The distribution and concentration of dopants in the core of an optical fiber, at low concentrations, particularly the rare earth dopants, are difficult to measure quantitatively. However, such information is critical to the determination of absorption cross sections of rare earth dopants in fiber amplifiers and the optimization of their performance. A number of different analytical techniques, such as secondary ion mass spectrometry (SIMS) and the electron probe microanalyzer (EPMA) were used here, along with prepared glass standards, to determine the Er concentration and distribution in optical fiber preforms containing Al, Ge and P. These results were compared with data obtained by neutron activation analysis (NAA) and x-ray fluorescence (XRF) which measure the average concentration of Er in the core. It has been shown that SIMS (and EPMA), in conjunction with NAA data can be used to establish, quantitatively, the Er concentration in the preform core, without the need for glass standards.