KWAME NKRUMAH UNIVERSITY OF SCIENCE AND TECHNOLOGY, KUMASI

COLLEGE OF ENGINEERING

DEPARTMENT OF MATERIALS ENGINEERING

A REPORT ON AAS AND SEM ANALYSIS IN ENGINEERING MATERIALS AT THE

MATERIALS ENGINEERING LABORATORY

BY GROUP 7

Abstract
This comprehensive report provides the various operations and analysis of AAS and SEM
information. The AAS gives information for numerous application such as for elemental analysis
for liquid samples while the molecular method for bulk specimen composition for the analysis of
solid materials of which the SEM is a key instrument for such purpose.

Introduction
The aim of this experiment is to familiarize with the basic operation principles, sample
preparation and result interpretation of the AAS and SEM. For AAS sample is introduced by
spraying into a flame with good reproducibility and with high efficiency in the higher regions of
the flame the thermal dissociation of the molecules occurs: ground state atoms are formed for
atomic absorption measurement.
The SEM on the other is also a powerful versatile instrument for analysis of solid materials. In
SEM, an electron beam is moved in a raster pattern across the surface of a sample and the beam
interacts with the sample which can be analyzed to provide useful information about topography,
composition, crystallography etc. the primary motivation for using SEM is to the fact that
electrons have a much shorter wavelength than light and uses longer focal length.

Theory
The magnification of an SEM is determined by the ratio of the linear size of the display screen to
the linear size of the specimen area being scanned

d = diameter of electron beam used in SEM,

f = focal length
The Atomic Absorption Spectrometry is based on when energy is transferred to the atoms of
certain gases, they emit a characteristic spectrum consisting of lines. Furthermore these atoms
can absorb light having the same wavelength as the wavelength of the emitted ones. Flames are
used in this process in the AAS.

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Instrumentation for AAS
Light Sources Hollow-Cathode Lamps, Laser
AtomizationFlames, Graphite furnaces, Plasma (ICP)
Detection Methods Photomultiplier tube (PMT)
Instrumentation for SEM
-Electron optical column
-A vacuum system
-Electronics

MODE OF OPERATION OF AAS AND SAMPLE PREPARATION

First, the sample (50-100mg) in the form of a liquid is passed through a capillary tube and into
the nebulizer. Here, it is converted into fine spray of droplets. These droplets are moved using
carrier gases into the burner slot which contains the flames.
In the flame, three major things happen to the sample. First, it undergoes desolation- burning out
of the solvent leaving only compounds. Afterwards, the compounds undergo decomposition due
to the intense heat in the flame. Finally, free atoms and ions are left in the flame. Light from the
hollow cathode lamp specific for each element to be detected- is passed through the base of the
flame for the excitation of electrons.
There is an electron detector which is so sensitive to recognize any changes in light intensity
between hollow cathode lamp and the extra light given off by the sample.

Figure 1 showing how AAS work.

Analysis of result
When light is absorbed by a sample, the radiant power P (energy per unit time per unit area) of
the beam of light decreases. The energy absorbed may stimulate rotation, vibration or electronic
transition depending on the wavelength of the incident light.
Concentration measurements can be made from a working curve after calibrating the instrument
with calculated and plotting it against calculated absorbance as shown in FIGURE 2 below.

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 Figure 2 showing a plot of concentration against absorbance

Conclusion
The AAS has been a very useful instrument that has many useful applications. The AAS can be
used in determining elemental compositional analysis in food analysis, Water analysis, analysis
of soil, analysis of additives in lubricating oil or grease and for Clinical analysis on blood
samples, whole blood, plasma.

SEM analysis
SEM is a type of electron microscope that images the sample surface by scanning it with a high-
energy beam of electrons. Scanning is done simultaneously in two perpendicular directions, a
square or rectangular area of specimen (known as a raster). A scanning electron microscope
consists of an electron gun and a series of electromagnetic lenses and apertures

Sample preparation
Material to test are turn on vacuum pump control and vent the specimen chamber. After pressure
equalization shake up the cover plate of specimen chamber the specimen is coated with gold
plate and are reassembled.
Minimal preparation of specimens in order to preserve features of their surfaces. Common
contaminants on the specimen surfaces are hydrocarbons from oil and grease, because an
electron beam decomposes any hydrocarbon and leaves a deposit of carbon on the surface.
Surfaces with oil or grease contamination should be cleaned by an organic solvent
such as methanol or acetone in an ultrasonic cleaner.

Mode of operation
The interaction of a high-energy beam with the specimen will produce various effects resulting
in a range of signals being emitted. The incidental electrons interact with specimen atoms and are
significantly scattered by them. Most of the energy of the electron beam will eventually end up
heating the sample. However, before electrons come to rest, they undergo two types of
scattering: elastic and inelastic.
Electron field between cathode and anode accelerate the electrons downward called primary
electrons and these electrons knock out specimen material and the knocked down electrons
produced are called secondary electrons

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Fig. 3 showing the interaction of electron on specimen surface

Discussion of result
A specimen for SEM analysis can be in any form. This is one reason that SEMs are more widely
used than TEMs. However, there are special problems in SEM specimen preparation such as
surface charging of specimens that have poor electric conductivity and dehydration requirement
for biological samples
When high energy electrons strike a specimen, they produce either elastic or inelastic scattering.
Elastic scattering produces the backscattered electrons (BSEs), which are incident electrons
scattered by atoms in the specimen
BSEs are typically deflected from the specimen at large angles and with little energy loss
BSEs are useful for formation of elemental composition contrast
BSEs are typically deflected from the specimen at large angles and with little energy loss
BSEs are useful for formation of elemental composition contrast

Fig 4. showing how signals are detected in SEM

The electron beam emitted from an electron gun is condensed to a fine probe for surface
scanning. The signal electrons emitted from the specimen are collected by a detector, amplified,
and used to reconstruct an image

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Conclusion
The SEM provides information such as topography, morphology, specimen composition
crystallography information.

REFERENCES
[1]- Materials Characterization: Introduction to Microscopic and Spectroscopic Methods, Yang
Leng, John Wiley & Son, Singapore, ISBN 978-0-470-082298-
[2]-City University of Hongkong Laboratory for undergraduates, Manual. Available at:
www6.cityu.edu.hk//AP5301Lab.PDF.

Laboratory Write-up
1. The most commonly used flames in flame spectrometry are; air-acetylene flame and
nitrous oxide system (N2O) acetylene flame.

2. Samples are first made liquid if they are not. Then they are passed through capillary tube
into the nebulizer where they are converted into spray and transferred by spraying in the
flame in the spectrometer

3. There is an electron detector (photomultiplier tube) which is so sensitive to recognize any

changes in light intensity between hollow cathode lamp and the extra light given off by
the sample. The principle is: Photons impacted to K photosensitive cathode product
electrons which flow towards the P1 dinode due to the potential between P1 dinode and
K cathode. Electrons impacting to P1 dinode creates a seconder electron emission of
which intensity is larger than the primer electron current. This process is repeated on the
dinodes until the anode.

4. A. Comprehensive calibration technique- It can be applied in case of big number samples

of the same type. The comprehensive solution series contain increasing quantity of the
examined elements. Moreover, the standards may contain other components present in
the samples in average concentration. Since the composition of validation series made by
this way is about the same with sample composition, the arising interfering effects will be
about the same. The parts of the calibration series are usually diluted from a stock
solution with exactly known concentration.

B. Standard addition- It is applied primarily in case of so called exponential interfering

components respectively. The point of the method is that the samples are divided into 3=5
equal parts. We give to each portion increasing amount of examined metal ion in the same
volume. To the first portion we dont add any metal ion solution thus it contains the
examined metal ion in the original concentration to the other members known increasing
amount of examined metal solution is given. The linear line fit to measure points
(intensity of emission or absorbance) intersects the abscissa axis beyond 0 in negative
range. The scale is the same than in positive range. The absolute value of the distance
between the intersect and the origin gives the metal ion concentration of the sample.

5. The stronger condenser lens causes more of the beam to be stopped by the objective
aperture and thus a reduction in probe current occurs. Beam current increases to the 8/3
power as probe diameter increases. Adequate current is essential to produce better

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 contrast images. Hence, accelerating voltage causes better images as well. Decreasing the
diameter of the aperture will: decrease lens aberrations and thus increase resolution. It
will also decrease the probe current, decrease the convergence angle of the beam and thus
increase depth of focus.

6. When high energy electrons strike a specimen, they produce either elastic or inelastic
scattering. Elastic scattering produces the backscattered electrons, which are incident
electrons scattered by atoms in the specimen. These are typically deflected from the
specimen at large angles and with little energy loss. They are useful for formation of
elemental composition contrast. Inelastic scattering produces secondary electrons which
are electrons ejected from atoms in the specimen. They are typically deflected at small
angles and show considerably low energy compared with incident electrons. These
electrons are the primary signals for achieving topographic contrast.

7. Carbon tape and Carbon paint can be used on the surface, to prevent the surface charging.

8. Specimens that have poor electric conductivity and dehydration requirement for
biological samples, experience a phenomenon known as surface charging. Here,
excessive electrons accumulate on the specimen surface where it is impinged by the
electron beam and they remain due to low conductivity of the specimen. Hence, the
introduction of the sputter coating makes the surface conductive in order to prevent this
phenomenon. The coating might become a problem when it is done on an already
conductive surface. This would cause more electrons to leave the sample quickly instead
of taking a while to knock electrons in the specimen. An image may therefore not be
clearly created.

9. Some of the trade- offs are; higher resolution, possibility of X-ray microanalysis and
EELS, among others.