Determinação dos índices de cristalinidade de fibras celulósicas

Tomaz, Rose Marry Araújo Gondim; Bittencourt, Edison; Sabino, Nelson Paulieri; Kondo, Julio Isao

doi:10.1590/S0006-87051994000100013

Resumos

No presente estudo, foi avaliada a introdução de métodos de análises de micro-estrutura de fibras celulósicas. O algodão utilizado, proveniente das variedades IAC 17, IAC 19 e IAC 20, foi colhido em dez localidades do ensaio regional de variedades do Estado de São Paulo, no ano agrícola de 1985/86. Amostras de fibras de viscose, rami e rami tratado quimicamente com ácido clorídrico, também foram usadas, a fim de estabelecer uma relação entre os dois sistemas de determinação dos índices de cristalinidade. Utilizaram-se os métodos empíricos de difratometria de raios X e espectroscopia de infravermelho para as determinações dos índices de cristalinidade: o obtido por espectroscopia de infravermelho permitiu a diferenciação de variedades de algodoeiro IAC, enquanto o proposto por difratometria de raios X não possibilitou essa diferença. As propriedades físicas das fibras de variedades de algodoeiro IAC não se correlacionaram com os índices de cristalinidade obtidos nos dois processos. Os métodos usados para a determinação de tais índices foram altamente correlacionados (r = 0,95), empregando-se amostras de celulose com tratamento diferenciado.

difração de raios X; espectroscopia de infravermelho; índice de cristalinidade

The purpose of this work was to develop analytical techniques for structural characterization of cellulosic fibers. To establish a relationship between the two methods that determine crystallinity index, three varieties of cotton (IAC 17, IAC 19, and IAC 20) and fibers of viscose, rami and rami chemical treated were used. Two empirical methods, x-ray diffraction and infrared spectroscopy, were used to evaluate the crystallinity index. Differentiation of IAC cotton varieties was possible with the crystallinity index obtained by infrared spectroscopy; but, not with the x-ray diffraction method. The crystallinity index obtained by these two methods had no correlation with physical properties of cotton fibers. When cellulose fibers with different treatment were assayed, there was a high correlation (r = 0.95) between the two methodologies used for the determination of crystallinity index.

X-ray diffraction; infrared spectroscopy; crystallinity index

XII. METODOLOGIA E TÉCNICAS EXPERIMENTAIS

NOTA

Determinação dos índices de cristalinidade de fibras celulósicas¹ 1 Parte da dissertação de mestrado em Engenharia Química apresentada pelo primeiro autor à Universidade Estadual de Campinas, em abril de 1989.

Crystallinity index determination on cellulosic fibers

Rose Marry Araújo Gondim Tomaz^{I, III, IV}; Edison Bittencourt^II; Nelson Paulieri Sabino^{I, III}; Julio Isao Kondo^I

^ISeção de Tecnologia de Fibras, Instituto Agronômico (IAC)

^IIUniversidade Estadual de Campinas (UNICAMP)

IIICom bolsa de pesquisa do CNPq

IVCom bolsa de pesquisa da CAPES e UNICAMP

RESUMO

No presente estudo, foi avaliada a introdução de métodos de análises de micro-estrutura de fibras celulósicas. O algodão utilizado, proveniente das variedades IAC 17, IAC 19 e IAC 20, foi colhido em dez localidades do ensaio regional de variedades do Estado de São Paulo, no ano agrícola de 1985/86. Amostras de fibras de viscose, rami e rami tratado quimicamente com ácido clorídrico, também foram usadas, a fim de estabelecer uma relação entre os dois sistemas de determinação dos índices de cristalinidade. Utilizaram-se os métodos empíricos de difratometria de raios X e espectroscopia de infravermelho para as determinações dos índices de cristalinidade: o obtido por espectroscopia de infravermelho permitiu a diferenciação de variedades de algodoeiro IAC, enquanto o proposto por difratometria de raios X não possibilitou essa diferença. As propriedades físicas das fibras de variedades de algodoeiro IAC não se correlacionaram com os índices de cristalinidade obtidos nos dois processos. Os métodos usados para a determinação de tais índices foram altamente correlacionados (r = 0,95), empregando-se amostras de celulose com tratamento diferenciado.

Termos de indexação: difração de raios X; espectroscopia de infravermelho; índice de cristalinidade.

ABSTRACT

The purpose of this work was to develop analytical techniques for structural characterization of cellulosic fibers. To establish a relationship between the two methods that determine crystallinity index, three varieties of cotton (IAC 17, IAC 19, and IAC 20) and fibers of viscose, rami and rami chemical treated were used. Two empirical methods, x-ray diffraction and infrared spectroscopy, were used to evaluate the crystallinity index. Differentiation of IAC cotton varieties was possible with the crystallinity index obtained by infrared spectroscopy; but, not with the x-ray diffraction method. The crystallinity index obtained by these two methods had no correlation with physical properties of cotton fibers. When cellulose fibers with different treatment were assayed, there was a high correlation (r = 0.95) between the two methodologies used for the determination of crystallinity index.

Index terms: X-ray diffraction; infrared spectroscopy; crystallinity index.

Texto completo disponível apenas em PDF.

Full text available only in PDF format.

Recebido para publicação em 8 de fevereiro e aceito em 29 de junho de 1994.

EGLE JUNIOR, C.J. An X-ray diffraction study of the conformation cellulose chain. Textile Research Journal, Princeton, 33(9):711-719, 1963.
EGLE JUNIOR, C.J. & GRANT, J.N. Interrelations of structure and physical properties of untreated cottons. Textile Research Journal, Princeton, 40(2):158-168, 1970.
HERMANS, P.H. & WEIDINGER, A. X-Ray studies on the crystallinity of cellulose. Journal of Polymer Science, New Orleans, 4:135-144, 1949.
HINDELEH, A.M. X-Ray characterization of viscose rayon and the signficance of crystallinity on tensile properties. Textile Research Journal, Princeton, 50(10):581-589, 1980a.
HINDELEH, A.M. Crystallinity, crystallite size, and physical properties of native egiptian cotton. Textile Research Journal, Princeton, 50(11):667-674, 1980b.
HINDELEH, A.M. & JOHNSON, D.J. Crystallinity and crystallite size measurement in cellulose fibers: I Ramie and Fortisan. Polymer, Leeds, 13:423-430, 1972.
HINDELEH, A.M. & JOHNSON, D.J. The resolution of multipeak data in fiber science. Journal Physics D: Applied Physics, New York, 4:259-263, 1971.
NELSON, M.L. & O'CONNOR, R.T Relation on certain infrared bands to cellulose crystallinity and crystal lattice type. Part I: Spectra of lattice types I, II, III and of amorphous cellulose. Journal of Applied Polymer Science, New Orleans, 8:1311-1324, 1964a.
NELSON, M.L. & O'CONNOR, R.T. Relation of certain infrared bands to cellulose crystallinity and crystal lattice. Part II: A new infrared ration for estimation of crystallinity in cellulose I and II. Journal of Applied Polymer Science, New Orleans, 8:1325-1341, 1964b.
O'CONNOR, R.T.; DUPRÉ, E.F. & MITCHAN, D. Applications of infrared absorption spectroscopy to investigation of cotton and modified cottons. Part I: Physical and crystalline modifications and oxidations. Textile Research Journal, Princeton, 28(5):382-392, 1958.
PATIL, N.B. X-Ray studies on the orientation of microfibrilus in the primary wall of cotton fibers. Textile Research Journal, Princeton, 40(7):667-668, 1970.
PETERLIN, A. & INGRAM, P. Morphology of secondary wall fibrils in cotton. Textile Research Journal, Princeton, 40(4):345-354, 1970.
RADHAKRISHNAN, T Relation between crystallite orientation and tensile properties of cotton. Textile Research Journal, Princeton, 29(4):322-343, 1959.
SABINO, N.P.; GRIDI-PAPP, I.L.; KONDO, J.I. & CARNEIRO, J.B. Maturidade da fibra de algodão determinada pelo fibrógrafo modelo 430. Bragantia, Campinas, 39(9):69-77, 1980.
SEGAL, L.; CREELY, J.J.; MARTIN, A.E. & CONRAD, CM. An empirical method for estimating the degree of crystallinity of native cellulose using the X-ray diffractometer. Textile Research Journal, Princeton, 29(10):786-794, 1959.
WAKELIN, J.H.; VIRGIN, H.S. & CRYSTAL, E. Development and comparison of two X-ray methods for determining the crystallinity of cotton cellulose. Journal Applied Physics, New York, 30(11):1654-1662, 1959.

1

Parte da dissertação de mestrado em Engenharia Química apresentada pelo primeiro autor à Universidade Estadual de Campinas, em abril de 1989.

Datas de Publicação

Publicação nesta coleção
16 Out 2007
Data do Fascículo
1994

Histórico

Aceito
29 Jun 1994
Recebido
08 Fev 1994

This work is licensed under a Creative Commons Attribution-NonCommercial 4.0 International License.

[1] EGLE JUNIOR, C.J. An X-ray diffraction study of the conformation cellulose chain. Textile Research Journal, Princeton, 33(9):711-719, 1963.

[2] EGLE JUNIOR, C.J. & GRANT, J.N. Interrelations of structure and physical properties of untreated cottons. Textile Research Journal, Princeton, 40(2):158-168, 1970.

[3] HERMANS, P.H. & WEIDINGER, A. X-Ray studies on the crystallinity of cellulose. Journal of Polymer Science, New Orleans, 4:135-144, 1949.

[4] HINDELEH, A.M. X-Ray characterization of viscose rayon and the signficance of crystallinity on tensile properties. Textile Research Journal, Princeton, 50(10):581-589, 1980a.

[5] HINDELEH, A.M. Crystallinity, crystallite size, and physical properties of native egiptian cotton. Textile Research Journal, Princeton, 50(11):667-674, 1980b.

[6] HINDELEH, A.M. & JOHNSON, D.J. Crystallinity and crystallite size measurement in cellulose fibers: I Ramie and Fortisan. Polymer, Leeds, 13:423-430, 1972.

[7] HINDELEH, A.M. & JOHNSON, D.J. The resolution of multipeak data in fiber science. Journal Physics D: Applied Physics, New York, 4:259-263, 1971.

[8] NELSON, M.L. & O'CONNOR, R.T Relation on certain infrared bands to cellulose crystallinity and crystal lattice type. Part I: Spectra of lattice types I, II, III and of amorphous cellulose. Journal of Applied Polymer Science, New Orleans, 8:1311-1324, 1964a.

[9] NELSON, M.L. & O'CONNOR, R.T. Relation of certain infrared bands to cellulose crystallinity and crystal lattice. Part II: A new infrared ration for estimation of crystallinity in cellulose I and II. Journal of Applied Polymer Science, New Orleans, 8:1325-1341, 1964b.

[10] O'CONNOR, R.T.; DUPRÉ, E.F. & MITCHAN, D. Applications of infrared absorption spectroscopy to investigation of cotton and modified cottons. Part I: Physical and crystalline modifications and oxidations. Textile Research Journal, Princeton, 28(5):382-392, 1958.

[11] PATIL, N.B. X-Ray studies on the orientation of microfibrilus in the primary wall of cotton fibers. Textile Research Journal, Princeton, 40(7):667-668, 1970.

[12] PETERLIN, A. & INGRAM, P. Morphology of secondary wall fibrils in cotton. Textile Research Journal, Princeton, 40(4):345-354, 1970.

[13] RADHAKRISHNAN, T Relation between crystallite orientation and tensile properties of cotton. Textile Research Journal, Princeton, 29(4):322-343, 1959.

[14] SABINO, N.P.; GRIDI-PAPP, I.L.; KONDO, J.I. & CARNEIRO, J.B. Maturidade da fibra de algodão determinada pelo fibrógrafo modelo 430. Bragantia, Campinas, 39(9):69-77, 1980.

[15] SEGAL, L.; CREELY, J.J.; MARTIN, A.E. & CONRAD, CM. An empirical method for estimating the degree of crystallinity of native cellulose using the X-ray diffractometer. Textile Research Journal, Princeton, 29(10):786-794, 1959.

[16] WAKELIN, J.H.; VIRGIN, H.S. & CRYSTAL, E. Development and comparison of two X-ray methods for determining the crystallinity of cotton cellulose. Journal Applied Physics, New York, 30(11):1654-1662, 1959.

Brasil

Brasil

Determinação dos índices de cristalinidade de fibras celulósicas

Crystallinity index determination on cellulosic fibers

Resumos

Datas de Publicação

Histórico