ANALYTICAL CHEMISTRY

APPLICATIONS & ITS FUTURE ASPECTS

Introduction:
Analytical chemistry is the branch of chemistry which deals with the study of
separation, identification and quantitative analysis (i.e., estimation) of the chemical
components of natural and artificial materials. E.g.:

1) Estimation of Ca, Fe content present in cement.

2) Estimation of Fe present in water.
3) To study the blending property and thermal stability of polymers.
4) To study the morphology of particle size i.e., dimensions of nano sized particles
used as nano fibres, nano clays, nano composites, nano antibacterial air purifier,
etc.
5) Application of sot gel method to metal oxides nano particles.
6) To study the contents of clay (which is alumino-silicates) which are bricks,
building stones, rock specimens, etc.
7) Determination of hardness of water i.e., estimation of Ca and Mg present in
hard water.
8) Detection of adulterants in common food stuffs.
E.g.: a) Detection of starch in milk.
b) Detection of yellow dye in turmeric powder.
c) Detection of Khesari dal in Besan.

In analytical chemistry a chemist have to perform two important steps-

i)Qualitative analysis- It is a quite simple step which involve only the

identification step methods or volumetric methods.

ii)Quantitative analysis- It is a more complicated step in comparision to qualitative

analysis. It can be classified depending upon the method of analysis or can be
categorized according to the scale of analysis. Qualitative analysis can be sub-
divided involving classical methods like gravimetry or volumetry or there
involving sophisticated instruments estimating with EDTA solution using
Eriochrome Black T indicator.

For getting reproducible results, some interfering elements come in the way of
quantative analysis and these problems have been solved by analytical chemists
having the knowledge of sampling and excellent methods of separation such as
solvent extraction, ion-exchange chromatography and other different methods of
 chromatography like TLC, paper, partition, HPLC, etc. These methods have
significantly helped an analytical chemist to mitigate these problems of
interference, a short review of which discussed below.

I) The Isolation and Purification step during analysis involves atomic

absorption spectroscopy.
II) The next step on analysis involves volumetric methods or gravimetric
methods if the sample is present in milligram concentration.
III) If the sample to be analyzed is present at very low concentration then the
analysis involves optical methods or spectroscopic methods like UV-
visible, IR- spectroscopy.
IV) The methods principally used for illusidation of structure involved NMR
and mass spectroscopy.
V) Thermo analytical and radiochemistry methods are used for quantitative
works.
VI) Another important set of methods uses available electro-analytical
techniques ie. Potentiometry, cyclic voltametry, Polarography,
Conductometry and Coulometric methods of analysis.

Chemical analysis and analytical chemistry:

Chemical analysis establishes the qualitative and quantitative composition of

materials. The constituents to be detected or determined are elements, radicals, functional
groups, compounds or phases. Analytical chemistry is concerned with much broader and
more general aspects of analysis, while chemical analysis is concerned with much
narrower and more specific aspects of analysis. The determinatio0n of one constituent in
the presence of several other similar materials is essential, e.g. the careful control of
conditions such as pH, complexation, change in oxidation state, is essentials. Several
advanced in analytical chemistry have been made possible due to the spectacular progress
in separation methods. Analysis is generally composed of quantitative analysis and
qualitative analysis. Usually qualitative analysis is carried out before quantitative
analysis.

Improving the accuracy of analysis:

There are several ways of achieving accuracy in the analysis. One can use small
blanks along with the sample during determination. The use of large blanks reduces the
precision.
Another way is to give a correction e.g. in weighing of filter paper, or weight of
precipitate unreacted or unignited. An analytical chemist should strive hard to improve
the existing methods by proper combination of methods of separation and determination
to increase accuracy. Real advances can only be made by abandoning old methods and
seeking newer ones. An analytical chemist should be an originator and innovator as well
as a repair person.

Applications of Analytical Chemistry:

No other branch of science finds such extensive applications as analytical

chemistry, purely for two reasons. Firstly it finds numerous applications in various
disciplines of chemistry such as inorganic, organ, physical and biochemistry and
secondly it finds wide applications another fields of sciences such as environmental
science, agricultural science, biomedical and clinical chemistry, solid state research and
electronics, oceanography, forensic science and space research. Hence analytical
chemistry plays a very important role in enhancing the human knowledge about natural
materials.

Some important methods which are used immensely in analytical chemistry are as
follows-

A) CHROMATOGRAPHY- It is defined as a method of deporting a mixture of

components into individual components through equilibrium distribution between two
phases. The name chromatography (Greek ‘chroma’-color and ‘graphy’ writing) means
color writing.

Principle: The technique of chromatography is based on the difference in the rate at

which the components of a mixture move through a porous medium ( called stationary
phase) under the influence of some solvent or gas ( called moving phase). In
chromatography, the stationary phase may be solid or a liquid and the mobile phase may
be liquid or a gas.

The various techniques of chromatography are summarized in the table below-

Techniques Stationary Phase Mobile Phase

i) Column Chromatography or Absorption Solid Liquid

ii) Partition Chromatography Liquid Liquid
iii) Paper Chromatography Liquid Liquid
iv) Thin Layer Chromatography (TLC) Liquid or Solid Liquid
v) Gas Liquid Chromatography (GLC) Liquid Gas
vi) Gas Solid Chromatography (GSC) Solid Gas
i) Applications of Column Chromatography:

a) Analytical uses- Capillaries made of glass or copper are used for analytical
purposes. Glass capillaries whose internal surfaces are treated with conc. NH3 at
500*c can separate amino acid using Butanone/Pyridine/Dil. Acetic Acid or
Xylose/Glucose/Maltose using Butanone/Acetic Acid/Water.
b) Deportation of Geometrical Isomers- It helps to separate cis and trans isomers.
c) Chromatography is also used in separation of tautomeric mixtures.

ii) Applications of Liquid-Liquid partition Chromatography:

a) Detergent removal from protein solution.

b) Separation of steroids, bile acids and microtoxin.
c) Removal of pesticides, phenols, incecticides.
d) Trace metal concentration from aq. solution.

iii) Applications of Thin Layer Chromatography:

a) TLC is used for checking the separation procedures and purification

process.
b) In organic chemistry, TLC is used in the isolation and separation of
individual components of a mixture. Besides this, it is applied on checking
the purity of sample, examination of reaction and for the identification of
organic compounds.
c) Recently TLC has been used for separating cationic, anionic, purely
covalent species and also some organic derivatives of the metals.

iv) Applications of Paper Chromatography:

These are most same as the applications of TLC.

v) Applications of Gas Liquid Chromatography (GLC)-

a) The detections of steroid drugs used by the athletes in international sports

competitions and the steroids administered to animals in races are being carried out
by GLC.
b) Hazardous pollutants such as formaldehyde, carbon monoxide,
bichloroethylene, benzene and acrylonitrile can be monitored by GLC.
c) In analysis of foods, the separation and identification of
lipids,proteins,carbohydrates,preservatives, flavors, colorants and texture, GLC
is frequently used.
 d) It is also possible to analyze the dairy products by GLC foraldehydes and
ketones, fatty acids
and milk sugar.

iv) Applications of Gas Solid Chromatography (GSC):

The apparatus and technique for GSC happen to be the same as for GLC. The only
difference lies in the nature of the stationary phase and the length of the column.
Information on the columns and therir applications is included in the table.

Column Deportation Gas

Carbon (Carbosieves) Light Hydrocarbons, H2 & O2.

Silica (Spherosil, Parasil) Light Hydrocarbons, H2 & O2.
Alumina Hydrocarbons.
Molecular Sieve H2, O2, N2 and branched chain
Hydrocarbons.

B) NANOTECHNOLOGY- Nanotechnology is considered to be the key technologies for

the current century. Efforts are being made worldwide to create smart and intelligent
textiles by incorporating various nano particles or creating nano structured surface and
intelligent textiles by incorporating various nano particles or creating nano structured
surface and nano fibres which lead to unprecedented level of textile performances, such
as strain resistant, self cleaning, antistatic, UV protective, etc.

There are two main techniques involved in nano technology-

i) Scanning Electron Technology (SEM)- The scanning electron microscope

that images the sample surface by scanning it with a high energy
beam of electrons. Conventional light microscopes use a series of
glass image while the scanning electron microscope creates the
magnified image by using electrons instead of light waves.

Applications of SEM:

a) The SEM shows very detailed 3D black and white images at

much high magnifications (up to 300000X) as compared to light
microscope (up to 10000X).
b) The surface structure of polymer nano particles and nano coating
can be imaged through SEM- with great clarity.
c) SEM can be used for antibacterial air purifier.
d) SEM technique can also be used to view dispersion of nano
particles such as carbon nano-tubes, nano clays and hybrid.
 ii) Transmission Electron Microscope (TEM)- Transmission electron
microscopy is a
Microscopy technique whereby a beam of electrons is transmitted
through an ultra thin specimen and interacts as passes through the
sample. An image is formed from the electron transmitted through the
specimens magnified and focused by an objective lens and appears on
an imaging screen.

Applications of TEM:

i. The TEM is used widely in both material science/metallurgy and

biological sciences. In both cases the specimens must be very thin and
be able to with stand the high vacuum present in side the instrument.
ii. The properties of nano composite depend to a large extent on
successful nano level dispersion or intercalation/exfoliation of nano
clays, therefore monitoring their morphology and dispersion is very
crucial.

C) THERMAL METHODS- Thermal methods of anlysis may be defined as those

techniques in which changes in physical and/or chemical properties of substance are
measured as a function of temperature.

The methods of thermal analysis have been widely accepted in analytical

chemistry.

The various techniques of thermal analysis are summarised in the table below-

NAME OF THE ABBREVIATI INSTRUMENT PARAMETE DRAWING

TECHNIQUE ON OF THE EMPLOYED RS OF THE
TECHNIQUE MEASURED CURVE
THERMO-GRAVITY TG THERMO- MASS Mass V/S
BALANCE Temperatu
re or Time
DERIVATIVE DTG THERMO- dm/dt dm/dt V/S
THERMOGRAVIME BALANCE Temperatu
TRY re
DIFFERENTIAL DTA DTA ∆T ∆T V/S
THERMAL APPARATUS Temperatu
ANALYSIS re
DIFFERNTIAL DSC CALORIMATE dH/dt d H/dt V/S
SCANNING RY Temperatu
CALORIMETRY re
 I)THERMOGRAVIMETRY (TG)- It is a technique whereby the weight of a substance in
an environment heated or cooled at a controlled rate, is recorded as a function of time or
temperature.
Applications of Thermogravimetry-
i) It helps in determining purity and thermal stability of
both the primary and secondary standard.

ii) It helps in determining the composition of alloys and

mixtures.

iii) In analytical chemistry use- analytical reagents

especially those used in titrimetric analysis as primary
standards e.g, sodium carbonate, sodium tetraborate
and potassium hydrogen phthalate have been
examined.

iv) Building materials- one of the intresting examples in

cement is the study of a ternary compound in the
system CaO-Al2 O3 –SiO2.

v) One of the most important applications of TG is in

examining the thermal stability of polymers. TG is also
capable of giving informations concerning polymer’s
identity.

II )
DERIVATIVE THERMOGRAVIMETRY(DTG)- In DTG curve, the first derivative of
the TG curve is plotted with respect ot eithr temperature or time.
This is produced electronically from the TG trace by the computer and represents
the dm/dt or occasionally the dm/dt as a function of time or T.
Applications of DTG-
i) The magnitude of DTG signal is directly proportional to the rate of
reaction, it allows the comparision of reaction rates and

ii) The DTG curve separates overlapping reactions more clearly than
the TG curve.
 III)DIFFERTIAL THERMAL ANALYSIS(DTA )- DTA though often considered an
adjunct to TG is infact far more versatile and yields data if a considerably more
fundamental nature. This technique is simple as it involves the techniques of recording
the defference in temperature between a substance and a reference material against time
or temperature.
Applications of DTA-
i) Thermal diffusivity- DTA has been used to determine the thermal
diffusivities by measuring the temperature difference, ∆Ts,
between the centre and surface of the sample, heated at a
uniform rate.

ii) Analytical chemistry use-

a) DTA has become an established technique for the

identification of clays.

b) In a reaction the products are identified by this specific DTA

curve.

c) An melting point can be easily determined by DTA.

d) DTA technique has been widely used for the quality control
of a large no. Of substaces like cement, glass, soil, catalysts,
textiles, resins etc.

iii)Miscellaneous applications- DTA has been made to detect energy

changes occuring during melting, polymorphic transitions, and
second order transitions.

IV) DIFFERENTIAL SCANNING CALORIMETRY(DSC)- It is a thermal method whereby

the energy necessary to establish a zero temperature difference between a substance and a
reference material is recorded as a function of temperature or time.
Applications of DSC-
i) DSC provides a rapid yet reliable method for determining the
purity of materials.

ii) Using DSC calorimeter a blend containing Nylon66, orlon and

vycron polyester can be determined.

iii)DSC can be used to determine calcium sulphate hydrates in

cement.
 iv)DSC can be used to study the no. and the temperature range of
polymorphs. Since each polymorphic transition causes an
energy change that may also be detected by DSC.

CONCLUSION- From the above discullion it can be concluded that the analytical
chemistry is an important tool in the hands of an analytical chemist for the quantitative as
well as qualitative analysis of a compound accurately. Analytical chemistry has various
aspects in the different fields of study. Now a days a chemist can not think of analysis of
substances used in our daily life and also which are naturally abundant without analytical
chemistry. In near futhre it is going to be the capstone of all the branches of chemistry.
All the materials used in our daily life i.e, hags, clothes, chair, aeroplane, fans etc. belong
to polymer family and the thermal stabiliyty of these po;ymers is a part of analytical
chemistry,. Now a days nano science and technology is growing in the field of chemistry.
The morphology i.e, size,dimensions, surface structure of the nanoparticles used as
nanofibres, nonocoatings, nanopolymers, nanocomposites etc. can be dermined by tools
and techniques which is an integral part of analytical chemistry. So, the analytical
chimistry is essential and integral part for the development of the future prospects of the
world.