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 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