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In recent years the development of new scientific instruments and techniques has made microanalysis an essential and powerful tool for the materials scientist. The ability to chemically characterize small, included particles or second-phase materials down to one micrometer (1 µm) in diameter and to determine the nature of surfaces with a depth resolution below 100A has led to the solution of serious materials problems and the development of new products and processes. This article, which is a review of the many techniques available, illustrates how the various techniques are related, when they can be most appropriately used and when they can be successfully combined in a single instrument. Such a review should: 1) aid the materials scientist in selecting the proper technique and instrument for his particular problem; 2) guide the novice in his initial efforts in the field of microanalysis; and 3) provide the expert with a critical review and state-of-the-art description of the field. Particular emphasis is placed on the quantitative capabilities of the various techniques so that the reader may obtain a full understanding of the capabilities and limitations of each. The problems associated with accuracy and precision in electron beam microanalysis are discussed so the investigator or user will be aware of potential problems. The following instruments and techniques or combinations thereof are discussed: electron probe analyzer, transmission electron microscope, scanning electron microscope, Auger electron spectroscopy, energy dispersive spectrometer, ion mass analyzer, automated instruments and quantitative metallography. Finally applications in many disciplines are presented to illustrate the vast potential of the techniques.