CONTENTS
Preface ix
Introduction 1
General problems in the analysis of ultra-light elements 2
BORON ANALYSIS
I Specific problems in the analysis of Boron 6
II Experimental procedures 14
II.1 Preparation and characterization of binary Borides 14
II.2 Mounting, polishing and cleaning procedures 17
II.3 Some details on the equipment used 18
II.4 Measurement of Area/Peak Factors (APFs) 18
II.5 Measurements of Peak k-ratios 19
III Results 21
III.1 Boron-K emission spectra 21
III.2 Area/Peak Factors for B-K relative to elemental Boron 38
III.3 Intensity ratios for metals and Boron 45
III.4 Relative emitted B-K intensities from the Boride specimens as a function of
accelerating voltage in relation to the mass absorption coefficients 57
IV Data reduction and comparison of correction programs 70
IV.1 Description of the “PROZA96” (z) correction program 70
IV.2 Performance of the new model 83
IV.2.1 Medium-to-heavy element analyses 84
IV.3 Results of this work 88
IV.3.1 Metal analysis in binary Borides 88
IV.3.2 Boron analyses 92
V Conclusions 98
Appendix
A Area/Peak factors as a function of peak position for a number of Borides 100
B Numerical details for the intensity measurements for metals and Boron 103
C Database for the analyses of Boron and metals 131
CARBON ANALYSIS
I Specific problems in the analysis of Carbon 137
I.1 Contamination and Background problems 141
II Experimental procedures 150
II.1 Preparation and characterization of Carbide specimens 150
II.2 Mounting, polishing and cleaning procedures 152
II.3 Details on the microprobe used and check on its operating conditions 152
II.4 Measurements of Area/Peak Factors 154
II.5 Measurements of Peak k-ratios between 4 and 30 kV 155
III Results 158
III.1 Carbon spectra in various Carbides; performance of W/Si multilayer
compared to that of conventional Stearate Crystal 158
III.2 Area/Peak Factors for C-K 178
III.3 Relative emitted intensities for C-K as a function of accelerating voltage 183
III.4 Comparison between performances of Ni/C and W/Si multilayer crystals 193
IV Data reduction and comparison of correction programs 209
IV.1 Performances of the various correction procedures 209
IV.1.1 Analysis of the metal X-ray lines in the Carbides 209
IV.1.2 Analysis of Carbon in the Carbides 211
V Some applications 226
V.1 Analysis of low levels of Carbon in Iron 226
V.2 Study of Carbon diffusion in binary Carbide systems 229
VI Conclusions 236
Appendix
1 Numerical details for the intensity measurements for metals and Carbon 237
2 Data base for the analyses of Carbon and metals 252
NITROGEN ANALYSIS
I Specific problems in the analysis of Nitrogen 257
II Experimental procedures 264
II.1 Preparation of Nitrides 266
II.2 Characterization of Nitride specimens 268
II.3 Mounting, polishing and examination procedures 271
II.4 Technical details of the microprobe used 272
II.5 Measurements of Area-Peak Factors 273
II.6 Measurements of Integral k-ratios between 4 and 30 kV 274
III Results 274
III.1 Oxygen contamination in the microprobe 275
III.2 New procedures for the analysis of Nitrogen in the presence of Titanium 280
III.2.1 Analysis of existing methods 280
III.2.2 The new method 282
III.2.3 Quantitative analysis of low Nitrogen contents in the presence of Titanium 292
III.3 Performance of LDE crystal as compared to conventional lead-stearate crystal 295
III.4 Area/Peak Factors for N-K relative to Cr2N 315
III.5 Emitted intensities for N-Kα radiation as a function of accelerating voltage 316
IV Data Reduction 327
IV.1 Analysis of the metal X-ray lines in the Nitrides 327
IV.2 Nitrogen analysis in the Nitrides 328
V Conclusions 338
Appendix
1 Numerical data on the intensity measurements of metal and Nitrogen X-ray lines 339
2 Final data base 357
OXYGEN ANALYSIS
I Introduction 361
II Problems in the analysis of Oxygen 363
III Experimental procedures 370
III.1 Origin of Oxide specimens 370
III.2 Check on the electrical conductivity of the specimens 371
III.3 Characterization of Oxide specimens 372
III.4 Mounting, polishing and examination procedures 373
III.5 Technical details of the microprobe used 374
III.6 Measurements of Area/Peak Factors 375
III.7 Measurements of Integral k-ratios 376
IV Results 376
IV.1 Performance of LDE crystal as compared to conventional lead-stearate crystal 376
IV.2 Area/Peak Factors for O-Kα relative to Fe2O3 392
IV.3 Emitted intensities for O-Kα radiation as a function of accelerating voltage 393
IV.4 Non-conducting Oxides 403
IV.4.1 Surface charging and its effects on the X-ray signals 404
IV.4.2 Influence of a coating on inter-elemental intensity ratios 408
IV.4.3 Influence of a coating on absolute emitted intensities 411
V Data reduction 417
V.1 Analysis of the metal X-ray lines in the Oxides 417
V.2 Oxygen analysis 418
V.3 Results obtained on notorious insulators 435
VI Conclusions 440
Appendix
1 Numerical data on the intensity measurements of metal and Oxygen X-ray lines 441
2 Final data base 471
References 479