New Horizon College of Engineering, Bangalore

MODULE III

Nanomaterials: Introduction, Size dependent properties. Classification based on dimensions (0D, 1D, 2D and
3D. Bottom up and top down approach of nano material synthesis, Synthesis and applications of copper oxide
nanoparticles by co-precipitation method, carbon nano tubes (CNTs) by chemical vapor deposition.
Applications of gold nano particles in cancer treatment.
Display systems: Liquid crystals - Introduction, classification, properties and application in Liquid Crystal
Displays (LCD’s). LED display system working and applications. OLED display system working and
applications. QLED display system working and applications.
Analytical Techniques: Introduction. Principle, instrumentation and applications of UV-Visible
spectrophotometry and conductometry.

NANOMATERIALS

Introduction: The word “Nano” means dwarf in Greek language. Use it as a prefix for any unit like a
second or a meter and it means a billionth of that unit. A nanosecond is one billionth of a second. And a
nanometer is one billionth of a meter—about the length of a few atoms lined up shoulder to shoulder.
This is a term that has entered into the general and scientific vocabulary only recently but has been
used at least as early as 1974 by Taniguchi. Nanotechnology is defined as technologies where
dimensions and tolerances are in the range of 0.1-100 nm (from size of the atom to about the wavelength
of light) play a critical role.
Popular definition for Nano technology is: “Nano technology relates to the ability to build functional
devices based on the controlled assembly of nano scale objects for specific technological applications.”

Difference between Nano science and Nano technology:

Study on fundamental relationships between physical properties and phenomena and material
dimensions in the nanometer scale referred to as Nano science.
But Nano technology is the application of these nano structures and principles behind them to make nano
scale devices and to produce new materials.
Size dependent properties of Nanomaterials

1. Chemical properties: Reactivity; Catalysis

2. Thermal property: Melting point temperature.

3. Electronic properties: Electrical conduction.

4. Optical properties: Absorption and scattering of light.

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1. Chemical Properties:

Based on the surface area to volume effect, nanoscale materials have:

a) increased total surface area.

b) Increased number of atoms accessible on the surface.

c) Increased catalytic activity of those large number surface atoms.

d) Different/ tunable surface catalytic properties by the change in shape, size and
composition. Hence, nanoscale catalysts can increase the rate, selectivity and efficiency of
various chemical reactions.
As particle sizes and layer thicknesses approach the nm size scale, special properties begin to emerge.
For example, as particles get smaller in diameter a greater percentage of the atoms in the particle reside
on the surface of the particle as shown below.

Smaller than 10nm, the number of surface atoms dramatically increases, increasing the reactivity of
these particles. At below 2nm diameter 50% of the atoms in the particle, and hence have more degree of
freedom because they have fewer constraints and they become more active additionally as the particle
become smaller, their relative surface areas increase, again making them more chemically active.

2. Thermal Properties:

The melting point of a material directly correlates with the bond strength. In bulk materials, the

surface to volume ratio is small and hence the surface effects can be neglected. However, in
nanomaterials the melting temperature is size dependent and it decreases with the decrease particle size
diameters. The reason is that in nanoscale materials, surface atoms are not bonded in direction normal to

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the surface plane and hence the surface atoms will have more freedom to move.
3. Electronic Properties:
In bulk materials, conduction of electrons is delocalized, that is, electrons can move freely in all
directions. When the scale is reduced to nanoscale, the quantum effect dominates. For nanomaterials, all
the dimensions are at the nanoscale and hence the electrons are confined nano space. Therefore no
electron delocalization (freedom to move) occurs. Due to electron confinement, the energy bands are
replaced by discrete energy states which make the conducting materials to behave like either
semiconductors or insulators.

4. Optical Properties:
Because of the quantum confinement in nanomaterials, the emission of visible light can be tuned by
varying the nanoscale dimensions. It is observed that the size reduction in nanomaterials shifts the
emission of peak towards the shorter wavelength (blue shift).

CLASSIFICATION OF NANOMATERIALS ON THE BASIS OF DIMENSION

On the basis of reduction in size of materials in different dimensions, nanomaterials are classified into
three groups.
1. Zero dimensional (0-D): These nanomaterials have Nano-dimensions in all the three directions.
Metallic nanoparticles including gold and silver nanoparticles and semiconductor such as quantam dots
are the perfect example of this kind of nanoparticles. Most of thesenanoparticles are spherical in size and
the diameter of these particles will be in the1-50 nm range. Cubes and polygons shapes are also found
for this kind of nanomaterials.
2. One dimensional (1-D): In these nanostructures, one dimension of the nanostructure will be outside
the nanometer range. These include nanowires, nanorods, and nanotubes. These materials are long
(several micrometer in length), but with diameter of only a few nanometer. Nanowire and nanotubes of
metals, oxides and other materials are few examples of this kind of materials
3. Two dimensional (2-D): In this type of nanomaterials, two dimensions are outside the nanometer
range. These include different kind of Nano films such as coatings and thin-film-multilayers, nano sheets
or nano-walls. The area of the nano films can be large (several square micrometer), but the thickness is
always in nano scale range
4. Three Dimensional (3-D): All dimensions of these are outside the nano meter range. These include
bulk materials composed of the individual blocks which are in the nanometer scale (1-100 nm).

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METHODS OF SYNTHESIS OF NANOMATERIALS

Role of Bottom-up and Top-Down approaches in Nanotechnology

There are two approaches for the synthesis of nanomaterials

and fabrication of nanostructures. Top down approach refers
to slicing or successive cutting of a bulk material to obtain
nanomaterials.
Bottom up approach refers to build of nanomaterials from
bottom: atom by atom, molecule by molecule or cluster by
cluster
There are advantages and disadvantages in both approaches.

Figure 1: Schematic representation of the building up of Nanostructures.

 The biggest problem with top down approach is the imperfection of surface structure and
significant crystallographic damage to the processed patterns.
 These imperfections which in turn leads to extra challenges in the device design and
fabrication.

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 But this approach leads to the bulk production of nano material. Regardless of the defects
produced by top down approach, they will continue to play an important role in the synthesis of nano
structures.
 On the contrary, top down approach most likely introduces internal stress, in addition to surface
defects and contaminations.

When structures fall into a nanometer scale, there is a little chance for top down approach, all the tools
we have possessed are too big to deal with such tiny subjects. Bottom up approach also promises a better
chance to obtain nano structures with less defects, more homogeneous chemical composition.

Precipitation method for the synthesis of copper oxide nanoparticles.

Precipitation is a technique in which two reagents mixed to get an insoluble material in the solid form
which precipitates out of the solution and settles down.

The precipitation technique of preparation of nano materials involves two steps

 Formation of the nuclei: Here the nuclei refers to group of atoms together – Initially as the
precipitation starts few particles will approach each other forming a small mass (called nuclei).
 Growth step: In the growth step the above formed nuclei attracts the particles present in the
solution thus increasing its size itself.
 The growth step decides that the material to be formed is a nano material or bulk material.
 By monitoring and restricting the growth of the nuclei we can prepare nano size particles.
if the growth is not controlled, leads to precipitation of bulk mass.
 The growth of the nuclei can be controlled by maintaining suitable concentrations, pH of the
medium and temperature.
1. A suitable copper precursor (CuCl2/CuSO4/Cu(NO3)2etc,) solution is prepared in a known
volume of water.
2. To the prepared homogeneous solution of copper, suitable precipitating agent like
NaOH/NH4OH was added slowly under constant stirring.
3. The precipitate obtained was allowed to age, the solution has to be washed several times till it
is free from counter ions.
4. Thus, obtained precipitate has to be dried, then should be subjected to calcination at the desired
temperature to obtain copper oxide nanoparticles.

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pH, temperature
CuCl2 + NaOH Cu(OH) 2 + NaCl
stirring rate and capping agents

 (Calcination)
Cu(OH)2 CuO

Advantages of Precipitation Process

1. Homogeneous mixing of reactant precipitates reduces the reaction temperature.
2. Simple direct process for the synthesis of fine metal oxide powders, which are highly reactive in low
temperature sintering.
Disadvantages of Precipitation Process
1. This process is not suitable for the preparation of high pure, accurate stoichiometric phase. 2. This
method does not work well, if the reactants have very different solubility as well as different precipitate
rate.
3. It is not having universal experimental condition for the synthesis of various types of metal oxides.

Chemical Vapour deposition method for the synthesis carbon nanotubes.

Chemical Vapour Deposition (CVD) Chemical vapour deposition of hydrocarbons over a metal catalyst
is a classical method that has been used to produce various carbon materials such as carbon fibres and
filaments for over twenty years. It is a versatile method that can produce bulk amounts of defect-free
CNTs at relatively low temperatures. In this process, thermal decomposition of a hydrocarbon vapour is
achieved in the presence of a metal catalyst. Hence, it is also known as thermal CVD or catalytic CVD.

A schematic diagram of the CVD set up is given in Figure 2. A substrate material like quartz or alumina
is taken, cleaned well in preparation for the catalyst deposition and placed in a tubular furnace. A porous
substrate is generally used as it enhances the rate of carbon nanotube growth. A catalyst like iron or
nickel is deposited on the surface of the substrate through thermal evaporation. The furnace is
maintained at a temperature between 600oC and 1200oC. The process involves passing a hydrocarbon
vapour (acetylene, ethylene, carbon monoxide, etc.) through the furnace. In the case of a liquid
hydrocarbon (benzene, alcohol, etc.), the liquid is heated in a flask and an inert gas is purged through it,
which in turn carries the hydrocarbon vapour into the reaction zone. If a solid hydrocarbon is to be used
as the CNT precursor, it can be directly kept in the low-temperature zone of the reaction tube. Volatile
materials (camphor, naphthalene, etc.) directly turn from solid to vapour, and perform CVD while
passing over the catalyst kept in the high-temperature zone.

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Heating coil
v
Tubular
furnace
Carbon
nanotubes

Hydrogen gas
Heating coil

Hydrocarbon

Argon
carrier gas

Figure 2: Schematic diagram of CVD setup

At these high temperatures, carbon dissociates from these precursor molecules and diffuses into the
catalyst. CNTs grow on the catalyst in the reactor, which are collected upon cooling the system to room
temperature.
There are two basic mechanisms proposed for the growth of nanotubes by the CVD method based on the
substrate bound catalyst Figure 3.
(i) Tip growth model (Top carbon diffusion): The decomposition of the carbon source on the exposed
surface of the metal catalyst results in the formation of carbon species. They dissolve in the catalyst and
diffuse through it until they precipitate at the end in the form of nanotubes. The catalytic particle sits
always on the top of the growing nanotube.
(ii) Base growth model (Bottom carbon diffusion): In this model, the catalyst stays on the substrate. The
carbon species dissolve in the catalyst and diffuse through it until they precipitate on top of the metal
particle in the form of nanotubes.

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Figure 3: Mechanism of CNT growth in CVD method.

NANOMEDICINE:
Application of gold nanoparticles in Cancer treatment

Usually, the body is constantly replacing old cells with new ones; the old, damaged cells are deliberately
killed in process called apoptosis. Sometimes, however, mutations occur so that some new cells form
when the body doesn’t need them old cells don’t die when they should – which by the way is a basic
definition of cancer. Cancer cells bypass apoptosis and form a mass of tissue called a tumor.
It is interesting to know that the processes leading to cancer occur at the nanoscale therefore nanoscale
devices (for example in the form of nanoshell) can easily use to detect and destroy cancer cells.

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Working of gold nanoshell for cancer treatment:

Summary of the mechanism schematic represented as follows.

1. Injected into the Body

2. Illuminated with IR

Nanogold shell can be used to kill cancer cell. To begin creation of gold nanoshell includes following
steps.
At first gold nanoparticle (10 – 15 nm) is coated to silica (glass, sio2) core and then this core is coated
(attached) with special amine. After the amines are attached to the core, the coated silica particles are
attached with gold nanoparticles (less than 2nm) to form gold – silica nanoshell (roughly 15mnm). This
shell can best absorb infrared light (800 – 1050 nm) and heated up. Finally, antibodies are attached to the
gold – silica nanoshell as shown in the figure.
When these nanoshells are injected into the body antibodies present in the nanoshell attaches to the
surface of the cancer cells. Upon illuminating nanoshelss with infrared light (as it is mentioned earlier
nano gold shell can absorb infrared wavelength) by absorbing infrared light gold nanoshell heated up
hence it destroys tumor cells. By this nanogold shell can absorb IR radiation and kill the cancer cells.

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DISPLAYSYSTEMS

LIQUID CRYSTALS

It was observed by an Austrian botanist; Freidrich Reinitzer that solid cholesteryl benzoate on heating
becomes a hazy liquid at 145.50C and on further heating turns into a clear, transparent liquid at178.50C.
Cholesteryl benzoate is said to exist as a liquid crystal between 145.5oC and 178.5oC.). On cooling, the
change from liquid crystal state to solid took place exactly at the same temperature.
Thus “liquid crystal is a state of matter between highly ordered crystalline solid state and
disordered liquid states.”

145.5oC 178.5oC
Cholesteryl benzene liquid crystal state liquid
Solid (mesophase)

 In crystalline state, not only do the molecules occupy specific positions but also tend to orient
in a preferred direction. Thus, the molecules have both positional and orientational order.
 In liquid state, the molecules neither occupy specific positions nor are oriented in any particular
manner. The molecules are free to move at random and collide with one another abruptly changing their
positions thus losing both positional and orientational order.
 Intermediate between the solid and the liquid state exists the liquid crystal phase, wherein the
molecules are free to move but are oriented in a particular manner. The molecules have no positional
order but retain some orientational order.

Solid Liquid crystal Liquid

Temperature

 Liquid crystal phase is also called mesophase and the molecules, which can exist in mesophase,
are called mesogens.
 Director: in liquid crystal state the molecules have no positional order but are oriented in a
particular direction. The preferred orientation of the molecules of a liquid crystal is called the Director.

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Classification of liquid crystals

Liquid crystals may bebroadly classified into two

 Thermotropic liquid crystals: are those that exhibit liquid crystalline state on change of
temperature alone. Example: paraazoxyanisole.
 Lyotropic liquid crystals: these exhibit liquid crystalline state in mixture and when the
concentration of one of the constituents is varied. Example: soap, DNA, Polypeptides

Difference between Thermotropic and Lyotrophic liquid crystals

Thermotropicliquidcrystals Lyotrophic liquid crystals

This type of Liquid crystals depends on This type of liquid crystals depends on
temperature concentration
They are optically active. Therefore, used in These are optically inactive, hence not
electronic display. used in electronic display.
This type of LC possesses definite texture These do not possess definite texture
It is single component system. It is double component system
ie. substance+water system
It must contain at least one benzene ring It may or may not benzene ring
Eg: Cholestryl Benzoate Eg:Phospolipids

Thus liquid crystals may be classified as follows

Liquid crystals

Thermotropic liquid crystals Lyotropic liquid crystals

Nematic Chiral nematic Smectic Discotic

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 Nematic liquid crystals:

 These have thread like texture. (Greek nematos= thread).
 These are formed from optically inactive compounds.
 The molecules do not have positional order but the molecules are arranged parallel
to one another and hence have orientational order.
 Less Viscous as they are less closely arranged
 Fluidity is more
 Example: p-azoxyanisole

Chiral Nematic or twisted Nematic or cholesteric liquid crystals:

 Cholesteric liquid crystals exhibit finger print texture.

 These are formed from optically active compounds.
 A group of molecules is oriented at an angle to the adjacent group of molecules such that
the director takes a helical path as it travels through the liquid crystal just as a nut is moved
onto a screw.
 The distance through which a director travels as it completes one full rotation is called the
pitch of the liquid crystal.
 Less Viscous as they are less closely arranged
 Fluidity is more
 Example: cholesterylbenzoate.

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Smectic Liquid crystals:

Greek smectos =soap

 Smectic liquid crystals exhibit focal conic(brokenfan) texture
 Molecules are arranged in layers. At any instant of time the number of molecules within a
layer is much more than the number of molecules between the layers.
 Highly Viscous as they are closely arranged
 Fluidity is less
 Depending of the orientation of the molecules (inclination to the director) smectic liquid
crystal s are called smectic A, B,C etc.
 Example:4,4’-di-n-Heptyloxyazoxybenzene

Discotic liquid crystals:

• Here the molecules are disk like.

• These may be columnar liquid crystal or discotic nematic liquid crystals

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• In columnar liquid crystals, the molecules are stacked one above the other forming a column.
• In discotic nematic liquid crystals the molecules have coin like shape and have no positional
order but possess orientational order. The columns form definite shape such as hexagon.
• Highly Viscous as they are closely arranged
• Fluidity is less
• Example: Benzene-hexa–n-alkanoates

Applications of Liquid crystals in Display systems (LCD)

Construction and working of Working of LCD:

An LCD panel is made up of six layers,

 First front layer is vertical polarizing plate,
 Second layer with thin grid wires adjoining the liquid crystals,
 third layer is thin liquid crystal layer,
 Fourth layer is horizontal grid wires on its surface
 Fifth layer is horizontal polarizer
 Sixth layer is reflector.
The principle behind the LCDs is that when an electrical field is not applied to the liquid crystal
molecules, the molecules in twisted position in the LCD cell. When the light passes through the first
polarizer, the light is polarized and twisted with the liquid crystal molecular layer by 90o and becomes
horizontal. When it reaches the second horizontal polarizer, it will pass through, the viewer sees the
display is bright.
When an electric field is applied to the liquid crystal molecules, all of them line up in a same direction
and thus they have no polarizing effect. So the liquid crystal molecules do not change the polarization of
transmitted light. In this case the vertically polarized light cannot pass through the horizontal polarizer.
The viewer sees the display is black.

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Polarisation is a process in which the vibration of light waves is restricted to a single plane, resulting in
the formation of light waves known as polarised light

Since liquid crystals do not produce light of their own, they need an external light source to work back
light or ambient light.

Types of LCD Display

There are three types of LCD displays, Transmissive, Reflective and Transflective display.

Transmissive LCD Display

Transmissive displays rely on a backlight to be visible. For this kind of display, light emitting from the
back of the display glass must pass through the LCD towards the front to light the pixels. Transmissive
LCDs are suitable in low-light environments since they rely on a backlight to be visible. These displays
are also used in applications where high-resolution images, videos, and high quality are important.

Reflective LCD display

Reflective displays rely on bright ambient light to be visible. There is no backlight source inside this kind of
display; instead, light is reflected from the surrounding environment for the pixels to be visible.

Reflective LCDs work by using a reflective layer along with the polarizing filter, to reflect the light back
to the user's eyes instead of emitting light from a backlight. Reflective LCDs are used in e readers,
digital watches, calculators, etc.

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Transflective LCD displays

Transflective displays combine backlighting and ambient light reflection to illuminate the pixels,
resulting in a display with both transmissive and reflective properties.

In a transflective LCD, a backlight is used to illuminate the screen in low-light conditions, such as
indoors or at night. In bright light conditions, such as outdoors or direct sunlight, the screen can be
viewed by reflecting ambient light off the surface of the LCD.

Transflective LCDs are commonly used in industrial and medical equipment, where it's essential to have
high visibility in any lighting conditions. They are also widely used in marine, military, and aviation
applications.

Light Emitting Diodes (LEDs)

A Light Emitting Diode (LED) is a semiconductor device, which can emit light when an electric current
pass through it. To do this, holes from p-type semiconductors recombine with electrons from n-type
semiconductors to produce light. The wavelength of the light emitted depends on the bandgap of the
semiconductor material. This effect is called electroluminescence, and the color of the light is
determined by the energy bandgap of the semiconductor.
Application of LEDs in Display systems:
LED display system is nothing but modified Transmissive LCD. In which fluorescent back light is used
in LED display LEDs are used for back light.
An LED display unit consists the following structure.
From backside

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 LED backlight
 vertical polarizing plate,
 TFT (Thin film transistor)
 liquid crystal layer,
 RGB color filter
 horizontal polarizer
 Front cover

A huge collection of light emitting diodes on a flat panel. These diodes are either red, blue or green
combination of these colors with varying ratio can create every color the spectrum.
Different types of LED displays
7 segment display – for numbers
14 segment display – For alpha numeric
Dot matrix LED display – Numbers, alphabets, characters and simple graphics
Complex LED display – TV, Computer monitors and other display systems where complete spectrum of
colors is required
Advantages of LED Displays
One third the thickness of the LED screens (Due to the tiny LEDs)
LED s consume minimal amount of electricity when compared with LCDs
Enhanced Image quality, they can produce true blacks and true whites
More life span as no moving parts
Wider Viewing angle as LED displays are evenly lit
Less eye strain

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OLED (Organic Light Emitting Diodes)

OLED is a flat light emitting technology, made by placing aseries of organic thin films between two
conductors. When electrical current is applied, a brightlight is emitted. OLEDs are emissive display that
do not require a backlight and so are thinner and more efficient than LCD displays (which do require a
white backlight).

OLEDs work in a similar way to conventional diodes and LEDs, but instead of using layers of n-type
and p-type semiconductors, they use organic molecules to produce their electron sand holes.

A simple OLED is made up of six different layers. On the top and bottom there are layers ofprotective
glass or plastic. The top layer is called the seal and the bottom layer the substrate. Inbetween those
layers, there's a negative terminal (cathode) and a positive terminal (called the anode). Finally, in
between the anode and cathode are two layers made fromorganic molecules called the emissive layer,
where the light is produced, which is next to the cathode and the conductive layer (next to the anode).

1. An OLED light up, we simply attach a voltage (potential difference) across the anode and cathode
2. As the electricity starts to flow, the cathode receives electrons from the power source and the anode
loses them.
3. Now, added electrons are making the emissive layer negatively charged (similar to the n-type layer
in a junction diode), while the conductive layer is becoming positively charged (similar to p-type
material).poly(p-phenylenevinylene) and polyfluorene.
4. Positive holes are much more mobile than negative electrons so they jump across the boundary from
the conductive layer to the emissive layer. When a hole (a lack of electron) meets an electron, the
two things cancel out and release a brief burst of energy in the form of a particle of light—a photon,
in other words, this process is called recombination, and because it's happening many times a
second the OLED produces continuous light for as long as the current keeps flowing.

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OLEDs have many advantages over LCDs

1. OLED display works without a backlight because it emits visible light.

2. OLED screen can achieve a higher contrast ratio.
3. Improved image quality-better contrast, higher brightness, fuller viewing angle, a wider color
range and much faster refresh rates.
4. Lowerpowerconsumption.
5. Simpler design that enables ultra-thin, flexible, foldable and transparent displays.
6. Better durability-OLEDs are very durable and can operate in a broader temperature range.

QUANTUM-DOT light emitting diode (QLED)

Quantum-dot, or QLED (Quantum dot LED), screens are essentially a new type of LED-backlit LCD,
and they make use of tiny phosphorescent crystals to react to light and electricity. Less than 500
nanometers in size, the “nanoparticles” can glow in a range of colors which is precisely determined by
the number of atoms within. And instead of using pure white backlights, the quantum dots emit red or
green when struck by blue light. This means you will see much more highly saturated and accurate
colors than an average LED screen.

Working of QLED

Every pixel on the monitor emits red, green, or blue light, or sometimes a combination of all three. The
accuracy of the color of each pixel is defined by wavelengths. And quantum dots can be easily tuned to
their determined size to release different specific wavelengths for the best color production.

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The quantum dots can be placed in tubes or more commonly arranged inside a film. The sheet is then
inserted between a blue LED unit and color liquid crystal display (LCD) filters. When the blue LED
shines on the quantum dots, they start glowing red and green. All three colors combine to produce the
“purest” white light. The white light offers the color filters a more precise source to filter out the three
colors efficiently and precisely.

The diagram above illustrates how the quantum dots are placed in a QLED display. The blue LED light
source emits light that passes through the film enhancement layer to produce gradations of red, green,
and blue. The different colored light goes through the LCD panel and color filter glass, and then to the
screen for image display.

Advantages of Quantum Dot Technology

The added quantum-dot layer brings your monitor a whole host of benefits.

Precise Color and Higher Peak Brightness

As quantum dots can be tuned to emit the precise amount of light, it means the color produced will be
more accurate. The nanocrystals can render a wider spectrum color at maximum brightness without
losing saturation. This allows pictures to be shown clearly even in brightly lit rooms.

Better Energy Efficiency

Quantum dots only require a small amount of energy to work, and this can be achieved by a single blue
light. In fact, they can produce a 30 percent increase in brightness while using about 30 to 50 percent less
power.

Longer Lifespan and Low Burn-In

As QLED displays are based on existing LCD technology, they benefit from having a longer lifespan as
they rely on modern and energy-efficient backlighting. Quantum dot technology also does not degrade
over time, meaning QLED displays are less prone to burn-in.

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Instrumental method of Chemical Analysis

Chemical Analysis involves “Qualitative and Quantitative characterization of materials. It finds

application in fields like environmental science, agricultural science, biomedical and clinical
chemistry, solid state research and electronics, forensic research and space research.

Qualitative analysis deals with the determination of the elements or ingredients present in a compound
or mixture. E.g. the constituents of an alloy can be determined by the qualitative analysis.

Quantitative analysis deals with the accurate measurement of the amounts or percentages of the
various components of a compound or a mixture. E.g. estimation of calcium and magnesium salts in
water sample. The quantitative analysis can be classified into two types, depending upon the
method of analysis.

1) Chemical methods of analysis or Classical method of analysis

2) Modern methods of analysis or Instrumental methods of analysis.

Chemical methods of analysis involve gravimetric and volumetric analysis. Gravimetric analysis
involves quantitative estimation by weight and volumetric or titrimetric analysis involves the estimation
of a test solution by titrating against a std solution. E.g. determination of percentage of CaO in cement
solution by titrating against standard EDTA solution.

Instrumental methods of analysis: In Instrumental methods of analysis, an instrument is used to

measure the physical property of a substance to determine its concentration. For example, conductivity
meter is used to measure the specific conductance of an acid to determine the concentration of the acid.
Advantages of instrumental methods over the classical methods.

The methods are much faster than the chemical methods

i. Small amount of the test sample can be used for the estimation.

ii. Find wide applications in industries

iii. The analytical process can be automated

iv. Complex mixture can be analysed either with or without their separation.

v. Sufficient reliability and accuracy of results are obtained by instrumental method

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Disadvantages of instrumental methods over the classical methods.

i. The instruments are expensive

ii. An initial or continuous calibration is required using a sample of material of known

composition
iii. The concentration range is limited

iv. Specialized training is needed for the operation of certain sophisticatedinstruments.

v. The sensitivity and accuracy depend upon the type of instrument.

Figure. Working of analytical instrument

Transducer: A device that converts variations in a physical quantity, such as pressure or brightness,
into an electrical signal, or vice versa.

Ultraviolet-visible spectroscopy

In UV-visible spectrophotometer, the concentration of the species in a given sample can be estimated
at very low concentrations.
The instrument measures intensity of light passing through a sample (I) and compares it with the
intensity of transmitted light (I0).
The method follows Beer-Lambert Law which states that when a monochromatic light of UV – visible
region is passed through a colored medium; the intensity of the absorbed light is directly proportional to
the concentration and thickness of the medium.
I/I0 = T (Transmittance) A (Absorbance) = -log T

A= ɛcl Where, A = absorbance

I0 = intensity of light incident upon sample cell I = intensity of light leaving sample cell
c = molar concentration of solute l = length of sample cell (cm)

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ɛ = molar absorptivity coefficient Instrumentation:

Figure: Instrumentation of UV-Vis spectrophotometer

UV spectrometers consist of the following components:

Light Source: Two light sources are required to scan the entire UV-Vis band: deuterium lamp covers the
UV region (-200 to 330) mμ, tungsten lamp covers the visible region (330- 700) mμ.

Monochromator: A means of isolating light of a single wavelength and getting it to the sample
compartment. It is composed of prisms and [Link] radiation emitted from the primary source is
dispersed with the help of rotating prisms.

Sample and reference cells: One of the two divided beams is passed through the sample solution and
second beam is passed through the reference solution taken in cuvettes made of silica or quartz.
(Glass cannot be used for the cells as it also absorbs light in the UV region).

Detector: Two photocells serve the purpose of detector in UV spectroscopy. One of the photocell
receives the beam from sample cell and second detector receives the beam from the reference.

The detector measures the difference between the transmitted light through the sample (I) and the incident
light (I0) and sends this information to the recorder.

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 New Horizon College of Engineering, Bangalore

Working:

In UV-VIS spectrophotometer, a beam of light is split into two equal halves. One – half of the beam (the
sample beam) is directed through a transparent cell containing a solution of the compound being
analysed and one-half (the reference beam) is directed through an identical cell that contains only the
solvent. The instrument compares the intensities of the two beams at each wavelength of the region. The
instrument gives output graph – a plot of the wavelength versus the absorbance (A) of the light at each
wavelength is known as absorption spectrum.

Figure: Absorption spectrum of a UV-Vis Spectrophotometer

Applications of UV spectroscopy
1) In Quantitative analysis: The given species can be estimated in micro/ nano gram range. The
stoichiometry of the complex can be estimated.
2) In determination of the purity of a substance: Purity of a substance can also be determined with
the help of UV spectroscopy. The absorption of the sample solution is compared with the
absorption of the reference solution.

3) Chemical kinetics: UV-Vis spectroscopy is used to study the kinetics of the reaction. Change in
concentration in terms of absorbance values during a reaction can be measured for the following
the kinetics of reaction, since the concentration is proportional to absorbance.
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 New Horizon College of Engineering, Bangalore

Conductometric Titrations

Principle: Conductometric titration is based on the fact that during the titration, one of the ions is
replaced by the other and invariably these two ions differ in the ionic conductivity with the result
that conductivity of the solution varies during the course of titration. The equivalence point may be
located graphically by plotting the change in conductance as a function of the volume of titrant
added.
Theory: The electrical conductance C of a solution is a measure of ability of the solution to conduct
electricity. It is otherwise defined as inverse of resistance.

C = 1/R and its unit is Siemens.

When AC current is passed in a solution the resistance of a solution containing a fixed
concentration of an electrolyte at constant temperature is directly proportional to distance between
two electrodes (l) and inversely proportional to area of cross section (A).

R α l/A

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 New Horizon College of Engineering, Bangalore

Where κ is specific conductance, it is defined “Conductance of a solution placed between two

electrodes which are unit distance apart and having unit cross sectional area”.

Instrumentation: It consists of conductivity cell having two platinum electrodes placed at 1cm apart
and each having a unit area of cross section. The cell is dipped in the electrolytic solution taken in the
beaker and its connected to the conductance measuring device. In conductivity meter we usually
measure specific conductance.

Figure : Instrumentation of conductivity meter

Application of conductometry in acid-base titration:

a) Strong acid with a Strong Base:

During the titration of strong acid with a strong base ( Eg. HCl Vs NaOH), the following
reaction takes place

(H+ + Cl-) + (Na+ + OH-) (Na+ + Cl-) + H2O

The highly conducting H+ ions are initially present in the solution are replaced by Na+ions having
much smaller ionic conductance. Therefore, the conductance first falls, and after the equivalence
point has been reached, rapidly rises with further addition of NaOH which furnishes Na+ ions and OH-

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 New Horizon College of Engineering, Bangalore

ions. The intersection of the two straight lines gives the end point.

Figure : Graph of conductometer titration of strong acid Vs. strong base

b) Strong acid with a weak Base:

During the titration of strong acid with a weak base (Ex. HCl Vs NH 4OH), the following reaction
takes place

(H+ + Cl-) + (NH4+ + OH-) (NH4+ + Cl-) + H2O

The highly conducting H+ ions are initially present in the solution are replaced by NH4+ ions having
much smaller ionic conductance. Therefore, the conductance first falls, and after the equivalence point
has been reached, the conductance almost remains constant, since the excess of ammonium hydroxide
added, does not ionize in the presence of ammonium chloride (common ion effect). The plot is
curved near the end point, due to the hydrolysis of the salt of strong acidand weak base (NH4Cl).

Figure: Graph of conductometer titration of strong acid Vs. weak base

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 New Horizon College of Engineering, Bangalore

Question bank

1. Write optical, size dependent, and catalytic properties of nanomaterials.

2. Write on classification of nanomaterials with example.

3. What is top-down and bottom-up approach of nanomaterial synthesis?

4. Explain the precipitation method for the synthesis of CuO nanoparticles.

5. How CNTs are synthesized using CVD method?

6. Differentiate between Thermotropic and Lyotropic Liquid Crystals with examples.

7. Write a note on Different types of Thermotropic liquid crystals.

8. Write the principal and working of LCDs.

9. Explain the construction and working of OLEDs. Write the advantages of OLEDs.

10. Briefly explain the working of QLEDs.

11. Explain the principle, instrumentation and working of UV-Vis spectroscopy using a neat diagram.

12. Explain the principle, instrumentation and working of Conductometry

13. Explain the conductometric titration curve for the following titrations:

(i) HCl vs. NaOH (ii) HCl vs. NH4OH (iii) Mixture of HCl and CH3COOH vs. NaOH

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