We have studied the mineral composition of the gloss and the ceramic body o
f three pieces of Attic Greek pottery by applying the techniques of high-re
solution powder diffraction using synchrotron x-rays. The measurements were
performed on Stations 2.3 and 9.1 at the Synchrotron Radiation Source, Dar
esbury Laboratory. High quality powder patterns from the bulk of the cerami
cs and from the gloss surfaces have been obtained. The diffraction results
show interesting variations of mineral composition between the gloss of the
different sherds as well as variations between the bulk and the gloss. Thi
s makes phase identification and comparison between different fabrics less
ambiguous. Spinel minerals are present in the gloss which are absent in the
main body of the ceramics. Diffraction lines from one surface match the pa
tterns of hematite, magnetite/maghemite and hercynite, while solid solution
s of spinel structures appear to be present in the gloss layer of another s
ample. Crystallite particle sizes and lattice parameters of the minerals in
the gloss layer of another sample. Crystallite particle sizes and lattice
parameters of the minerals in the gloss layer have been accurately determin
ed. Supplementary scanning electron microscopy (SEM) reveals the gloss thic
kness to be approximately 20 mum but with variations down to 5 mum. Analysi
s of the diffraction profile for the hematite component reveals a particle
size int he order of 0.027 mum.