Selecting Suitable Standards for the MAN Calibration

EPMA Xtreme Probe

Selecting Suitable Standards for the MAN Calibration

To start with you should have some idea of the range of Z-bar of your unknown samples. For silicates this will normally be in the 10.5 to 14 or 15 range, for oxides 10 or 12 to 20 or 22, for other samples use the Standard program to calculate the ranges or just look at a copy of the periodic table and estimate in your head (average atomic number is approximately calculated using the sum of the weight fractions of the atomic numbers in a compound). You then select standards (usually simple synthetic oxides or metals of high purity that will cover the range of Z-bar for both the standards and unknowns that you will be analyzing.

For example, in a silicate analysis of olivine the range of Z-bar will be from forsterite (10.6) to fayalite (18.7). Therefore you would select several standards in that range to use as MAN backgrounds including for instance MgO (Z-bar=10.4), Al2O3 (Z-bar=10.6), SiO2 (Z-bar=10.8), TiO2 (Z-bar=16.4) and NiO (Z-bar=21.2). These standards adequately cover the range of Z-bar for olivine analysis. Other pure oxides of similar Z-bar could, of course, be used also.

 

To begin manually collecting data on a MAN background (let's say MgO, which was given a standard number of 12 in the standard database), create a new unknown sample from the Acquire! window. Click OK and the sample will display in the log window.

Note that "Set 1" means the first time you have collected data for this standard sample in this run. You can now manually start the counters, and collect a series of lines or points of data. Each data line or point of data represents a single unit of counting time. These lines or points are grouped together into samples each containing 100 or fewer "lines" (usually 3 to 5). All lines are numbered sequentially, and these line numbers are used frequently for reference purposes.

The line number, "status" of each line, beam counts and the x-ray counts on each channel are typed on the screen as the data is collected. The status of every line is initially "G" for good. If you see a bad line (epoxy, etc.) you can disable it at any time from the Analyze! window. This will change the status of that line to "B" for bad, and it will be ignored in all calculations. It may later be enabled if you change your mind.

When you have collected a sufficient number (5-10) of good lines for this background sample, proceed to the next one. Note that as each point is acquired, the program will print out a summary of the current sample. The summary includes average counts, the standard deviation and the one sigma (predicted standard deviation) of the average counts on successive lines. If the scatter in the counts is due totally to counting randomness, the standard deviation of the number of counts should equal to or less than the one sigma values. If the standard deviation is much larger it indicates scatter due to other causes, such as sample inhomogeneity etc.

Continue collecting data on the MAN background samples until you are done. Although the background due to the continuum usually drifts very little, the program will automatically correct the MAN background correction for drift, if more than one set of MAN backgrounds are acquired. If it is suspected that the background is drifting, possibly due to a change in the P-10 gas purity for instance, simply acquire an additional set of MAN background samples and the program will automatically calculate a linear drift correction before each quantitative analysis. For a description on the form of the drift correction see the section above titled "Automatic Standard Drift Correction".