Analytical Laboratory Evaluations

In the hands of our engineers and chemists, these tools also provide clear root cause answers to forensic investigations of why a catalyst performance has declined.  Equipped with an understanding of the root cause, our engineers help customers avoid or minimize the causes, reverse them, and extend catalyst operating life.

MIRATECH has a facility in one of the great science centers of the U.S. Home to the Department of Energy’s Oak Ridge National Laboratory, the University of Tennessee, the Tennessee Valley Authority, and numerous supporting technical businesses, this area has the most advanced analytical laboratories available anywhere.  MIRATECH collaborates with these laboratories to bring benefits and value to its customers.

Analytical methods used by MIRATECH include the following:

• Chemisorption
• EDS – Energy Dispersive X-Ray Spectroscopy
• ICP-MS – Inductively Coupled Plasma/Mass Spectroscopy
• ICP-OES – Inductively Coupled Plasma/Optical Emission Spectroscopy
• SEM – Scanning Electron Microscopy
• SEM-EDS – Scanning Electron Microscopy with Energy Dispersive X-Ray Spectroscopy
• TEM – Transmission Electron Microscopy
• TEM/STEM-EDX – Transmission Electron Microscopy/Scanning Transmission Electron Microscopy with EDS Energy Dispersive X-Ray Spectroscopy
• TGA/DTA – Thermal Gravimetric Analysis/Differential Analysis
• TOF-SIMS – Time-of-Flight Secondary Ion Spectrometry
• WDS – Wavelength Dispersive Spectroscopy
• XPS – X-Ray Photoelectron Spectroscopy
• XRD X-Ray Diffraction
• XRF – X-Ray Fluorescence
• BET Surface Area

A typical diagnostic approach would include the following steps:

• Customer removes a catalyst test coupon or full size element and ships to MIRATECH’s Knoxville laboratory along with specific information that may be related to performance decline, such as normal and maximum operating temperatures, fuel type and sulfur content, etc.
• MIRATECH’s engineering technician carefully removes a very small portion of the catalyst coating from the catalyst substrate for use as a diagnostic sample.  The catalyst function is not affected and can be returned to service.
• Using strict chain of custody, the coating samples are submitted to approved independent analytical laboratories for measurement of specific catalyst characteristics.
• Depending on initial findings, MIRATECH may submit additional samples for other types of characterization analysis.
• An MIRATECH engineer produces a report for the customer summarizing and interpreting the analytical results along with specific recommendations for minimizing or preventing future catalyst degradation, and for reversing the degradation and restoring catalyst performance.

The analytical methods selected for the evaluation are selected based on the type of catalyst, operating service, and other engine-specific information that could relate to a decline in catalyst performance.  The analyses are done in a stepwise sequence to identify an obvious cause of the degradation at the lowest cost.  Normally, an initial set of analyses (Phase 1) are performed that identify the cause.  If the results are not conclusive, additional analyses would be recommended to the customer.

Phase I (one or more of the following)

• Elemental analysis to detect the presence of and measure the concentration of possible catalyst masking agents and poisons.
• Internal surface area and porosity of wash coat to determine if thermally or chemically induced changes have occurred.
• Chemical speciation to further define/confirm thermally or chemically induced changes.
• Nano-scale microscopic analysis to further define catalyst masking agents or poisons.

Phase 2
Additional analyses that may be necessary include further nano-scale microscopic elemental analysis and techniques to measure precious metal dispersion.  Customer authorization is required before this additional work is undertaken.