Sampling Techniques

SAMPLING TECHNIQUES AND and Preservation

PRESERVATION
The process of sampling consists of drawing a very small portion of the material as a
representative of the bulk of the material. It may involve an elaborate array of
operations, such as, crushing, grinding, subdivision, etc. The collected sample should
be suitable for convenient transport and laboratory testing.

SAMPLING
A sample is a portion of the material taken from the consignment in such a way that it
possesses the essential characteristics of the bulk An ideal sample would be identical
in all of its intensive properties of the bulk of the material from which it is removed.

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 Thus, a single drop, removed from a tanker of a completely mixed liquid, may be a
sample. In practice a sample is satisfactory if its properties correspond to the
.

Digest
Name three important factors of prime importance in a sampling plan.

Gases

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The gas samples are usually collected in cylindrical containers made of glass and fitted
with stopcocks at both ends. At one of the ends some arrangement may be made to
evacuate the container or some other device required to filling the container. The
stopcocks should be carefully cleaned and lubricated.

The following three methods, in general, are used for collecting gaseous samples.
(i) Flushing
(ii) Displacement with liquid
(iii) Expansion into an evacuated container

When sampling from atmosphere, a single sample would supply little information.
Therefore, a large number of samples taken at various locations and at various times
will be required in any study of atmospheric pollution. In most cases of atmospheric
sampling, large volumes of air are passed through the collecting apparatus. Many
solids and liquids may be very finely divided and remain suspended in the air, such
solids may be removed by suitable filters and liquids are either adsorbed or reacted
with liquids or solids present in the sampling apparatus. In order to know the total
volume of air that is represented by the collected sample, a used. Sometimes, a manual
pump is used that delivers a definite volume of air through the sample tube with each
stroke of the pump.

15 .3.2 Liquids
The sampling of homogeneous liquids or pure liquid does not pose any problem. A
regular sample can be collected either by pouring the liquid into container or by
dipping the container into bulk of the liquid.

However, when the samples are to be collected from the various depths, the equivalent
volumes from the top, middle and bottom portions of the well-stirred bulk liquids are
collected with the help of a special device, which consists of a bottle with a two-hole
stopper. One hole is fitted with a short piece of tubing which is slightly longer than
the depth of the bulk liquid. The longer tube is fitted with a stopcock. To collect the
sample the stopcock is closed, the bottle is dipped in the liquid and the shorter tube is
lowered to the desired depth. The stopcock is then opened. As the air escapes through
the long tube (on opening the stopc ock) the liquid fills the bottle through the shorter
tube. This method can be applied for sampling emulsions and suspensions that are
fairly stable.

The accurate sampling of immiscible liquids is very difficult. For sampling

immiscible liquids the above method can be applied but each layer is sampled
separately. A composite sample is then prepared by mixing the different samples in
proportions to the relative volume of different layers in the bulk mixture of liquids.

15 .3.3 Solids
It is impossible to give general methods of sampling that are applicable to all solid
materials and to all conditions of sampling, since large variations exist within solid
materials. Hand sampling is often used to have a gross sample of bulk material such
as coal or ores. A laboratory sample is then prepared by reduction of the gross sample
to a convenient weight. Hand sampling, though inaccurate, is sometimes the only
available means of collecting a sample. It requires a careful plan for the material and
conditions of sampling and also careful supervision of the worker.

Material consisting of discrete lots is sampled by taking a random selection of such

lots. The particle size of the collecting solid material also introduces a variable that

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Non - Instrumental does not occur in the sampling of liqu ids or gases. This factor is of direct importance
Methods of Analysis to the analyst because it may be involved in the laboratory preparation of the sample
for analysis. The amount of impurity may vary in different sized particles. The
difficulty may be avoided by grinding the large particles to a smaller size and then
passing through a sieve, which has a nominal opening of about 0.05 mm.

Sampling of solids depends upon the physical properties and geometry of the material.
The procedure of sampling from solids in compact form, such as slabs, sheets or blocs,
can be made on random basis, sheet of metal, for example, can often be sampled by
clamping a number of sheets together with edges, flush and milling across the edges to
obtain an edge sample. Sometimes, the sampling procedure from a block follows to
drill or punch holes at regularly spaced intervals along the diagonal of a block,
alternately from one side and then from the other.

15 .3 .4 Precautions
Sampling requires adequate precautions that can be summarized as follows:

1. Label every bottle containing the sample with appropriate information including
the name of collector, date, exact location and any other data relevant to analysis
of the sample. Labeling of samples prevent misidentification.
2. Before filling a liquid sample, rinse sample bottle with the liquid being
collected.
3. While filling the container preferably leave an air space of about 1% of
container capacity to allow for thermal expansion.
4. Take adequate precautions during sampling and sample handling, if there is a
chance of sample constituents being toxic, wear gloves, apron or other
protective apparel. When toxic vapours might be present, sample only in well
ventilated areas. Always wear eye protection.
5. In a laboratory, make use of fume hood to open the sample container.
6. Never put food materials near samples.
7. If inflammable compounds are suspected to be present keep sparks and flames
away from samples and sample locations.
8. Take special safety measures for handling samples with radioactive
contaminants.
9. Operations that change the composition of the sample should be avoided as far
as possible.
10. Use plastic container if sample contains fluoride or strong alkalis.

SAQ 2
How the liquid samples are collected from various depths?
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15.4 CONTAINERS
The container of a suitable material is of great importance for sampling since the
nature of the material that is being sampled and also the tests are to be made on the
sample may be affected by the material of the container if it is not inert to the sample.
Usually, containers used for sample collection are made of plastic or glasses. One
material may be preferred over the other depending on the contamination present in
the sample. Avoid glass containers for samples of high pH and containing substances

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 Sampling Techniques
that affect glass. Plastic containers should be used for such samples. However, avoid
and Preservation
plastic containers, if samples contain organic compounds that affect plastic.

Metal containers may be used for sampling many materials, but they must also be used
with caution. Materials that will corrode the container or that will react with the metal
should not be sampled in such containers. For example, for storing acetylene a copper
container cannot be used, since it will cause explosion due to the formation of copper
acetylide.

Many materials must be protected against light, atmosphere, moisture, temperature

etc. Dark bottles are frequently used to protect material from light, use of tight
stoppers or sometimes by sealing with paraffin may give a sufficient protection against
the atmosphere. In more severe cases it may be necessary to seal in glass in an
atmosphere of nitrogen or helium.

15.5 COLLECTION AND PRESERVATION OF WATER

SAMPLES
Collection of water samples and its preservation is very important for the analysis of
water, specially for chemical purpose.

15 .5.1 Collection of Water Samples

Sampling is necessary to examine waters of a wide range of quality that includes water
suitable for domestic use, water suitable for industrial supplies, ground water, surface
water from rivers, lakes, rain water, municipal waste water, industrial water, saline
water etc.

It is not practical to use the same procedure for sampling all types of water. Collection
and preservation of water samples depend on the source, purpose of examination, and
the analytical procedure used for determination. Special precautions are necessary for
microbiological, organic and trace metal analysis. The constituents present may be
totally or partially lost if proper sampling and preservation procedures are not
followed.

Collection of water samples may be manual or automatic. In manual sampling no

equipment is involved, but this type of method may be time consuming for routine or
large scale sampling programs. Whereas in automatic sampling specifically designed
equipment is needed and human errors can be eliminated. This method may provide
the means for more frequent sampling.

Water sampling procedure depends on source also. For example, when a sample is
collected from tube well, the collection should be made after the well has been
pumped sufficiently so that the sample represents the ground water source. And when
a sample is collected from river, the collection should be made at different times from
different places and from different depths, since river water has rarely the same
composition throughout the year.

15 .5.2 Preservation of Water Samples

Analytical determinations may be affected by sample storage before analysis,
chemical and biological changes take place continuously after sample collection.
Change in pH and in amount of dissolved gases (oxygen, carbon dioxide) is very
common. Growth of microorganisms may take place, when the interval between
sample collection and analysis is long enough. Certain cations are subject to loss by
adsorption on, or ion exchange with, the walls of glass containers.

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Non - Instrumental To avoid the aforesaid changes, proper preservation of water samples should be made.
Methods of Analysis Nevertheless, complete preservation of water samples is a practical impossibility. At
best, preservation techniques can retard the possible chemical and biological changes
that occur during the sample storage.
Samples should be kept under conditions that will preserve the sample with as little
change as possible. Common preservation techniques used are:

(i) Refrigeration
(ii) Chemical preservation
(iii) pH control
(iv) Keeping in dark

Analyse samples as quickly as possible on arrival at the laboratory. If immediate

analysis is not possible store samples as cool as possible without freezing. Storage at
4°C is recommended for most samples. Cooling minimizes the, potential for
volatilization or biodegradation during storage.

Chemical preservatives may be used in certain cases. Before adding such

preservatives make sure that they do not interfere with the analysis being made. The
choice of the preservative be made taking due regard to determinations. When the
preservatives are used, they are added to the sample bottle initially so that the whole
sample is preserved as soon as collected.

Since pH plays an important role in many reactions, therefore, pH control is essential.

Sometimes, pH may change significantly in a matter of minutes. However, methods
of pH control are limited to the addition of acids (e.g. H2SO 4, HCl) or bases (e.g.,
NaOH).

Changes caused by growth of microorganisms are retarded by keeping the sample in

the dark and at a low temperature. The use of amber and opaque bottles is quite
satisfactory to avoid photochemical reactions required for the growth of
microorganisms.

SAQ 3
Name some of the preservation techniques used for water samples.
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15.6 SAMPLING OF SOIL

Sampling of soil is by far the most significant part of soil analysis. Sampling of soil
depends on various conditions, such as, the purpose for which the sample is required,
the nature of the soil, the analytical determinations to be made, the area and the depth
from which the samples are drawn etc.

Soil is the material occupying the outermost part of the earth's crust and possessing
different mineralogical and chemical properties resulting from its unique position on
the surface of the earth and the environmental factors existing at that position. The
properties of soil vary with lateral and vertical displacement. The individual layers of
soil that exhibit distinct variation with depth are called soil horizons where as the
vertical cross-sections as prof iles. Soil may be classed on the basis of the size of the
particles and as sand, silt and clay. The coarse sand has particles of diameter of 2-0.2

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 Sampling Techniques
mm, which are taken as fine sand. The silt particles below 0.002 mm diameter size are
and Preservation
clay particles.

The soil samples are usually collected in plastic, jute or cloth bags. Calico bags are
convenient to collect the soil samples. Such bags are numbered and labeled to give
required information, such as, different horizons, location, date, time etc. For most
purposes 1-2 kg sample weights are collected.

Samples should be taken from the face of a freshly dug pit sufficiently deep to permit
the collections from different horizons. Samples are collected from different areas
with the help of a suitable tool by breaking the lumps, if any, into smaller pieces and
mixing thoroughly. Pass the collected soil through nylon or stainless steel sieves with
holes of 2 mm. Crush the bigger particles again and again till the aggregate particles
are fine enough to pass through the sieves. The bigger particles left as stones and
gravels are discarded after weighing.

Area for digging should be chosen with the consideration of such factors as, degree of
erosion, surface drainage, color, texture, etc. Sampling of soil should be done in broad
daylight and the soil should be reasonably dry. Before sampling, all fitter should be
removed from the surface of the area chosen for sample collection, but do not remove
the organic matter embedded in the horizon. Collect the samples from different depths
as required. The depth of choice depends on the purpose of study. For example, to
study the fertility status the samples of upper 6" of 9" depth soil are suitable, whereas
for salinity and alkalinity studies samples of low depths are more important than that
of surface soil.

To take a composite sample representation of the area collect sample from each
important and distinctly different soil stratum at different depths. Thoroughly mix
each composite sample and dry in a well ventilated place. Pass the sample through a
stainless steel or nylon sieve to collect the particles of diameter less than 2mm.

For sampling soil a suitable tool is essential. An ideal sampling tool should be such
that it gives an uncontaminated reproducible sampling unit of approximately uniform
cross-section to the desired depth. Augers were often used in past but they are not very
satisfactory. Sampling tubes are usually used for sampling surface horizons.
Instruments such as towel and knife are frequently used to collect samples from
suitable depths after digging a pit.

15.7 SUMMARY
In this unit you learnt that:

• Sampling is to collect a very small portion of material such that it is a

representative of the bulk. It should be suitable for convenient transport and
laboratory testing.
• In a sampling plan the factors of prime importance are: nature of the sample, its
physical state, its toxicity and the cost of the test compared with the value of the
product.
• Gas samples are collected by flushing or by displacement with a liquid or
expansion into an evacuated container.
• A regular liquid sample can be collected either by pouring the liquid into container
or by dipping the container into bulk of the liquid.
• Sampling of solids depends upon the physical properties and geometry of the
material.
• Sampling of water depends on source, purpose of examination and the analytical
procedure used for determination.

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Non - Instrumental • Sampling of soil depends on the area and depth from which the sample is drawn,
Methods of Analysis the nature of the soil and the purpose for which the sample is required.

15.8 TERMINAL QUESTIONS

1. What kind of container will be used if a water sample contains fluoride or strong
alkalis?

2. For storing acetylene a copper container cannot be used. Why?

15.9 ANSWERS
Self Assessment Questions (SAQs)
1. (i) Nature of the sample
(ii) The physical state of the sample
(iii) The toxicity of the sample

2. The liquid samples are collected from various depths with the help of the special
device by which the equivalent volumes from the top, middle and bottom
portions of the well stirred bulk liquid are collected.

3. Refrigeration, chemical preservation, pH control and keeping in dark.

Terminal Questions
1. Plastic containers should be used for each sample.

2. Since it will cause explosion due to the formation of copper acetylide.

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