UNIT V
OTHER TESTING
Thermal Testing: Differential scanning calorimetry, Differential thermal analysis. Thermo-
mechanical and Dynamic mechanical analysis: Principles, Advantages, Applications. Chemical
Testing: X-Ray Fluorescence, Elemental Analysis by Inductively Coupled Plasma-Optical
Emission Spectroscopy and Plasma-Mass Spectrometry.
Materials Testing – Measurement of the characteristics and behaviour of substances like metals,
ceramics, plastics, etc.
Categories of Material Testing
Testing for physical and chemical properties
Testing for thermal properties
Testing for electrical properties
Testing for resistance to corrosion
Testing for Radiation and Biological deterioration
Thermal Analysis
It is a form of analytical technique most commonly used in the branch of materials science
where changes in the properties of materials are examined with respect to temperature.
Thermal Properties
Thermal Conductivity – Temperature as a function of time along the length of a bar.
Specific Heat – Heat absorbed per unit mass per degree change in temperature.
Thermal Expansion - Tendency of matter to change its shape, area, volume, and density in
response to a change in temperature.
Thermal Stress – Stress experienced by a body due to thermal expansion.
Thermo-Elastic Effect - Temperature change resulting from stretching or contracting of an elastic
material.
Thermal Shock - A mechanical load caused by a rapid change of temperature of a certain point.
Melting Point or Heat Resistance - Ability to resist and remain unaffected by heat.
Emissivity of Materials - The measure of an object's ability to emit infrared energy.
Latent Heat of Fusion of Materials - the enthalpy change of any amount of substance when it
melts.
Latent Heat of Vaporization of Materials - the heat consumed or discharged when matter
disintegrates, changing stage from fluid to gas stage at a consistent temperature.
Thermal Testing Parameters
Thermal analysis is a branch of material science for studying the thermophysical and
kinetic properties of materials with temperature. Thermal properties can be measured as
function of temperature or time over a wide temperature range from − 150°C to 1600°C.
Sl. No Method Parameter Testing
1 Thermogravimetric Analysis Mass Changes
2 Differential Thermal Analysis Temperature Difference
3 Differential Scanning Calorimetry Heat Difference
4 Evolved gas analysis Gas Decomposition
5 Thermo Mechanical Analysis Deformation and Dimension
6 Dilatometer Volume
7 Dielectric Thermal Analysis Electrical Properties
8 Thermo Optical Analysis Optical Properties
Thermogravimetric Analysis
Thermogravimetric analysis (TGA) is an analytical technique used to determine a material's
thermal stability and its fraction of volatile components by monitoring the weight change that
occurs as a sample is heated at a constant rate.
Thermogravimetric analyzer
A typical thermogravimetric analyzer consists of a precision balance with a sample pan located
inside a furnace with a programmable control temperature. The temperature is generally
increased at constant rate to incur a thermal reaction. The thermal reaction may occur under a
variety of atmospheres including ambient air, vacuum, inert gas, oxidizing/reducing gases,
corrosive gases, carburizing gases, vapors of liquids as well as a variety of pressures including:
a high vacuum, high pressure, constant pressure, or a controlled pressure.
Types of TGA
Isothermal or static thermogravimetry
Quasistatic thermogravimetry
Dynamic thermogravimetry
Thermogravimetric Analysis
Differential Scanning Calorimetry
Differential scanning calorimetry (DSC) is a thermo-analytical technique in which the difference
in the amount of heat required to increase the temperature of a sample and reference is measured
as a function of temperature.
Types of DSC
Heat-flux DSC
Power differential DSC
Modulated DSC
Hyper DSC
Pressure DSC
Differential Scanning Calorimetry
Differential Thermal Analysis
DTA involves heating or cooling a test sample and an inert reference under identical
conditions, while recording any temperature difference between the sample and reference. This
differential temperature is then plotted against time, or against temperature, permitting the
calculation of the heat flow difference between reference and sample, which are kept in almost
identical environments (DTA furnace). Therefore, changes in the sample which lead to the
absorption or evolution of heat can be detected relative to the inert reference.
Differential Thermal Analysis
Thermo-Mechanical Analysis
The measurement of a change of dimension of the sample with a negligible force acting on the
sample while it is subjected to a temperature is called thermodilatometric analysis (TDA).
Thermo mechanical Dynamic Analysis
It is most useful for studying the viscoelastic
behavior of polymers. A sinusoidal stress is
applied and the strain in the material is measured.
The temperature of the sample or the frequency
of the stress are often varied, leading to variations
in the dynamic modulus. This approach can be
used to locate the glass transition temperature of
the material, as well as to identify transitions
corresponding to other molecular motions.
Chemical Analysis
It is used to identify the contents, composition and quality of the materials used in product
development, manufacturing and Testing.
Chemical Properties
Toxicity - the degree to which a substance or mixture of substances can damage an organism.
Reactivity – tendency of a substance to undergo chemical reaction.
Coordination Number – the number of neighbor atoms with respect to a central atom.
Oxidation States – the charge of an atom if all bonds it formed were ionic bonds.
Flammability – the ability of a chemical to burn or ignite, causing fire or combustion.
Acidity - the tendency of a compound to act as a proton/H+ donor.
Basicity - ability to accept a proton/Hydrogen ion.
Radioactivity - the particles which are emitted from nuclei as a result of nuclear instability.
Gas Chromatography
Chemical Testing Chromatography
Ion Chromatography
Technique
Chemical testing tells us what a certain material Liquid
or product is made of. Various chemical testing Chromatography
methods are used across a wide range of
Gas Chromatography
Chemical Composition
industries to help manufacturers and suppliers Mass Chromatography
ensure their products comply with regulatory Mass Spectroscopy
Technque
safety requirements. Inductively Coupled
Plasma
Tests
FTIR
X-Ray-EDS &XRF
Analysis
Spectroscopy Inductively Coupled
Technique Plasma
Wet Chemistry Atomic Absorption
Technique Graphic Furnace
Spark Atomic
Emissions
X-Ray Fluorescence
An X-ray fluorescence (XRF) spectrometer is an x-ray instrument used for routine, relatively
non-destructive chemical analyses of rocks, minerals, sediments and fluids. It works on
wavelength-dispersive spectroscopic principles that are similar to an electron microprobe
(EPMA). However, an XRF cannot generally make analyses at the small spot sizes typical of
EPMA work (2-5 microns), so it is typically used for bulk analyses of larger fractions of
geological materials.
Types
Energy Dispersive X-Ray Fluorescence with direct excitation
Energy Dispersive X-Ray Fluorescence with polarized excitation
Wavelength Dispersive X-Ray Fluorescence
Elemental Analysis
Elemental analysis is a process where a sample of some material (e.g., soil, waste or drinking
water, bodily fluids, minerals, chemical compounds) is analyzed for its elemental and sometimes
isotopic composition.
Methods of Elemental Analysis
CHNX Analysis – determination of carbon, hydrogen, Nitrogen and heteroatoms.
Nuclear Magnetic Resonance (NMR), Mass Spectrometry Chromatographic,
Combustion Analysis
Quantitative Analysis – determination of the mass of each element.
Gravimetry Analysis, Optical atomic Spectroscopy, Neutron activation Analysis
Qualitative Analysis – to determine which element present in the sample
Atomic Spectroscopy, Inductively coupled plasma mass spectroscopy, X-Ray
Fluorescence, Particle-induced X-Ray emission, X-Ray Photolectron spectroscopy,
Auger electron Spectroscopy, Sodium fusion test
Plasma
An electrical conducting gaseous mixture containing significant amount of cations and electrons.
(net charge approaches zero)
Types of Plasma
Direct current plasma (DCP)
Microwave-induced plasma (MIP)
Capacitively Coupled Microwave plasmas (CMP)
Inductively Coupled plasma (ICP)
Advantages
Increased atomization
Wider range of elements
Simultaneous multielement analysis
Wide dynamic range
Inductively-coupled plasma (ICP)
An inductively coupled plasma (ICP) or transformer coupled plasma (TCP) is a type of plasma
source in which the energy is supplied by electric currents which are produced by
electromagnetic induction, that is, by time-varying magnetic fields.
IT is an ionization source that fully decomposes a sample into its constituent elements and
transforms those elements into ions. It is typically composed of argon gas, and energy is
"coupled" to it using an induction coil to form the plasma.
Optical Emission Spectroscopy
Optical emission spectrometry involves applying electrical energy in the form of spark
generated between an electrode and a metal sample, whereby the vaporized atoms are brought to
a high energy state within a so-called "discharge plasma“.
Classification
Inductively coupled optical emission spectroscopy.
Glow discharge optical emission spectroscopy (GD-OES) or Glow discharge MS (GDMS).
Arc spark optical emission spectroscopy
Flame emission spectroscopy
Inductively coupled optical emission spectroscopy
Inductively coupled plasma atomic emission spectroscopy (ICP-AES), also referred to as
inductively coupled plasma optical emission spectrometry (ICP-OES), is an analytical technique
used for the detection of chemical elements. It is a type of emission spectroscopy that uses the
inductively coupled plasma to produce excited atoms and ions that emit electromagnetic radiation
at wavelengths characteristic of a particular element. The plasma is a high temperature source of
ionised source gas. The plasma is sustained and maintained by inductive coupling from cooled
electrical coils at megahertz frequencies. The source temperature is in the range from 6000 to
10,000 K. The intensity of the emissions from various wavelengths of light are proportional to the
concentrations of the elements within the sample.
Construction
Sample Introduction – Nebulizer, pump, spray champers, Drains.
Production of Emission – Torches, Radiofrequency generators.
Collection and detection of emission – Transfer optics, Wavelength dispersive devices, Detectors.
Signal processing and Instrument control – Signal processing, Computers and processors, Software.
Inductively coupled optical emission spectroscopy
Inductively coupled Plasma mass spectrometry
Inductively coupled plasma mass spectrometry (ICP-MS) is a type of mass spectrometry that
uses an Inductively coupled plasma to ionize the sample. It atomizes the sample and creates
atomic and small polyatomic ions, which are then detected. It is known and used for its ability to
detect metals and several non-metals in liquid samples at very low concentrations. It can detect
different isotopes of the same element, which makes it a versatile tool in Isotopic labeling.
Summary
Elemental Analysis
Material Testing
Plasma
Thermal Analysis
Inductively coupled plasma (ICP)
Thermal Properties
Optical Emission Spectroscopy
Thermal Testing Parameters
Inductively coupled optical
Thermogravimetric Analysis emission spectroscopy
Differential Scanning Calorimetry Inductively coupled Plasma mass
Differential Thermal Analysis spectrometry
Thermo-Mechanical Analysis
Thermo mechanical Dynamic
Analysis
Chemical Testing
X-Ray Fluorescence
