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Spectroscopic Methods

Spectroscopic Methods. PART 3. IR Instrumentation. IR Instrumentation. Absorption Spectrometer. Signal Processor Readout. Source. Sample. Wavelength Selector. Detector. IR Instrumentation. Components of Optical Instruments. (a) Construction materials.

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Spectroscopic Methods

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  1. Spectroscopic Methods • PART 3

  2. IR Instrumentation

  3. IR Instrumentation Absorption Spectrometer SignalProcessor Readout Source Sample WavelengthSelector Detector Dr. S. M. Condren

  4. IR Instrumentation

  5. Components of Optical Instruments (a) Construction materials Dr. S. M. Condren

  6. Components of Optical Instruments (b) wavelength selectors for spectroscopic instruments.

  7. Components of Optical Instruments (c) Sources. Dr. S. M. Condren

  8. Components of Optical Instruments (d) Detectors for spectroscopic instruments. Dr. S. M. Condren

  9. Sources IR Region Nernst glower - rare earth oxides globar - silicon carbide rod incandescent wire - nichrome wire Dr. S. M. Condren

  10. Wavelength Selection Filters interference filters interference wedges absorption filters Dr. S. M. Condren

  11. Wavelength Selection Monochromators Components entrance slit collimating element (lens or mirror) prism or grating as dispersing element focusing element (lens or mirror) exit slit Dr. S. M. Condren

  12. Wavelength Selection “Two types of monochromators: (a) Czerney-Turner grating monochromator (b) Bunsen prism monochromator." Dr. S. M. Condren

  13. Prism Monochromators UV-Visible-Near IR Quartz IR NaCl Cornu type Littrow type

  14. Angular dispersion of prisms dq dq dn --- = -----· ----- dl dn dl whereq => angle l => wavelength n => refractive index Dr. S. M. Condren

  15. Resolving Power ofPrism Monochromators R => resolving power l dn R = ------ = b· ----- dl dl where b=> length of prism base Dr. S. M. Condren

  16. Interference and Diffraction Diffraction Monochromators

  17. Diffraction Video 1 If l is large compared to the aperture, the waves will spread out at large angles into the region beyond the obstruction. Video 2 Diffraction increases as aperture size   Eugene Hecht, Optics, Addison-Wesley, Reading, MA, 1998.

  18. Diffraction Pattern From a Single Slit Ingle and Crouch, Spectrochemical Analysis

  19. Diffraction Pattern From a Single Slit For Destructive Interference: x = /2 W sin  =  Ingle and Crouch, Spectrochemical Analysis

  20. Diffraction Pattern From a Single Slit For Destructive Interference: x = /2 W sin = 2  Ingle and Crouch, Spectrochemical Analysis

  21. Diffraction Pattern From a Single Slit For Destructive Interference: W sin  = m  m = ±1, ±2, ±3, … Ingle and Crouch, Spectrochemical Analysis

  22. Diffraction Gratings Plane or convex plate ruled with closely spaced grooves (300-2400 grooves/mm). Eugene Hecht, Optics, 1998. http://www.olympusmicro.com/primer/java/imageformation/gratingdiffraction/index.html

  23. Grating Equation Two parallel monochromatic rays strike adjacent grooves and are diffracted at the same angle (b). Difference in optical pathlength is AC + AD. For constructive interference: m = (AC + AD) m = 0, 1, 2, 3, … Ingle and Crouch, Spectrochemical Analysis

  24. Grating Equation m = (AC + AD) AC = d sin a AD = d sin b Combine to give Grating Equation: d(sin a + sin b) = m Grating Equation only applies if: d > l/2 Ingle and Crouch, Spectrochemical Analysis

  25. Are you getting the concept? At what angle would you collect the 1st order diffracted light with l = 500 nm if a broad spectrum beam is incident on a 600 groove/mm grating at qi = 10°? For l = 225 nm? For l = 750 nm?

  26. Fourier Transform IR (FTIR) • Modern infrared spectrometers are very different from the early instruments that were introduced in the 1940s. Most instruments today use a Fourier Transform infrared (FT-IR) system.

  27. Fourier Transform IR (FTIR) • In early experiments infrared light was passed through the sample to be studied and the absorption measured. • This approach has been superseded by Fourier transform methods. • A beam of light is split in two with only half of the light going through the sample. • The difference in phase of the two waves creates constructive and/or destructive interference and is a measure of the sample absorbance.

  28. Fourier Transform IR (FTIR) • The waves are rapidly scanned over a specific wavelength of the spectra and multiple scans are averaged to create the final spectrum. • This method is much more sensitive than the earlier dispersion approach.

  29. Fourier Transform IR (FTIR) • A Fourier transform is a mathematical operation used to translate a complex curve into its component curves. In a Fourier transform infrared instrument, the complex curve is an interferogram, or the sum of the constructive and destructive interferences generated by overlapping light waves, and the component curves are the infrared spectrum.

  30. Fourier Transform IR (FTIR) • An interferogram is generated because of the unique optics of an FT-IR instrument. The key components are a moveable mirror and beam splitter. The moveable mirror is responsible for the quality of the interferogram, and it is very important to move the mirror at constant speed. For this reason, the moveable mirror is often the most expensive component of an FT-IR spectrometer.

  31. Michelson Interferometer

  32. Fourier Transform IR (FTIR) • The beam splitter is just a piece of semi-reflective material, usually mylar film sandwiched between two pieces of IR-transparent material. The beam splitter splits the IR beam 50/50 to the fixed and moveable mirrors, and then recombines the beams after being reflected at each mirror.

  33. Fourier Transform IR (FTIR) Michelson Interferometer "Schematic of a Michelson interferometer illuminated by a monochromatic source." Dr. S. M. Condren

  34. Fourier Transform IR (FTIR) "Illustrations of time doamin plots (a) and (b); frequency domain plots (c), (d), and (e)." Dr. S. M. Condren

  35. Fourier Transform IR (FTIR) “Comparison of interferograms and optical spectra.” Dr. S. M. Condren

  36. FT-IR Dr. S. M. Condren

  37. Video

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