Polymer Analytical Laboratory

You will find comprehensive support for your development of Nylon 66 (PA66) products and processes through Solutia's Polymer Analytical Laboratory.  You gain access to the experienced industry experts who staff our lab and a broad range of material characterization and measurement equipment and techniques within our state-of-the-art laboratory facilities.  Available techniques include:

The microscopy capabilities available to support your developmental activities include:

Optical microscopy is often the first tool you will use to examine a sample.  In addition to the usual bright-field illumination analysis, you can also take benefit from our various types of illumination and discrimination techniques:

• Ultraviolet light illumination allows you to observe fluorescent species, such as certain polymer gels and some chemicals.
• Cross-polarized illumination detects molecular orientation within a sample.
• Dark-field illumination is useful for imaging particulates in a thin cross-section.
• Phase contrast images show differences in refractive indexes.
• Differential interference contrast is often used to image gel globules in a sample.  This technique distinguishes differences in optical-path lengths.
• Through hot-stage microscopy, you can determine the temperature of certain phase transitions, including melting of crystals, using cross-polarized light.

Various specialized sample preparation and staining techniques are also available.

Major instrumentation includes:

• AusJENA-JenaLumar Fluorescence Illumination
• AusJENA-JenaPol and Nikon MicroPhot-FX
• Nikon Differential Interference Contrast Microscope
• Nikon MRC-600 Confocal Microscope
• Mettler FP82HT/FP90 Hot Stage
• Jena-Mach-Zender Interference Microscope
• Wild Makroskop M420 and Meiji Stereo Microscopes
• Leica CM1800 Cryo Microtome
• Leica RM2025 Rotary Microtome
• Reichert Jung Sledge Microtome
• Reichert Jung Ultracut E Ultra-Microtome with Cryo Attachment
• Digital Imaging Using Hitachi Color Video and Sony Cats Eye Digital Photo Cameras
• Image Pro Plus and Sigma Scan Pro Image Analysis Software

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Scanning electron microscopy (SEM) involves irradiating the surface of a sample with a finely focused electron beam.  With SEM, you can examine features that are too small to be seen with an optical microscope.

• You can achieve magnifications up to 500,000X.
• Surface examination reveals features, such as processing damage, domains with different crystalline or amorphous character, and variability in surface coatings.
• The field-emission SEM (FE-SEM) provides high magnification with low-beam intensity.  FE-SEM provides high-resolution images of delicate surface morphology, such as organic coatings that can be damaged by conventional SEM.
  • Freeze-fracture, selective dissolution, and microtomy techniques enable you to examine the interior regions of samples.
  • Metal coating with various elements including Osmium is available if your application requires it.
• Both SEM microscopes are equipped with Energy Dispersive Spectrometers (EDS), which allow you to identify elements with atomic numbers higher than Boron.  This allows for elemental determination and compositional mapping of the different features in a specimen.

Major microscopy instrumentation includes:

• LEO 982 FE-SEM
• JEOL 5300LV SEM
• Oxford EDS Systems
• Emitech K550 Sputter Coater
• OPC 80 Osmium Plasma Coater

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Infrared spectroscopy (IR) and Fourier transform-infrared spectroscopy (FT-IR) provide information about the functional groups and chemical structure of a compound.  It determines these properties by examining the frequencies of infrared radiation that the material absorbs.  IR and FT-IR are often useful in identifying polymers and chemical additives.

Special accessories make it possible to obtain spectra by placing the surface of an object into contact with a diamond window, which provides non-destructive testing and eliminates sample preparation problems.

For very small specimens, an FT-IR-microscope is available.  This instrument maps chemical composition across a region of interest in a sample, for instance, to determine the distribution of an additive or contaminant.

Major instrumentation includes:

• Nicolet Nexus 670 FT-IR Spectrometer with DuraSampl/IR Horizontal ATR Cell
• PerkinElmer AutoImage FT-IR microscope / Spectrum One FT-IR Spectrometer

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Thermal analysis (TA) techniques measure changes in one or more physical properties of a sample, while the sample is being heated or cooled. The temperature range and rate of heating or cooling are controlled.

The Polymer Analytical Laboratory is equipped with a variety of state-of-the-art instruments:

• Differential scanning calorimetry (DSC) measures heats of melting, crystallization and reaction, as well as heat capacity.  Two varieties of temperature modulated DSC (TM-DSC) are available.  This technique separates the effects caused by "reversing" and "non-reversing" processes.  For example, it allows you to separate a glass transition ("reversing" process) from an accompanying solvent evaporation ("non-reversing" process).
• Thermogravimetric analysis (TGA) measures the weight loss of materials versus temperature or time.  Differential thermal analysis (DTA) identifies the endothermic or exothermic character of events.  Simultaneous TGA and DTA measurement allows you to identify the endothermic or exothermic character of weight-change events.  Mass spectrometric identification of gases evolved from TGA experiments (TGA/MS) can be employed to identify volatile components or decomposition products.
• Thermomechanical analysis (TMA) measures the mechanical responses of materials subjected to a constant stress.
• Dynamic mechanical analysis (DMA) measures the mechanical responses of materials subjected to a periodically varying stress.  Various measurements can be made over a wide temperature range, as low as -150 C and as high as 1,100 C, depending on the instrument and the technique employed.  In most cases, the sample can be exposed to either an oxidizing gas or an inert gas.

Major instrumentation includes:

• Perkin-Elmer Pyris 1 DSC w/ Liquid Nitrogen Cooling Accessory and IntraCooler II
• TA Instruments DSC 2920 Modulated DSC w/ Refrigerated Cooling System (RCS)
• Perkin-Elmer DSC-7 Differential Scanning Calorimeter w/ Robotic Autosampler
• Mettler SDTA 851e Simultaneous TGA/DTA w/ Gas Switching Accessory and Autosampler Perkin-Elmer TGA 7 Thermogravimetric Analyzer w/ Gas Switch
• TA Instruments TGA 951 Interfaced to an INCOS 50 Quadrupole Mass Spectrometer
• TA Instruments TMA 2940
• Perkin-Elmer DMA7e Dynamic Mechanical Analyzer w/ Intracooler II Cooling Accessory
• Omnical Model CRC90 Reaction Calorimeter

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Polymer chromatography includes the use of high-performance liquid chromatography (HPLC) techniques for absolute molecular weight determination of polymers using triple-detection methods.  HPLC is also used to characterize additives, impurities, and decomposition products.

Various mobile phases are used, including hexafluoro isopropanol (HFIP), which is an excellent solvent for polyamides.

Components that have no useful UV absorption can be detected and quantified using an evaporative light scattering (ELS) detector.

The components responsible for specific HPLC peaks can be deposited onto a silicon disc and then IR-analyzed off-line using an LC-transform accessory.  Ion chromatography (IC) can identify ionic additives in polymers.

Major instrumentation includes:

• Hewlett Packard 1090 and 1100 HPLC Systems
• Waters 410 Differential Refractive Index Detector
• Viscotek T50 Differential Viscosity Detector
• Dionex CD25 Conductivity Detector
• Polymer Laboratories PL-ELS 1000 Evaporative Light Scattering Detector
• LC-Transform Accessory

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