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There are two main infrared (IR) spectrophotometers: dispersive IR spectrometers and Fourier transform infrared (FTIR) spectrometers. In a dispersive IR spectrometer, a beam of infrared radiation produced by a hot wire is divided into two parallel equal-intensity beams using mirrors. One beam passes through the sample, while another is a reference beam. The beams then move through the monochromator, which separates the radiations into a continuous spectrum of different frequencies. The...
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Peripheral thermosensation is the perception of external temperature. A change in temperature (on the surface of the skin and other tissues) is detected by a family of temperature-sensitive ion channels called Transient Receptor Potential, or TRP, receptors. These receptors are located on free nerve endings. Those detecting cold temperatures are closer to the surface of the skin than the nerve endings detecting warmth. These thermoTRP channels, while temperature selective, have relatively...
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Body temperature can be assessed using various devices and measured in Celsius or Fahrenheit.
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Atomization, converting samples into gas-phase atoms and ions, is essential for atomic spectroscopy. The flame temperature required for atomization affects the efficiency of the atomic spectroscopic methods by increasing the atomization efficiency and the relative population of the excited and ground states.
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Inductively coupled plasma (ICP) is the common plasma source used in atomic emission spectroscopy (AES), a technique that detects and analyzes various elements in a sample. This method is often called inductively coupled plasma atomic emission spectroscopy (ICP-AES).
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Atomic Absorption Spectroscopy: Instrumentation01:22

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An atomic absorption spectrophotometer (AAS) comprises several components: a radiation source, an atomizer, a monochromator, and a detector. The radiation source can be a hollow-cathode lamp (HCL) or an electrodeless-discharge lamp (EDL), both of which provide a narrow emission line of the required wavelength. However, some instruments use continuum sources and high-resolution monochromators to achieve a narrow range of radiation.
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Variable temperature infrared spectroscopy with a button sample holder and thermoelectric heating/cooling.

Jaspreet Singh1, Robert L White1

  • 1Department of Chemistry and Biochemistry, University of Oklahoma, Norman, 73019, USA.

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|February 22, 2022
PubMed
Summary

This study introduces a new apparatus for variable temperature infrared spectroscopy, enabling precise analysis of liquids and powders across a wide temperature range. The method enhances spectral measurement accuracy and reveals temperature-dependent structural changes in samples.

Keywords:
Acetylsalicylic acidButton sample holderKaoliniteMontmorilloniteThermoelectric heating/coolingVariable temperature infrared spectroscopy

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Area of Science:

  • Analytical Chemistry
  • Materials Science
  • Spectroscopy

Background:

  • Infrared spectroscopy is a powerful technique for analyzing molecular structure and composition.
  • Variable temperature measurements are crucial for understanding temperature-dependent phenomena in materials.
  • Existing methods may have limitations in temperature control, sample handling, or applicability to volatile substances.

Purpose of the Study:

  • To develop and validate a novel apparatus for variable temperature infrared spectroscopy.
  • To enable precise temperature control for analyzing liquids and powders from -50 to 100 °C.
  • To demonstrate the apparatus's capability in characterizing temperature-induced structural changes and phase transitions.

Main Methods:

  • Utilized a Peltier thermoelectric device for precise heating and cooling of neat samples in a stainless steel holder.
  • Developed customized temperature profiles, including linear ramps and isothermal steps, for dynamic and static measurements.
  • Investigated volatile liquids by controlled cooling to minimize evaporation during spectral acquisition.

Main Results:

  • Achieved reproducible infrared spectra for volatile liquids at 10 °C, comparable to thin film transmittance spectra.
  • Observed and correlated temperature-dependent variations in spectral data with specific sample structural changes during temperature ramps.
  • Successfully differentiated between reversible and irreversible sample changes using difference spectra from isothermal measurements.

Conclusions:

  • The developed apparatus and methodology provide a sensitive and versatile platform for variable temperature infrared spectroscopy.
  • The system effectively monitors temperature-induced structural modifications in various materials, including clays and drug-excipient mixtures.
  • This technique offers enhanced capabilities for studying dynamic processes and phase behaviors in condensed matter.