The Auger electron spectroscopy (AES) peak heights, sputtering yields, and line shapes of well‐characterized TiSiyfilms were examined. Analysis of AES peak‐to‐peak heights showed that the total correction factor (KT) used for quantification varied linearly by a factor of 10 as the mole fraction of Si (XSi) changes from 0 to 1. TheKTvariation was attributed primarily to preferential sputtering although line‐shape variations also had some effect. The line shapes of the derivative SiLVVand TiLVVspectra were examined as a function ofXSi. The TiLVVline shape did not change significantly with composition. However, the characteristic features (peak height, peak width, skewdness, etc.) of the SiLVVline shape were shown to vary linearly with silicide composition. The average sputtering rates and yields of the titanium silicides were shown to vary by a factor of 2 asXSivaries from 0 to 1. The average sputtering yields of the silicides varied linearly with composition while the sputtering rates did not. The use of peak height, line‐shape, and sputtering yield calibration lines for quantitative concentration and depth determinations is discussed.