SPEctroscopy, Characterisation and Experimental Laboratory

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Penelope King

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Infrared spectroscopy

Infrared is commonly used to:

  • Identify inorganic compounds, including minerals
  • Quantify H2O, OH-, CO2, CO32- and SO42- in solids like minerals and glasses
  • Determine the spectral signatures of materials relevant to remote sensing
  • Quantify functional groups in pharmaceutical, agricultural, medical and manufactured materials
  • Identify historical art media and archaeological artifacts

Top reasons to use IR:

  • Useful for molecules with a dipole moment like polar groups, substituents on organic molecules, bonds in solids (e.g., Si-O, Al-O, B-O, H-O, C-O, C-H, N-O, S-O)
  • Samples can be crystalline, microcrystalline, amorphous or liquid
  • Very small samples can be analysed (<6μm lateral resolution)
  • Fast (1-10 minutes)
  • Qualitative ID is straightforward
  • Quantitative molecular abundances may be determined

FTIR spectrometer with microscope & mapping stage

  • Mid-IR: 400-5600 cm-1 (1.8-25 μm)
  • Reflectance, transmittance and attenuated total reflectance
  • Dry air purge
  • Microscope (15x and 36x objectives) with mapping stage that provides automated collection of spectra with ≥ 1μm step over 1cm2

Environmental chamber

  • Diffuse reflectance in a controlled-temperature reaction chamber
  • -150 to 500ºC
  • Vacuum or gas flow
  • Analysis of powders and reaction products (including surface species) in situ during experiments

Small-scale environmental chamber

  • Environmental stage for in situ transmission or reflectance IR micro-analyses
  • -196 to 900ºC with vacuum or gas flow

Field equipment

Portable or mounted FTIR

  • Reflectance, grazing angle and attenuated total reflectance analysis
  • Rapid analysis of powders, films and flat surfaces
  • Used in the field or lab

Geochemical and field equipment

  • Multi-meter with probes for measuring pH, ionic species, conductivity, dissolved O2, total dissolved solids, temperature and barometric pressure
  • Humidity-temperature data loggers

X-ray diffraction laboratory

Bragg-Brentano & transmission diffractometers

  • Powders or flat solid samples (>1μmg)
  • Phase identification and quantification including clay minerals
  • Crystal structure (Rietveld) refinement

Thermal analysis equipment

  • Thermogravimetric analyser <1200ºC
  • Differential thermal analyser <1200ºC
  • Differential scanning calorimeter <725ºC

Materials preparation facility

  • Horizontal tube furnaces (<1650ºC)
  • High-temperature box furance + ovens

Current projects include:

  • In situ analyses to characterise reactions as a function of temperature and gas atmosphere
  • Detecting rock art coatings appropriate for dating
  • Spatially mapping water diffusion in crystals and glasses
  • In situ temperature-dependent reaction rates
  • Investigating relationships between silicate glass structure, composition, thermal effects and spectra