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Instrumentation in infrared (IR) spectroscopy

A spectrometer is an instrument used to measure properties of light over a specific portion of the electromagnetic spectrum, typically used in spectroscopic analysis to identify materials.

1. Sources of Radiation:

  • The source in an IR spectrophotometer provides the necessary IR radiation which will pass through the sample.

  • The source should be stable, have a long lifetime, and cover the desired wavelength range.

A. Globar:

  • It's a silicon carbide rod which, when electrically heated, emits radiation in the mid-IR region. Its spectral radiance is nearly constant over this range.

B. Nernst Glower:

  • Made of rare earth oxides, this source has a spectral radiance that increases with wavelength.

  • It's a ceramic rod which, when electrically heated, emits radiation in the mid-IR range.

C. Tungsten Filament:

  • This is generally used for the near-IR region. It emits over a broad range, covering both the visible and NIR region.

D. Mercury Arc Lamp:

  • This is useful for the far-IR region.

2. Wavelength Selectors:

  • These devices separate the broad spectrum emitted by the source into individual frequencies, allowing for the sequential or specific analysis of each frequency.

A. Monochromators:

  • These use prisms or gratings to disperse radiation.

  • As the radiation passes through, different wavelengths are bent by different amounts, effectively separating them.

B. Interferometers:

  • Used in Fourier Transform Infrared (FTIR) Spectrometers.

  • They split the radiation beam into two, reflecting them off mirrors, and then recombine them.

  • The resulting interference pattern (interferogram) contains information about all wavelengths at once, which is then Fourier transformed to give the spectrum.

3. Detectors:

  • Detectors are devices that convert the IR radiation, which is transmitted or reflected by the sample, into an electrical signal.

A) Golay Cell (Pneumatic Detector):

  • It's a thermal detector that operates on the principle of constant volume gas thermometry.

  • It consists of a closed-ended, mirrored cylinder with a diaphragm at the end. The chamber is filled with a gas, and IR radiation heats the gas, causing a pressure change that moves the diaphragm. This movement is detected and converted into an electrical signal.

  • Application: Widely used in FTIR due to its wide frequency range and fast response.

B) Bolometer:

  • It employs a blackened platinum or gold strip maintained at constant temperature.

  • When it absorbs IR radiation, the temperature rises and resistance changes.

  • Application: Used for detecting far-IR radiation because of its high sensitivity in this region.

C) Thermocouple:

  • It consists of two different metals joined together. When one junction is heated by IR radiation, a small voltage is produced.

  • Application: Suitable for the mid-IR range due to its moderate sensitivity and wide frequency response.

D) Thermistor (Thermal Resistor):

  • Made from semiconducting materials whose resistance changes significantly with temperature. When IR radiation heats it, this resistance change is measured.

  • Application: Used in the mid-IR range, it provides higher sensitivity than thermocouples.

E) Pyroelectric Detector (e.g., DTGS - Deuterated Triglycine Sulfate):

  • These detectors generate a voltage when they are heated or cooled. When IR radiation falls on the detector, it heats up and produces a voltage proportional to the change in temperature.

  • Application: Widely used in FTIR instruments due to their broad spectral response and compatibility with room temperature operation.


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