Chemistry Division

Solid Analysis

  • Solid State Nuclear Magnetic Resonance (NMR) Spectroscopy

FTIR Avatar 360, including spatial imaging and ATR capability TA24, Bldg 24, Rm B33

FTIR spectroscopy is a common technique used for polymer analysis as it provides a unique chemical (vibrational) fingerprint of each individual material. FTIR provides useful information that can help to identify unknown materials, determine sample quality, and quantify components in a mixture. FTIR spectroscopy can be used to analyze bulk solids and liquids, thin films, and gases. Our FTIR microscopy capability can analyze single points in a material at a spatial resolution down to 10 μm. This technique is particularly useful for the analysis of coatings and polymeric materials when small quantities are used. The ability of the instrument to perform analyzes at a micro-scale level makes it very useful in the analysis of polymer aging. In addition, FTIR microscopy provides information about the uniformity of a substrate through spatial mapping experiments. This technique is also commonly used in kinetic reaction studies, such as curing experiment on a substrate or migration of impurities.

FTIR spectroscopy has recently been used by CDE to characterize a number of polymeric materials, including Halthane, Wilethane, Silane Foams, VCE, and polyurethane.

For Halthane, FTIR-ATR was used to determine the appropriate mixing time and degassing times, and determine sample stochiometry. Peaks unique to prepolymer and Asilamine 170 were used to determine uniformity of mixing and the most effective mixing methods.

For Wilethane, the percent cure of the binary mixed adhesive was determined based on a quantitation method from PXRPT-04-14., and also determined quantitatively by establishing a correlation between the NCO and OH peak intensities. Continuing studies examined curing differences and compared adhesion properties.

A combination of IR (Meadows) and NMR (Labouriau) was used to characterize individual starting materials of silane foam LK3626, and their reaction rates, intermediates, products, and mixing characteristics. Temporal IR and NMR data gathered during mixing provided information on reaction intermediates. IR was used to identity and quantity of functional groups on post-cured and non post-cured LK3626 foams and extracts. This provided baseline spectroscopic characteristics used in continuing aging studies and to characterize foams chemistry vs. formulation. Filled and unfilled VCE and cured and uncured LK3626 were also investigated by IR microscopy.

Additionally, we have conducted studies of hydrogen bonding in polyurethanes by IR spectroscopy.

  • X-Ray Flouresence (XRF) Spectroscopy

Contact: Dan Kelly (505) 665-7388

Thermal Analysis: Thermal Gravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC), TGA and DSC coupled with mass spec (TGA/MS & DSC/MS)TGA coupled with infrared analysis (TGA/FTIR)

Thermogravimetric Analysis (TGA) is s method to accurately monitor the temperature affects of a material by precise weight loss measurements. This method is generally used to study the decomposition of a material in an inert of oxidative atmosphere to characterize the molecular and physical properties. Differential Thermal Analysis (DTA) allows for a comparison of two materials at the same time. The complementary information obtained allows differentiation between endothermic and exothermic events with no associated weight loss (e.g. melting and crystallization) and those that involve a weight loss (e.g. degradation). It can be use to compare original materials to modified (aged) samples. Differential Scanning Calorimetry (DSC) is similar to TGA analysis with the addition of characterizing the endo/exothermeric properties of the material as the heat is increased resulting in obtaining enthalpy properties of the material. This DSC method and be used similarly to the DTA to compare two samples. The system can also incorporates a Mass Spectometer (MS) or FTIR to analyze the produced gases during heating. This detector adds additional information to the molecular properties identification. The method produces qualitative and quantitative results.

  • SEM coupled with energy dispersive spectrometer (EDS)

Contact: Dan Kelly (505) 665-7388

Carbon-Hydrogen-Nitrogen (CHN, CHNS & Oxygen) Analysis

  • One analyzer with three modes of operation: CHN, CHNS and Oxygen
  • Advanced combustion design for handling virtually any type of sample
  • Frontal Chromatography for simple, reliable and accurate measurements
  • NEW EA 2400 Data Manager software for easy data handling

The PerkinElmer 2400 Series II CHNS/O Elemental Analyzer (2400 Series II) is a powerful instrument for the rapid determination of the carbon, hydrogen, nitrogen, sulfur or oxygen content in organic and other types of materials. It has the capability of handling a wide variety of sample types in the field of pharmaceuticals, polymers, chemicals, environmental and energy, including solids, liquids, volatile and viscous samples.
Contact: Dan Kelly (505) 665-7388

Laser Induced Breakdown Spectroscopy (LIBS)

LIBS (Laser-Induced Breakdown Spectroscopy) is a laser based technique that involves the use of a focused pulse laser beam to generate a microplasma. The emission from the plasma is wavelength resolved using a spectrograph / detector / computer system to determine the elemental composition of the samples of interest. Advantages of LIBS include: (1) little to no sample preparation is required, (2) analysis can be accomplished in minutes, (3) it is a highly configurable technique, portable, fixed lab, and transportable field deployable systems are possible and remote analysis in harsh environments using conventional or fiber optic cables in hotcells and gloveboxes can be performed, (4) element ratios and isotopic measurements are possible, and (5) all of the elements in the periodic table can be analyzed with varying degrees of precision and accuracy. Relative to polymer analysis LIBS can be used to determine: (1) the elemental composition of the polymer, (2) trace elements in the polymer moiety including metal atom inclusions, and (3) particle and elemental inclusions using LIBS microscopy with a spatial resolution of a few microns.
Contact: James Barefield (505) 665-5195

Febuary 2012

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