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The magnitude of systematic and statistical errors in electron probe microanalysis due to faulty specimen preparation is discussed theoretically and experimentally. It is shown that this error increases as the energy of the X-ray line being monitored decreases and also as the X-ray emergence angle decreases. Specific specimens are chosen to illustrate various preparation problems in metallurgy, petrography, and biology. Generalizing from these, certain useful instrumental adjuncts can be listed; these adjuncts tend to allow the effects of the specimen surface on the analysis to be controlled more rigorously. Several conductive coatings commonly used are evaluated in terms of electron and optical transparency, adherence, X-ray attenuation, and thermal and electrical conductivity. Finally, a brief survey of standards employed in electron probe microanalysis is made. Situations for which nonelemental standards are required are outlined. The choice of standards for various types of work is discussed.
specimen preparation, electron probes, metallography, petrography, microanalysis, X-ray analysis
Institute for Materials Research, National Bureau of Standards, Washington, D. C.