Scanning Electron Microscopy and X-Ray Microanalysis

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3.0

0

1 000

2 000

3 000

4 000

0

5 000

10 000

15 000

20 000

a

b

5 000

3.2 3.4 3.6 3.8 4.0 4.2 4.4 4.6 4.8 5.0

Photon energy (keV)

Counts

Counts

5.2 5.4 5.6 5.8 6.0 6.2 6.4 6.6 6.8 7.0

0.0 1.0 2.0 3.0 4.0 5.0

Photon energy (keV)

6.0 7.0 8.0 9.0 10.0

Benitoite_10kV20nA7%DT

Residual_Benitoite_10kV20nA7%DT

Benitoite_10kV20nA7%DT

Residual_Benitoite_10kV20nA7%DT

. Fig. 20.7 a SDD-EDS spectrum of BaTiSi 3 O 9 (benitoite) (red) at E 0 = 10 keV (11,137,000 counts) and residual (blue) after DTSA II analysis using
BaSi2O 5 (sanbornite) and Ti as fitting references and standards. b Expanded view
. Table 20.7 Analysis of BaTiSi 3 O 9 (benitoite) at E 0 = 10 keV with Ti and sanbornite (BaSi 2 O 5 ) as fitting references and standards;
integrated spectrum count = 11,366,000. Analysis performed with O K- L2,3, Si K-L2,3, Ti K-L2,3 and Ba L 3 -M4,5

O Si Ti Ba

Cav (atom frac) 0.6416 0.2149 0.07096 0.07256

Z-correction 0.955 0.953 0.947 0.943

A-correction 0.804 1.041 0.989 1.004

F-correction 1 1 1.007 1

σ (7 replicates) 0.000269 0.00016 0.000176 0.000176

σRel (%) 0.04 % 0.07 % 0.25 % 0.24 %

RDEV (%) −0.20 % 0.28 % −0.66 % 1.60 %

C (mass frac, single analy-

sis)

0.3462 0.2032 0.1143 0.3356

Counting error, std 0.0002 0.0001 7.10×10–5 0.0006

Counting error, unk 0.0002 0.0001 0.0004 0.0009

A-factor error 0.0142 0.0003 2.10×10–5 3.50×10–5

Z-factor error 0.0003 2.40×10–5 1.10×10–6 2.80×10–6

Combined errors 0.0142 0.0003 0.0004 0.0011

20.4 · The Need for an Iterative Qualitative and Quantitative Analysis Strategy