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1 This rticle ppered in journl pulished y Elsevier. The ttched copy is furnished to the uthor for internl non-commercil reserch nd eduction use, including for instruction t the uthors institution nd shring with collegues. Other uses, including reproduction nd distriution, or selling or licensing copies, or posting to personl, institutionl or third prty wesites re prohiited. In most cses uthors re permitted to post their version of the rticle (e.g. in Word or Tex form) to their personl wesite or institutionl repository. Authors requiring further informtion regrding Elsevier s rchiving nd mnuscript policies re encourged to visit:

2 Aville online t Journl of Moleculr Structure (2008) Chrcteriztion of henequen nturl fier y using two-dimensionl correltion spectroscopy Seong Ok Hn, Young Mee Jung, * Nno Mterils Reserch Center, Kore Institute of Energy Reserch, Dejeon , Repulic of Kore Deprtment of Chemistry, Kngwon Ntionl University, Chunchon , Repulic of Kore Received 5 Octoer 2007; received in revised form 19 Decemer 2007; ccepted 19 Decemer 2007 Aville online 31 Decemer 2007 Astrct In this presenttion, we hve pplied principl component nlysis-sed two-dimensionl (PCA2D) correltion spectroscopy to the IR spectr of electron em irrdition (EBI) or NOH solution treted henequen fiers to investigte in detil, the effects of EBI nd lkli tretment on henequen fiers. PCA2D correltion spectr with eigenvlue mnipultion trnsformtion (EMT) opertion y lowering the power of set of eigenvlues showed tht the spectrl chnges with EBI tretment re distinctly different from those for lkli tretment on henequen fiers. The crystlline nd morphous stretching nds re oserved t 1722 nd 1735 cm 1, respectively, for EBI tretment, while t 1728 nd 1739 cm 1 for lkli tretment. By lowering the power of set of eigenvlues ssocited with the originl dt, the sutle fetures hidden within spectrl dt set re reveled much more clerly thn the originl dt, which re difficult to oserve even y conventionl 2D correltion nlysis. Ó 2008 Elsevier B.V. All rights reserved. Keywords: Biocomposites; Henequen fiers; Electron em irrdition; Alkli treted; Two-dimensionl correltion spectroscopy; PCA2D correltion spectroscopy; Eigenvlue mnipulting trnsformtion (EMT) 1. Introduction Nturl fiers, such s kenf nd henequen fiers, hve ctively een pplying for utomoiles nd construction industries s reinforcement of environmentl friendly iocomposites. Nturl fier hs comprle specific mechnicl properties to glss fier nd lso dditionl dvntges of environmentl friendliness, low cost, renewle nd iodegrdle properties [1 3]. Henequen fier (Agve fourcroydes) is composed of pproximtely 77% cellulose, 4 8% hemicelluloses, 13% lignin nd 2 6% pectin nd wxes y weight. Henequen hs een used extensively to mke twins, ropes, crpet nd cordges for long period of time [4]. The structurl rrngement of lignin nd cellulose inside the fier is sed * Corresponding uthor. Tel.: ; fx: E-mil ddress: (Y.M. Jung). fundmentlly on tht lignin which cts s cementing mtrix for the cellulose component tht hs its own seprted structure. The cellulose fier is the rigid prt of the fier nd the mechnicl properties of henequen fier such s stiffness nd strength re minly influenced y its structurl rrngement [5]. The surfce of henequen fier is covered with wx, impurities which induce the poor dhesion etween the hydrophilic nturl fier reinforcement nd the hydrophoic polymer mtrix. The properties of nturl fier reinforcement re closely relted to the performnce of iocomposites, therefore, surfce modifiction of nturl fier with lkli or silne tretment is effective to enhnce dhesion etween the polymer mtrix nd the nturl fier reinforcement [6]. Wheres the chemicl tretment is wet nd energy consuming process, electron em irrdition (EBI) hs een proved s dry, efficient nd environmentl friendly tretment process of nturl fier. EBI technique hs een utilized for surfce modifiction nd properties enhncement /$ - see front mtter Ó 2008 Elsevier B.V. All rights reserved. doi: /j.molstruc

3 S.O. Hn, Y.M. Jung / Journl of Moleculr Structure (2008) of vrious polymer mterils like fiers, films nd composites for mny yers ecuse it is dry, clen nd cold process with energy sving, high speed nd environmentl friendliness [7]. Also, EBI cn mintin the inner pore structure of nturl firil, compred to the destruction of pore structure of nturl fier treted y lkli solution. It gives the dditionl dvntge of iocomposite ecuse the pore structure of nturl fier cn result in the insultion nd collision soring effects, when iocomposites pply to utomoile nd construction industries [8]. Therefore, the chrcteristics comprison of EBI nd lkli tretment on nturl fier is necessry to develop the est energy sving nd the efficient tretment. In this study, the chrcteristics comprison of EBI nd lkli tretment on nturl fier will e investigted y two-dimensionl (2D) correltion spectroscopy. Generlized 2D correltion spectroscopy is well-estlished nlyticl technique tht provides considerle utility nd enefit in vrious spectroscopic studies of polymers [9 11]. Some of the notle fetures of generlized 2D correltion spectr re: The simplifiction of complex spectr consisting of mny overlpped peks; n enhncement of the spectrl resolution y spreding peks long the second dimension; the estlishment of unmiguous ssignments through the correltion of nds tht re selectively coupled y vrious interction mechnisms; nd the determintion of the sequence of the spectrl pek emergence. The detils of this technique were descried previously [9 11]. To improve the dt qulity for 2D correltion nlysis, we recently proposed powerful development in generlized 2D correltion spectroscopy which involves the incorportion of multivrite chemometrics techniques [12 17]. Principl component nlysis-sed 2D (PCA2D) correltion showed the gret dvntge, noise suppression for generlized 2D correltion spectroscopy. We formulted the reconstructed dt mtrix A * (A * =W V T ), which no longer contins the residul (i.e., noise) contriutions, from few selected significnt scores nd lodings derived from PCA of the originl set of perturtion-dependent spectr A. Here, W nd V re score mtrix nd loding mtrix, respectively. The nottion V T stnds for the trnspose of V. The reconstructed dt mtrix, A *, otined y the product of score nd loding vector of from few selected significnt principl components, is used insted of the originl rw spectrl dt mtrix, A, for susequent 2D correltion nlysis. Recently, we hve proposed n ide of eigenvlue mnipulting trnsformtion (EMT) for further improving the generlized PCA2D correltion nlysis [12,14 16]. The PCA-reconstructed dt mtrix A * cn e expressed y singulr vlue decomposition (SVD) s, A * =USV T. Here, U, S, nd V re, respectively, then orthonorml mtrix of left singulr vectors (i.e., eigenvectors of A * A *T ), digonl singulr vlue mtrix, nd the mtrix of right singulr vectors (i.e., eigenvectors of A *T A * ), which re equivlent to the loding vectors. S =(W T W) 1/2 is digonl mtrix, where ech digonl element corresponds to the positive squre root of principl component eigenvlue. In EMT, new reconstructed dt mtrix A ** = U S ** V T, which is otined y mnipulting nd replcing eigenvlues of A *, is used insted of A * for the clcultion of enhnced 2D correltion spectr. Here, S ** is given y vrying the corresponding eigenvlues in S y rising or lowering them to the power of m, ss ** = S m. The EMT opertion chnges the emphsis of fetures contined in the originl dt set. By uniformly lowering the power of set of eigenvlues ssocited with the originl dt, the smller eigenvlues now ecomes more prominent nd the contriutions of minor components ecome mplified. More sutle difference of spectrl ehvior for ech component is now highlighted. Modifiction of 2D correltion spectr my e possile to selectively enhnce certin correltionl fetures, y systemticlly mnipulting the eigenvlues which re nothing ut weight fctors of informtion contriution to the reconstructed dt mtrix. However, y uniformly rising the power of set of originl eigenvlues, the influence of fctors ssocited with mjor eigenvlues ecomes more prominent, while the minor eigenvectors primrily rising from the noise component re no longer strongly represented. Thus, this trnsformtion of dt mtrix ecomes grdul noise reduction scheme with ttrctive flexiility of continuously fine-tuning the lnce etween the desired noise suppression nd retention of pertinent spectrl informtion. The noise contriutions, however, re lredy sustntilly suppressed y the originl PCA-sed dt reconstruction using limited numer of principl components. In this study, we pplied PCA2D correltion spectroscopy to IR spectr of EBI or lkli treted henequen fiers. We lso considered the EMT technique y lowering the power of set of eigenvlues ssocited with the originl dt to ccentute ny sutle differences in EBI or lkli treted henequen fiers, which is difficult to oserve y ordinry 2D correltion nlysis. The smll difference in EBI or lkli treted henequen fiers cn e much more gretly emphsized thn the originl dt if we mgnify the minor eigenvlues. 2. Experimentl Henequen fiers (Agvo fourcroydes), originted from Mexico, in cm long filment form, were used s reinforcement throughout this reserch. For EBI tretment henequen fiers were put into polyethylene g, nd then they were irrdited y n electron em ccelertor (ELV- 4 type, e-tech Co. Ltd., Dejeon, Kore) [18]. The henequen fiers were irrdited with different EBI dosges of 10, 30, 50, 100, 200 nd 500 kgy, respectively. For lkli tretment henequen fiers were wshed nd soked in NOH solutions of 2, 5 nd 10 wt% for 1 h, respectively. Then, the treted fiers were wshed with distilled wter, neutrlized with 2 wt% cetic cid, wshed with distilled wter gin, nd then finlly dried t room temperture

4 144 S.O. Hn, Y.M. Jung / Journl of Moleculr Structure (2008) for 3 dys. Untreted (0 kgy) henequen fiers were lso used for comprison. Fourier trnsform infrred spectr were mesured t spectrl resolution of 4 cm 1 with FT-IR-610 spectrometer (Jsco Co.). The fiers were mounted on n ATR ccessory nd the ATR-FTIR spectr were otined with n ccumultion of 128 scns for high signl-to-noise rtio. Prior to PCA clcultion, the men centering opertion ws pplied to the dt mtrix. To preserve the mplitude informtion of the vrition of spectrl intensities, which ecomes importnt lter for 2D correltion nlysis, other steps commonly used in PCA, such s normliztion scling of dt ccording to the stndrd devition, were not crried out. PCA nlysis ws performed in Pirouette softwre (Infometrix Inc.). Synchronous nd synchronous 2D correltion spectr were otined using the sme softwre s t descried previously [9,12 17]. 3. Results nd discussion The EBI-treted nd NOH-treted FTIR spectr of henequen fiers in the region of cm 1 re shown in Fig. 1 nd, respectively. Fig. 1 shows tht the EBItreted FTIR spectr of henequen fiers re virtully indistinguishle from the NOH-treted spectr. The FTIR spectr of henequen fiers showed the nds t 1738 cm 1 from cronyl group stretching, t 1608 cm 1 from free cronyl ond, t 1373 cm 1 from OAH in plne ending, t, 1246 nd cm 1 from CH deformtion, t 1204 cm 1 from CAO stretching, t 1157 cm 1 from the skeletl stretching virtions including the CAOAC stretching, nd t 1104 cm 1 from ring virtion [19 24]. No significnt chnge ws oserved in the spectr etween untreted nd the EBI treted henequen fiers. On the contrry, the henequen fier undergoes very different chemicl chnges y the lkli tretment. For the lkli treted henequen fiers, the intensity of nds t 1373 cm 1 from OAH in plne ending ws reduced ecuse of the formtion of glycoside onding. Also, the intensity of nd t 1737 cm 1 from cronyl group stretching ws reduced due to hemicellulose removl. The decrese of the intensity of nd t 1608 cm 1 cn e explined y the removl of OH ending in the sored wter molecules y lkliztion [19,20]. To investigte the effects of electron em irrdition nd lkli tretment on henequen fiers, we pplied PCA2D correltion spectroscopy to the FTIR spectr of EBI nd lkli treted henequen fiers. The originl spectrl dt sets (Fig. 1) were decomposed into scores nd loding vectors y stndrd PCA nlysis. For FTIR spectr of EBI treted henequen fiers, PC1, PC2, nd PC3 ccounts for 96.96%, 2.03%, nd 0.94%, respectively, of the contriution to the dt, while 99.03%, 0.65%, nd 0.31% for FTIR spectr of lkli treted henequen fiers. Thus, we formulted PCA-reconstructed dt set with only three significnt PCs tht hve essentilly ll informtion needed to descrie FTIR spectr of EBI nd lkli treted henequen fiers. Synchronous nd synchronous PCA2D correltion spectr constructed from the PCAreconstructed dt with three PCs for EBI treted henequen fier re shown in Fig. 2 nd, respectively. The corresponding 2D correltion spectr for lkli treted henequen fier re shown in Fig. 3 nd. The overll fetures of the synchronous spectr for EBI nd lkli treted henequen fiers re similr. However, differences, such s the sequence of intensity chnges with EBI nd lkli tretments, re oserved in synchronous spectr. This indictes tht the effect of EBI tretment on henequen fiers is completely different from lkli tretment. To etter understnd the detils of different effects of EBI nd lkli tretment on henequen fiers, we performed n EMT opertion y lowering the power of set of Asornce (.u.) 0.12 HQ 10 kgy 30 kgy kgy 70 kgy kgy 200 kgy 500 kgy Asornce (.u.) 0.12 HQ NOH 2% NOH 5% NOH 10% Fig. 1. FTIR spectr of EBI-treted () nd NOH-treted () of henequen fiers in the region of cm 1.

5 S.O. Hn, Y.M. Jung / Journl of Moleculr Structure (2008) Fig. 2. Synchronous () nd synchronous () PCA2D correltion spectr constructed from the PCA-reconstructed dt with three PCs for EBI-treted henequen fiers. The solid nd dshed lines represent positive nd negtive cross peks, respectively. Fig. 3. Synchronous () nd synchronous () PCA2D correltion spectr constructed from the PCA-reconstructed dt with three PCs for NOHtreted henequen fiers. The solid nd dshed lines represent positive nd negtive cross peks, respectively. eigenvlues ssocited with the originl dt. The new EMT-reconstructed dt mtrix A ** ws used insted of the usul PCA-reconstructed dt mtrix A * for the 2D correltion nlysis. Such EMT-reconstructed dt mtrix will emphsize the sutle contriutions from minor eigenvectors much more strongly thn the originl dt. Fig. 4 shows the synchronous 2D correltion spectr from the newly trnsformed dt mtrix A ** otined y replcing the eigenvlues of A * for EBI treted henequen fier. The power spectrum long the digonl line in the synchronous spectrum is lso shown in Fig. 4. The corresponding 2D correltion spectr for lkli treted henequen fier re shown in Fig. 5. Fig. 4 clerly shows tht y ccentuting the minor PCs, the intensity chnges of nds t 1735, 1722, 1650, 1024 nd 987 cm 1 with EBI-tretment re indeed quite significnt. However, y ccentuting the minor PCs, the intensity chnges of nds t 1739, 1728, 1713, 1660, 1644, 1632,, 1591, 1028, 1011, 992, nd 947 cm 1 re significnt with lkli tretment s shown in Fig. 5. The intensity chnges of nds in cm 1 region y ccentuting the minor PCs for lkli tretment re much greter thn those for EBI tretment. Sutle differences in the effects of EBI or lkli tretment on henequen fiers, which re difficult to oserve even y

6 146 S.O. Hn, Y.M. Jung / Journl of Moleculr Structure (2008) c d Fig. 4. Synchronous PCA2D correltion spectr constructed from the EMT reconstructed dt y vrying the vlue of power prmeter m, s m = 1 (), 1/2 (), 1/4 (c), nd 0 (d) for EBI-treted henequen fiers. The solid nd dshed lines represent positive nd negtive cross peks, respectively.

7 S.O. Hn, Y.M. Jung / Journl of Moleculr Structure (2008) c d Fig. 5. Synchronous PCA2D correltion spectr constructed from the EMT reconstructed dt y vrying the vlue of power prmeter m, s m = 1 (), 1/2 (), 1/4 (c), nd 0 (d) for NOH-treted henequen fiers. The solid nd dshed lines represent positive nd negtive cross peks, respectively.

8 148 S.O. Hn, Y.M. Jung / Journl of Moleculr Structure (2008) conventionl 2D correltion nlysis, re ccentuted much more strongly. Furthermore, there re two distinct nds in the stretching nd, crystlline nd t 1722 cm 1 nd n morphous nd t 1735 cm 1 for EBI tretment, which re not redily detectle in 1D spectr. While crystlline nd t 1728 cm 1 nd n morphous nd t 1739 cm 1 for lkli tretment re oserved [25,26]. 4. Conclusion In this study, the effects of electron em irrdition nd lkli tretment on henequen fiers were investigted for the first time y using PCA2D correltion spectroscopy. From the PCA2D correltion spectr, we conclude tht the spectrl chnges with EBI tretment re distinctly different from those for lkli tretment. The crystlline nd morphous stretching nds re oserved t 1722 nd 1735 cm 1, respectively, for EBI tretment, while t 1728 nd 1739 cm 1 for lkli tretment. By lowering the power of set of eigenvlues ssocited with the originl dt, the sutle fetures hidden within spectrl dt set, which re difficult to oserve even y conventionl 2D correltion nlysis, re reveled clerly. Acknowledgements The reserch ws finncilly supported from the CDRS R&D Center (CJ2-101) (the 21st Century Frontier R&D Progrm) y the Ministry of Science nd Technology, Kore. References [1] A.K. Bledzki, J. Gssn, Prog. Polym. Sci. 24 (1999) 221. [2] D. Cho, S.G. Lee, W.H. Prk, S.O. Hn, Polym. Sci. Tech. 13 (2001) 460. [3] R. Joffe, J. Andersons, L. Wllstrom, Composites A 34 (2003) 603. [4] M. Aguilr-Veg, C.A. Cruz-Rmos, J. Appl. Polym. Sci. 56 (1995) [5] M.N. Czurng-Mrtinez, P.J. Herrer-Frnco, P.I. Gonzlez-Chi, M. Aguilr-Veg, J. Appl. Polym. Sci. 43 (1991) 749. [6] A.K. Mohnty, M.A. Khn, G. Hinrichsen, J. Mter. Sci. 35 (2000) [7] Y.H. Hn, S.O. Hn, D. Cho, H.I. Kim, Compos. Interfces 14 (2007) 559. [8] S.O. Hn, D. Cho, W.H. Prk, H.I. Kim, Compos. Interfces 13 (2006) 231. [9] Y.M. Jung, I. Nod, Appl. Spectrosc. Rev. 41 (2006) 515. [10] I. Nod, Y. Ozki, Two-Dimensionl Correltion Spectroscopy: Applictions in Virtionl Spectroscopy, John Wiley & Sons, Inc., New York, [11] I. Nod, Appl. Spectrosc. 47 (1993) [12] Y.M. Jung, H.J. Kim, D.Y. Ryu, S.B. Kim, J.K. Kim, J. Mol. Struct. 779 (2006) 96. [13] Y.M. Jung, Vi. Spectrosc. 36 (2004) 279. [14] Y.M. Jung, S.B. Kim, I. Nod, Appl. Spectrosc. 57 (2003) 850. [15] Y.M. Jung, S.B. Kim, I. Nod, Appl. Spectrosc. 57 (2003) 557. [16] Y.M. Jung, S.B. Kim, I. Nod, Appl. Spectrosc. 57 (2003) 564. [17] Y.M. Jung, H.S. Shin, S.B. Kim, I. Nod, Appl. Spectrosc. 56 (2002) [18] [19] S.Y. Oh, D.I. Yoo, Y. Shin, G. Seo, Crohydr. Res. 340 (2005) 417. [20] V.O.A. Tnoe, T.H.D. Syndenstricker, M. Munro, S.C. Amino, Poly. Test. 24 (2005) 474. [21] R. Bdulescu, V. Vivod, D. Jusovec, B. Voncin, Crohydr. Polym. 71 (2008) 85. [22] B. Tomšič, B. Simončič, B. Orel, A. Vilčnik, H. Spreizer, Crohydr. Polym. 69 (2007) 478. [23] A.M.A. Nd, S. El-Sherief, A. Nsr, M. Kmel, J. Mol. Struct. 841 (2007) 1. [24] M. Åkerholm, B. Hinterstoisser, L. Slmen, Crohydr. Res. 339 (2004) 569. [25] Y.M. Jung, H. Sto, I. Nod, Anl Sci. 23 (2007) 881. [26] J. Zhng, H. Sto, I. Nod, Y. Ozki, Mcromolecules 38 (2005) 4274.

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