Data were obtained to demonstrate whether the metallurgical structure affected the accuracy with which copper, gold, and lead concentrations could be determined on small samples (É46 1 gram) from ancient silver specimens. The data were taken from objects mainly assigned to the Sasanian period. Analytical methods included x-ray fluorescence, electron microprobe, and thermal neutron activation analyses. The data demonstrated that the accuracy is directly related to the uniformity of the metallographic structure. Surface sampling techniques tend to underestimate the copper concentration, and care must be taken in interpreting gold analyses from surface rubbing techniques to ensure that the object had not previously been gilded. Emission spectroscopic analyses tend to overestimate the lead concentration.