Qualitative Elemental Analysis by Energy Dispersive X-Ray Spectrometry

Before attempting automatic or manual peak identification, it is critical that the EDS system be properly calibrated to ensure that accurate energy values are measured for the characteristic X-ray peaks. Follow the vendor’s recommended procedure to rigorously establish the calibration. The calibration procedure typically involves measuring a known material such as copper that provides characteristic X-ray peaks at low photon energy (e.g., Cu L3-M5 at 0.928 keV) and at high photon energy (Cu K-L3 at 8.040 keV). Alternatively, a composite aluminum-copper target (e.g., a copper penny partially wrapped in aluminum foil and continuously scanned so as to excite both Al and Cu) can be used to provide the Al K-L3 (1.487 keV) as the low energy peak and Cu K-L3 for the high energy peak. After calibration, peaks occurring within this energy range (e.g., Ti K-L3 at 4.508 keV and Fe K-L3 at 6.400 keV) should be measured to confirm linearity. A well-calibrated EDS should produce measured photon energies within ±2.5 eV of the ideal value. Low photon energy peaks below 1 keV photon energy should also be measured, for example, O K (e.g., from MgO) and C K. For some EDS systems, non-linearity may be encountered in the low photon energy range. Figure 18.1 shows an EDS spectrum for CaCO3 in which the O K peak at 0.523 keV is found at the correct energy, but the C K peak at 0.282 keV shows a significant deviation below the correct energy due to non-linear response in this range.