Chem 302 Lab Instrumental Analysis Laboratory

AY 2015-2016

Perkin-Elmer FT-IR Spectrometer Spectrum Two

Spectrum Two
Perkin-Elmer
Perkin-Elmer Instruments (Philippines) Corporation
(02) 637 0180

Prepared by:
GROUP 4
13 Dimaculangan, Reyza Kathleen A.
14 Domingo, Emmanuel Ramil A.
15 Espejo, Anna Dominique S.
16 Florin, Neil Anthony D.
3Chem

Introduction:
Infrared Spectroscopy has always been an important technique for material analysis in the
laboratory. An infrared spectrum represents a fingerprint of a sample with absorption peaks
which correspond to the frequencies of vibrations between the bonds of the atoms making up
the material. Because different materials possess a different combinations of atoms, no two
compounds produce the exact same infrared spectrum. Therefore, infrared spectroscopy results
to a positive identification (qualitative analysis) of every different kind of material. But it can also
make quantitative analysis because the size of the peaks in a spectrum indicates the amount of
a specific material is present.
The development of infrared spectrometers up until the existence of fourier transform
infrared spectrometer has been filled loops, turns and adjustments. The first generation IR
spectrometer was invented in late 1950s. It utilizes prism optical splitting system. The prisms
are made of sodium chloride. The requirement of the samples water content and particle size is
extremely strict. Furthermore, the scan range is narrow. Additionally, the repeatability is fairly
poor. As a result, the first generation IR spectrometer is no longer in use. The second
generation IR spectrometer was introduced to the world in 1960s. It utilizes gratings as the
monochrometer. The performance of the second generation IR spectrometer is much better
compared with IR spectrometers with prism monochrometer, but there are still several
prominent weaknesses such as low sensitivity, low scan speed and poor wavelength accuracy
which rendered it out of date after the invention of the third generation IR spectrometer, the
fourier transform infrared spectrometer.

The preferred method of infrared spectroscopy for the present generation is the fourier
transform infrared spectroscopy. It follows the same principle for infrared spectroscopy, IR

radiation is passed through a sample. Some of the infrared radiation is absorbed by the sample
and some of it is passed through (transmitted). The resulting spectrum represents the molecular
absorption and transmission, creating a molecular fingerprint of the sample which makes
infrared spectroscopy very useful for several types of analysis. It can be used in identifying
unknown materials, determine its consistency or quality, and determine the amount of
components of the mixture. FTIR spectrometers (Fourier Transform Infrared Spectrometer) are
widely used in organic synthesis, polymer science, petrochemical engineering, pharmaceutical
industry and food analysis. In addition, since FTIR spectrometers can be hyphenated to
chromatography, the mechanism of chemical reactions and the detection of unstable
substances can be investigated with such instruments.
A common FTIR spectrometer consists of a source, interferometer, sample
compartment, detector, amplifier, A/D converter, and a computer. The source generates
radiation which passes the sample through the interferometer and reaches the detector. Then
the signal is amplified and converted to digital signal by the amplifier and analog-to-digital
converter, respectively. Eventually, the signal is transferred to a computer in which Fourier
transform is carried out. At 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 and, ultimately, to the detector. The beam enters the interferometer where the
spectral encoding takes place. The resulting interferogram signal then exits the interferometer.
When the interferogram signal exits the interferometer, it will be transferred to the A/D converter
which stands for analog to digital converter. It transforms the data from an analogue one, which
is the signal, to a digital data where the computer can read the information and process the data
for displaying in the screen.
FTIR is only one of the many types of spectrometer like absorption spectrometer,
fluorescence spectrometer, X- ray spectrometer, Flame spectrometer, and many others. Like all

spectrometers, Fourier Transform Infrared Spectrometer also records and measures spectra for
data analysis, but FTIR is useful for matching unknown substances to known materials to help
identify them. Since it also reads spectra, it also provides a clue of the substances structure.
Since like all analysis method, FTIR methods also need another method for its data to be
precise and will help for further characterization of the unknown substance.
There are five types of spectrometer, namely Optical Spectrometer, Mass Spectrometer,
Time-of-Flight Spectrometer, and magnetic spectrometer. Optical Spectrometer uses different
intensities of light to obtain data from the sample. Mass Spectrometer uses mass-to-charge ratio
and abundance of gas-phase ions to get the amount and type of a substance. Time-of-Flight
Spectrometer uses the time of flight between two detectors to obtain the energy spectrum of a
known substance. Magnetic Spectrometer uses magnetic fields where the sample will be
passed through to obtain the relative content of the various masses of the sample. FTIR falls
under optical spectrometer since it uses optical methods to get the spectra of the unknown
substance.
Block Diagram:

Fixed
Moving
Mirror
Sourc

Collimat

Sample
Compartm
ent
Detect
or

Schematic Diagram:

Operating Instruction
Start-up Procedure
1
2
3
4
5
6
7
8
9

Turn ON the computer

Open the Spectrum program
Click the Instrument tab in the right side of the screen
Click the Setup Instrument Basics tab
Set the required Abscissa units, Ordinate units, Start and End, Scan type, Resolution
and Accumulations
Setup Instrument Advance tab and Check CO2/H2O box
Open background
Place the sample at the top of ATR crystal
Then obtain the sample and SCAN

Shut-down Procedure
1
2
3
4

Save the file and print the spectra obtained

Close the software
Turn OFF the Computer
Remove the KBr disc holder or ATR stage

Precaution and Hazard

1
2
3
4
5
6
7

Make sure that the instrument are not connected with any voltage sources before
opening
Wear safety goggles to protect the eyes from burning liquid nitrogen
Exposure to liquid nitrogen may cause skin burn
Avoid any contact to flammable or toxic solvent
Do not touch the infrared resource (it may be very hot)
Do not place anything at the top of spectrometer
Avoid staring at the laser beam

Instrument Maintenance
1.
2.
3.
4.

Any optical surface of the instrument should not be touched.

Use damp cloth and mild detergent when cleaning the instrument.
Use grease, damp cloth and mild detergent to clean the Display of the instrument.
Condensation may occur when the instrument is moved from a cooler environment to a
warmer one and this may cause damage to the instrument. To avoid such damage,
protect the windows with fresh bags of dessicant and allow the instrument to equilibrate

with the surrounding temperature before removing the dessicant.

5. Do not use flammable gas when purging the instrument.
6. Never connect the purge tubing to a gas cylinder or anything with a high pressure
supply.
7. Before opening the instrument cover, switch off the mains power supply and wait 60
seconds and disconnect power cable.
8. Do not open main cover if >75% humidity for an instrument with KBr optics and >45 for
an instrument with CsI optics.
9. When replacing the source, avoid touching the bulb as its lifespan may shorten.
10. When replacing the windows, be careful not to get moisture on the surface.
11. Do not separate the laser from the power supply.
References:
D.A. Skoog, D.M. West, F.J. Holler & S.R. Crouch. Fundamentals of Analytical Chemistry, 8th
edition. Thomson learning, Inc.,Brooks/Cole 2004.