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 dif fractometric 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 con stant. 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.
Get full access to this article
View all access options for this article.
References
1.
Atalla, R.H. , The Crystallinity of Cellulosic Fibers, in "Preservation of Paper and Textiles of Historic and Artistic Value II," Advances in Chemistry Series, no. 193, J. C. Williams, Ed., American Chemical Society, Washington, D.C., 1981, pp. 69-176.
2.
Beers, Y., "Introduction to the Theory of Error," Addison-Wesley , New York, 1958.
3.
Berry, G.M., Hersh, S.P., Tucker, P.A., and Walsh, W.K., Reinforcing Degraded Textiles, Part I: Properties of Naturally and Artificially Aged Cotton Textiles, in "Preservation of Paper and Textiles of Historic and Artistic Value," Advances in Chemistry Series, no. 164, J. C. Williams, Ed., American Chemical Society, Washington, D.C., 1977 , pp. 228-248.
4.
Caulfield, D.F. , and Steffes, R.A., Water Induced Recrystallization of Cellulose , Tappi52 (7), 1361-1366 (1969).
5.
Chidambareswaran, P.K., Sreenivasan,, S., and Patil, N.B., Quantitative Analysis of Crystalline Phases in Chemically Treated Cotton Fibers, Textile Res. J.57, 219-222 (1987).
6.
Conrad, J., Final Voyage, Am. Hist. Illustrated72 (3/4), 58-65 (1991).
7.
Foreman, D.W. , and Jakes, K.A., X-ray Diffractometric Measurement of Cellulose Microcrystallite Size, in "Cellulose '91 Proceedings ," Ellis Horwood, West Sussex, England (in press).
8.
Gröbe, A., Properties of Cellulose Materials, in "Polymer Handbook ," 3rd ed., J. Brandrup and E. H. Immergut, Eds., John Wiley & Sons, New York, 1989 , p. 117.
9.
Herdendorf, C.E., Discovery in an Alien EnvironmentAm. Hist. Illustrated72 (3/4), 66-71 (1991).
10.
Hermans, P.H. , and Weidinger, A., Quantitative X-ray Investigations on the Crystallinity of Cellulose Fibers, A BackgroundAnalysis , J. Appl. Phy. 19, 491 ( 1948).
11.
Hindeleh, A.M. , Crystallinity, Crystallite Size, and PhysicalProperties of Native Egyptian Cotton , Textile Res. J.20, 667-674 (1980).
12.
Hindeleh, A.M. , and Johnson, D.J., The Resolution of Multipeak Data in Fiber Science, J. Phys. D. Appl. Phys.4, 259-263 (1974).
13.
Hindeleh, A.M. , and Johnson, D.J., An Empirical Estimation of Scherrer Parameters for the Evaluation of True Crystallite Size in Fibrous Polymers , Polymer21, 929-935 (1980).
14.
Jakes, K.A. , and Mitchell, J.C., On the Recovery and Drying of Textiles from a Deep Ocean Historic Shipwreck, J. Am. Ins. Cons.31, 343-353 (1992).
15.
Jakes, K.A. , and Wang, W.The Characteristics of Textile Fibers and Fabrics Recovered from a Historic Deep Ocean Site, Ars Textrina ( in press).
16.
Jones, D.W., X-ray and Electron Diffraction, Cellulose I Structure Studies, in "Cellulose and Cellulose Derivatives," vol. V, N. Bikales, N. and L. Segal, Eds, Wiley-Interscience, New York, 1954, pp. 117-180.
17.
Kasper, J. S., and Lonsdale, K., Eds. "International Tables for Crystallography ," vol. II, Kynoch Press, Birmingham, England, 1967, p. 51.
18.
Khalifa, B.A. , Abdel-Zaher, N., Shoukr , F.S., Crystalline Character of Native Chemically Treated Saudi Arabian Cotton Fibers, Textile Res. J.61, 602-608 (1991).
19.
Mann, J., Roldan-Gonzales, L., and Wellard, H.J., Crystalline Modifications of Cellulose, Part IV: Determination of X-ray Intensity Data, J. Polym. Sci.42, 165-171 (1960).
20.
Perel, J., AnX-ray Study of Regain-dependent Deformations in Cotton Crystallites, J. Textile Inst.81, 241-244 (1990).
21.
Pugh, E.M., and Winslow, G.H., "The Analysis of Physical Measurements," Addison-Wesley , Reading, MA, 1966.
22.
Rau, R.C., "Advances in X-ray Analysis," vol. V, Plenum Press, University of Denver, 1962, pp. 104-116.
23.
Ruland, W., X-ray Determination of Crystallinity and Diffuse Disorder Scattering , Acta Cryst.14, 1180-1185 (1961 ).
24.
Scallan, A.M. , A Quantitative Picture of the Fringed Micellar Model of Cellulose, Textile Res. J.41, 47-653 (1971).
25.
Scherrer, P. , Bestimmung der Grosse und inneren Struktur von Kolloidteilchen mittels Rontgenstrahlen, Nach. Ges. Wiss.Göttingen2, 8-100 (1918).
26.
Segal, L., Creely, J.J., Martin, A.E., and Conrad, C.M., An Empirical Method for Estimating the Degree of Crystallinity of Native Cellulose Using the X-ray Diffractometer, Textile Res. J.29, 786-794 (1959).
27.
Shenouda, S.G., The Structure of Cotton Cellulose, in "Applied Fibre Science ," vol. 3, F. Happey , Ed., Academic Press Inc., NY, 1979, pp. 275-309.
28.
Tripp, V.W., and Conrad, C.M., X-ray Diffraction, in "Instrumental Analysis of Cotton Cellulose and Modified Cotton Cellulose," R. T. O'Connor , Ed., Marcel Dekker, Inc, NY , 1972, pp. 339-379.
29.
Varma, I.K. , Anantha Krishnan , S.R., and Krishnamoorthy, S., Effect of Chemical Treatment on Density and Crystallinity of Jute Fibers, Textile Res. J.59, 368-370(1989).
30.
Wakelin, J.H. , Virgin, H.S., and Crystal, E., Development andComparison of Two X-ray Methods for Determining the Crystallinity of Cotton Cellulose , J. Appl. Phys.30, 1654-1662 (1959 ).
31.
Ward, K., Crystallinity of Cellulose and Its Significance for the Fiber Properties , Textile Res. J.20, 363-372 (1950).
32.
Warren, B.E. , and Briscoe, J., The Structure of Silica Glass by X-ray Diffraction Studies, J. Am. Ceram. Soc.21, 49-54 (1938).
33.
Young, H.D., "Statistical Treatment of Experimental Data," McGraw-Hill , New York, 1962.
