A Beginner FTIR + SEM

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A Beginner’s Guide to FTIR Testing:

Interpreting & Analyzing Results


July 16, 2018 by Jennifer Mathias Leave a Comment

Fourier transform infrared spectroscopy (FTIR) is an incredibly versatile materials


analysis technique, helping identify organic and some inorganic materials that could be
the source of product contamination or cause a malfunction. As a result, we often
recommend FTIR testing to our clients as the first step in the testing process.

But when it comes to understanding and analyzing FTIR results, how we interpret FTIR
spectra is a common question.

Your materials testing lab should be providing you with clear, detailed, and actionable
insights and recommendations in an easy to understand format—something Innovatech
Labs is dedicated to.

With that said, we’ve developed this helpful guide to interpreting FTIR spectra to help
our customers—and anyone else who’s interested—know how to analyze FTIR data.

The Analysis
In order to understand FTIR results, it’s helpful to know a little bit about how FTIR
works.

Essentially, by applying infrared radiation (IR) to samples of materials, FTIR analysis


measures a sample’s absorbance of infrared light at various wavelengths to determine
the material’s molecular composition and structure. The Fourier transform spectrometer
works to convert the raw data from the broad-band light source to actually obtain the
absorbance level at each wavelength.
FTIR spectroscopy can be used on solid, liquid, and gaseous samples. Usually, the
amount of material required for a viable analysis is very small and most analyses can
be done relatively quickly with little sample preparation.

How to Read FTIR Results Graphs


The X-Axis: The Infrared Spectrum
The x-axis—or horizontal axis—represents the infrared spectrum, which plots the
intensity of infrared spectra. The peaks, which are also called absorbance bands,
correspond with the various vibrations of the sample’s atoms when it’s exposed to the
infrared region of the electromagnetic spectrum. For mid-range IR, the wave number on
the infrared spectrum is plotted between 4,000 to 400 cm-1.

The Y-Axis: Absorbance or Frequency


The y-axis—or vertical axis—represents the amount of infrared light absorbed or
transmitted by the material being analyzed.
The Absorbance Bands
Typically, absorbance bands are grouped within two types: Group frequencies and
fingerprint frequencies.

Group frequencies are characteristic of small groups of atoms or functional groups such
as CH₂, OH, and C=O. These types of bands are typically seen above 1,500cm-1 in the
infrared spectrum (See top spectrum in the graph below) and they’re usually unique to
a specific functional group, making them a reliable means of identifying functional
groups in a molecule.

As for fingerprint frequencies, these are highly characteristic of the molecule as a


whole; they tell what is going on within the molecule. These types of absorbances are
typically seen below 1500cm-1 in the infrared spectrum (See bottom graph of figure
below); however, some functional groups will absorb in this region as well. As a result,
this region of the spectrum is less reliable for identification, but the absence of a band is
often more indicative than the presence of a band in this region.
How to Interpret FTIR Spectra
Once the initial testing and spectrum collection is complete, interpretation of FTIR
spectra comes next.

Typically, interpreting FTIR spectra starts at the high frequency end to identify the
functional groups present. The fingerprint regions are then studied to positively identify
the compound. Thankfully, there are vast libraries of infrared spectra available, allowing
our team to compare unknown materials to ensure quick and accurate identification.
Scanning electron microscopy (SEM) is a powerful analytical technique to perform analysis
on a wide range of materials, at high magnifications, and to produce high resolution
images. TWI’s extensively equipped electron microscopy suite allows many different types
of sample to be analysed, giving resolution greatly exceeding that of conventional light
microscopy.

SEM Imaging
SEM relies on the detection of high energy electrons emitted from the surface of a sample after
being exposed to a highly focused beam of electrons from an electron gun. This beam of electrons
is focussed to a small spot on the sample surface, using the SEM objective lens. Variables like the
accelerating voltage used, size of aperture employed and the distance between the sample and
electron gun (working distance) can be optimised to achieve the best quality images.

There are two modes of electron detection which allows for different types of imaging and
analysis, each giving vital insights. Backscattered electrons can be detected to give contrast
based on different chemical compositions across an image. Secondary electrons, emitted close to
the surface of the sample, give information about the surface topography.

Energy-Dispersive X-Ray Spectroscopy


Each of our SEMs are equipped with energy-dispersive X-ray (EDX, also referred to as EDS)
spectroscopy facilities. When exposed to the electron beam, an atom emits characteristic X-rays
unique to its atomic number; this allows a sample’s elemental composition to be analysed,
whether at a single point or over a large region, including line scanning and elemental mapping.
Semi-quantitative analysis can also be performed to assess the chemical composition of a sample.
TWI also has capabilities for wavelength-dispersive X-ray (WDX) analysis to detect light elements,
such as oxygen, nitrogen etc. Combined with conventional SEM analysis, EDX can give a fuller
insight into the local composition of a sample.

Electron Back-Scattered Diffraction


One of the most powerful quantitative techniques is electron back-scattered diffraction (EBSD),
which produces microstructural maps, presenting high-resolution crystallographic data and
analysis of phase distribution, misorientation (strain), grain size and distribution, and preferred
crystallographic orientation (texture). Once a highly specialised technique, this can now be
performed routinely. The technique is highly dependent on excellent sample preparation, which
can be arranged through our metallography laboratories.

TWI’s Electron Microscopy Suite


Environmental Scanning Electron Microscope (Zeiss EVO LS15 SEM)

 
This high-performance LaB6 environmental scanning electron microscope (SEM), fitted with EDX
and WDX detectors, allows for imaging alongside SEM chemical analysis of a wide range of
specimens. It is also equipped with a large sample chamber to accommodate many different
sample dimensions.

Field Emission Gun Scanning Electron Microscopy (Zeiss Σigma FEGSEM)


This scanning electron microscope allows very high-resolution imaging, with clear SEM images
and electron microscopy analysis beyond 50,000× magnification, allowing analysis from micron to
nanometre scale. This can be an essential tool for characterisation of test samples, failure
analysis, fractography in materials including metals, polymers and ceramics, and analysis of
deposits, contaminants and powders. Equipped with EBSD facilities, simultaneous EBSD and
EDX data acquisition can be performed.

Knowledge and Capabilities


With close links to industries in many sectors and a wealth of knowledge and experience, TWI
offer a range of high quality scanning electron microscopy (SEM) analysis and imaging services.
This ranges from small-scale rapid-response material characterisation from one of our
experienced experts to combination as part of a larger project for compliance testing or failure
analysis.

This ranges from small-scale rapid-response material characterisation from one of our
experienced experts to characterisation work as part of a larger project for compliance testing or
failure analysis.

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