This course covers qualitative and semi quantitative analysis, beginning with the generation of background and characteristic of x-rays, nomenclature, and peak family ratios.
Details
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Targeted Participants
Individuals who are, or soon will be, expected to operate an SEM, choose appropriate parameters for EDS, and perform qualitative and semi quantitative analysis on materials samples.
Format
Lecture, demonstration and hands-on practice, as well as round table discussion. Participants are encouraged to bring their own samples, if possible.
Main Curriculum
- Generation and nomenclature of x-ray lines
- Spectral artifacts
- Deconvolution of peak overlaps
- Qualitative analysis
- Semi quantitative analysis
- Hardware settings/function
- Setup and operation of SEM for BSE imaging and spectral acquisitions
- Sample requirements for BSE/EDS
Instruments Available
- Hitachi S3500
- Bruker Esprit (SDD)
- MAC Element Standards
- COXEM SEM EM-30N
Enrollment Note
Registration will be limited to a maximum of 15 participants.
EMS will provide samples to those who prefer not to bring their own.
X-Ray Microanalysis: A Complete Picture
The nondestructive elemental identification of a sample’s micro-composition is a powerful tool for the microscopist. This technique can detect elements from boron to uranium with a minimum concentration delectability of 1000 ppm in solid samples.
Collection parameter settings of both the EDS system and microscope, their effect on the spectrum and quality of the subsequent quantification are of primary importance. The non-variable parameters of working distance and tilt will be demonstrated as well as the effect of accelerating voltage on background shape, x-ray spatial resolution, over-voltage requirements, and accuracy of ZAF matrix corrections examined. With the advent of the silicon drift detector (SDD) the pulse processor time constant and beam current (spot size) settings to control % dead time are almost a moot point but will be introduced for those who work with a SiLi detector.
Identification of individual elemental lines as well as methods used for determining peak overlaps such as peak shape, peak family ratio anomalies, and the presence of a peak unassociated with known elements will be paid particular attention.
Quantitative analysis will be limited to the use of ZAF and PhiRhoZ routines but the collection of standards and their use in a full quant will be discussed. Backscattered (BSE) imaging will be correlated with x-ray maps and spectral imaging results. Energy calibrations will also be preformed.