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In photo acoustic spectroscopy, the energy absorbed from the infrared radiation is measured by sensing the mechanical vibration produced, and by employing an appropriate acoustic measuring device. A diagram representing the photo acoustic spectroscopic sensing system is shown in figure 23.
The incident radiation is allowed to fall on the sample contained in a suitable enclosure. When the modulated infrared radiation is absorbed by the sample, the substance heats and cools in response to the radiation received. Situated in the enclosure is an acoustic sensing device, which may be a simple microphone or a piezoelectric sensor. The sensor detects the acoustic pulses (caused by the heating of the surrounding gas) as they are generated by the different IR frequencies that are absorbed. The advantage of this type of IR measurement is that it can be used effectively with very black or highly absorbing samples.
Lloyd et al [6] employed a simple micro phonic detector as the sensor, to scan a TLC plate. The thin layer sheets were either aluminium or poly(ethylene terephthalate) backed, and both silica and alumina were used as a thin layer about 250 μm thick. 1 cm diameter discs were excised from the plates and placed in the sample compartment of the microphonic cell. The cell was sealed in a glove bag after purging for 15 minutes with helium The cell itself was fabricated from polished stainless steel with a sodium chloride window, and was supported on vibration-free mounts. It had a total volume of about 0.4 cm3. The IR output from a Nicolet 7199 FTIR spectrometer was focused through the sodium chloride window onto the plate surface. The acoustic waves were detected with a Brüel and Kjoer 4165 microphone, which was exposed to the helium in the cell, through a pipe 10 mm long and 1 mm I.D. Some spectra of tetraphenylcyclopentadienone taken by this procedure are shown in figure 24.
The figure shows the actual spectra as taken, the background spectra of the plate, and the difference spectra of the sample alone. It is seen, by comparison with the spectra obtained from the KBr pellet sample, that reasonably fine structure is disclosed. However, as might be expected, the signal to noise ratio is not very satisfactory, and consequently the absolute sensitivity is not as good as that obtained by other scanning procedures.
About the Author
RAYMOND PETER WILLIAM SCOTT was born on June 20 1924 in Erith, Kent, UK. He studied at the
University of London, obtaining his B.Sc. degree in 1946 and his D.Sc. degree in 1960.
After spending more than a decade at Benzole Producers, Ltd. Where he became head of
the Physical Chemistry Laboratory, he moved to Unilever Research Laboratories as
Manager of their Physical Chemistry department. In 1969 he became Director of Physical
Chemistry at Hoffmann-La Roche, Nutley, NJ, U.S.A. and subsequently accepted the position
of Director of the Applied Research Department at the Perkin-Elmer Corporation, Norwalk, CT, U.S.A.
In 1986 he became an independent consultant and was appointed Visiting Professor at Georgetown
University, Washington, DC, U.S.A. and at Berkbeck College of the University of London; in 1986
he retired but continues to write technical books dealing with various aspects of physical chemistry
and physical chemical techniques. Dr. Scott has authored or co-authored over 200 peer reviewed
scientific papers and authored, co-authored or edited over thirty books on various aspects of
physical and analytical chemistry. Dr. Scott was a founding member of the British chromatography
Society and received the American Chemical society Award in chromatography (1977), the
M. S. Tswett chromatography Medal (1978), the Tswett chromatography Medal U.S.S.R., (1979),
the A. J. P. Martin chromatography Award (1982) and the Royal Society of Chemistry Award in
Analysis and Instrumentation (1988).
Dr. Scott’s activities in gas chromatography started at the inception of the technique,
inventing the Heat of Combustion Detector (the precursor of the Flame Ionization Detector),
pioneered work on high sensitivity detectors, high efficiency columns and presented fundamental
treatments of the relationship between the theory and practice of the technique.
He established the viability of the moving bed continuous preparative gas chromatography,
examined both theoretically and experimentally those factors that controlled dispersion
in packed beds and helped establish the gas chromatograph as a process monitoring instrument.
Dr. Scott took and active part in the renaissance of liquid chromatography,
was involved in the development of high performance liquid chromatography and invented
the wire transport detector. He invented the liquid chromatography mass spectrometry
transport interface, introduced micro-bore liquid chromatography columns and used them
to provide columns of 750,000 theoretical plates and liquid chromatography separations
in less than a second.
Dr. Scott has always been a “hands-on” scientist with a remarkable record of accomplishments in chromatography ranging from hardware design to the development of fundamental theory. He has never shied away from questioning “conventional wisdom” and his original approach to problems has often produced significant breakthroughs.