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Chapter 2
EXPERIMENTAL TECHNIQUES IN
CHEMISTRY
Analytical chemistry:
The branch of chemistry which deals with the chemical characterization (qualitative and
quantitative analysis) of a compound is called "analytical chemistry.
Separation Techniques
Filtration:
The process in which insoluble particles (suspended particles and precipitates) are separated from
liquids is called filtration.
Filter media:
Filtration can be performed with several types of filter media. Nature of the precipitate and other factors
dictate which filter medium must be used. Following filter media are frequently used for filtration.
Filter paper
Filter crucibles
Cotton
Paper pulp
Cloth
Sand as used as filter media
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4. The filter paper should be large enough so that it is one-fourth to one-half full of precipitate at the
end of filtration.
5. The funnel should be large enough for its rim to extend 1to 2 cm above the top circumference of the
paper.
6. If the process of filtration is to run smoothly, the stem of the funnel should remain continuously full
of liquid as longs as there is liquid in the conical portion.
7. The stem of funnel should be several inches long so that it can extend a few centimeters down into
the receiving beaker, and tip should touch the sides of beaker. In this way, the filtrate runs down the
side of beaker without splashing.
1.
2.
3.
4.
5.
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In this way, we increase the surface area of filter paper. As a result the rate of filtration increases.
Gooch crucible:
1.
2.
3.
4.
5.
It is made up of porcelain.
It has a perforated bottom which is covered with paper pulp or a filter paper cut to its size.
Quick filtration can be done by placing the crucibles in a suction filtering apparatus.
It is useful for the filtration of precipitates, which need to be ignited at higher temperature.
If its perforations are covered with asbestos mat then it may because to filter solutions that react with
paper e.g. concentrated HCl and KMnO4 (alkaline) solutions.
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Crystallization
Definition:
The process in which a crude product is purified and is obtained in the form of crystals is called
crystallization."
Principle:
The basic principle of crystallization is that solute should be soluble in a suitable solvent at high
temperature and excess amount of solute is thrown out as crystals when it is cooled.
1) Choice of solvent:
Solvent is chosen on hit and trial basis. It is necessary o try a number of solvents before arriving at a
conclusion.
Combination of Solvents:
If none of the solvents is found suitable for crystallization, a combination of two or more miscible
solvent may be employed.
Precautionary Measures:
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If the solvent is inammable then, precaution should be taken while heating the solution so that it
does not catch fire. In such cases, water bath is used for heating purpose.
After selecting a suitable solvent, the substance is then dissolved in a minimum amount of solvent
and is heated directly or on a water bath with constant stirring.
Add more solvent to the boiling solution if necessary until all the solute has dissolved.
3) Filtration:
The insoluble impurities in saturated solution are then removed by filtering the hot saturated
solution, through a normal or fluted filter paper. Thus avoid the premature crystallization of the solute hot
water funnel should be used for this purpose.
4) Cooling:
The hot filtered solution is then cooled at a moderate rate so that medium sized crystal is formed.
Slow cooling yields bigger crystals which are likely to include considerable amount of solvent
carrying impurities with it and complicating the drying process.
5) Collecting of crystals:
Filtration: When crystallization is complete, the mixture or crystals and mother liquor is filtered
through a Gooch crucible using vacuum pump. Full suction is applied in order to drain the mother
liquor from the crystals as effectively as possible.
Pressing: The filters cakes is rigid enough, it is pressed firmly with a cork to drain the left-over
liquid.
Washing: The crystals are then washed with a small portion of cold solvent and the process is
repeated for several times.
Evaporation: The mother liquor is quite often concentrated by evaporation and cooled to obtain a
fresh crop of crystals.
Success of Operation: The process of crystallization appears to be very simple yet the success of
operation lies in the amount or percentage of crystallized product obtained from the crude substance.
several times dries the crystallized substance. This process has the disadvantage that the crystals
crushed into fine powder and sometimes the fibers of filter paper contaminate the product.
Drying in an oven: The crystals are dried in an oven provided the substance does not melt or
decompose on heating at 100C.
Vacuum Desiccator: A safe and reliable method of drying crystals is through a vacuum desiccators.
In this process, crystals are spread over the watch glass and kept in vacuum desiccators for several
hours.
Drying agents: In desiccators are CaCl, silica gel or phosphorous pent oxide (P205) [con. H2SO4
also].
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Sometimes during the preparation of a crude substance, the colouring matter or resinous products
effect the appearance of product and it may appear coloured. Such impurities are conveniently removed by
boiling the substance in the solvent with sufficient quantity of finely powdered animal charcoal and then
filtering the hot solution. The coloured impurities are adsorbed by animal charcoal and the pure decolorized
substance crystallizes out from the filtrate on cooling.
SUBLIMATION
Definition:
The process in which a solid upon heating directly converts into gaseous phase and condenses back
into solid phase on cooling without passing through liquid phase is called sublimation. It is frequently used
to purify a solid.
Examples:
Benzoic acid, naphthalene, iodine (I2), ammonium chloride (NH4Cl), dry ice (solid CO2).
Sublimand:
The solid substance which is being sublimed is called sublimand.
Process of sublimation:
To carry out the process, the substance is taken in watch glass, covered with an inverted funnel. The
substance is then slowly heated over a sand bath and funnel is cooled with wet cotton. The pure solid
deposits on the inner side of funnel.
SOLVENT EXTRACTION:
Definition:
It is technique in which a solute can be separated from a solution by shaking the solution with a
solvent in which the solute is more soluble and the added solvent does not mix with the solution."
Objectives:
The objectives of solvent extraction are:
Separation of organic compounds from water,
Separation of the compound which is volatile or thermally unstable.
Distribution law:
A solute distributes itself between two immiscible liquids in a
constant ratio of concentrations irrespective of amount of solute added.
Solvent extraction L
Liquid phase chromatography
Distribution Co-efficient:
The ratio of concentration of solute dissolved in two immiscible
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Process: -
Solvent extraction is an important technique in chemical analysis. Usually, it is done by placing the
solution and the second liquid into a separating funnel. The funnel is stoppered and the two liquids are
shaken together.
Ether extraction:
The most common laboratory example of solvent extraction is ether extraction. This is used to
separate products of organic. synthesis from water. In a typical organic synthesis, the aqueous solution
containing the organic product is shaken up with ether in aseparating funnel and allowed to separate. The
inorganic impurities remain in the aqueous phase whereas the organic compound goes to ether layer. The
ether layer is separated and the organic compound is obtained by evaporating ether.
CCI4 Extraction:
The distribution of iodine between two immiscible solvents, water in the presence of KI and CCI4.
Iodine reacts with iodide ion to produce tri-iodide in a reversible reaction. The following dynamic
equilibrium is established.
I2 + I
Soluble in CCL4
I3
Soluble in water
At this point, the rate at which iodine passes from CCI2 to water equals the rate at which it passes from
-
water to CCl4. i lSo, if we add CCI4 to an aqueous solution of I 3 ions, the iodine will transfer from the
aqueous layer into organic layer. As a result, the brown colour of tri-iodide ions fades and the purple colour
of free iodine molecules appears in the organic phase. To achieve good separation, the two liquids are gently
shaken to increase there are a of contact and improve the chances of transferring, iodine molecules. No
matter how much iodine is used, the ratio of the nal concentrations at equilibrium is constant. The constant
is called distribution coefcient, K and is given By:
At 25C, the value of K for this equilibrium is 85. This means that the concentration
of Iodine in CCI4 is 85 times more than in water.
CHROMATOGRAPHY
Denition:
It is a technique of separation in which components of a mixture are separated.
Meanings:
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The word chromatography is derived from a Greek word khrornatos meaning colour writing.
This is because the earliest chromatographic methods were conned to separation of coloured substances
from their mixture.
Phases in chromatography:
Chromatography involves tho distribution of a solute between two phases:
(i) Statiqnary Phase:
It may be solid or liquid supported as a thin lm on the surface of an inert solid
Examples:
Alumina, silica gel, filter paper, acetone, water, ethyl alcohol etc.
PARTITIONH CHROMATOGRAPHY
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PAPER CHROMATOGRAPHY
It is a technique of partition chromatography. Here the stationary phase is a liquid (say H20)
adsorbed on paper. The adsorbed water behaves as an immiscible liquid towards the mobile, phase,
which passes over the paper. The mobile phase is usually an organicliquid.
There are three ways of carrying out paper chromatography namely:
Descending
Ascemding
Radial/circular
In the ascending type, the solvent is in a pooliat the hottom of a vessel in which the paper is supported and
the solvent travels upward by capillary action. A solvent mixture, specially composed in accordance with the
sample to be separated, is poured into the chromatographic tank. Cover the tank to homogenize its inner
atmosphere. Take about 20 cm strip ' of Whatmanns chromatographic paper No. I and draw on it a thin
pencil line about 2.5 cm from one end. Spot a point on the pencil line with the sample mixture solution. To
facilitate the identication of components of the mixture, spotsof the known compounds may also be placed
alongside. When the spots here dried, suspend the paper with dips so that the impregnated end dips into the
solventmixture to a depthof 5.6 mm. Cover the tank. As the solvent front passes the spots, the solutes begin
to move upward. The rate at which they move
depends on their distribution coefficients. When the solvent front has risen
to about 3/4th of the length of thepaper, remove the strip, mark the solvent
front with a pencil and allow the strip to dry.
Chromatogram:
The nished dried product with the colour bands of various
components of a mixture obtained in chromatographic experiment is called
chromatogram.
Development of chromatogram:
If the components of a mixture are colourless, then the chromatogram has to be developed by
Chemical Methods By using locating agents such as H2S, ninhydrin and rubeanic acid etc.
Physical Methods By heating or by throwing ultra violet radiations, we can identify the spots.
Retardation Factors(Rf):
It is the mathematical ratio which is obtained by dividing distance travelled by a component from
original spot and the distance travelled by the solvent from original spot.
Equation:
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Uses of chromatography:
(i)
The techniques of chromatography are very useful in organic synthesis for separation, isolation
and purications of products.
(ii)
They are equally important in qualitative and quantitative analysis.
(iii) This techniqueis used for the determination of the purity of a substance.
KEY POINTS
Chemical characterization includes both qualitative and quantitative analysis. 4 steps are in
quantitative analysis. Second step Separation of desired constituent from sample is discussed here.
Filtration removes insoluble Apanicles from liquid by passing through various porous materials.
For smooth ltration (a) In funnel, oaper should t tightly (b) lter paper can be folded in uted
manner or (e) stem of funnel should remain lled as long as liquid is in conical region.
Gooch crucible or sintered glass crucible can also be used for convenient ltration.
Crude product or impufe solid can bc puried by Crystallization providing solute is more soluble in
hot solvent than in cold state.
Solvent should be inexpensive, easy to handle, easy to remove and form well shaped crystals.
Firstly saturated solution is prepared, ltered, then cooled to get crystals. Desiccation is best drying
method. Unwanted colour is removed by animal charcoal.
Sublimation puries a substance that can be converted directly into vapours and then can be condensed
back into solid without passing through liquid state. e.g., Iodine, naphthalene, benzoic acid, camphor or
ammonium chloride.
Solvent extraetion separates a solute from solution by mixing with immiscible solvent in which solute
is more soluble.
Separating funnels is used for this purpose.
Repeated extraction is more efcient.
It is govemed by distribution law.
Chromatography separates components of a mixture on the basis of their distribution between a
stationary and mobile phase.
Adsorption and partition chromatography are used.
Paper chromatography is a partition technique done in three ways.
Rf value of components can be calculated from developed chromatogram.
Chromatography is used in isolation, purication and clinical analysis.
A pure substance has one spot on chromatogram.