Applied Chemistry

Module-4: Spectroscopic and diffraction techniques

Syllabus: Fundamental concepts in spectroscopic and diffraction

techniques – Principle, instrumentation, and applications of UV-Visible and
powder XRD determination of crystallite size, numerical
 Spectroscopy
What is spectroscopy?
The interaction of electromagnetic radiant energy with matter is called spectroscopy.
Quantitative and qualitative analysis of inorganic, organic, and biological compounds.
Spectroscopic data represent the response as a function of wavelength/frequency.

Spect Opt
rum ics

Sir Isaac Newton introduced the word spectrum in 1672 to describe the rainbow of colors.
Fraunhofer made significant contributions to optics and spectroscopy in 1814.
Kirchhoff demonstrated spectroscopy's utility in chemical analysis in 1859.
Spectroscopy has significantly advanced in the fields of chemistry, physics, and astronomy since its
discovery.
 Fundamental concepts in spectroscopic and
Spectroscopymicroscopic
Basics: techniques
Spectroscopy is used as a tool for studying the structures of atoms and molecules.
The basic principle shared by all spectroscopic techniques is to shine a beam of EM
radiation onto a sample, and observe how it responds to such a stimulus. The response
is recorded as a function of radiation wavelength.
Con
 Regions of EMR, Molecular Effects and
Applications

1eV = 96.48
 Electromagnetic Radiation
Energy is defined as the capacity to do work.
Energy Transfer Methods
Conduction refers to the transfer of heat from one
substance to another through direct contact.
Convection refers to the transfer of heat through a
fluid due to molecular motion.
Radiation refers to the energy transmitted through
rays, waves, or particles.

The dual nature of radiation was proposed by de Broglie in

1923,
EMR behaves as a wave in space and as a particle in matter
interaction.
The wave nature is measured in terms of frequency, wave-
length, and velocity.
The particle nature is expressed in individual photons, which are
discrete energy packets.
 Properties of EMR
Wave length (λ) refers to the distance between the
adjacent crests of a wave ( cm).
The frequency (v) is the number of oscillations per unit
time, denoted by hertz (Hz).

Velocity (c) is the speed of propagation in vacuum,

c=2.9979x108 m.s-1.

The energy carried by an EMR or photon is directly proportional

to its frequency, as E=hv
Photons are discrete packets of energy .

Spectroscopy Basics:
Spectroscopy is used as a tool for studying the structures of atoms and molecules.
The basic principle shared by all spectroscopic techniques is to shine a beam of EM
radiation onto a sample, and observe how it responds to such a stimulus. The response
is recorded as a function of radiation wavelength.
 Interaction of EMR with Matter
Absorption: EMR interacts with matter, causing
molecules and atoms to absorb energy and reach a
higher energy state.
Emission: It occurs when a substance emits
electromagnetic radiation.
Transmission: The process by which incident
radiation passes through matter without measurable
attenuation.
Reflection: Measures the amount of energy reflected
by matter.
Scattering: EMR scattering occurs when radiation
interacts with matter, causing the energy to be Wave nature explains reflection,
reradiated in different directions, not along the path of refraction, diffraction.
the radiation. Light absorption and emission due
to particle nature in individual
Refraction: Refers to the deflection or bending of EM photons.
waves as they pass from one transparent medium to
another.

These processes form the basis for detection or spectroscopic measurement techniques
Types of EM radiation interaction with matter:
If matter is exposed to EM radiation e.g. IR light (Fig. shown below), the radiation can be either absorbed,
transmitted, reflected, scattered or undergo photoluminescence.
Photoluminescence is a term used to designate a number of effects including fluorescence, phosphorescence and Raman
scattering.
Complement of the absorbed light gets transmitted.
Color of an object that we see is due to the wavelengths transmitted or reflected. Other wavelengths are absorbed. The
more absorbed, the darker the color (more concentrated solution).

Fig. Schematic
representation of interaction
of radiation and matter

Interaction of EM radiation with matter is a quantum phenomenon and is dependent on both the properties of
radiation and appropriate structural parts of the samples involved.
Origin of EM radiation is due to energy changes within matter itself.
In spectrochemical methods, we measure the absorbed radiation.
 Spectroscopy

Electroma Alpha Beta Proto Acousti Seismi

gnetic particl particl ns c c
spectrum es es Neutro waves waves
ns
Neutron Neutron-Induced
radiography gamma
Neutron spectroscopy
spectroscopy

Radio Microw Infrare UV- AAS X-Ray Gamma

ave d Visible Diffraction ray

Con
 Principle and Classification of Spectroscopy
Electromagnetic energy is transferred to atoms, ions, or molecules in the sample, resulting
in a transition to a higher energy state.
Energy required of a photon to give this transition.

hν= ∆E =
E1-E0
 Numerical Problems
The speed of a wave is equal to its wavelength time its
frequency : C= λν
1. What is the frequency of radiation with a wavelength of 5.00 x
10¯8 m? In what region of the electromagnetic spectrum is this
radiation?

Use λν = c to determine the frequency:

(5.00 x 10¯8 m) (ν) = 3.00 x 108 m/s = 6.00 x 1015 s¯1
Frequency in Middle Ultraviolet Region

2. Calculate the wavelength of radiation emitted from radioactive

cobalt with a frequency of 2.80 x 1020 s¯1. What region of the
electromagnetic spectrum does this lie in?

Use λν = c to determine the wavelength:

λν = c
λ (2.80 x 1020 s¯1) = 3.00 x 108 m.s-1
λ = 1.07 x 10¯12 m
 Spectroscopic Instruments in Space Exploration
Exploration Rovers Launch Missions
Searching and analyzing rock and soils.
Utilizing multiple spectrometers for sample analysis.

Mars Mission
Mini-TES: miniature thermal emission
spectrometer (examine rock, soil & atmosphere)
MB: Mossbauer Spectrometer (examine
mineralogy of rocks & soils)
APXS: Alpha Particle X-ray Spectrometer (analyzes
elements in rocks & soils)

Chandrayaan 3 mission
Seismometer, Langmuir Probe
Thermal Probe, Retroreflector
X-ray Spectrometer. Laser-based Spectrometer
Spectro-polarimeter
Principle, Instrumentation and Applications of
UV-visible Spectroscopy
 Contents
UV Visible Light Absorption Region
Absorption and Emission
Electronic Transitions
Terms and Shifts used in UV Spectroscopy
Color-absorption relationship
Principles of UV Spectroscopy-Absorption Law
Instrumentation
Applications
Numerical Problems
Summary
 UV-Visible Light Absorption Region
The process involves the absorption of light from 200 nm to 700 nm by molecules or atoms.
UV and visible light are involved with electronic excitation.
UV-Vis radiation has the potential to excited valence electrons in molecules or atoms.

Near UV/UVA: Long-wave UV or black light, not

absorbed by O3 layer
Medium UV/UVB: medium-wave UV, mostly
absorbed by O3 layer
 Absorption and Emission
Absorption and emission processes involve transitions between different energy levels.
Incidence photon must equal energy difference between states; hν= ∆S = S1-S0.
Energy absorption allows transition to the excited state.
The energy of molecular orbitals is specific to each group or chemical function.
Absorption wavelength is thus correlated to the type of chemical bonds.
 Electronic transitions and Absorption Bands
After excitation by EMR, valence electrons take part in electronic transitions.
Intensity
Four different transitions are allowed between σ, π and lone pair electrons.

1. Transition σ → σ*
occurs only for simple bonds (C-H or C-C for example)
Requires high energy and found in 100 nm-150 nm
2. Transition n → σ*
occurs for atoms with lone pair electrons (N, O, S….)
requires a high quantity of energy, and is thus found between 150
and 250 nm.
3. Transition n → π*
Only occurs for atoms with lone pair electrons and unsaturated
functions. (250nm- 500 nm)
4. Transition π → π* (aromatics) σ → σ*>n → σ*>π →
π*>n → π*
occurs only for atoms with unsaturated functions Forbidden transition: ε ≤ 10
are locatedbands
Absorption in the UV and visible
intensity domain
linked to (200 to 700 nm)
electronic Partly allowed transition: 10 ≤ ε ≤
1000
transition probability. Allowed transition:1000 ≤ ε ≤ 100000
Molar absorption coefficient valid for one wavelength. Highly allowed transition:ε ≥ 100000
 Terms involved in UV Spectroscopy
A chromophore is any isolated covalently
unsaturated bonded group that shows a
characteristic absorption of EMR in the UV or Auxochrome
Visible region.
Na+ O O
O O Na+
S S
Organic molecules containing >C=C<, >C=O, - O O
N=N- and -NO2
In Greek : Chroma = color, and phoros= bearer. HO
An auxochrome is a group of atoms attached to a Chromogen Auxochrome
N
chromophore that modifies the ability of that N
chromophore to absorb light. Chromophore

Organic molecules containing:- COOH, -OH,-

SO3H, -NR2 -NH2 O S O
In Greek, Auxo= increase and chrome=color. O
Auxochrome
Chromogen is the chromophore and auxochrome Na+
together.
 Shifts Involved in UV Spectroscopy
Bathochromic Shift (Red Shift)
Shifts absorption maximum towards longer wavelength.
Caused by auxochrome presence or solvent change.
Hypsochromic Shift (Blue Shift)
Shifts absorption maximum towards shorter
wavelength.
Caused by the removal of conjugation and solvent
polarity.
Hyperchromic shift
Increases absorption maximum intensity.
Auxochrome usually boosts absorption intensity.
B-band shifts from 275 mμ to 262mμ.
Emax for 2-methyl pyridine increases to 3560.
Hypochromic Shift
Decreases absorption maximum intensity.
Caused by group distorting molecule geometry.
 Colour-absorption Relationship
Methylene blue absorbs 600-700 nm in orange-red, so that it looks blue to us
Cong red absorbs maximum at 500 nm in green, so that it looks like red for us.
Red and blue light are absorbed by chlorophyll and so it appears its complementary
colour, green.
Methylene
0. blue
75
Congo
0.
red
5
0.
A 25
b 0
s 40 50 60 70 80
o 0 0 Wavelengt
0 0 0
r h (nm)
b
The complement of the absorbeda light gets transmitted. O- Na +
n
The colour of an object that we see is due to the wavelengths N Cl- NH2
O
S O
c
transmitted or reflected. Other
e
wavelengths are absorbed. The H3C
N N
CH3 N
N
N
N
more absorbed, the darker the colour (more concentrated CH3 CH3
O
S O H2N
solution). + Na - O
 Principles of UV Spectroscopy-Absorption Law
Beer–Lambert law or Beer–Lambert–Bouguer law.
The law combines discoveries made by Bouger, Lambert, and Beer ( 1729-1852)
At a wavelength maximum, absorption is proportional to the concentration of absorbing
molecules and the path length of the light through the sample.
A = εLC
A = absorbance of the sample, log10 (I0 /I)
I0 = intensity of the radiation entering the sample
l = intensity of the radiation emerging from the
sample
L = length of the light path through the sample, in
centimeters
C = concentration of the sample, in moles/liter
ε = molar absorptivity (Litre mol-1 cm-1 )

It applies to all forms of electromagnetic radiation, not just visible light.

 Instrumentation
Arnold O. Beckman's created Spectrophotometry in 1940

A "single-beam" spectrophotometer is
made up of:
a polychromatic source
a wavelength selector and eventually a
source selector
a sample compartment
a detector
a screen and/or a computer.
Instrumentation-Double-beam spectrophotometer
 Applications
1. Quantitative analysis of analyte: Determination of the concentration of a
compound in solution using Beer’s law.
Determination of percent content of Vitamin A1 and Vitamin A2 in natural fats and oils by
measurement of intensities of peaks at λmax=325 nm and 351 nm, respectively.
2. Distinction in conjugated and non-conjugated compounds: if an
organic compound does not show λmax above 200 nm, it cannot contain a
conjugated chromophore, aldehyde, keto group, or benzene ring.
3. Distinction between Cis and Trans geometrical isomerism: The Trans
isomer shows a longer absorption wavelength and Higher intensities than the
cis isomer.
4. Distinction between keto-enol tautomerism: Keto form shows low
intensity band at 275 nm (ε=20) due to isolated keto-carbonyl group while
enol shows high intensity band at 245 nm (ε=1800) due to conjugated double
bond.
5. Study of charge transfer complex: Charge transfer complexes are formed
when an electron-rich molecule (tetracyanoethylene iodine) is mixed with an
electron acceptor molecule (aniline, benzene). The charge transfer complex is
responsible for new absorption peaks.
 Numerical Problems
1.A sample has a maximum absorbance of 275 nm and molar
absorptivity of 8400 M-1cm-1. A spectrophotometer measures
absorbance of 0.70 using a cuvette that is 1 cm wide. Find the
solution concentration.
Use the equation A = εcL and solve for concentration (c):
c = A/εL
c = (0.70) / (8400 M-1cm-1)(1 cm) = 8.33 x 10-5 mol/L = 8.33 x 10-5 M
2. Indicate the functional groups shown in the compound below
whether they are auxochrome or chromophore groups
D
A C

HO CH3
B NH2
E
N O
3. What sort of electronic transitions are possible for each of the
following compounds? (a) cyclopentane (b) acetaldehyde (c)
dimethyl ether (d) triethyl amine (e) cyclohexene
Types of EM radiation interaction with matter:
If matter is exposed to EM radiation e.g. IR light (Fig. shown below), the radiation can be either absorbed,
transmitted, reflected, scattered or undergo photoluminescence.
Photoluminescence is a term used to designate a number of effects including fluorescence, phosphorescence and Raman
scattering.
Complement of the absorbed light gets transmitted.
Color of an object that we see is due to the wavelengths transmitted or reflected. Other wavelengths are absorbed. The
more absorbed, the darker the color (more concentrated solution).

Fig. Schematic representation of

interaction of radiation and matter

Interaction of EM radiation with matter is a quantum phenomenon and is dependent on both the properties of radiation
and appropriate structural parts of the samples involved.
Origin of EM radiation is due to energy changes within matter itself.
In spectrochemical methods, we measure the absorbed radiation.
(ii). Principle and applications of UV-Visible spectroscopy technique
Principle: Different molecules absorb radiation of different wavelengths depending on their
structure. An absorption spectrum will show a number of absorption bands corresponding to
structural (functional) groups within the molecule. For ex. absorption by carbonyl group in
acetone is of the same wavelength as the absorption by carbonyl group in diethyl ketone.
In UV-Vis spectroscopy, energy is absorbed by a molecule in the UV region (1-400 nm) or the
visible region (400-750 nm), resulting in an electronic transition of valence electrons.

Components of a UV-Vis
Spectrophotometer
Source Lamp Sample Holder Photometer/Detector

Monochromator Signal Processor and Readout

Beer-Lambert Law
When light passes through a molecular material, absorption can occur. The absorption of light, as it passes through a
medium, varies linearly with the distance the light travels and with concentration of the absorbing medium.
The extent of absorption is given by Beer-Lambert Law, as expressed by A = εcl, where A is the
absorption, ε is the absorptivity coefficient, l is the path length, and c is the
concentration of the specific analyte. Absorptivity characterizes the amount of light absorbed by a specific
molecule at a specific wavelength.
Beer-Lambert Law

IT
Io

Path
length (l)

Chromophore: any isolated covalently bonded group that shows a

characteristic absorption in the UV-Vis. region. The only molecular moieties likely
to absorb light in the 200 to 800 nm region are π-electron functions and hetero
atoms having non-bonding electron pairs. ~ λmax: 280
NH2
nm
Auxochrome
~ λmax: 255
Auxochrome: group of nm
atoms attached to a
chromophore which modifies N N
N N

the ability of that

chromophore to absorb light.
Ex. COOH, -OH, - C2H5 O ~ λmax: 385
SO3H, -NH2, -NH-R, - ~ λmax: 320
Principle, Instrumentation and Applications of XRD
 Contents
X-rays and Energy.
Continuous and Characteristics X–
rays.
Production of X-rays.
Diffraction and Interference.
Principles of X-ray Diffraction (XRD).
Bragg’s Law.
X-ray Diffractometer.
X-ray Diffraction Pattern Analysis.
Crystallite Size from XRD.
Numerical problems.
Applications, Advantages and
Disadvantages.
 X-rays and Energy
It is basically energetic high-frequency EMR. Discovered by W.C. Rontgen in 1895.
Part of electromagnetic spectrum: Nobel Prize in 1901.
Wavelength: 0.01 -10 nm shorter than UV X-radiation (X-rays) or Röntgen radiation.
and greater than gamma.
Energy: 1keV-100 keV higher than UV and Types of X-rays: Hard X-rays (0.01 to 1 nm)
lower than gamma. and Soft X-rays (0.1 to 10 nm).
Frequency: 3x1016 Hz -3x1019 Hz. Analytical purpose: 0.7 to 2 nm
First example of ionizing radiation.

Anna Bertha Ludwig, wife of Rontgen

First human body radiographic image
 Continuous and Characteristics X-rays
Continuous (Bremsstrahlung, breaking
radiation) X-rays
Nucleus field interaction: Bremsstrahlung
Arises from electron deceleration.
Electrons near the nucleus slow down KE.
Loss of KE compensated by X-ray emission.
Polychromatic, continuous, or white radiation.
The phenomenon was discovered by Nikola Tesla.

Characteristic X-rays
Inner shell interaction produces characteristic radiation.
Created when a hole in inner shell filled by higher energy
electron.
K-shell electron knocked out fills vacancy by L-shell (Kα) or
M-shell (Kβ) electron.
K-lines are most useful in X-ray diffraction.
Cu Kα is commonly used on lab scale x-ray instruments:
Energy is 8.04 keV, corresponding to 1.5406 Å X-ray λ.
. Used for the crystal structure study by XRD.
Discovered by Charles Glover Barkla in 1909.
Question: Distinguish between Continuous and Characteristic X
ray Spectrum
 Production of X-rays
Evacuated glass/metal bulb.
Seals cathode and anode electrodes on each end of the tube.
Cathode (-ve): Tungsten (W) ( Filament type).
Anode ( +ve) : Cu/ Cr/Mo/W/ depending type of applications (disk type).
Electrons are produced by the heated cathode via the thermionic process to hit the anode.
Accelerating potential is applied between the cathode and anode (25-150 kV).
X-rays are produced when a fast-moving stream of electrons is rapidly decelerated.
Characteristics Kα, (Å) of different anodes: Cr(2.29), Fe (1.94), Co (1.79), Cu (1.54), Mo (0.71), and W (2.13).

Tungsten features :
o High atomic number of 74.
o Efficient electron release.
o Good thermionic emitter.
o Manufactured as thin wires.
o High M.P. of 3422 0C.

Recent Old model Crookes

model tube
 Interference and Diffraction
Interference is the interaction of the two waves:
Reinforcing interaction = Constructive interference
Two waves are in phase, results in greater amplitude wave
Canceling interaction = Destructive interference
Two waves are out of phase, cancel each other then no net motion remain

Bending of light around the

corners of door and windows.

Diffraction occurs when a light wave passes through a physical slit or corner that is
smaller than or equal to its wavelength.
What is diffraction?
Diffraction refers to a phenomena when a wave encounters an
obstacle.
In classical physics, the diffraction phenomenon is described as the
apparent bending of waves around small obstacles and the spreading
out of waves past small openings.
Interference of diffracted waves
Interaction between diffracted waves is called interference.
Constructive Interference: Waves are in-phase when each of their crests and troughs occur
exactly at the same time. Those type of waves stack together to produce a resultant wave that has
a higher amplitude. For constructive interference, path difference should be multiples of n*λ.
Destructive Interference: If the waves are out of phase by multiples of (n/2)*λ, then destructive
interference occurs and the amplitude of the resultant wave will be reduced.

path difference = path difference = multiple

 Principles of X-ray Diffraction (XRD)
Microstructure of solid materials
Crystalline: Entire solid is made of up atoms in an
orderly array.
Polycrystalline: Completely ordered in segments.
Amorphous: No recognizable long range order.

“Every crystalline substance gives a pattern; the same

substance always gives the same pattern; and in a mixture
of substances each produces it’s independently of others”.
The XRD pattern of pure substances resembles a
fingerprint of the substance.
It is based on the scattering of X –rays by crystals.
The atomic planes of crystal cause an incident beam of X-
rays to interfere with one another as they leave the crystal
is described by the famous law called Braggs law.

Chemical formula of SiO2

Crystal structures vary.
 Bragg’s Law
The atomic planes of a crystal cause an incident
beam of X-rays to interfere with one another as they
leave the crystal is called X-ray diffraction.
Two parallel rays create angle ϴ with crystal planes.
When the total path difference is 2dsin θ equals to nλ,
diffraction occurs:
Path difference (δ)=CB+ BD
For Δ ACB; Sin θ= CB/AB= CB/d= CB=dSin θ
Similarly, Δ ADB; Sin θ= BD/AB= BD/d= BD= dSin θ
So, dSin θ + dSin θ= 2dSin θ
Bragg’s law: δ = 2dSin θ= nλ
Where
δ : Path difference between the reflected x-ray waves.
λ : Incident X-ray wavelength.
n= an integer ( 1,2,3…).
d= distance between lattice planes.
Θ: angle between the indent X-ray and the lattice. Nobel Prizes in Physics:
Max von Laue: 1914 Nobel Prize for X-ray
diffraction discovery.
W.H. Bragg and W.L. Bragg: 1915 Nobel prizes for
X-ray crystal structure analysis.
02-10-2025
 X-Ray Diffractometer
It is the instrument used to
produce monochromatic x-rays.
Focuses beam on sample.
Scans through a 2θ range.
Detects reflected x-rays and their
intensity.
Attached to a goniometer for
simultaneous scanning.
Optics focus x-ray beam on sample.
Reflects x-rays into detector.
Detector: Gas-filled, scintillation, or
semiconductor.
Records peak position and intensity
during constructive interference.
Displayed on a diffractogram.

A goniometer is an instrument for the precise measurement of angles, especially one used to measure the angles
between the faces of crystals.
 Components of a XRD
instrument
Incident-beam
X-ray tube: source of X-rays
Receiving-side
optics optics Incident-beam optics:
condition the X-ray beam before it hits the sample.
Goniometer: platform that holds and moves the
sample, optics, detector, and/or tube.

Sample holder
Receiving-side optics: condition the X-ray beam
after it has encountered the sample.
Detector: count the number of X-rays scattered by
the sample.

Incident angle (ω) is defined between the X-ray

source and sample.
Diffracted angle (2θ) is defined between the incident
beam and the detector angle.
Incident angle (ω) is always ½ of the detector angle
2θ i.e. θ.
In a typical XRD instrument, the X-ray tube is fixed,
the sample rotates at θ°/min and detector rotates at
2θ°/min.

(In
ter
 1111 1111
11 1111
1 1111
111 1111
111 11
1111
1111
1

X-ray
tube
1111111111 aavvaaac1
Detect
ω θ 2 or
θ
X-ray Diffraction Pattern Parameters and Analysis
XRD Plot: Signal intensity at two theta positions.
Peak Intensity and Peak position
Two theta positions atoms within a lattice structure.
Intensity of peaks correlates with number of atoms in
phase.
Greater peak intensity indicates more crystals or
molecules with specific spacing.
Peak Width and Crystal Size
Peak width inversely proportional to crystal size.
Thinner peak indicates larger crystal.
Broader peak suggests smaller crystal, defect, or
amorphous nature.

Diffraction Pattern Database Confirmation

Matches unknown compound patterns with literature and
experimental values.
Verifies element identity by matching location, width, and
relative heights of diffraction patterns. Joint Committee on Powder Diffraction
Standards (JCPDS)
International Crystal Structure Database
(ICSD)
 Crystallite size from XRD
Crystallite:
Small crystal composed of multiple atoms/molecules.
A crystallite is that portion of the crystal which diffracts light
coherently.
Calculated using XRD diffractogram using Scherrer's formula.
Grain:
During crystal growth, multiple nucleation centers
responsible for grain formation.
Grain contains multiple crystallites.
Grain size is detected using SEM.
Particle:
Consists of single crystal or agglomeration of several grains.
Grains combine to form particles.
Particle size always larger than crystallite size.
Particle size is detected using TEM.
 Crystallite Size
Crystallite size: D= k λ/β cos θ.
β=FWHM in radians, θ= Bragg angle, λ= X-ray wavelength.
k=Scherrer constant depends on shape.
0.94 For FWHM of spherical crystals with cubic symmetry.
Full width at half maximum (FWHM)

P.H.
Scherrer
(1890-
1969)
 XRD numerical problems
1. If X-rays of wavelength 0.9 Å are diffracted at an angle of 7 0 in
the first order, what is the spacing between the adjacent planes of
the crystal in Å? According Bragg’s law
Solution: 2dsin θ= nλ
Wavelength of X-rays= 0.9 Å = 0.9x10-10 m 2 x d x sin(70)= 1x 0.9x10-10
Angle (θ)= 70 2x d x 0.1218 = 1x 0.9x10-10
First order reflection=n=1 d= 0.9x10-10/0.2436
Spacing between the adjacent planes=d=? d=3.6946x10-10 cm
3.6946 Å

2. Estimate the crystallite size of the given nanomaterial using p-XRD data: Peak
position 2θ = 21.61o, FWHM of sample = 2.51o, k = 0.9 and λ = 1.5406 Å (degree to
radian = Degree × π/180).
Given: According to Scherrer’s equation D= : kxλ
2θ = 21.61o (θ = 10.805o) βx Cosθ
β= FWHM = 2.51o (0.043825 radian) Crystallite size= 0.94x0.15406
k = 0.94 0.043825x0.982257
λ = 1.5406 Å (0.15406 nm) D = 3.22 nm
XRD patterns for 3 different forms
of SiO2

These three phases of SiO2

are chemically identical.
The amorphous glass does
not have long-range atomic
order and therefore produces
only broad pattern.

Cristobalite form polycrystalline

structure.
Quartz form single crystal
structure.
 Applications, Advantages and Disadvantages
Applications:
Distinguishing between crystalline and amorphous materials.
Details unit cell dimensions, atom positions, and crystal symmetry.
Determining the texture of polygrained materials.
Measuring strain and small grain size.
Advantages:
Lowest cost, convenience, and widely used for crystal structure determination.
No significant air absorption, requiring no evacuated chamber.
. Nondestructive technique
Disadvantages:
X-rays do not interact very strongly with lighter elements