Procedures were developed to enable standard x-ray diffractometric equipment to be used to study and compare textile fiber crystallographic characteristics. The approach was based on fitting diffractometric data to the Gaussian distribution by weighted regression analysis, which also supported an assessment of error propagation. Crystallite dimensions were obtained through the Scherrer method using analytically derived spectral line breadths. Percent crystalline component was determined by summing background-corrected amorphous and crystalline components of the spectra. A diffractometric analysis was made of samples of rare textiles recovered from a 133-year old shipwreck, as well as modem fabrics submerged for three months at the same deep ocean site. The microcrystallite size of the historic textile materials increased, while the percent crystalline component decreased and unit cell dimensions remained constant. The crystallite sizes of modern linen immersed for three months with iron, copper, or alone did not increase, while the percent crystalline component decreased and the unit cell dimensions remained constant. While x-ray diffractometric studies of fibers have been conducted for years, the work we report here concerns a data processing method we have developed to assess experimental errors through regression analysis and propagation of error techniques applied to the Scherrer method of crystallite size evaluation. We have included in the method a scheme with which to weight the observed intensity values, as well as a mechanism for calculating the percent crystalline component. This study significantly builds on our preliminary work [ 7 ] .As an example of the method, we subjected a group of textiles recovered from a deep ocean environment to diffractometric analysis. One group was recovered from the interior of a trunk that sank to the ocean floor in 1857 and was raised in 1990. A second group we examined was composed of modem textiles submerged at the same deep ocean site for a period of three months and retrieved in October 1991.Review of Literature X-ray diffractometric analysis of cellulosic fibers yields data useful in deducing the arrangement of polymer molecules within those fibers. Cellulose fiber structures contain highly ordered crystalline domains interposed among amorphous zones and, in varying degree, ordered along the fiber axis [ 27,16 ] .Determinations of crystal size and of percent crystalline composition have been used to support the validity of proposed structure models, as well as to describe structural consequences of degradation or chemical treatment of fibers [ e.g., 5, 20 ] . In addition, crystal size and percent crystallinity have been linked to the physical performance properties of fibers and fabrics [ e.g., 31, 13] and related to physical property changes as a consequence of degradation of cellulosic polymers [ e.g., 31, 1 ] . Rau [22] has summarized the Scherrer technique for determining crystallite size and demonstrated the general method for crystallites ranging from 20 to ...