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CONTENTS
Preface ixIntroduction 1General 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
