Scene 9 · Figure · Grain-scale evidence

At grain scale, the same atoms appear together.

The macroscopic correlations Ni–Mn (r² = 0.66) and Ni–Ca (r² = 0.86) have a microscopic mechanism. Sample F2-3 from Nachfilter 4 of Wasserwerk Breyell carries the highest nickel mass-percent of the study: the green crosshair in the SEM micrograph marks the point where nickel co-localises with a manganese-oxide-rich grain interior.

1.82 % Ni K mass-percent · F2-3 FOTO 11
44.43 % Mn K mass-percent · F2-3 FOTO 11
3.10 % Ca K mass-percent · F2-3 FOTO 11
In-chamber TV view of the LEO Zeiss 1530 Gemini FESEM showing the multi-stub holder loaded with filter-material granules. Methods illustration.
SEM micrograph of sample F2-3 at 105 times magnification, 200 micrometre scale bar. The green crosshair marks the EDX measurement point in the manganese-oxide-rich grain interior. FOTO 11, LEO Zeiss 1530 Gemini FESEM, 17 March 2011.
EDX spectrum of sample F2-3, Spektrum 1, energy axis 0 to 11 keV. The dominant peak is manganese at 5.9 keV; nickel is detectable at 7.5 keV and calcium at 3.7 keV.
Ca · 3.10 %
Mn · 44.43 %
Ni · 1.82 %
The molecular signature
1.82 % Ni on a grain interior of 44.43 % Mn — the highest Ni mass-percent in the study and the atomic-scale mechanism of the macroscopic r² = 0.66 (Ni–Mn) correlation.
0 · multi-stub holder in the FESEM chamber
Figure (Scene 9). Three-stage grain-scale chain on sample F2-3 from Nachfilter 4 of Wasserwerk Breyell. The sequence begins with the multi-stub specimen holder inside the LEO Zeiss 1530 Gemini FESEM chamber, proceeds to the SEM micrograph at 105× magnification, 200 µm scale bar, with the green crosshair marking the EDX measurement point in the grain interior (FOTO 11, 17 March 2011), and concludes with the EDX spectrum (Spektrum 1). The composition recorded at the marked point — Ni K = 1.82 %, Mn K = 44.43 %, Ca K = 3.10 % (thesis pages 117–118) — is the highest nickel mass-percent measured across the entire REM-EDX dataset of the study (Kandemiroglu, 2011). The grain-scale co-localisation of nickel with manganese oxide provides direct molecular-scale support for the bulk-sample correlation r² = 0.66 (Fig 6, Ni–Mn) reported in Wisotzky, Kandemiroglu & Plassmann (2012); the calcium peak at 3.7 keV indicates the simultaneous presence of co-precipitated calcite within the same measurement volume, consistent with r² = 0.86 (Fig 7, Ni–Ca).