Experimental techniques in chemistry
The branch of chemistry
which gives a complete characterization of substance that is the qualitative
and quantitative analysis of a substance
Qualitative analysis:
The type of analysis in
which identification of elements in a compound is carried out for example
detection of elements by the sodium fusion test and salt analysis and mixture
analysis
The type of analysis in
which relative amounts of different elements are carried out for example
volumetric analysis (titration)
The main steps in the quantitative analysis are involved
·
Obtaining a sample for
analysis
·
Separation of the
desired component
·
Measurement and
calculation of the result
·
Drawing conclusion from
the analysis
Filtration:
The separation of
insoluble particles precipitate from the liquid by passing the mixture through a the filter medium is called filtration
Filter medium:
The porous medium which is used to separate insoluble solid particles from a solution or a mixture is called filter medium
Filtrate:
The liquid part of a solution that passed through the filter medium is called filtrate
Residue:
The insoluble particles
which cannot pass through the filter medium is called Residue
Selection of a filter medium
·
Nature of precipitate
·
Size of precipitate
Fluted filter paper
increase the rate of filtration because alternate elevations and depressions on
a filter paper provides an increased area for filtration Hans it increases the
rate of filtration
Gooch crucible:
Composition: it is made of porcelain having a perforated bottom which is covered with the paper pulp are filter paper are asbestos mat cut to its size. Filtration is useful for the filtration of the precipitate which needs to be ignited at heart temperature. If its perforation is covered with asbestos mad then it may be used to filter solution that reacts with paper
For example: concentrated hydrochloric acid and potassium permanganate solution
Sintered glass crucible: is made up of Glass having a porous glass disc sealed into bottom
Advantages:
It is convenient to use
because no preposition is needed as with the crucible moreover the process is
very e smooth
Crystallization:
Crystallization is the
removal of solid from a solution by increasing its concentration above the
saturated point in such a manner that the excess solid separate out in the form
of crystals
Why there is a need to crystallize the crude product
There is a need to crystallize the crude
product for the purification
• Choice of solvent
• Preparation of saturated solution
• Filtration
• Cooling
• Collecting of crystals
• Drawing to the crystalline substance
• Decolorizing of undesired colors
Write the steps for the choice of solvent in crystallization
• It should not react chemically with the solute
• It should either not dissolve the imperative are the
impurities should not crystallize from it along with the solute
• On cooling it should deposit well-formed crystals of the
pure compound
• It should be inexpensive
• It should be safe to use
• It should be easily removable
Note: If none of the solvents is found suitable for crystallization a combination of two or more miscible solvents may be employed
Drying agents:
• Calcium chloride
• Phosphorus pentoxide
• Silica Gel
Decolorizing of undesirable color:
Sometimes during the
preparation of crude substance that coloring matter are resonance product
affect the appearance of the product and it may appear color Such color
impurities are conveniently removed by boiling the substance in the solvent
with the sufficient quantity of finely powdered animal charcoal and then
filtering the hot solution impurities are absorbed by the animal charcoal and the
pure decolorize substance crystallizes out from the filter on the cooling
Animal Charcoal is used to decolorize the
undesirable color from crystallizing substances
A process in which a
solid when heated vaporized directly without passing through the liquid phase
and these vapors can be condensed from the solid again
For example Iodine, ammonium
chloride, naphthalene, benzoic acid, and dry ice
Sublimand:
The substance whose
sublimation is required or impure substance for sublimation is called sublimand
Sublimate:
The pure substance after
sublimation is called sublimate
Define solvent extraction
Solvent extraction:
The technique in which a solute is separated from a solution by shaking it with an immiscible solvent in
which the solute is more soluble is called solvent extraction
Define distribution law
Distribution law:
Solvent extraction is an
equilibrium process and it is controlled by distribution law or partition La
which is defined as
“A solute distributes
itself between two immiscible liquids in a constant ratio of concentration
irrespective of the amount of solute added”
Define distribution coefficient K
Distribution
Coefficient k:
The ratio of the concentration of solute in an
organic solvent to the concentration of solute in an aqueous solution is called
distribution Coefficient and it is represented by k
A process that is used
to separate the components of a mixture on the basis of their difference in a
relative affinity with two faces that is stationary and the mobile phase is called
chromatography
The word chromatography original from the Greek words Chroma toes which means color and graphene which means writing so chromatography means color writing
Differentiate between the stationary phase and
mobile phase
Stationary phase:
The stationary phase is a solid or liquid spotted as a thin film on the surface of an inert solid. This phase is in rest and the mobile phase flows over it. Component of a mixture with a small value of k mostly remains in this phase
Example: Glass Silica or Alumina
The mobile phase may be
liquid or a gas. It flows over the surface of a stationary phase. Component of
a mixture with a great value of k mostly remains in this phase
Example: helium argon nitrogen
and organic solvents
Distribution coefficient:
The distribution of
components of a mixture between the two phases are governed by the distribution coefficient is the ratio of the component in a mobile phase and a concentration of that component in a stationary phase
A smaller value of k:
The component of a mixture with a small value
of k mostly remains in the stationary phase and the mobile phase flows over it
The greater value of k:
The component with a the greater value of k largely remains dissolved in the mobile phase and pass over
the stationary phase quickly
• Adsorption
chromatography
• Paper
chromatography
Differentiate between adsorption chromatography
and partition chromatography
Adsorption chromatography:
A type of chromatography
in which the stationary phase is solid. In this type, a substance leaves the
mobile Phase to become absorbed on the surface of the solid phase
For example a thin layer
chromatography and column chromatography
Partition chromatography:
It is a type of
chromatography in which the stationary phase is liquid in this type the a substance being separated are distributed throughout both the stationary and
mobile phase
For example paper chromatography
Chromatogram: once the paper is dried the pattern on the paper is called a chromatogram
Retardation factor:
Each component has a
specific retardation factor called Rf value this value is related to its
distribution Coefficient and is given by
Write important uses of chromatography
Uses of
chromatography
It is used for separation and purification
It is used for checking the purity of
components
It is used in the qualitative and quantitative
analysis
It is used for the separation and
identification of colored pigments
It is used for the identification of amino
acids