Historic Textile and Paper Materials II - American Chemical Society

Chapter 15

Nondestructive Evaluation of Aging in Cotton Textiles by Fourier Transform Reflection—Absorption Infrared Spectroscopy

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Jeanette M. Cardamone Department of Clothing and Textiles, College of Human Resources, Virginia Polytechnic Institute and State University, Blacksburg, VA 24061

Specular Reflectance FTIR has been used to follow the chemical changes in cellulose when cotton cloth was aged for 2, 4, 7, 11, 14, 23, and 31 hours at 190°C in air and in nitrogen. The infrared absorptions of carbonyl and carboxylate groups were measured from the 1600-1750 cm-1 region. After 31 hours of aging in air and in nitrogen, the extent of carboxylate formation was approximately the same although oxidation proceeded more rapidly in air. The rate of aging in nitrogen proceeded at a uniform rate over 31 hours whereas in air, a leveling off point was reached after 11 hours. The dependence of the formation of carboxylate on the accessibility of OH groups is discussed. These results indicate the exceptional use of Specular Reflectance absorbance infrared spectroscopy for rapid, sensitive, and nondestructive detection of oxidation degradation in cotton textiles. The aging of c e l l u l o s i c t e x t i l e s includes a complex set of reactions involving oxidation, h y d r o l y s i s , c r o s s l i n k i n g . and chain s c i s s i o n . (1-3) Slow degradation at room temperature i s cumulative and can be followed by a chemical change i n the c e l l u l o s e structure or by a physical change i n some measured parameter. Often a r t i f i c i a l heat-aging i s used to simulate the natural aging process assuming that s i m i l a r changes occur.(4-7) These changes from thermal aging in a i r . in nitrogen, or i n vacuo affect c e l l u l o s e s t r u c t u r a l morphology, chemical a c c e s s i b i l i t y , and the extent of degradation. (8-11) General Infrared Spectroscopy Background Infrared spectroscopy i s recognized as a universal instrumental method for analyzing changes i n chemical structure. (12-13) There are a v a r i e t y of infrared techniques which include Transmission. 0O97-6156/89/0410-O239$O6.00/0 ο 1989 American Chemical Society

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Diffuse Reflectance, Attenuated Total R e f l e c t i o n or M u l t i p l e Internal Reflection* Photoacoustic (PAS). Phototheraal Beam D e f l e c t i o n . Specular R e f l e c t i o n Absorption, and f o r e n s i c applications w i t h the diamond c e l l and the Fourier transform infrared (FTIR) microscope. In museum l a b o r a t o r i e s . FTIR applications have been used f o r problems of i d e n t i f i c a t i o n and degradation i n a r t and archeology. (14) Several spectroscopic approaches have been used t o examine t e x t i l e s . In Transmittance FTIR an i n f r a r e d transparent sample may be s u i t a b l e f o r placement d i r e c t l y i n the infrared beam or may be ground or pulverized, mixed w i t h KBr or KC1 and pressed as a p e l l e t or d i s c . The sample can be mulled or deposited as a f i l m . (15-17) The D i f f u s e Reflectance technique requires dispersing the f i n e l y divided substrate i n a s c a t t e r i n g s a l t such as KBr or KCl. This method has been applied t o examine h i g h l y s c a t t e r i n g glass f i b e r s . (18) Attenuated and M u l t i p l e Reflectance FTIR have been used t o study f i n i s h treatments on t e x t i l e s . (19-20) These reflectance methods are complicated because yarn i n t e r l a c i n g s and c l o t h i n t e r s t i c i e s prevent close contact w i t h the r e f l e c t i n g prism surfaces. Other FTIR a p p l i c a t i o n s include Photothermal Beam Detection (21) and the use of diamond c e l l s f o r microsampling of micrograms of museum objects. (22-23) Photoacoustic FTIR spectroscopy i s i d e a l f o r measuring absorptions from s o l i d samples because i t i s unaffected by s c a t t e r i n g r a d i a t i o n . (24) The theory and technique are described elsewhere. (25-26) In Figure 1. wavenumber versus r e l a t i v e photoacoustic i n t e n s i t y f o r cotton p r i n t c l o t h (#400 Ό T e s t f a b r i c s , Inc.) i n the bottom spectrum i s compared to the spectrum of n a t u r a l l y aged cotton c l o t h from 1250 - 1300 A.D. (26). The spectral changes with aging shown i n the 1600 - 1750 cm-1 region are t y p i c a l of those found by others. (27-28) Cut samples were analyzed from the cotton c o n t r o l . Tarn fragments. 0.5 cm long were analyzed from the n a t u r a l l y aged cotton f a b r i c . Specular reflectance FTIR has been used t o examine s o l i d s and semi-solids, adhesives. and coatings. There are three systems based on reflectance angle o r i e n t a t i o n s : grazing f o r t h i n f i l m s , surface contaminates, and l u b r i c a n t f i l m s ; v a r i a b l e angle f o r t h i n films and highly r e f l e c t i v e surfaces and coatings, and f i x e d angle f o r coatings and r e f l e c t i v e surfaces. Surface a p p l i c a t i o n s include following photochemical changes of bulk and polymer coated metal and metal oxide i n t e r f a c e s (29). oxidation degradation of the surface l a y e r of a composite sample (30). and evaluation of degradation and reactions at metal polymer i n t e r f a c e s due to environmental f a c t o r s . (31) Reflectance FTIR has been used as a nondestructive and reproducible method f o r determining the amount of l u b r i c a n t on the surface of magnetic d i s c s . (32) A search of the t e x t i l e l i t e r a t u r e showed no a p p l i c a t i o n of specular reflectance FTIR f o r t e x t i l e s . The Specular Reflectance FTIR study presented here follows from e a r l i e r work where methodology using property-kinetics was developed to estimate extent of degradation. (33) Specular reflectance FTIR was examined f o r possible use i n applying the methodology nondestructively by monitoring carboxylate development f o r future c o r r e l a t i o n with strength l o s s . Although the Photoacoustic study of n a t u r a l l y and a r t i f i c i a l l y heat-aged cottons proved t o be a rapid


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Aging in Cotton Textiles

and s e n s i t i v e method f o r monitoring c e l l u l o s e degradation; the specular reflectance method was investigated because i t requires no sample taking.


Experimental Cotton p r i n t c l o t h was heat-aged at 2 ,4, 7, 11, 14, 23, and 31 hours i n a i r and i n nitrogen at 190°C. The procedure i s described elsewhere.(33) Infrared absorption was measured as a function of wavelength to d i s t i n g u i s h carbonyl and carboxylate groups which absorb from 1600 - 1750 cm-1. The Fourier transform i n f r a r e d spectrometer i s described i n d e t a i l with theory and methods i n G r i f f i t h and de Haseth's book on the subject. (34) The Specular Reflectance spectra presented here show high signal-to-noise and were c o l l e c t e d by placing a 1 3/4" χ 2" c l o t h sample on top of the 1/2" diameter opening of a reflectance sample c e l l holder which was placed i n the infrared beam. The sample c e l l was configured w i t h two f i x e d mirror planes meeting at an apex below the opening which directed the i n f r a r e d beam h o r i z o n t a l l y and upward at an incidence angle, being directed to the detector by the second mirror plane. A l l measurements were of absorbance by peak height values. A Mattson S i r i u s model 100 FTIR interferometer and computerized data c o l l e c t i o n , storage, and data manipulation system was used to c o l l e c t a l l spectra into i n d i v i d u a l data f i l e s . A mercury cadmium t e l l u r i d e detector with transmission window of 4000 to 500 cm-1 was used. A computer program was w r i t t e n to co-add 16 mirror scans i n the foward d i r e c t i o n and 16 i n reverse. Each s i n g l e pass of the mirror recorded 256 scans f o r a t o t a l of 8,192 data c o l l e c t i o n s each at 2 cm-1 r e s o l u t i o n . These data c o l l e c t i o n s were c o l l e c t e d through a 16 b i t A/D converter and were s i g n a l averaged i n t o 32 b i t words f o r f u r t h e r computations. In Figure 2A a mirror spectrum was c o l l e c t e d to represent the background. A mirror spectrum was c o l l e c t e d at the beginning of each session of data c o l l e c t i o n and were were used to r a t i o singlebeam spectra. This normalization corrected f o r instrument v a r i a b i l i t y . Figure 2B i s the Fourier transform of the interferogram (singlebeam spectrum) of the unheated c o n t r o l sample. Figure 2C i s the absorbance spectrum obtained by r a t i o i n g Β to A. A l l other absorbance spectra were obtained by r a t i o i n g a singlebeam spectrum to the mirror spectrum. These other spectra are represented by Figure 3A, 2 hours i n a i r , 3B, 31 hours i n a i r , 4A, 14 hours i n a i r , and 4B, 14 hours i n nitrogen. In Figure 5 the development of the carboxylate band at 1730 cm-1 i s ratioed against the CH s t r e t c h i n g band i n the 2900 cm-1 region. The 2900 cm-1 band was used as a second normalization standard f o r each sample since i t showed no appreciable change with aging. Normalizing to t h i s i n t e r n a l standard provided a c o r r e c t i o n f o r changes i n r e f l e c t i v i t y due to changes i n sample p o s i t i o n i n g . In Figure 6 the 1730 cm-1 carboxylate band i s compared to the OH s t r e t c h i n g absorptions which represent intermolecular hydrogen bonding at 3300 cm-1 f o r an i n d i c a t i o n of the interdependence of these f u n c t i o n a l groups during aging.


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Wavenumbers (cm ) Figure 1 - Photoacoustic FTIR spectra of fibers from new cotton c l o t h (lower Spectrum) and approximately 700 year old cotton (upper spectrum). The aged cotton f i b e r was sample #3019 (circa A . D . 1250-1300). Both spectra were obtained by averaging 1000 interferometer scans. Note the presence of new absorption bands i n the C=0 region in the aged sample. * Reproduced with permission from reference 26. Copyright 1987 T e x t i l e Research Journal.

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Figure 2B - Singlebeam Spectrum of Unheated Cotton Cloth

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Figure 3Α - Cotton Cloth Aged f o r 2 hours in a i r at 190 C

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Figure 3B - Cotton Cloth Aged for 31 hours in a i r at 190°C


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Figure ΑΑ - Cotton Cloth Aged f o r 14 hours i n a i r at 190 C

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Figure 4B - Cotton Cloth Aged f o r 14 hours i n nitrogen at 190 C


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1.2 -

Development of 1730cm- with 2900cm-' as Reference (1730/2900cm-') in Air ~ and in Nitrogen ""S~" 1

Figure 5 - Development of 1730 cm-1 with 2900 cm-1 as Reference (1730/2900 cm-1) i n A i r and i n Nitrogen

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Time versus l730/3340cm-' Absorbance in Air at I90°C. Figure 6 - Time versus 1730/3340 cm-1 Absorbance in A i r at 190°C


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Discussion and Results There i s a vide variety of complex c e l l u l o s e oxidation reactions. Oxidation products. oxycelluloses. can form from s e l e c t i v e oxidations of the C-6 OH. C-2 OH. and C-3 OH groups to carbonyl and carboxyl groups (35). These OH groups on c e l l u l o s e have different r e a c t i v i t i e s . It can be reasoned that oxidation w i l l cause reducing end group conversion from OH at the reducing end of a polymer chain to aldehyde to acid carboxylate (36). Different r e a c t i v i t i e s and a c c e s s i b i l i t i e s can be found i n different parts of the f i b e r . An extensive body of l i t e r a t u r e has been amassed to describe the effects of various oxidizing agents including 21% oxygen i n a i r on the formation of oxycelluloses under widely diverse conditions of time, temperature, and concentration. During low temperature degradation of c e l l u l o s e the glycosyl u n i t s . C(l) -0 - 0 ( 4 · ) . decompose with the formation of water, carbon monoxide, and carbon dioxide. (37.) With the cleavage of the gylcosyl u n i t s , shorter c e l l u l o s e chains form which can lead to a loss i n t e n s i l e strength. Certain measured parameters such as weight l o s s , degree of polymerization, strength retained, and color change have been used to follow the k i n e t i c effects of heat-aging i n a i r . (8.38) The thermal degradation of c e l l u l o s e i s thought to f i t an o v e r a l l pattern or series of steps which describe the rate of attack on the glycosyl linkages. The f i r s t i n i t i a l stage affects weak linkages. This i s followed by a slower rate where these linkages in the amorphous regions are affected. In the f i n a l stage the slowest rate of attack i s proposed for the c r y s t a l l i n e regions where a l e v e l i n g off degree of polymerization (LODP) i s described. (39) Specular Reflectance FTIR Spectra. When the spectra are examined for the effects of aging, the unheated cotton control in Figure 2C contains the sharp band at 3600 cm-1 assigned for free OH stretching (non-hydrogen- bonded OH). (40) The sample was free of water and the spectrum was collected after a long purge of the o p t i c a l bench where the samples were stored under the drying effect of l i q u i d nitrogen used to cool the detector. A l l samples were handled inside a glove bag sealed to the opening to the sample compartment. By contrast, the broad hydrogen bonded absorption at 3300 cm-1 i n Figure 3A indicates that after two hours of aging there are definite morphology changes brought about by inter-and intra-molecular hydrogen bonding which can lead to c r o s s l i n k i n g . Another c r i t i c a l spectral region i s 1630 cm-1 where water absorption bands have been reported (41) In this study this band develops from chemical change and not from absorbed water. This i s supported by the spectral changes i n 3360 and 1630 cm-1 which do not p r o c è d e on the same time frame, consequently the chemical changes i n these groups are not due to the same chemical species. The assignment of the 1630 cm-1 absorption as carbonyl i s consistant with the spectra of -glucose i n i t s aldohexose form. (41) When the Specular Reflectance spectra in Figures 3A and 3B are compared to the PAS spectrum i n Figure 1. the Reflectance spectra show somewhat better spectral d e t a i l because of a higher resolution (2 cm-1 versus 4 cm-1. and a higher number of data c o l l e c t i o n s . 8.192 versus 1000).

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Compared t o t h e PAS s p e c t r a o f c o t t o n c l o t h , i n t h e S p e c u l a r R e f l e c t a n c e s p e c t r a , t h e s i g n a l - t o - n o i s e i s h i g h e r and any n o i s e i s low enough t o show c l e a r l y t h e s p e c t r a l f e a t u r e s d e s c r i b e d h e r e . Even though t h e r e a r e d i f f e r e n c e s due t o t h e change i n s a m p l i n g c o n d i t i o n s , t h e s p e c t r a c a n be compared f o r a o n e - t o - o n e c o m p a r i s o n and i d e n t i f i c a t i o n o f a b s o r p t i o n b a n d s . Note however t h a t i n t h e PAS spectrum r e l a t i v e i n t e n s i t i e s a r e d i s p l a y e d and t h a t t h e Specular Reflectance spectra show an absolute response and measurement w h i c h l e a d s t o a b e t t e r p o s s i b i l i t y f o r q u a n t i f i c a t i o n and a more r i g o r o u s t r e a t m e n t o f t h e d a t a . The f o l l o w i n g summarizes t h e changes r e v e a l e d by S p e c u l a r R e f l e c t a n c e s p e c t r o s c o p y when c o t t o n c l o t h i s h e a t - a g e d : A i r a g i n g a f t e r 31 h o u r s l e a v e s t h e c l o t h i n a f r i a b l e and b r i t t l e s t a t e where t h e e x t e n t o f d e g r a d a t i o n i s v e r y h i g h . In n i t r o g e n a f t e r 31 h o u r s , c a r b o x y l a t e forms t o t h e same e x t e n t as a f t e r 31 hours i n a i r ( F i g u r e 5 ) . T h e r e i s a d i f f e r e n c e i n t h e r a t e o f a g i n g when t h e a i r and n i t r o g e n e n v i r o n m e n t s a r e compared. T h e r e i s g r e a t e r c a r b o x y l a t e a b s o r p t i o n i n a i r a t 14 h o u r s t h a n i n n i t r o g e n i n 14 h o u r s . .. A f t e r 11 h o u r s o f a g i n g i n a i r . a l e v e l i n g o f f p o i n t for c a r b o x y l a t e development i s r e a c h e d . Up t o 31 h o u r s o f aging, there is no l e v e l i n g off for c a r b o x y l a t e development when c o t t o n c l o t h i s aged i n n i t r o g e n . When the 1730/3340 cm-1 a b s o r p t i o n r a t i o s a r e p l o t t e d v e r s u s wavenumber t h e r a t e o f c a r b o x y l a t e f o r m a t i o n i s f a s t e r t h a n t h e r a t e o f change i n OH ( F i g u r e 6 ) . I n f a c t t h e r e i s l i t t l e change i n t h e OH r e g i o n o v e r 2 t o 31 hours o f a g i n g . Conclusions The h e a t - a g i n g o f c o t t o n c e l l u l o s e i n n i t r o g e n i n v o l v e s c a r b o n y l and c a r b o x y l a t e group f o r m a t i o n s w h i c h can be m o n i t o r e d by t h e i n f r a r e d a b s o r p t i o n s a t 1600 - 1750 cm-1 w i t h S p e c u l a r R e f l e c t a n c e F T I R . Not a l l p r i n c i p a l bands undergo change. F o r example, t h e r e i s little change i n t h e r e g i o n s f o r OH a b s o r p t i o n a t 3340 c m - 1 . CH a t 2900 cm-1. and c a r b o n y l a t 1630 cm-1 o v e r 2 t o 31 hours o f a g i n g i n a i r and i n n i t r o g e n . The pronounced i n c r e a s e i n t h e 1730 cm-1 band f o r c a r b o x y l a t e i n d i c a t e s t h a t the o x i d a t i o n may not form by d i r e c t c o n v e r s i o n o f t h e s e o t h e r f u n c t i o n a l groups whose a b s o r p t i o n s change o n l y s l i g h t l y . I t i s p o s s i b l e , however, t h a t t h e r e may be a s t e a d y s u p p l y o f t h e s e g r o u p s w h i c h becomes a v a i l a b l e i f t h e s e g r o u p s a r e i n v o l v e d i n t h i s c h e m i c a l c h a n g e . F o r example, the a c c e s s i b i l i t y o f t h e OH groups i n t h e amorphous r e g i o n s may i n c r e a s e w i t h a g i n g . By F i g u r e 6. more OH groups c o u l d become a v a i l a b l e a t a s l o w e r r a t e t h a n t h e f o r m a t i o n o f t h e c a r b o x y l a t e g r o u p s . I t c a n be reasoned t h a t a p o s s i b l e s o u r c e f o r t h e i n c r e a s e i n 1730 cm-1 a b s o r p t i o n i s t h e c o n v e r s i o n o f t h e r e d u c i n g a l d e h y d i c end groups t o a c i d g r o u p s . O t h e r s o u r c e s o f c a r b o x y l a t e s may be b y g l y c o s y l bond c l e a v a g e and t h e subsequent f o r m a t i o n o f s h o r t e r c h a i n s w i t h end g r o u p s h a v i n g OH and a l d e h y d e w h i c h o x i d i z e t o c a r b o x y l a t e . The l e v e l i n g o f f p o i n t i n F i g u r e 6 has been found by o t h e r s and has been c h a r a c t e r i z e d a t t h e p h y s i c a l l e v e l as the l i m i t o f a c c e p t a b l e s t r e n g t h . (39) L e v e l i n g o f f has been e x p l a i n e d as t h e end



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of the attack i n the amorphous regions and the r e s i s t i v i t y to chemical attack of the remaining highly ordered m i c r o c r y s t a l l i n e regions (39). The spectral data collected for Figure 5 support what others have found, that air-aging p r o c è d e s faster than nitrogen-aging but that in both environments, an endpoint can be reached. (8) The oxycelluloses which form i n c e l l u l o s e with aging are therefore time and temperature dependent. The rate at which they develop can be controlled to a limited degree by choosing a nitrogen environment to slow the process. With t h i s exceptional use of Specular Reflectance FTIR. i t may be possible to follow the aging process nondestructively and to estimate the extent of degradation which corresponds to the end of a t e x t i l e ' s useful l i f e . Acknowledgments Professor James 0. Alben. Director of the Biospectroscopy Laboratory. The Ohio State University (NIH Grants: HL28144 and RR01739) provided the f a c i l i t y and t r a i n i n g for the author. Salary and research support were provided i n part by state and federal funds appropriated to the Ohio A g r i c u l t u r a l Research and Development Center and to the V i r g i n i a A g r i c u l t u r a l Experiment Station.

Literature Cited 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

13.

Hebeish, Α.; El-Aref, A. T.; El-Alfi, Ε. Α.; and El-Rafie, M. H. J . Appl. Polm. Sci. 1979, 23, 453-462. Philipp, B.; Baudisch, J.; and Ruscher, C. TAPPI J. 1969, 52, (4), 693-698. McGinnis, G. D.; Shafizadeh,; Casey, J . P. Ed. In Pulp and Paper Chemistry and Chemical Technology. 3rd ed. Wiley-Interscience: New York, 1980; Vol 1. Chapter 1. Rasch, R. H.; Scribner, B. W. Res. Nat. Bur. Stand., 1933, 11, (5), 727-732. Scribner, B. W. J . of Res. Nat. Bur. Stand., 1939, 23 (3), 405-413. Richter, G. Α.; Wells, F. L. TAPPI J, 1956, 39, 603- 608. Block, I. J . Amer. Inst. Conserv., 1982, 22, 25-36. Shafizadeh, F.; Bradbury, A. G. W. J. Appl. Polym. Sci., 1979, 23, 1431-1442. Parks, E. J . TAPPI J., 1971, 54 (4), 537 - 544. Fairbridge, C.; Ross, R. Α.; Sood, S. P. J . Appl. Polym. Sci., 1978, 22, 497 - 510. Zeronian, S.H. In Cellulose Chemistry and Technology; ACS Symposium Series 48; American Chemical Society: Washington, D.C. 1977; pp. 189-205. Morris, N.M.; Berni, R.J. In Polymers for Fibers and Elastomers; Arthur,J . C., J r . , Ed.; ACS Symposium Serives No. 260, American Chemical Society: Washington, D.C., 1984; 62-74. Yang, C.Q.; Bresee, R.R.; Fately, W.G.; Perenich, T. A. In The Structures of Cellulose; Atalla, R. H. Ed.; ACS Symposium Series No. 340, American Chemical Society: Washington,D.C., 1987; 214- 232.


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Historic Textile and Paper Materials II - American Chemical Society

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