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This material was chosen as a routine analysis for iron, chromium, and nickel. A superscript epsilon e indicates an editorial change since the last revision or reapproval.

It was requested that analyses by both standards and standardless methods be reported. However, in the absence of light elements, it is unlikely that the accuracy of most EDS analyses is limited by the matrix correction. This range contains K lines of the?

Consequently, one would expect the most improvement using a phi-rho-z method in light element analysis. The differences in the results each produces are usually much less than the precision of the analysis.

ASTM E – 12a Standard Guide for Quantitative Analysis by Energy-Dispersive Spectroscopy

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? In like manner, deconvolution routines work well in most cases, but not when the overlapped lines arise from elements present in widely different concentrations.

Link to Active This link will always route to the current Active version of the standard. Last previous edition approved in as E — If standards are used, they must be collected under the identical geometrical conditions as the unknowns. For a more detailed ee1508 of the subject, see Goldstein, satm al.

Practice E s1508 used to analyze the round-robin data for consistency and calculates intralaboratory repeatability and interlaboratory reproducibility statistics. Longer counting times and increased beam current produce more counts. It calls attention to problems such as elements not speci? The larger the active area of the detector, the more counts will be collected, but at the expense of spectral resolution.


Whichever method is used, all elements present must be speci? For the highest accuracy, standards should be as similar as possible to the unknowns to minimize matrix effects. It asstm both methods that use standards as asgm as standardless methods, and it discusses the precision aatm accuracy that one can expect from the technique. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

These values are given in Table 5. Higher count rates can be achieved by lowering the shaping time on the system ampli? ASTM B atm 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.

This method is not based on any model and, therefore, is more general. To ensure reproducible results, calibration should be checked periodically. This is because a correction is necessary asrm account for the effect of other elements the matrix present in the specimen.

Aastm the unknown and standard were identical, each of these factors would equal one. The intensity of such X rays is proportional to the mass fraction of that element in the specimen. As such, the precision obtained should be representative of the technique. 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.

Two methods in common use are 1 the method of overlap factors and 2 the method of multiple least squares. The interlaboratory reproducibility under standard conditions averaged 8. The actual accelerating voltage of the electron beam does not always correspond with the voltage selected on the instrument. Light Element Analysis Carbon that appears to be tan in aatm on the awtm surface, or on a piece of?

For quantitative analysis, a shaping time of about 10? Even though one cannot see the individual components of a peak envelope in a spectrum, there are computer methods of deconvolution. Both specimens were analyzed by various metal producers, EDS system manufacturers, and one university. Precision and Bias Wstm limits of detection are possible with longer counting times, but the precision of trace element analysis is poorer than when the element is present at the percent level.


It would also be informative to mention the type of window on the EDS detector, if other than a conventional beryllium window. There are, however, effects of atomic number, absorption, and?

Six Sigma: Scanning Electron Microscopy & Energy Dispersive Spectroscopy

The presence of eight elements also added to the difficulty in analyzing this material. However, two artifacts that are commonly seen are pulse pileup peaks and silicon escape peaks. Requiring set parameters had little effect on the repeatability but improved the reproducibility for chromium and iron, but not for nickel.

The background in the spectrum is not linear and simple interpolation is inadequate. Evaporated carbon is usually the most suitable coating material.

It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. In many cases, the results are similar, and the standardless method may be used for convenience.

The inherent precision of the EDS method is controlled by counting statistics. The specimen must be? Some sources of bias that are under operator control are as follows.

ASTM E1508 – 12a

If the X-ray intensity of each element is compared to that of a standard of known composition and suitably corrected for the effects of other elements present, then the mass fraction of each element can be calculated. Lowering the beam current to lower the count rate usually eliminates the problem.

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.

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