Fourier Transform Infrared Spectroscopy

ABOUTFTIR BACKGROUND USES ADVANTAGES

DISADVANTAGES
TYPES OPERATIONPRINCIPLE DEVICE MECHANISMPROCESS TRANSMISSIONTECHNIQUES

SAMPLE PREPARATION
DATAANALYSIS

ABOUTFTIR

FT-IR stands for Fourier Transform InfraRed. Named after J.B.J. Fourier

Includes the absorption, reflection, emission, or photoacoustic spectrum obtained by Fourier transform of an optical interferogram.

ABOUTFTIR

ABOUTFTIR

Identification of unknown materials Determination of the quality or consistency of a sample Determination of the amount of components in a mixture

DEVELOPMENTALBACKGROUND

late 1880s Albert A. Michelson invented the Michelson Interferometer.

Performed the experiment to determine the speed of light. (Michelson Morley experiment).
1907 Michelson received the Nobel Prize in Physics Michelson could not take advantage of the field of Fourier Transform Spectroscopy (FTS).

SCHEMATIC DIAGRAMMICHELSON INTERFEROMETER

DEVELOPMENTALBACKGROUND

1940s Practical Fourier Transform Spectroscopy Used to measure light from celestial bodies.

1949 first Fourier transform spectrum

Different types of interferometers had been developed Lamellar grating Fabry-Perot interferometers

DEVELOPMENTALBACKGROUND

1960 growing interest in interferometric spectroscopy J. W. Cooley and John Turkey fast Fourier Transform (FFT) algorithm
Allowed Fourier transforms to be computed easily on computers available.

DEVELOPMENTALBACKGROUND

1966 the first near infrared planetary spectra was recorded 1969 high resolution and high quality spectra of the planets
first commercial FT-IR spectrometer was sold by Digilab.

DEVELOPMENTALBACKGROUND

1970 commercial fourier transform spectometers became widely accessible. The first FT-IR spectrometers were large and expensive. 1981 Robert Z. Muggli adapted a microscope to a FT-IR spectrometer. 1983 Digilab and Spectra-Tech developed the first commercial FT-IR microspectrophotometer.

DEVELOPMENTALBACKGROUND

First low-cost spectrophotometer capable of recording an infrared spectrum was the Perkin-Elmer Infracord in 1957. Covered the wavelength range from 2.5 m to 15 m Lower wavelength limit - highest vibration frequency due to a fundamental molecular vibration. Upper wavelength limit - spectral region or rock-salt region. Later instruments used potassium bromide prisms and caesium iodide.

DEVELOPMENTALBACKGROUND

Region beyond 50 m is the farinfrared region Merges into the microwave region. diffraction gratings replaced prisms as dispersing elements. More sensitive detectors detect low energy radiation. Electronic computer needed to perform the required Fourier transform.

USES&APPLICATIONS

Identify unknown materials Determine the quality or consistency of a sample Determine the amount of components in a mixture Analysis of liquid chromatography fractions.

Acquire spectrum of light emitted by the sample.

Photocurrent spectra.

USES&APPLICATIONS

Functional Group Analysis

Surface Molecular Composition Chromatographic Effluents Mixture Compound Determination Stereochemistry Molecular Orientation Fingerprinting Identification of Reaction components Identification of Polymer, Resins, and Plastics Formulation of Insecticides and Polymers

USES&APPLICATIONS

ADVANTAGES

Non-destructive technique Provides a precise measurement method which requires no external calibration Increase speed, collecting multiple scans simultaneously Little Sample Preparation Identifies structural isomers

Increase sensitivity and wavelength accuracy

Has greater optical throughput and resolution

Mechanically simple

DISADVANTAGES

FTIR do not measure spectra, only interferograms which are difficult to interpret. Cannot use advanced electronic filtering techniques (lower S-N Ratio than Dispersive) Noise sensitive - affects the radiation from infrared source Uses a single beam changes in infrared absorbing gas can affect results

TYPESofFTIR

FAR-INFRARED FTIR developed for far-infrared range for mechanical tolerance needed for good optical performance. A typical instrument was the cube interferometer developed at the NPL and marketed by Grubb Parsons.

TYPESofFTIR

NEAR-INFRARED FTIR The near-infrared region spans the wavelength range between the rock-salt region and the start of the visible region at about 750 nm. Fundamental vibrations can be observed in this region. It is used mainly in industrial applications such as process control and chemical imaging.

OPERATIONPRINCIPLE

I is the constant level with no modulation present. The second term - spectrum.

The lower integration limit can be set to - since B() = 0 for all negative .
I(x) is defined as the modulated part of the interferogram.

OPERATIONPRINCIPLE

I() is the light source intensity distribution

B() is the modified source function.

DEVICE

Three basic spectrometer components in an FT system: Radiation source

Interferometer
Detector

DEVICE

IMV-4000 The newest most rapid FTIR Array micrscope.

DEVICE

PARTS OF MICHELSON Interferometer

DEVICE

Interferometer
produces a unique signal which contains infrared frequencies encoded into it

Mirrors
reflects the beam transmitted

Beam Splitter
takes the incoming infrared beam and divides it into two optical beams

Detector
where all radiation incident on the interferometer is registered.

DEVICE

Spectrometer Layout

DEVICE

Spectrometer Layout

SPECTROMETERDESIGN

SPECTROMETERDESIGN

SPECTROMETERDESIGN

MECHANISM

1. The Source: Infrared energy is emitted from a glowing black-body source. This beam passes through an aperture which controls the amount of energy presented to the sample 2. The Interferometer: The beam enters the interferometer where the spectral encoding takes place. The resulting interferogram signal then exits the interferometer.

MECHANISM

3. The Sample: The beam enters the sample compartment where it is transmitted through or reflected off of the surface of the sample, depending on the type of analysis being accomplished. This is where specific frequencies of energy are absorbed.

MECHANISM

4. The Detector: The beam finally passes to the detector for final measurement. The detectors used are specially designed to measure the special interferogram signal. 5. The Computer: The measured signal is digitized and sent to the computer where the Fourier transformation takes place. The final infrared spectrum is then presented to the user for interpretation and any further manipulation.

MECHANISM

MECHANISMPROCESS

A collimator is irradiated with monochromatic light yielding a parallel ray of light.

The ray is split into two components in the beam splitter. Following reflection in the mirrors another passage through the beam splitter occurs Rays are added on the detector.

TRANSMISSIONTECHNIQUES

Solid Samples: KBr Disk Technique Quantitative analysis of organic or inorganic substances in powder form.

Thin-Film Technique Polymeric qualitative and quantitative analysis for substances in film form.
Solution Technique Primarily qualitative analysis of substances dissolved in solvent. Uses liquid cells

TRANSMISSIONTECHNIQUES

Liquid Samples: Liquid Film Technique Qualitative analysis of viscous and nonvolatile substances Solution Technique Qualitative analysis of liquids that dissolve in solvent and nonvolatile substances

RELATEDTECHNIQUES

Nuclear magnetic resonance Additional information on detailed molecular structure Mass spectrometry Molecular mass information and additional structural information Raman spectroscopy

Complementary information on molecular vibration.

Facilitates analysis of aqueous samples.

SAMPLEPREPARATION

Samples State Any solid, liquid or gas sample Amount Solids:50 to 200 mg is desirable, but 10 g ground with transparent matrix

1 to 10 g minimum is required if solid is soluble in suitable solvent.

Liquids: 0.5 L is needed if neat, less if pure.

Gases: 50 ppb is needed

Preparation Little or no preparation is required; suitable solvent

SAMPLEPREPARATION

Analysis Time
Estimated time: 1 to 10 min depending on the type of instrument and the resolution required.

Samples are prepared 1 to 5 min.

DATAANALYSIS

Emission Spectrum from a light source

obtained by passing the light through a monochromator,

Intensity of remaining light is measured. Intensity that was directly measured.

DATAANALYSIS

Absorption spectrum
Light source with continuous spectrum in a broad wavelength range. Gas sample placed between the beam splitter and the detector. Measurement Background acquired without the sample cell Measurement done with the cell place in sample compartment. Difference of the measurements measure of the absorption.

DATAANALYSIS

The spectrum of light of blue flame of butane torch.

Horizontal axis is the wavelength of light Vertical axis represents amount of light emitted

DATAANALYSIS

DATAANALYSIS