SAMPLING AND SAMPLE HANDLING

A chemical analysis is most often

performed only on a small fraction of the
material whose composition is of
interest. The process by which a
representative sample is obtained is
called sampling. Often sampling is the
difficult step in the entire analytical
process. Sampling also limits the
accuracy of the procedure.

SAMPLING UNITS
The sampling process must ensure that the
items are representative of the bulk material.
The items chosen for analysis are called
sampling units or sampling increments.
For example: Consider a population of 100
coins and our aim is to know the average
composition of lead in the collection of coins.
Our sample consists of five coins. Each coin is
a sampling unit or sampling increment

GROSS SAMPLE

A gross sample is a collection of

individual sampling units. It must be
representative
composition
distribution.

of
and

the
in

whole
particle

in
size

SIZE OF THE GROSS SAMPLE

Gross sample weight is determined by (1)
the uncertainty that can be tolerated
between the composition of the gross
sample and that of the whole, (2) the degree
of heterogeneity of the whole and (3) level of
particle size.
A well mixed solution of a gas or liquid is
heterogeneous only on the molecular scale
and the weight of the molecules themselves
governs the minimum weight of the gross
sample.

A particulate solid such as an ore or

soil,
represents
the
opposite
situation.
In
such
materials,
individual pieces of solid differ from
each other in composition. In such
cases gross sample may weigh a gram
or more. The number of particles
required in a gross sample ranges
from a few particles to 10 12 particles.

SAMPLING OF LIQUIDS AND GASES

Well mixed solutions of liquids and

gases require only a very small
sample
because
they
are
homogeneous upto the molecular
level. Whenever possible The liquid or
gas to be analysed should be stirred
well before sampling to make sure
that the gross sample is homogeneous.

Gases can be sampled in several

ways. In some cases, the sampling
bag is simply opened and filled
with the gas. In other cases, gas
can be trapped in a liquid or
adsorbed onto the surface of a
solid

SAMPLING OF PARTICULATE SOLIDS

It is often difficult to obtain a random

sample from a bulky particulate
material. Random sampling can be
done during the transferring of the
material.

SAMPLING OF METALS AND ALLOYS

Samples of metals and alloys are

obtained by sawing, milling or drilling.
Solid material from the interior and
exterior
must
be
sampled.
Representative sample can be obtained
by sawing across the piece at random
intervals and collecting the sawdust as
the sample. Alternatively by drilling
the sample and collect the drillings.

LABORATORY SAMPLE

For heterogeneous solids, the gross

sample may weigh from hundreds of
grams
to
kilograms
or
more.
Reduction of the gross sample to a
finely ground powder by crushing,
grinding, mixing and dividing. The
finely ground sample is called
laboratory sample.

Laboratory samples of solids often

contain water that is in equilibrium
with the atmosphere. The common
practice is to remove moisture from
solid samples prior to weighing.
Traditionally drying is accomplished
by heating the sample in an oven or
vacuum oven and by storing in a
decicator

FORM OF WATER IN SOLIDS

Essential water:
It is the water that is an integral part
of a solid chemical compound in a
stoichiometric amount.
Eg. BaCI2 2H2O, CaC2O4 2H2O

Water of constitution is a second type

of essential water.
KHSO4 (s) = K2S2O7(s) + H2O(g)
Ca(OH)2 (s) = CaO (s)+ H2O (g)
These
compounds
yield
stoichiometric amounts of water
when heated

Nonessential water:
It is the water that is physically retained
by a solid.
It
is
not
necessary
for
the
characterisation
of
the
chemical
constitution of the sample.
Adsorbed water is a type of nonessential
water that is retained on the surface
solids. Another type of nonessential
water is called sorbed water amounting
to about 20% of the total mass of the solid.

Occluded water:
Liquid
water
entrapped
in
microscopic
cavities
spaced
irregularly throughout solid crystals.
Such cavities often occur in minerals,
rocks and gravimetric precipitates.