electronprobemicroanalysisepma-uw-geoscience.pptVIP

* * * * * * * * * * * Higher order reflections Recall nl = 2d sinq. Higher order reflections are possible in your specimens, and must be avoided to prevent errors in your analyses. Reed (1993) reports that LIF can show a strong second order peak, up to 10% of the first order peak. In 1999, the 777 class examined the higher order reflections of Cr Ka lines. On PET, 2nd and 3rd order peaks were present, and decreased ~an order of magnitude with increasing n. UW- Madison Geology 777 UW- Madison Geology 777 On TAP, up to the 8th order peak was present. Here, the intensity of the odd numbered orders was less than the following even order, e.g. the 5th order Ka had 30% fewer counts than the 6th order line. Differential mode of pulse height analysis (PHA) may be used to ignore counting higher order X-rays. n 3 4 5 6 7 8 counts 1563 327 75 102 31 97 Pulse Height Analysis If a higher order reflection falls upon a peak (or unavoidable background) position, the analyst has the option of using Pulse Height Analysis, i.e. setting up a window and not counting any X-rays that have energies greater than the window’s upper limit. There is a lower limit (baseline, usually 0.5 volts). The window stretches above it (here 4 volts), and thus a second order reflection should have a pulse height around 6 volts, and would not be counted. There are some situations where operation in differential mode can introduce errors (pulse height depression), so the normal mode is integral. And if differential is used, it is good to do some tests first to get a feeling of how comprehensive its filtering action is. window baseline UW- Madison Geology 777 Integral vs Differential PHA Goldstein et al, p.507-8 Analysis of ‘light elements’ such as C is complicated because of the long wavelength (44 ?) which means that higher order reflections of many elements can interfere. At top, where the PHA is set to the “count everything” integral mode, the 3rd order reflec