Introduction to FTIR spectroscopy

FTIR spectroscopy offers a vast array of analytical

opportunities in academic, analytical, QA/QC and forensic
labs. Deeply ingrained in everything from simple compound
identification to process and regulatory monitoring, FTIR
covers a wide range of chemical applications, especially for
polymers and organic compounds. Learn more about the
basics and the value of this popular technique by watching
the tutorials below. Videos also provide an overview of two
common detectors and the apodization function.

What is FTIR?

STRETCHIN BENDING TWISTING

DEFORMATION

FTIR stands for Fourier transform infrared, the preferred

method of infrared spectroscopy. When IR radiation is passed
through a sample, some radiation is absorbed by the sample
and some passes through (is transmitted). The resulting signal
at the detector is a spectrum representing a molecular
fingerprint of the sample. The usefulness of infrared
spectroscopy arises because different chemical structures
(molecules) produce different spectral fingerprints.

So, what is FTIR?

 The Fourier Transform converts the detector output to an
interpretable spectrum.

The FTIR generates spectra with patterns that provide

structural insights.

How does FTIR work and why use it?

The FTIR uses interferometry to record information about a

material placed in the IR beam. The Fourier Transform results
in spectra that analysts can use to identify or quantify the
material.

An FTIR spectrum arises from interferograms being

decoded into recognizable spectra

Patterns in spectra help identify the sample, since

molecules exhibit specific IR fingerprints
FTIR sampling introduction

There are four major sampling techniques in FTIR:

Transmission

Attenuated Total Reflection (ATR)

Specular Reflection

Diffuse Reflectance

Each technique has strengths and weaknesses which motivate

their use for specific samples

Sampling and applications of FTIR

FTIR can be a single purpose tool or a highly flexible research
instrument. With the FTIR configured to use a specific
sampling device transmission or ATR for instance the
spectrometer can provide a wide range of information:

Most commonly, the identification of an unknown

Quantitative information, such as additives or

contaminants

Kinetic information through the growth or decay of

infrared absorptions

Or more complex information when coupled with other

devices such as TGA, GC or Rheometry

Ultimately, FTIR can be a cost-effective answer machine.

Fourier-transform infrared spectroscopy (FTIR) is a
technique used to obtain
an infrared spectrum of absorption or emission of a solid,
liquid or gas. An FTIR spectrometer simultaneously collects
high-spectral-resolution data over a wide spectral range. This
confers a significant advantage over
a dispersive spectrometer, which measures intensity over a
narrow range of wavelengths at a time.
The term Fourier-transform infrared spectroscopy originates
from the fact that a Fourier transform (a mathematical
process) is required to convert the raw data into the actual
spectrum. For other uses of this kind of technique, see Fourier-
transform spectroscopy.

COMPONENTES:

IR sources
FTIR spectrometers are mostly used for measurements in the
mid and near IR regions. For the mid-IR region, 225 m
(5000400 cm1), the most common source is a silicon carbide
element heated to about 1200 K. The output is similar to a
blackbody. Shorter wavelengths of the near-IR, 12.5 m
(100004000 cm1), require a higher temperature source,
typically a tungsten-halogen lamp. The long wavelength
output of these is limited to about 5 m (2000 cm1) by the
absorption of the quartz envelope. For the far-IR, especially at
wavelengths beyond 50 m (200 cm1) a mercury discharge
lamp gives higher output than a thermal source.

Detectors
Mid-IR spectrometers commonly use pyroelectric detectors
that respond to changes in temperature as the intensity of IR
radiation falling on them varies. The sensitive elements in
these detectors are either deuterated triglycine sulfate (DTGS)
or lithium tantalate (LiTaO3). These detectors operate at
ambient temperatures and provide adequate sensitivity for
most routine applications. To achieve the best sensitivity the
time for a scan is typically a few seconds. Cooled
photoelectric detectors are employed for situations requiring
higher sensitivity or faster response. Liquid nitrogen cooled
mercury cadmium telluride (MCT) detectors are the most
widely used in the mid-IR. With these detectors an
interferogram can be measured in as little as 10 milliseconds.
Uncooled indium gallium arsenide photodiodes or DTGS are
the usual choices in near-IR systems. Very sensitive liquid-
helium-cooled silicon or germanium bolometers are used in
the far-IR where both sources and beamsplitters are
inefficient.
Beam splitter
An ideal beam-splitter transmits and reflects 50% of the
incident radiation. However, as any material has a limited
range of optical transmittance, several beam-splitters may be
used interchangeably to cover a wide spectral range. For the
mid-IR region the beamsplitter is usually made of KBr with a
germanium-based coating that makes it semi-reflective. KBr
absorbs strongly at wavelengths beyond 25 m (400 cm1) so
CsI is sometimes used to extend the range to about 50 m
(200 cm1). ZnSe is an alternative where moisture vapor can
be a problem but is limited to about 20m (500 cm1). CaF2 is
the usual material for the near-IR, being both harder and less
sensitive to moisture than KBr but cannot be used beyond
about 8 m (1200 cm1). In a simple Michelson interferometer
one beam passes twice through the beamsplitter but the other
passes through only once. To correct for this an additional
compensator plate of equal thickness is incorporated. Far-IR
beamsplitters are mostly based on polymer films and cover a
limited wavelength range.[9]

Attenuated total reflectance (ATR)

ATR is one accessory of FTIR spectrophotometer to measure
surface properties of solid or thin film samples rather than
their bulk properties. Generally, ATR has a penetration depth
of around 1 or 2 micrometers depending on your sample
conditions.

Fourier transform
The interferogram in practice consists of a set of intensities
measured for discrete values of retardation. The difference
between successive retardation values is constant. Thus,
a discrete Fourier transform is needed. The fast Fourier
transform (FFT) algorithm is used.
ADVENTAGES OF FTIR

Some of the major advantages of FT-IR over the dispersive

technique include:
Speed: Because all of the frequencies are measured
simultaneously, most measurements by FT-IR are made in a
matter of seconds rather than several minutes. This is
sometimes referred to as the Felgett Advantage.
Sensitivity: Sensitivity is dramatically improved with FT-IR
for many reasons. The detectors employed are much more
sensitive, the optical throughput is much higher (referred to as
the Jacquinot Advantage) which results in much lower noise
levels, and the fast scans enable the coaddition of several
scans in order to reduce the random measurement noise to
any desired level (referred to as signal averaging).
Mechanical Simplicity: The moving mirror in the
interferometer is the only continuously moving part in the
instrument. Thus, there is very little possibility of mechanical
breakdown.
Internally Calibrated: These instruments employ a HeNe
laser as an internal wavelength calibration standard (referred
to as the Connes Advantage). These instruments are self-
calibrating and never need to be calibrated by the user