scholarly journals The Analysis of Sensitive Materials Using EBSD: The Importance of Beam Conditions and Detector Sensitivity

2019 ◽  
Vol 25 (S2) ◽  
pp. 2394-2395 ◽  
Author(s):  
Pat Trimby ◽  
Angus Bewick ◽  
Daniel Abou-Ras ◽  
Pietro Caprioglio ◽  
Dieter Neher ◽  
...  
Keyword(s):  
Author(s):  
E. B. Steel

High Purity Germanium (HPGe) x-ray detectors are now commercially available for the analytical electron microscope (AEM). The detectors have superior efficiency at high x-ray energies and superior resolution compared to traditional lithium-drifted silicon [Si(Li)] detectors. However, just as for the Si(Li), the use of the HPGe detectors requires the determination of sensitivity factors for the quantitative chemical analysis of specimens in the AEM. Detector performance, including incomplete charge, resolution, and durability has been compared to a first generation detector. Sensitivity factors for many elements with atomic numbers 10 through 92 have been determined at 100, 200, and 300 keV. This data is compared to Si(Li) detector sensitivity factors.The overall sensitivity and utility of high energy K-lines are reviewed and discussed. Many instruments have one or more high energy K-line backgrounds that will affect specific analytes. One detector-instrument-specimen holder combination had a consistent Pb K-line background while another had a W K-line background.


CrystEngComm ◽  
2013 ◽  
Vol 15 (11) ◽  
pp. 2091 ◽  
Author(s):  
Noriaki Kubota ◽  
Masanori Kobari ◽  
Izumi Hirasawa

1969 ◽  
Vol 52 (6) ◽  
pp. 1231-1237
Author(s):  
M C Bowman ◽  
Morton Beroza

Abstract Residues of fenthion, disulfoton, and phorate may each consist of the parent insecticide and five metabolites formed by oxidation of the thionophosphate and sulfide groups in each molecule. The analysis of these residues has been simplified and speeded by oxidizing the insecticide and its metabolites to the oxygen analog sulfone with m-chloroperbenzoic acid. After removal of the acid on an alumina column, the compound is determined by GLC with a flame photometric detector. Sensitivity (twice noise) is at least 0.001 ppm. When equal amounts of the six compounds were added to corn, milk, grass, and feces at levels of 0.2 to 5.0 ppm, the recoveries were 95–96% for fenthion and 74–82% for disulfoton and phorate. In analyses of field-treated samples, recoveries were 89–92% of those obtained by previous procedures, which are much more time-consuming.


1999 ◽  
Vol 5 (S2) ◽  
pp. 90-91
Author(s):  
E D Boyes

For a number of years we have used in our laboratory a simple extension to light elements of the classical ClifF-Lorimer approach using stoichiometric compound standards containing pairs of heavier elements to determine independently the EDS detector sensitivity contribution to quantitative analysis in the AEM. It is now also extended to direct light element LVEDS analysis in the SEM at low voltage (<5kV). This approach may be more practical, accessible and easily reproducible for routine use than the elegant custom thin film fabrications reported by Egerton, but the latter method has other substantial advantages, including well defined thicknesses, in the most sophisticated applications. As the types of advanced materials have expanded to include ceramics and polymers the requirements for analysis have also changed. In many cases the light elements are now the majority species in advanced materials and the corrections based on older standards are huge; and therefore inevitably rather limited in accuracy.


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