untethered atom · TEM

Which oxidation state? Reading valence from the shape of an EELS edge

Three standards that look alike can trade places in a fit. The mean valence still comes out right.

The height of an edge tells you how much of an element is there. Its shape, the energy-loss near-edge structure (ELNES), tells you the oxidation state. Here you build a Mn L2,3 spectrum from states you choose, then read the valence back three ways: fit it with references (MLLS), take the L3/L2 ratio, or find the L3 peak position. Change the counts, the energy calibration or the references, and watch which answer breaks.

Try a lesson:
1Raw spectrum. Blue band: background fit window (Γ). Dashed: power-law fit A·E−r, carried under the edge.
2Edge after background. Red: MLLS fit. Thin: each reference's share. Bottom: residual. Grey band: MLLS fit window.
3MLLS fractions. Outline: true. Filled: fitted. Bar: spread over 40 repeats.
4L3/L2 ratio. Dots: your references. Band: measured ratio. Read down to the valence.
5L3 position. About 1 eV per valence. Any energy shift goes straight into it.
Hover over a spectrum to read the numbers at that energy.

Specimen the truth you put in

Acquisition

Counts per energy channel at the top of the white line, above background. Energy shift: how far the unknown's energy axis sits from the references' (drift between sessions). Worse resolution: the unknown recorded with a wider zero-loss peak (ZLP FWHM) than the references.

Processing

DualEELS correction on: the unknown is shifted back using the zero-loss peak (ZLP) recorded at the same time as the edge. The references are always on a calibrated axis.

Numbers

The method in six steps

StepWhat you doKnob on this pageWhat goes wrong
1 RecordRecord the unknown and your references at the same energy, dispersion, resolution and collection angle.counts, worse resolution (ZLP)Too few counts: the answer wobbles. Different resolution: fractions shift.
2 Energy shiftRemove the energy shift so every spectrum sits on the same energy axis, ideally with a zero-loss peak (ZLP) recorded at the same time (DualEELS).energy shift, DualEELS correction0.5 eV of drift moves the L3 position by half a valence.
3 BackgroundFit A·E−r in a background fit window (Γ) just before the edge and subtract it.background fit window (Γ)A window that touches the edge rise, or is very short, gives a wrong exponent.
4 MLLSFit the edge as a non-negative sum of your references over a window that covers both white lines.MLLS fit window, MLLS referencesA missing reference cannot be fitted. Watch the residual.
5 RatioRemove a 2:1 step continuum, integrate L3 and L2, compare the ratio with your references'.(automatic)The ratio depends on the step model and windows. Use the same ones for references and unknown.
6 ReportReport the mean valence with its spread, the residual, and how the references were recorded.table aboveSeparate fractions of three similar states are poorly fixed, even with no noise.

Do it on your own spectra

  1. Record reference spectra of known valence on your instrument, in the same session and at the same settings as the unknown.
  2. Record the zero-loss peak (ZLP) with each spectrum (DualEELS), and use it to remove the energy shift.
  3. Pick a background fit window (Γ) at least 15 to 20 eV wide that ends a few eV before the edge starts to rise.
  4. Fit with only the references that could be there. Check the residual: it should look like noise, with no shape.
  5. Repeat on several regions or frames. The scatter is your error bar.
  6. Cross-check MLLS against the L3/L2 ratio. If they disagree by more than their spread, look for an energy shift or a missing state.
  7. Keep the thickness low (t/λ under about 0.5). Plural scattering broadens the white lines. Deconvolve if you cannot.

Scope and limits

The three references here are made-up shapes with white-line ratios (about 4.1, 3.2 and 2.2 after processing) and L3 positions (640, 641 and 642 eV) in the range reported for manganese oxides. They are not a copy of one paper's data. For real work the references must be your own, recorded like the unknown. The edge model has no multiplet structure, no crystal-field splitting and no oxygen K edge nearby. There is no plural scattering, so thickness effects are not shown. The noise is counting noise only; real detectors add readout noise and gain variation. MLLS here uses non-negative least squares with no extra terms; some people also fit a small linear background term or the first derivative of each reference to absorb a small energy shift.

On this site: Reading the EELS spectrum · EELS core-loss quantification · EELS thickness calculator · EFTEM elemental mapping

Questions people ask

Which method should I trust?

None of them alone. MLLS uses the whole shape and gives the smallest spread, if your references are right. The L3/L2 ratio is simpler and less sensitive to a small energy shift. The L3 position is quick but needs a perfect energy axis. If two methods agree within their spread, you can report the valence with some confidence.

Why are my fitted fractions so unstable?

Mn2+, Mn3+ and Mn4+ spectra look alike. A mix of Mn2+ and Mn4+ can look almost the same as Mn3+ (lesson 5). The mean valence is fixed much better than the separate fractions. Report the mean valence, or fit only two states if you know the third is absent.

How many counts do I need?

Use lesson 2: set the counts, read the spread in the table. The spread falls as one over the square root of the counts. Then check that your sample survives that dose (see the beam damage page).

How is this different from the core-loss quantification page?

That page uses the edge area to find how many atoms of an element are there. This page uses the edge shape to find their oxidation state. You can run both on one spectrum.

References

Show the 8 references
  1. D. B. Williams and C. B. Carter, Transmission Electron Microscopy, 2nd ed., Springer (2009): chapter 39 (high energy-loss spectra and images) and chapter 40 (fine structure and finer details).
  2. R. F. Egerton, Electron Energy-Loss Spectroscopy in the Electron Microscope, 3rd ed., Springer (2011): chapter 4 (background fitting) and chapter 5 (near-edge structure).
  3. H. Tan, J. Verbeeck, A. Abakumov and G. Van Tendeloo, Oxidation state and chemical shift investigation in transition metal oxides by EELS, Ultramicroscopy 116, 24 (2012).
  4. D. H. Pearson, C. C. Ahn and B. Fultz, White lines and d-electron occupancies for the 3d and 4d transition metals, Physical Review B 47, 8471 (1993).
  5. P. A. van Aken and B. Liebscher, Quantification of ferrous/ferric ratios in minerals by electron energy-loss spectroscopy, Physics and Chemistry of Minerals 29, 188 (2002).
  6. H. K. Schmid and W. Mader, Oxidation states of Mn and Fe in various compound oxide systems, Micron 37, 426 (2006).
  7. Z. L. Wang, J. S. Yin and Y. D. Jiang, EELS analysis of cation valence states and oxygen vacancies in magnetic oxides, Micron 31, 571 (2000).
  8. A. Gubbens et al., The GIF Quantum, a next generation post-column imaging energy filter, Ultramicroscopy 110, 962 (2010). Introduces DualEELS.
Cite this page: Tripathy, Manisha. “EELS Fine Structure and Oxidation State.” untethered atom, 2026, https://untetheredatom.com/tem/eels-fine-structure-oxidation-state.
BibTeX
@misc{tripathy2026eelsfinestructure,
  author = {Tripathy, Manisha},
  title  = {EELS Fine Structure and Oxidation State},
  year   = {2026},
  howpublished = {\url{https://untetheredatom.com/tem/eels-fine-structure-oxidation-state}},
  note   = {Interactive web tool}
}
Last updated 23 September 2026.