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FTIR talk letter vol. 17

Others | 2012 | ShimadzuInstrumentation
FTIR Spectroscopy
Industries
Energy & Chemicals
Manufacturer
Shimadzu

Summary

Significance of Topic


Rapid and non-destructive spectroscopic techniques play a key role in real-time monitoring of gas composition, thin-film coatings, and process control. Infrared (IR) and Raman methods offer complementary molecular information, while modern UV-VIS spectrophotometers extend analyses into the near-infrared, supporting research, industry QA/QC, and environmental monitoring.

Objectives and Overview of Articles


These articles present:
  • Comparative analysis of gas chromatography and FTIR gas spectroscopy
  • Automated FTIR quantitation in process control
  • Specular reflection FTIR for thin films and coatings
  • Q&A contrasting Raman and infrared spectroscopy
  • Introduction to enhanced UV-VIS spectrophotometer models

Methodology and Instrumentation


Gas Analysis by FTIR:
  • Transmission FTIR gas cell—integration times, resolution, pathlength adjustments
  • Multipath gas cells for extended optical path and MCT detectors cooled by liquid nitrogen
  • Standard gas calibration and pressure correction

Automated Quantitation System:
  • FTIR interfaced with DCS and PLC for start/stop signals, 4–20 mA output
  • Macro programming for background/sample alternation and endpoint detection

Specular Reflection FTIR:
  • SRM-8000 specular reflectance attachment (10° incidence)
  • Absolute reflectance accessory with V/W mirror arrangements
  • Kramers–Kronig analysis for converting reflectance to absorption
  • Interference fringe analysis for film thickness calculations

Raman Spectroscopy:
  • 532 nm laser excitation, Raman shift spectra (cm⁻¹)
  • Selection rules based on polarizability changes
  • Complementary information to IR, glass-capillary and aqueous solution compatibility

UV-VIS Spectrophotometry:
  • UV-2600 single monochromator (up to 1400 nm with integrating sphere)
  • UV-2700 double monochromator for 8-Abs range and ultra-low stray light
  • Compact design, energy saving, validation software included

Main Results and Discussion


FTIR gas analysis achieved ~1 min multi-component detection without carrier gas or sample pretreatment. Sensitivity differences among gases were linked to molecular dipole activity; multipath cells and integration control improved limits to ppm–ppb levels. Automated FTIR in a reaction furnace demonstrated reliable DCS control and unmanned operation. Specular reflection FTIR identified epoxy resins on aluminum, measured acrylic and polyester film absorption via K-K processing, and determined thickness (~26.4 µm) from interference fringes. Raman spectroscopy distinguished modes invisible to IR, notably C=C vibrations, confirming its complementarity. New UV-VIS models combined extended wavelength range, low noise, and high photometric range in a small footprint.

Benefits and Practical Applications


  • Continuous, non-destructive gas monitoring in environmental and process control
  • Direct thin-film analysis without sample destruction or special pretreatment
  • Automated integration with plant control systems for endpoint detection
  • Complementary IR/Raman datasets enhance substance identification in complex matrices
  • Versatile UV-VIS platforms adaptable to research, QA/QC, and routine analysis

Future Trends and Opportunities


  • Miniaturized and portable spectrometers for field and inline use
  • Advanced detector technologies (e.g., uncooled MCT alternatives, quantum detectors)
  • Enhanced multipath and waveguide cells for sub-ppm gas detection
  • AI-driven spectral libraries and automated peak assignment
  • Integration of IR, Raman, and UV-VIS into unified multi-modal platforms

Conclusion


Infrared gas analysis and specular reflection FTIR offer rapid, versatile, and non-invasive techniques for quantitative and qualitative monitoring of gases and surface films. Automated FTIR systems improve process control, while Raman spectroscopy provides complementary vibrational insights. Modern UV-VIS spectrophotometers extend analytical capabilities into the near-infrared with high sensitivity. Together, these technologies support advanced research and industrial applications.

Used Instrumentation


  • FTIR spectrometer with gas cell and multipath accessories
  • SRM-8000 specular reflectance attachment and absolute reflectance accessory
  • MCT (HgCdTe) detector cooled by liquid nitrogen
  • Raman microscope with 532 nm laser
  • UV-VIS spectrophotometers UV-2600 and UV-2700
  • Distributed control system (DCS) and PLC interfaces

References


  • David Welti (1970) Infrared Vapour Spectra: Heyden & Son Ltd.
  • Sadtler Database, Bio-Rad Laboratories, Inc.
  • Introduction to Spectroscopy Series, Vol. 6 – IR and Raman Spectroscopy, Spectroscopical Society of Japan
  • Masayuki Tanaka, Norio Teramae, IR Spectroscopy, Kyoritsu Shuppan Co., Ltd.
  • Mitsuo Tasumi, FT-IR Fundamentals and Actualities, Tokyo Kagaku Dojin
  • Yukihiro Ozaki (ed.), NIR Spectroscopy, Japan Scientific Societies Press

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