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For example, trace element analysis is sensitive to background subtraction because the computer is looking for a small peak above the continuum. Guidelines are given in Methods Ast 3. When analyzing hard and soft X rays in the same specimen, analyses at two voltages may be necessary. When these standard deviations are divided by the mean concentration for each element, the result is a measure of relative precision within and between laboratories. The compositions of both alloys, as determined by wet chemical analysis, are given in Table 2.
Although data can be generated on these casual surfaces, the results would be of astmm
ASTM E1508 – 12a
Lowering the accelerating voltage may reduce or eliminate the effect of charging in some samples, but applying a conductive coating is still the most common method. Sr SR r R Nickel 9. For quantitative analysis, a shaping time of about 10? Specimens mounted in a nonconducting asstm must make electrical contact with the microscope stage.
The beam current must remain stable throughout the analysis, because the counts collected are directly proportional to the beam current. For the most accurate analysis, standards and unknowns should be coated at the same time to assure equal coating thicknesses.
Heavy metals such as f1508 that are often used for SEM imaging are less suitable because they heavily absorb X rays; if the coating is thick enough, X-ray lines from those metals will be seen in the spectrum. On the MA alloy, the reproducibility among laboratories was much less than that of the standards technique R in Table 4.
It is the responsibility of the user of this standard to establish appropriate safety and aastm practices and determine the applicability of regulatory limitations asgm to use.
The count rate incident on an X-ray detector is directly proportional to the size of the solid angle de? All distances must be in the same units. Two methods in common use are 1 the method of overlap factors and 2 the method of multiple least squares.
The specimen must be? These approach the problem of matrix correction using more fundamental physics and sometimes combine the effects of Z and A into one, but they too require a set of fundamental parameters optimized to each program. And even though the average errors compared with the reference composition Table 5 are not great, they are probably the result of positive and negative errors among laboratories canceling each other.
Precision and Bias The nominal composition of each specimen was also included for reference. For the alloy MAthe average was 3. A number in parentheses indicates the year of last reapproval. Two approaches to this problem commonly used in commercial systems are background modeling and digital? Current edition approved Nov. If the unknown and standard were identical, each of these factors would equal one. More accurate interaction axtm can be computed by Monte Carlo computer methods to generate random electron trajectories, but Eq asm provides a reasonable estimate for most purposes.
Summary of Practice 4. It does not affect spatial resolution for X-ray analysis in the same way it detracts from electron image resolution. The operator must also be aware of the possibility of spurious X rays from parts of the chamber, polishing compound elements, or from adjacent phases or a combination thereof. Quantitative light element analysis is less precise than that of heavier elements, because the count rate of soft X rays is lower. Additionally, in the windowless mode any light, such as from cathodoluminescence, can be picked up by the crystal and will contribute to the overall noise of the system.
If they are etched, the operator must make sure that the composition in the region to be analyzed has not been altered and that the region to be analyzed is? This method lets the user pass judgment on the quality of f1508 model by comparing the model atm the actual spectrum.
It calls attention to problems such as elements not speci? The artifact cannot occur at energies below the absorption edge of the Si K line, and it becomes negligible at higher energies such as the Cu Ka line.
A total of nine laboratories participated in the study. In like manner, deconvolution routines work well in most cases, but not when the overlapped lines arise from elements present in widely different concentrations. Although results of the standardless analyses were rather good on the Type stainless steel, they may be considerably inferior on other types of specimens. It would also be informative to mention the type of window on the EDS detector, if other than a conventional beryllium window.
Standardless methods were about equivalent to those using standards for this specimen. Requiring set parameters had little effect on the repeatability but improved the reproducibility for chromium and iron, but not for nickel. Most sources of bias are either insigni? The alloy awtm both high and low atomic number elements necessitating the use of K, L, and M lines.
The inherent precision of the EDS method is controlled by counting statistics. Evaporated carbon satm usually the most suitable coating material.
Standard Guide for Quantitative Analysis by Energy-Dispersive Spectroscopy
It was not possible to specify all of these conditions because some are inherent to the system used. There are, however, effects of atomic number, absorption, and? For the highest accuracy, standards should be as similar as possible to the unknowns to minimize matrix effects.
Even though one cannot see the individual components of a peak envelope in a spectrum, there are computer methods of deconvolution. However, most matrix correction programs are sufficiently accurate to permit the use of pure element standards.