Infrared and Raman
Instrumentation |
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Infrared
The
Perkin-Elmer Spectrum Spotlight 300 infrared imaging microscope is a fully
integrated system, which can be employed in both array and point detector
imaging modes. The array detection mode allows one to generate molecular
specific images over a total area of 1.64 cm2 consisting of up to 260K
spectra. Pixel resolution in this mode is either 6.25 or 25 micrometers
allowing images to be collected more rapidly than the serial collection
point detector. The array detector provides a useful spectral range of
7800 to 720 cm-1, while the point detector affords a range of 7800 to
580 cm-1. Transmission, reflection and ATR spectra and images can be collected
in the point mode, while only transmission and reflectance capabilities
are available with the array detection. ATR mapping using the array detector
is currently being developed in our laboratory.
The MML has recently acquired this imaging microscope as part of a research agreement with Spectral Dimensions, Inc. The system is based on the Spectra-Tech ImageMax microscope, a stepscan interferometer, and a 64 X 64 MCT focal plane array detector. System features include both transmission and reflection sampling modes with a theoretical spatial resolution of 6 micrometers. The range of the detector provides spectral coverage from 5000 to 900 cm-1. An auxiliary macro sampling compartment is available for use on larger samples. The system can also be employed for ATR imaging on both the micro and macro configurations.
The Perkin-Elmer
Autofocus microscope is the work horse of the MML. This multipurpose system
can be used to collect transmission, reflection absorption, diffuse reflectance
and Attenuated Total Internal Reflectance (ATR) spectra on samples as
small as 5 micrometers in diameter. The system features an Infrared Microspectroscopy
Automated Graphical Environment (IMAGE) which permits automated mapping
analyses to be conducted on a wide variety of samples. Two dimensional
images based on either infrared or visible wavelengths can be collected
and displayed in a wide variety of formats. These formats include band
ratios, functional group maps, spectra from individual pixels and profiles
or cross-sections. The standard detector employed on the microscope is
a medium band HgCdTe detector which yields a spectral range of 4400 to
580 wavenumbers. A Harrick Split-Pea micro-ATR sampling accessory is also
integrated to the system for extended wavelength coverage down to 450
wavenumbers.
Raman
Confocal Raman spectra are collected with a Renishaw System 2000 Raman Imaging Microscope. This highly efficient system employs a variety of lasers and Peltier cooled CCD detector for excitation and detection of Raman scattered light, respectively. The system features fast full range scanning (100 to 4000 wavenumbers) and direct 2-D Raman imaging. Spatial resolution (x,y) of 1 micrometer and axial resolution of 2 micrometers can be achieved with the use of the confocal feature. The system has also been modified to obtain confocal images and spectra in both fluorescence and visible modes.
The MML has recently designed and constructed a third generation refracting microscope for use on the Perkin-Elmer System 2000. This instrument has been fully optimized as a FT-Raman spectrometer. Spatial resolution (x,y) of the microscope is 4 micrometers. The system employs a 1 watt diode pumped ND/YAG laser for excitation and a high sensitivity InGaAs detector. In addition to microsampling, Raman spectra of macro samples can be obtained in either the 90 or 180 degree scattering geometries. This instrument is typically employed for samples which fluoresce or are highly colored. The above example demonstrates the analysis of an Aleve pharmaceutical tablet. The spectra show that titanium dioxide is incorporated into the surface of the tablet.
A recent addition to the laboratory is a Renishaw MKIII process control Raman microprobe. The fiber coupled probe head which is tethered to a 2 meter fiber optic cable allowing it to be used in a wide variety of sample situations. The system is based on a short focal length spectrograph that yields a resolution of 12 cm-1. A Lexel Argon ion laser serves as the excitation source producing powers of up to 500 milliwatts at the sample.
The MML has recently
constructed a UV/VIS microprobe based on an Ocean Optics S2000 miniature
spectrograph. The Olympus BH-2 coupled to this spectrograph has both transmitted
white light and reflectance illumination modes, which can be utilized
for UV/VIS and fluorescence spectroscopies. The system is confocal and
provides a 5 micrometer spatial resolution, which is dictated by the entrance
slit of the spectrograph. The system is usable over the range of 350 to
1100 nm. We have employed the system for mainly geologic thin sections
and the measurement of film thickness via thin film interference.
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