THE

STRUCTURE OF JUTE FIBRE BY X-RAY DIFFRACTION METHOD.

By K. BANERJEE,D.Sc., F.N.I. and AJIT KUMARRAY, M.Sc., Dacca University. (Read August 29, 1941.)
ABSTRACT.

Jute fibres of different varieties have been studied by means of X-rays. It has been found that the cellulose contained in jute is identical with that in ramie as regards the internal arrangement of atoms in micelles. Lignin docs not enter into the micelles as its presence in or absence from the jute fibres does not produce any change in the cell dimensions or the relative intensities of spots. The size of the micelles determined by measuring the half-intensity width by means of a recording rnicrophotometer has been found to be much smaller than that in ramie.

INTRODUCTION. The method of X-ray diffraction for studying the ultimate structure of cellulose fibres was first applied by Polanyi (1921) and more thoroughly by Meyer and Mark (1928, 1929) and by Herzog and his collaborators (1928). They found that the fibres as revealed by X-rays are crystalline, in the sense that they contain countless small crystallites. The properties of the fibre depend to a great extent on the sizes of these minute crystallites. Cellulose is a carbohydrate of very high molecular weight and is represented by the formula (C6HlO05)n. Both X-ray investigations and the chemical work of Haworth (1929) and Staudinger (1929) have shown that the cellulose molecule is built up of parallel chains of 'glucose residues' C6HlO06 .. Each glucose residue is connected to the next through an oxygen atom and the structure is shown in fig. 1. These units are repeated at regular intervals along the length of the fibre to form one long fibre molecule. Several such molecular fibres are arranged sideways as in a crystal to form one' micelle'. These micelles are arranged parallel to each other along the chain length in the fibres. So if the fibres are irradiated by X-rays a photograph quite similar to a rotation photograph is obtained since micelles are present in all kinds of orientations obtained by rotation about the fibre axis. So spots are obtained arranged in layer lines, the axial length determined by Polanyi is 10·3A.U. From accurate measurements of the positions of the spots as well as by taking a Weissenberg goniometer photograph of a simple cellulose fibre Meyer and Mark concluded that the elementary unit of cellulose structure is monoclinic with a = 8'3,
b

=

10·3 and c

=

7·9 A.U. and

f3 =

96°.

The space-group is C; with four

glucose units in the unit cell. Considering the micelles to be single crystals, Herzog determined their sizes by measuring the widths of the diffraction
VOL. VII-No.3.
[Published December 15th, 1941.

. with differences in micellar size. /OH CH CH : ! : o "'CH/ I CH I ! "'OH HO".·· I I rj 1 / CH2". CH CH CH o I I ~ ~ j OR : I 0 I ! 1 : HO/ "'CH/ 0························· .378 K. The question whether cellulose in different forms is identical or not as regards chemical constitution has been solved by the X-ray method. \~'. cotton and flax. (2) Whether the jute cellulose has identical structure with cellulose obtained from other sources such as ramie. This was done more accurately by Hengstenberg and Mark (1928) who found that in ramie the lengths are 120 to 200 glucose units while the cross-sections contain from 200 to 250 units. indicating identical chemical oonstitution. BANERJEE & A.. K. /'~*' /CH... in order to decide the following points:(1) Whether the lignin present in jute enters into chemical combination with the cellulose or modifies the cellulose lattice in any way. cotton and flax. RAY: THE STRUCTURE OF 0··························. the diffraction patterns are quite similar except for the sharpness of the spots.:1- 1 . The following varieties of jute which have been kindly supplied to us by the Manipur Govt.············.. /CH2". (3) Whether the micellar sizes have relation with the physical properties of the fibres.. 1. It is found that for the different types of cellulose studied such as ramie. /CR". spots. In this paper the results of X-ray investigations on different varieties of jute are described.·· : I I ! ._ .. Agricultural Farm have been studied :- .. HO /CH"... FIG.

386). . The axial length along the fibre axis b obtained from the photographs are given in Table 1.. Sample No. T>\BLE 1. It is a late variety (D. ·.386 ·. 2. The other constituents are uronic acid. 3. ·. (3) After removal of lignin.O. Capsularis and is known to be the best quality jute grown in Fanduk in Tipperah (G. (2) After removal of fats.. It is a fixed type and a cross between samples 4 and 6. ·. 154). Sample No. . 4.. Sample of Jute. 370). Capsularis. VI and VII. Lattice Structure of Jute Fibres.-Same as Sample 3. 5. Sample No. 1.-Belongs to C. 6. Selected from Faridpur deep water jute. It is a selected strain giving the highest yield among the olitorius varieties (Plot No..JUTE FIBRE BY X-RAY DIFFRACTION METHOD. Jute fibre mainly consists of cellulose combined with a complex substance called lignin and also with other simpler gummy substances called hemicelluloses. but early variety (X-Early). ·. 10·30 10·34 10·25 10·28 10·27 10·25 10·28 10·32 10·30 2. ·. . Three fibre photographs were taken for each variety of jute at the three stages of chemical treatment.). The photographs are reproduced as figs. etc. . .-Belongs to C. It is a pure line selection from Serajganj Kakia Bombai (D. Ordinary Fat free Delignified Ordinary Fat free Delignified Ordinary Fat free Delignified ·. ·.-Belongs to C. 379 Sample No.. Sample No. ·.-Belongs to C. etc. 3. but before removing lignin. Plot No. ·. . viz.(1) Ordinary clean jute fibre before removing fats. 370 ·. pectin and small amounts of fat and resin.. Variety. Fats.. Sample No. X-Late . Axial length in A. The fibres were then freed from lignin by the action of chlorine peroxide. It is a late variety with high yield (X-Late). Capsularis. D. ·. waxes and resins were then extracted with a (1 . Olitorius. The middle portions of the fibres were taken and were separated as far as possible into individual fibres and washed with a solution of Pears' soap and dried.-Belongs to C. I.U. 1-6 on pls. Capsularis.. 1) mixture of alcohol and benzene in the Soxhlet apparatus.

V. 0·256 0·392 0·747 0·785 0·569 0 0·187 0·403 0·187 0·372 0·392 S.. Axial length in A. and this agrees very well with the value 10·3 A. V.W. 101 002 400 004 212 020 120 221 130 230 042 .W.W. V. 6. K.380 K. V. . . . G. V. 10·33 10·30 10·:36 10·33 10·32 10·34 10·24 ]0·31 ]0'.. 4. TABLE Sample of Jute.W. Tan".O. RAY: THE STRUCTURE OF I-continued. ·.W. obtained by Meyer and Mark for ramie cellulose. ·. M. the TABLE II.W. W. ·. The first and the second columns in Table II give the measured value of tan cp and the estimated intensity.S. ·. 'V.U. V. Ordinary Fat free Delignified Ordinary Fat free Delignified Ordinary Fat free Delignified ·. ·.S. V. Thus the values of cp were determined for all the spots and compared with those for ramie obtained by Meyer and Mark. M.U. Jute cellulose. ·.W.S. Variety. ·. V.W. W.S. The number of spots and their positions are identical in all the different photographs. BANERJEE & A. ·. 'I'ari e. I From the above table it is observed that within the limits of experimental error.154 ·.. Estimated intensity. (diffuse) V. D. V. Ramie cellulose (Meyer and Mark). V.~9 5. W. ·. This can be seen by actual superposition of the different photographs on each other and also by measurements.W. the values of the axial lengths 'b' remain the same. Then the azimuthal angle cp is given by x tan cp = R where R is the distance of the photographic plate from the fibre. M. Indices. ·. 0·260 0·386 0·768 0·567 0 0·190 0·396 0·188 0·370 0·388 V. ·.W. Let us represent the position of a spot by the co-ordinates x and y along the equatorial layer line and its perpendicular.. Reflecting planes in Jute cellulose. ·.S. Estimated intensity. X-Early ·. M.

The corrections for finite slit size and the absorption of the material are neglected as in the photographs used for this purpose the bundle of fibres used was very thin and a very narrow slit was used. In order to determine mI. it will be enough if we regard f1 to be a right angle. For cellulose the axial angle f1 is 840 according to Meyer and Mark. Laue deduced expressions for other systems of crystals.JUTE FIBRE BY X-RAY DIFFRACTION METHOD. while the spots are fairly broad. ms are the numbers of units repeated in the crystal particles in those directions. The spots used for this purpose are (101). where 0 is the angle at maximum intensity and 01 is the anglc at half intensity. To further test whether there is any effect due to these causes a powder photograph of an aluminium wire was taken under the same conditions and very sharp lines were obtained indicating that the possible errors were inappreciable. Since . The identity of the positions of the diffraction spots as regards positions and relative intensities in the photographs for the different stages of the same variety shows the unaltered nature of the cellulosestructure in these processes. The relations between the sizes of the diffraction spots and the sizes of the crystal particles have been developed first by Scherrer for cubic lattices and cubic particles. of sizes of the micelles of jute. m2. lignin and the fatty materials do not enter into the cellulose micelles so as to form either a chemical compound or solid solution. Determination. This completely disproves the contention of a school of chemists that lignin enters into chemical combination with cellulose in j ute and similar fibres. the particles being bounded by planes parallel to crystallographic faces. m2 and ms we thus require three equations and therefore measurements have to be made on three spots. (002) and (120). and ml. Thc relation between the size of the spot (h k l) and the average dimensions of the crystal particles is given by 8 = sin Ol-sin 0. For the purpose of deducing the sizes of the micelles to our order of approximation. The results show that the structure of jute cellulose is identical with that of ramie. No filter was used as the white radiation from the X-ray tube was extremely low compared with the characteristic radiation. 381 3rd and 4th columns give the corresponding quantities for ramie as measured by Meyer and Mark and the 5th column gives the indices assigned to these spots by Meyer and Mark. The widths for half intensity were determined by means of a Zeiss Recording Microphotometer. This shows definitely that in jute.

A139. Chem. 2. (1929). RAY: THE STRUCTURE OF JUTE FIBRE. ·. REFERENCES. Staudinger (1929). 8. o. 12° 8' 8°41' Ilo16' n- 8' 7°28' 10°13' The values of m1. I. ZeUs. Actually different photographs were used so that each of the spots could have the optimum exposure. f. Zeits. 69. 7. TABLE III. 42. Naturwiss. 3. 271. ·. 288.. 431. Zeitsf. Haworth (1929). 69. Celluloschemie. Chem. Hengstenberg and Mark (1928). B2. j.. (Angew) Ohem. Herzog and Jancke (1928). so there are twelve glucose units per micelle along the length of the fibre. Phys. 6 and 5 respectively. Zeits. Phys.382 K. Zeits. The Constitution of Sugar. Mark and Susich (1929)... The X-Early variety of jute was used for the purpose after the removal of fat and lignin. m2 and ma calculated from the above table are found to be 3. The cross-section contains 2 glucose units per unit cell and 15 cells per micelle and hence 30 glucose units per micelle. the blackening of the film is not proportional to the intensity of irradiation so the photometric curve of the usual standard wedge was used for determining the positions of half intensity in the photometric curve of the spot. Since along the length of the chain there are two glucose units per unit cell. 9. Chem. . London. Krist. On comparing with ramie fibre we find that the micelles of jute are -(0 of ramie micelles in length and -to in volume. 8 Indices. B4. 115.. 81 002 101 120 ·. 4. Meyer and Mark (1928). Phys. The values of 81 that were obtained are given in the second column of Table III and the third column gives the corresponding values of B. Our thanks are due to the Fibre Expert of Manipur Government Agricultural Farm for kindly supplying us with the different samples of jute studied.. 6. underexposed photographs Weretaken so that no position of the spots should be overexposed. BANERJEE & A. 235. As the three planes mentioned above give strong reflections.f. K. Polanyi (1921). 9. 61.

Sei. Vol. 370 Ia Ib Ie D.BANERJEE & RAY. Kat. VII. No. India. Inst. Lignin and Fat .Present. Fat Removed. Lignin and Fat Removed. Plate VI. Pt. Lignin Present. 3c . Proc.386 2a :2b 20 X-Late 3a 3b Fibre Photographs of -Jutc.

D.I54 4a 4b 4c . Lignin and Fat Removed.nduk 6a 6b Fibre Photographs of Jute. Lignin Present.BANERJEE (\: RAY. 60 . Lignin and Fat Present.. Fa.t Removed.c Fa.

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