a filtration
using vacuum is faster
than using gravity alone,
but
requires
some
additional equipment.
Since the technique relies
on producing a partial
vacuum in the receiving
flask, a thick-walled filter
flask with a side arm,
often called a Buchner
flask, must be used.

Calibration of
Pipette

Pipet
te

Calibration of Pipette
The pipette is first rinsed with distilled water
and the pipette is filled with distilled water.
The water in the pipette is then drained into a
clean, weighed stoppered weighing bottle.
The draining should be done slowly by keeping
the tip of the pipette in contact with the side of
the bottle.
The draining from the pipette is completed when
the meniscus comes to rest slightly above the
end of the pipette tip.
The
weighing
bottle
is
reweighed.
The
temperature of the water is noted.
The exact volume of the pipette is obtained from
the weight of the water drained using Table1

Calibration of pipette
The volume and weight of water
contained in the pipette depends
upon the temperature.
Volume occupied by 1.0g of water weighed
S.No

Temperature (C)

Volume (ml)

10

1.0013

11

1.0014

12

1.0015

13

1.0016

14

1.0018

Calibration of Burette

Burette

Calibration of Burette
The burette is filled with distilled water.
The water level in the burette is adjusted to
the zero mark.
The water is then drained fully into clean dry
stoppered weighed 100cm3 flask.
Any drop adhering to the tip must be
removed by touching the neck of the flask
against the tip.
Restopper and reweigh the flask. Find out the
weight of water drained and note it carefully.
Repeat this procedure for for every cm 3 or
every 5 cm3 in a 50cm3 burette.

Calibration of Burette
Note the temperature of the water
and find out the volume delivered at
each point from the weight using
Table 1
Volume occupied by 1.0g of water
weighed
S.No
Temperature (C)
Volume (ml)
1

10

1.0013

11

1.0014

12

1.0015

13

1.0016

14

1.0018

Calibration of standard measuring

flask

Calibration of standard measuring

flask
The standard flask is first thoroughly
cleaned and dried.
Deionised water is then added slowly
in to the flask through a small funnel
until the mark is reached.
When water is near the graduation
mark, using a dropping tube, water is
added drop wise until the meniscus
stands on the graduation mark.
The stopper is replaced and the flask
is reweighed.
The actual volume of the water filling

Chemical
Balance

Weighing process in a chemical

balance
In using analytical balance usually the following sequence is
followed.

Sit opposite the balance, so that you face the centre of

the balance.
Remove any dust on the pans gently using a brush.
Release the beam carefully without jerk and check that
the pointer swings equally on either side of the zero
reading on the scale. Otherwise adjust carefully to obtain
this condition.
Arrest the beam and then gently place the objects on the
centre of the left side pan and close the balance case.
Place suitable weights on the right side pan and check for
equal oscillation. The pointer should swing through four
or five divisions beyond the mid-point of the scale. At the
final stage, rider must be used

Weighing process in a chemical balance

When it is necessary to add more of solid or
liquid, this must be done outside the balance
case.
Adding and removing the weights is done with
minimum disturbance on the pan and always on
the arrested position of the beam.
The pans must on no account be touched while
the beam is swinging.
When the oscillation is equal, note carefully the
weight of the object correct to 0.1mg.
Arrest the beam, return the weights to the
weight box, remove the object from the pan and
clean the pans and the floor of the balance
gently with the brush. Remember to close the
balance case before you leave the balance room.

Single pan balance

Weighing in a single pan balance

Rotate the arrest knob to the full release position and
adjust the zero adjusting control until the illuminated scale
indicates a reading of zero.
Arrest the balance and place the object to be weighed on
the pan. After turning the arrest knob to its partial release
position, rotate the dial controlling the heaviest likely
weight for the object until the illuminated scale changes
position.
The removal of the correct range of weight is indicated by
the gentle movement of the illuminated scale being in view.
Inadequate or excessive removal will make the illuminated
scale disappear from the illuminated window

Weighing in a single pan balance

When weights equivalent to the weight of
the object have been removed, turn the
arrest knob to its full release position
and allow the balance to achieve
equilibrium.
The weight of the object is found by
taking the sum of the weights indicated
on the dials and that which appears on
the illuminated scale.
A vernier is use in reading the scale to
the nearest tenth of a milligram.