Single-Crystal X-Ray Diffraction                     Powder X-Ray Diffraction                     Thermal Gravimetric Analysis                     Surface Area Analysis

Microwave Reactor                     Gas Chromatography-Mass Spectrometry


INOMAR instruments are available for usage. Please see our User Cost List and read below for information about these instruments, services, and contact information.

 Single-Crystal X-Ray Diffraction

DSC09513sSingle-crystal x-ray diffraction is a non-destructive analytical technique which provides detailed information about the internal lattice of crystalline substances, including unit cell dimensions, bond-lengths, bond-angles, and details of site-ordering. Directly related is single crystal refinement, where the date generated from the x-ray analysis is interpreted and refined to obtain a crystal structure. 

Single-crystal x-ray diffraction is most commonly used for precise determination of a unit cell, including cell dimensions and positions of atoms within the lattice. Bond-lengths and angles are directly related to the atomic positions. The crystal structure of a mineral is a characteristic property that is the basis for understanding many of the properties of each mineral.

Specific applications of single-crystal diffraction include:

DSC09511s

  • New mineral identification, crystal solution and refinement
  • Determination of unit cell, bond-lengths, bond-angles and site-ordering
  • Characterization of cation-anion coordination
  • Variation in crystal lattice with chemistry
  • With specialized chambers, structures of high pressure and/or temperature phases can be determined
  • Determination of crystal-chemical vs. environmental control on mineral chemistry
  • Powder patterns can also be derived from single-crystals by use of specialized cameras (Gandolfi)

  Powder X-ray Diffraction

DSC09522s

DSC09523s

X-ray powder diffraction is most widely used for the identification of unknown crystalline materials (e.g. minerals, inorganic compounds). Determination of unknown solids is critical to studies in geology, environmental science, materials science, engineering, and biology. Other applications include: X-ray powder diffraction (XRD) is a rapid analytical technique primarily used for phase identification of a crystalline material and can provide information on unit cell dimensions. The analyzed material then is finely ground, homogenized, and average bulk composition is determined.

  • Characterization of crystalline materials
  • Identification of fine-grained minerals such as clays and mixed layer clays that are difficult to determine optically
  • Determination of unit cell dimension
  • Measurement of sample purity
  • With specialized techniques, XRD can be used to:
  • Determine crystal structures using Rietveld refinement
  • Determination of modal amounts of minerals (quantitative analysis)
  • Characterize thin films samples by making textural measurements, such as the orientation of grains, in polycrystalline samples
  • Determine the lattice mismatch between film and substrate and infer stress and strain
  • Determine the dislocation density and quality of the film by rocking curve measurements
  • Measure superlattices in multilayered epitaxial structures
  • Determine the thickness, roughness, and density of films using glancing incidence x-ray reflectivity measurements
 Thermal Gravimetric Analysis

DSC09496sThermal analysis measures physical or chemical changes in a material as a function of temperature. The common complimentary techniques of thermal analysis offered by thermogravimetric analysis (TGA). TGA is a technique for measuring changes in mass as a function of temperature and is primarily used to determine the composition of substances. Applications of TGA include:

  • Polymers-weight loss vs. temperature; loss of water from nylon and other hygroscopic polymers; determination of fillers, reinforcements, and pigments; analysis of rubber compositions; volitilization of additives; kinetics of decomposition; and oxidative stability studies.
  • Electronics-resin content of printed circuit boards; volatilization curves for fluxes; thermal decomposition of wire insulation and components
  • Pharmaceuticals-water and volatives content of solid dosage forms
  • Inorganic materials and minerals-determination of temperatures of dehydration, elimination, and decomposition; quantification of volatiles loss
  • Composites-system decomposition curves; filler and reinforcement analysis; oxidative stability; lifetime prediction

 Particle Surface Area and Pore Size Distribution Analysis
DSC09505s

Particle surface area measurements provide date for a range of solid samples, including catalyst and adsorbent materials such as molecular sieves. Algorithms are available for isotherm data analysis, including the Langmuir and Brunauer-Emmett-Teller (BET) models.

Particle Surface Area Testing: 

  • BET surface area
  • Langmuir surface area
  • Correlation coefficient
  • Micropore surface area
  • Micropore volume
  • Adsorption pore size distribution
  • Total pore volume

Applications include: 

  • Catalysts
  • Activated carbon
  • Carbon black
  • Pharmaceuticals
  • Fuel cells
  • High-tech ceramics and more 
Microwave Reactor

CEMMicrowave reactors are used to apply microwave radiation to a variety of chemical reactions and applications. The CEM Focused TM Synthesis, Discoverer SP System is specifically designed for reaction rate acceleration, achieving milder reaction conditions, performing green chemistry processes, reaching higher chemical yields, lowering energy usage, and realizing different reaction selectivities. In short, this instrument allows for the facile performance of synthetic processes under controlled conditions in a laboratory. The microwave reactor has widely been used in polymer synthesis, organic chemistry, nanotechnology, as well as solid-state chemistry. The following are several practical uses for microwave-based processes:

  • Polymerizations (including, but not limited to, free radical polymerization, step-growth polymerizations, living radical polymerization, ring opening polymerizations, and sol-gel polymerizations
  • Solvothermal synthesis of metal-organic frameworks and similarly related materials
  • Microwave-assisted organic chemistry
  • Microwave-assisted nanoparticle synthesis
  • Microwave-assisted synthesis of inorganic materials
  • Green chemistry applications

Gas Chromatograhy-Mass Spectrometry

Gas chromatography-mass spectrometry (GC-MS) is an analytical method that combines the features of gas-liquid chromatography and mass spectrometry to separate and characterize each of the components within a test sample. By combining the two techniques, an analytical chemist can both qualitatively evaluate a solution containing a number of chemicals.

gaschromotography-massspecApplication includes:

  • Catalyst
  • Organic synthesis
  • Drug detection
  • Environment analysis
  • Identification of compounds from mixtures

Columns Available for Use:

  • DB-1MS, 30m, .32mm, .25µm: for methanol, formaldehyde, formic acid, etc.
  • CP-Sil 5 CB, 30 m x 0.32 mm x 0.25 µm: for methanol, formaldehyde, formic acid, etc.
  • PoraPLOT Q, 25 m x 0.32 mm x 10 µm with 1PT: analysis of polar/apolar volatile compounds
  • HP-Chiral-20B, 30 m x 0.32 mm x 0.2 µm: enantiomeric separation
  • HP-5ms, 30 m x 0.25 mm x 0.1µm: aromatic compounds 

 

 For more information on the usage of these instruments please contact: