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This article is also available online at: http://trj.sagepub.com/cgi/reprint/75/9/645 SEPTEMBER 2005 645 Fourier Transform Infrared Analysis of Trehalulose and Sticky Cotton Yarn Defects Using ZnSe-Diamond Universal Attenuated Total Reflectance

NOUREDDINE ABIDI AND ERIC HEQUET International Textile Center, Texas Tech University, Lubbock, TX 79409, U.S.A.

ABSTRACT The universal attenuated total reflectance Fourier transform infrared (UATR-FTIR) equipped with a ZnSe-diamond composite crystal accessory was used to investigate the implication of trehalulose in the formation of yarn defects during rotor spinning of moderately sticky cotton mixes. One cotton bale contaminated with aphid honeydew and one contaminated with whitefly honeydew were selected. Mixes having moderate levels of stickiness were prepared from these two bales by mixing sticky cotton with non-sticky cotton. These cotton mixes were processed and the yarn defects were collected and analyzed using UATR-FTIR. The results obtained showed a high correlation between the FTIR spectra of the yarn defects from the whitefly honeydew-contaminated mixes and the spectra of artificial reconstituted whitefly honeydew. No significant difference was seen between the spectra of yarn defects from aphid honeydew-contaminated cotton and those of non-contaminated cotton. The FTIR and Raman studies of the hydration process of trehalulose showed a drastic impact of moisture absorption on the intensities of the vibration modes of trehalulose. These results all indicate that trehalulose is the primary concern when forming yarns from cotton with moderate honeydew contamination.

Cotton stickiness caused by excess sugars on the We reported in previous work on the implication of lint, from the plant itself [4] or from insects [9], is a trehalulose in the residue build-up on the textile equip very serious problem that affects all segments of 'the ment during processing of moderately sticky cotton [3]. cotton industry [6, 11]. Stickiness is a worldwide We have demonstrated that because of its high hygro contamination problem with around one-fifth of the scopicity, low-melting point, and film-like structure world production affected to some degree [10]. The (hydrated form), trehalulose was the main source of sugar composition of water extracts from honeydew concern in textile processing. It slowly contaminates the contaminated cottons analyzed by high-performance machinery: first sticking to surfaces, then catching dust, liquid chromatography (HPLC) is extremely complex. silica, etc. Among the identifiable sugars, the disaccharide treha In this work, our objective was to evaluate the useful lulose and the tri-saccharide melezitose are specific to ness of the universal attenuated total reflectance Fourier insects and are not found in the plant. In general, a transform Infrared (UA TR-FTIR) equipped with a high percentage of melezitose along with a low per ZnSe-diamond composite crystal accessory to investi centage of trehalulose reveals the presence of aphid gate the implication of trehalulose in the formation of the (Aphis gossypU Glover) honeydew. Conversely, a yarn defects during processing of moderately sticky cot dominance of trehalulose indicates contamination by ton. The advantage of ZnSe-diamond sampling acces whitefly (Bemisia argentifolii Bellows and Perring [= sory is that no sample preparation is required and it is not B. tabaci (Gennadius) strain B]) honeydew. Hendrix et destructive (the measurements are performed directly on al. [3] analyzed the honeydew from insects and found the yarn). that the aphid honeydew contained around 38.3% me lezitose plus 1.1 % trehalulose, while the whitefly hon eydew contained 43.8% trehalulose plus 16.8% me Experimental lezitose. However, these relative percentages will vary MATERIALS depending on the environmental or feeding conditions. In other studies, it has been demonstrated that the One commercial cotton bale contaminated with aphid severity of stickiness incidents in the textile mill is honeydew and another contaminated with whitefly hon related to the type of sugars present on the lint [8] eydew were selected, based on trehalulose and melezi-

TABLE J. High·performance liquid chromatography results on aphid honeydew- and whitefly boneydew-contaminaled bales.

G F Treh. S M Total sugars

Aphid honeydew contaminated cotton: % of the fi ber weight 0.067 0. 162 0.209 0.001 0.0 10 0.0 16 0.465 % of (he total sugars 14.4 34.8 44.9 0.21 2.2 3.4 Whitefly honeydew contaminated cotton: % of the fiber weight 0.068 0.071 0. 134 0.244 0 0.109 0.626 % of (he total sugars 10.8 11.3 21.4 38.9 0 17.4

I. Inositol, G, Glucose; F, Fructose; Treh .. Trehalulose. S. Sucrose; M. Melezitose. tose contents as determined by HPLC (Table I). Their amount of pressure is applied for 25 seconds with the stickiness levels were evaluated with the high speed heating element (53°C) in contact with the cotton. The stickiness detector (H2SD). The bale contaminated with second station is a cool press, where the same fixed aphid honeydew had an H2SD reading of 2 I, while the pressure is applied for 25 seconds at ambient tempera bale contaminated with whitefty honeydew had an H2SD ture. This fixes the sticky points to the aluminum foil. reading of 76. In addition, two bales of non-contami Next follows the cleaning station, where the non-sticky nated cotton were selected for mixing with the contam material is removed by a combination of a cleaning roll inated cotton, in order to obtain mixes that exhibited and suction. The fourth station is an image analysis moderate stickiness levels. The mix referenced as "mix chamber, where the sticky points are automatically aphid" was obtained by mixing 150 pounds of aphid counted and reponed. honeydew-contaminated cotton with 150 pounds of non sticky cotton. The mix referenced as "mix whitefty" was HIGH PERFORMANCE LIQUID CHROMATOGRAPHY obtained by mixing 257 pounds of non-sticky cotton with 43 pounds of whitefly honeydew-contaminated cotton. Eacb fiber sample was placed into a plastic bag and 20 Each sample was tested with the high volume instrument rnL of 18.2-megohm water was added. A sample of the (HVI 9OOA; Uster, Knoxville, TN) and tbe H2SD. Table aqueous solution was taken fTOm the bag with a 1O-cm - 3 II shows the HVI and H2SD readings of the two mixes. syringe (Becton Dickinson and Company, Franklin Lakes, NI), to whicb a 0.2-p.m fi lter (nylon membrane HIGH SPEED STICKINESS DETECTOR polypropylene housing) (National Scientific, Scottsdale, AZ) was attached. A 1.5-rnL fi ltered sample was depos The high-speed stickiness detector is an automated ited into J.5-mL autosampler vial (C4013-15A; National instrument derived from the sticky cotton thermodetector Scientific). Sugars were separated on the columns (Car (CIRAD, Montpellier, France), which was approved as a boPac PA I anion-exchange analytical columns; Dionex reference test by the International Textile Manufacturers Corporation) in series with a gradient eluent system. Federation in 1994 [2]. Frydrych el al. first described the Eluent I was 200 mM NaOH and eluent 2 was 500 mM H2SD in 1994 [I]. The general procedure is as follows: sodium acetate (C3H3NaOz, 3HzO) and 200 mM NaOH. after conditioning the fiber samples for at least 12 hours, Three replications were performed on each sample. The a 3.5-g specimen of lint is fed into the instrument to be results were expressed in percentage of the fiber weight. mechanically opened. [t fonns a pad of 130 mm by 170 mm, which is then automatically transferred onto a strip UATR-FTIR AND RAMAN SPECJl!.OSCOPIES of aluminum foil originating from a roU. The aluminum is rolled along a conveyor belt, which delivers sample FTIR Spectrum-One equipped with a universal atten sequentially to each station. The aluminum foil is roUed uated total reflectance (UA TR) accessory was used in up at the other end of the machine. The H2SD bas four this research (Perkin Elmer, USA). The UATR is an distinct stations. The first is a hot press, where a fixed internal reftection used to simplify the analysis of solids,

TABLE n. HVI aDd H2SD readings of the four mixes.

UMHL Unif. Strength E1on. H2SD Mix ID Mike (rom ) (%) (eN/lex) (%) Leaf Rd (%) + b read ings

Mi x aph id 4.5 24.9 78.6 23 .9 6.8 1.0 75.6 11.0 12.7 Mix whitefly 4.8 25.4 79.3 23.4 6.7 1.0 76.1 10.8 15.3 SEPTEMBER 2005 647 powders, gels, and liquids. It is a rapid and flexible FTIR spectra at different hydration times (from 0 to 300 hours sampling technique, which consists of placing a sample with 5-min increments) at 65 ::t: 2% relative humidity on top of the ZnSe-diamond composite crystal with a and 21 ::t: 1°C. The spectra were analyzed and the peaks high refractive index. The infrared radiation from the that show a significant increase with the hydration time instrument is passed into the accessory and up into the (located at 3280 and 10 18 cm -I) were integrated to get crystal. It is then reflected internally in the crystal, and the peak intensities. All measurements were perfonned then back toward the detector which is located in the without changing the amount of trehalulose or the pres spectrometer. When the beam is reflected within the sure on the top of the ZnSe crystal. Thus, any change crystal, it penetrates into the sample by approximately 2 observed in the FTIR spectra of trehalulose during /Lm. Figure 1 illustrates this process. The mid-infrared the hydration process is attributed to the effect of the detector is a deuteurated tri-glycine sulphate (DTGS). humidity. Sugars and yarn defects were placed on top of the ZnSe diamond crystal. Pressure was applied on the sample to ensure a good contact between the sample and the inci SPINNING EXPERIMENTS dent IR beam and to prevent loss of the IR beam. The FTIR spectra were collected at a spectrum resolution of The mechanical process used to make the yarn is 4 cm -I, with 32 scans, over the range of 650 -4000 described in Figure 2 [6]. The opening, carding, drawing, cm -I. A background scan of clean ZnSe-diamond crys roving, and rotor spinning machines used were all indus tal was acquired before acquiring the spectra of the trial machines. The yam manufactured was 26.84 6 sample. The Perkin-Elmer software was used to perform X 10- kg m- J (26.84-tex or 22 English number) on a the necessary spectra correlation and peak integration. Rieter R20 rotor spinning frame. Ten spinning positions were used and each mix was run for 20 hours. After each end-down. the two yarn ends were collected for further Pressure microscopic and infrared evaluation.

Hunter Weigh Pan Hopper Feeder t Monocylinder B4/1 Roll Speed = 750 rpm Incident radiation Reflected radiation --.Detector Dust Remover• FIGURE 1. Principle of the UATR-FI'lR. t ERM B5/5 Condenser RlOIl 0 Beater Speed = 850 rpm

Raman spectra of trehalu10se were collected using a AMHtBJender Raman System 2001 equipped with a miniature fiber Rieter Atrofeed optic with a 785 nm laser (Ocean Optics, USA) ~ uc~ute . Rieter C4 Ca rd Production Rate = 45.36 kglhour Trashmaster Sliver Weight = 4.25 ktex HYDRATION PROCESS OF TREHALULOSE t Trehalulose crystal was dehydrated at room tempera Rieter RSB 851 Delivery Speed = 400 m/min ture under vacuum for 48 hours. Then it was deposited Draw Frame Sliver Weight =4.25 ktex on the UATR-ZnSe crystal and a pressure was applied to t ensure a good contact between the sample and the IR Rieter R20 Rotor Rotor Speed = 100,000 rpm beam. The corresponding FTIR spectrum was recorded Spinning Frame Count = 19.68 tex immediatelY between 650 and 4000 cm- I using 32 scans Twist Multiplier = 4.8 with a spectrum resolution of 4 em -1. This spectrum constitutes the FTIR spectrum at t = O. Then, an auto ROURE 2. Outline of the mechanical process for rotor matic acquisition was performed to collect the FTIR spinning tests. 648 TEXTILE RESEARCH JOURNAL

ARTIFICIAL HONEYDEW MIXES trehalulose, sucrose, and melezitose). Among the sugars tested, trehalulose has the highest hygroscopicity and The selected sugars used to prepare artificial honey very fast hydration kinetic. After the eqUilibrium was dew were inositol, fructose, glucose, sucrose, trehalu reached, at 65 ± 2% relative humidity and 21 ± 1°C, the lose, and melezitose. Trehalulose was obtained from amount of absorbed water corresponded to 3 molecules Cornell University; the other sugars were purchased of H 0 per molecule of trehalulose. Furthermore, the from Sigma Chemical Company (St. Louis, MO). The 2 differential scanning calorimetry study of thermal prop mix referenced as "mix I" was composed of 1% treha erties of these sugars showed that trehalulose has a very lulose, 15% sucrose, 15% glucose, 19% fructose, 45% low melting point [5]. These characteristics explain why melezitose, and 5% inositol. The mix referenced as "mix we expected trehalulose to accumulate on the spinning 45" was composed of 45% trehalulose, 15% sucrose, equipment. In fact, the HPLC tests performed on the 10% glucose, 10% fructose, 15% melezitose, and 5% residues collected from the textile equipment after pro inositol. In preparing these two mixes, the dehydrated cessing sticky cottons showed very high concentrations sugars were weighed and mixed with a spatula, then the of trehalulose [5], thereby confirming the hypothesis of open containers containing mixed sugar samples were selected accumulation of trehalulose on the textile equip stored in controlled atmosphere, 65 ± 2% relative hu ment. It follows that trehalulose could also become a midity and 21 ± 1°C for more than 1 month (720 hours) [5]. The FTIR spectra of mix 1 and mix 45 were acquired precursor for yarn defects during processing of contam and stored in the FTIR software library. inated cotton with whitefly honeydew. Hydrated trehalulose and artificial whitefly honeydew mix were analyzed by scanning electron microscopy. SCANNING ELECTRON MICROSCOPE The micrograph of hydrated trehalulose shows an amor The yarn defects causing ends-down were identified phous film-like structure appearance (Figure 3). The and collected. The samples were mounted in the stub and artificial honeydew mix has a similar appearance, al coated with a layer of gold by means of thermal evapo though it contains only 45% of trehalulose. The high ration in a vacuum coating unit. They were examined in hygroscopicity of trehalulose leads to the formation of a the scanning electron microscope (Model S500;, Hitachi, polymeric film that readily adheres to the textile equip Tokyo, Japan) using an accelerating voltage of 20 kV. ment. It also causes cotton fibers to stick together initi ating the formation of yarn defects.- ' Results and Discussion Figure 4 shows the UATR-FUR spectrum of trehalu lose in its dehydrated state. All vibration bands are very UATR-FTIR AND RAMAN STUDY OF TREHALULOSB weak (absorption < O.OO~).This could mean that infra HYDRATION red vibrations of trehalulose are not active in 'this state, Sugars belong to the carbohydrate class and are hy However, the exp~~ure of ~rehal~lose to humidity re drophilic because of several hydroxyl groups that estab sulted in an incrt?ase of the intensity of all vibration lish hydrogen bonding with water molecules. In previous bands with increasing hydration time, particularly for the work [5], we evaluated the hygroscopic properties of 3280 and 1018 cm- 1 bands (Figure 5). After 77 hours of sugars found on sticky cotton (inositol, glucose, fructose, exposure to 65% relative humidity at 21°C, the intensity

FIGURE 3. Scanning electron microscopy of: (a) hydrated trehalulose, (b) artificial whitefly honeydew mix. 648 TEXTILE RESEARCH JOURNAL

ARTIFICIAL HONEYDEW MIXES trehalulose, sucrose, and melezitose). Among the sugars tested, trehalulose has the highest hygroscopicity and The selected sugars used to prepare artificial honey very fast hydration kinetic. After the equilibrium was dew were inositol, fructose, glucose, sucrose, trehalu reached, at 65 ± 2% relative humidity and 21 ::t 1°C, the lose, and melezitose. Trehalulose was obtained from amount of absorbed water corresponded to 3 molecules Cornell University; the other sugars were purchased of H 0 per molecule of ~rehalulose. Furthermore, th~ . from Sigma Chemical Company (St. Louis, MO). The 2 differential scanning calonmetry study of thermal prop mix referenced as "mix I" was composed of 1% treha- erties of these sugars showed that trehalulose has a very 11Ilose, 15% sucrose, 15% glucose, 19% fructose, 45% low melting point [5]. These characteristics explain why melezitose, and 5% inositol. The mix referenced as "mix we expected trehalulose to accumulate on the spinning 45" was composed of 45% trehalulose, 15% sucrose, equipment. In fact, the HPLC tests performed on th~ 10% glucose, 10% fructose, 15% melezitose, and 5% inositol. In preparing these two mixes, the dehydrated residues collected from the textile equipment after pro! sugars were weighed and mixed with a spatula, then the cessing sticky cottons showed very high ·concentra~oris open containers containing mixed sugar samples were of trehalulose [5], thereby confirming the hypotheSIS of stored in controlled atmosphere, 65 ::t 2% relative hu selected accumulation of trehalulose on the textile equip midity nnd 21 ± 1°C for more than 1 month (720 hours) ment. It follows that trehalulose could also become ·a: [5]. The FTIR spectra of mix 1 and mix 45 were acquired precursor for yarn defects during processing of contam- and stored in the FTffi. software library. inated cotton with whitefly honeydew. ' Hydrated trehalulose and artificial whitefly honeydeW . SCANNINO ELECTRON MICROSCOPE mix were analyzed by scanning electron microscopy" The micrograph of hydrated trehalulose shows an amor The yarn defects causing ends-down were identified phous film-like structure appearance (Figure 3). The and collected. The samples were mounted in the stub and artificial honeydew mix has a similar appearance, .al. coated with a layer of gold by me<).l1S of thermal evapo though it contains only 45% of trehalulose. T?e hIgh ration in a vacuum coating unit. They were examined in hygroscopicity of trehalulose leads to the form~tIon o~ !l the scanning electron microscope (Model S500;, Hitachi, polymeric film that readily adheres to :he texule e~v~~: Tokyo. Japan) using an accelerating volta~e of 20 kV. ment. It also causes cotton fibers to stIck together lID . t .~ ; ating the formation of yarn defects' i ' 1~u: Results and Discussion Figure 4 shows the UATR-FfIR spectrum of treh , ; UATR·FfIR AND RAMAN STUDY OF'I'REHAWLOSE : lose in its dehydrated state. All vib~ation bands are.v~rY, HYDRATION weak (absorption < 0.009); This ·could mean thatuwri , . . thi tate" red vibrations of trehalulose are not active 10 . ~ ~ n 4 Sugars belong to the carbohydrate class hnd are hy Howe~~~, fu~ ·exposure of trehalulose to humi~tXfri drophilic because of several hydrOXyl groups that estab. s'uIted in an increase of the intensity of all vIbr~ttq~. lish hydrogen bonding with water molecules. In previous bands with increa;ing hydration time, particularly for th..i work [5], we evaluated the hygroscopic properties of 3280 and 1018 cm-I bands (Figure 5). Mter 77 ?OUfs,.O sugars found on sticky cotton (inositoL, gluc9~e,fructose, expqsure to 65% relative humidity at 21 °C, the. lllteJl~lt . . - , ~

. scopy of: FIGURE 3. Scanning electron ~c:~ whitefly (a) hydrated trehalulose, (b) art! CI • • honeydew mix. . , , . SEPTEMBER 2005 649 of the FTIR spectra of hydrated trehalulose is approxi relative humidity and 23 :t 1°C. In contnlst to the FTIR mately 60 times higher than the intensity of the spectra of spectra of hydrated trehalulose. the intensity of the Ra trehalulose in dehydrated state for the peak at 3280 man vibration bands decreased when trehalulose was I cm- . exposed to humidity.

300 0.010

1 17 250 0.008

~ 200 0.006 a t.: .. c: .9 .. c: 150 .c 0.004 c.. ..e .! < ~ 100 0.002

1800 1600 1400 1200 1000 800 600 400 200 3500 3000 1500 Raman shift, em" Wavenumber, em-!

FIGURE 6. Raman spectra of trehalulose: (a) dehydrated, nnd (b) nfler FIGURE 4. FfIR spectra of dehydrated trehalulose. 10 minutes at 62 ± 2% relative humidity and 23 ± 1°C.

The absorption of water on trehalulose sugar wa" 1018 measured by observing the FfIR peaks at 3280 and 1018 0.5 cm -I. The peak located at 3280 em -I is attributed to the O-H stretching vibration of absorbed water molecules. 0.4 while the peak located at 1018 cm - I is attributed to C-O ..~ stretching vibration in the primary alcohol (-H2C-OH) . of 0.3 In order to obtain the integrated intensity at each hydra .c~ tion time, the peak located at 3280 cm - 1 was integrated < 0.2 from 3000 and 3700 cm- I and the peak at 1018 cm- I was integrated from 1095 and 941 cm -1. The integrated 0.1 intensities 13280 and 11018 as a function of hydration time are shown in Figure 7a. The evolution ofI3280 and 11018 may be divided into two regions, from 0 to 50 hours and 3500 3000 1500 1000 from 50 to 300 hours. For both integrated intensities. a Wavenumber, em-! first equilibrium was reached at 25 hours and a second at 150 hours of hydration. This behavior suggests that two FIGURE 5. FTIR spectra of trehalulose at different hydration time: (a) mechanisms are probably involved in the effect of water I = 7 hours. (b) 1 = 21 hours. (e) t = 31 hours. (d) t = 57 hours, (e) I = 70 hours. and (f) t = 77 bours. on trehalulose. As shown in Figure 7b, the weight gain of trehalulose in percent [5] and the integrated intensity 13280 of the peak at 3280 em -1 follow the same trend for Since infrared and Raman spectroscopies complement the hydration time < 50 hours. This could be attributed each other, we investigated the effect of humidity on the to a simple absorption mechanism of water molecules on Raman vibrations of trehalulose. Thus. the very weak trebalulose (three molecules of water per molecule of infrared vibrations obtained for trehalulose in the dehy trehalulose). The weight gain of trehalulose reached drated state could mean that the vibration modes of eqUilibrium and no further increase is noticed (not trehalulose are not active in infrared but are active in shown). However, the integrated intensity 13280 contin Raman. Figure 6 shows a comparison between the Ra ued to increase after 50 hours of hydration (Figure 7a), man spectra of dehydrated trehalulose and hydrated tre which indicates that another mechanism takes place after halulose after only to minutes exposure to at 62 ± 2% the water absorption process. 650 TEXTILE RESEARCH JOURNAL

~------r40 ing ends-down during rotor spinning of the cotton con taining aphid honeydew versus the cotton containing ~ co 30 ~ whitefly honeydew. The micrographs reveal that the cot § ton fibers in the yarn defects resulting from the aphid

> ~: :

FIGURE 8. Scanning electton microscopy of . yam defects causing ends-down during rotor spinning of: (a) aphid honeydew contaminated mix; and (b) whitefly honeydew contaminated , mix (X 1000). . • . SEPTEMBER 2005 651 significant difference between the integrated intensities TABLE III. Variance anulysis: Effect of yarn defect type on the integrated intensities 13280 and 11018, 13280 and 11018 of the spectra of yarn defects from aphid honeydew-contaminated cotton mix and the spectra of Peak 3280 cm - I the cotton yarn without defects. However, for yarn de dft Probability fects of the mix contaminated with whitefly honeydew Ft 1:'280 the integrated intensities of both peaks are significantly Intercept I 2387.044 0.000001 higher. Therefore, according to these results and for the Group 2 452.775 0.000001 Cotton yarn 19.822 b:j: stickiness level tested, the contamination with aphid hon Mix aphid 19.954 b eydew seems to cause no detrimental effects on yarn Mu whitefly 66.104 a quality. Indeed, the detailed analysis of yarn quality Error 98 showed that aphid honeydew contamination did not Peak 1018 cm- I translate into negative effects on either yarn quality or productivity up to 26 H2SD spots [7]. However, for the dft Ft Probability 11018 whitefly honeydew-contaminated cotton even 12 H2SD Intercept I 1523.679 0.000001 spots had drastic negative impact, producing unaccept Group 2 198.014 0.000001 Cotton yarn 8.744 b:j: able yarn quality and productivity loss [7]. Mix aphid 10.814 b Mix whitefly 25.649 a Error 98 0.7 1 8 t df. degrees of freedom; F. variance mtio. *Values not fol- lowed by the same letter are significantly different with a :: 5% 0.6 (according to the Newman-Keuls test).

0.5 100 40 ..u [; 0.4 !! ;;00 of .::/ 80 .;;t <:> 30 1l 0.3 k ... k." -< ...: 60 .....1:1 0.2 .9- 20 .5 'i 40 i... 0.1 -l:! l! 10 ~ 20 ...to 0.0 .EI- ...1:1 3500 3000 1500 1000 0 0 Wavenumber, em-' ~~ # ~ ~f? d>" ~ ':}'" .p ~~ ...a~ *'t ~-t:i ~...,. FIGURE 9. FI1R spectra of colton yarn and yarn defects causing ,l ~ .p ~ ends-down: (a) cotton yarn without defect; (b) yarn defect from aphid honeydew-contaminated cotton; (c) yarn defect from whitefly honey dew-contaminated cotton. FIGURE 10. Comparison between integrated intensities (13280 and 11018) for cotton yarn without defect (Cotton yam); yarn defects from aphid honeydew-contaminated cotton (Mix Aphid); yarn defects from The FTIR spectra of the yarn defects causing ends whitefly honeydew-contaminated cotton (Mix whitefly); artificial whitefly honeydew (Mix 45); and trehalulose (Vertical bars denote 0.95 down were compared with the spectra of artificial hon confidence intervals). eydew mix 1 and mix 45, previously stored in the library, to find the closest match. The matching coefficient be tween the spectra of the yarn defects produced during Conclusions rotor spinning of whitefly honeydew-contaminated mix exhibit higher correlation (0.84) with the reconstituted The VA TR-FfIR was successfully used to study the whitefly honeydew mix 45. This is in agreement with hydration process of trehalulose and analyze the yarn HPLC results of the cotton fibers used to make this mix defects causing ends-down during rotor spinning cotton (Table I). However, the matching coefficient between the mixes with modemte honeydew contamination. The ex spectra of the yarn defects from aphid honeydew-con posure of trehalulose to the humidity resulted in a drastic taminated mix and reconstituted aphid honeydew mix 1 change on the FTIR and Raman spectra. The absorption was only 0.61. These results are in agreement with the of water on trehalulose molecules could initiate struc previous finding that aphid-contaminated cotton seems to tural and/or conformational changes. The results also cause no yarn defects for the level of stickiness tested. showed very good correlation between the FfIR spectra 652 TEXTtLE R ESEARCH JOURNAL of the yarn defects obtained during rotor spinning of the 4. Hendrix, D. L. Steele, T. L., and Perkins Ir., H. H., Bemisia whitefly honeydew-contaminated cotton mix (trehalu Honeydew and Sticky Cotton, in "Bemisia: Taxonomy, lose-rich) and the artificial w hitefly ho neydew mix. This Biology, Damage, Control and Management", D. Gerling, indicated that trehalulose is the dominant sugar in the and R. T. Mayer, Eds. Intercept, Andover, UK, pp. 189- yarn defects. These results continned our previous con 199, 1995. 5. Hequet, E., and Abidi, N., Processing Sticky Cotton: Im clusions that trehalulose is the main concern during pro plication of Trehalulose in Residue Build-up. J. COttOIl Sci. cessing cotton with moderate honeydew contamination. 6( I), 77-90 (2002). 6. Hequet. E., Ethridge, D., Cole, B., and Wyatt, B., How ACKNOWLEDGEMENTS Colton Stickiness Measurements Relate to Spinning Effi The authors woul d like to thank Cotton Incorporated ciency, in "Proc. 13'" Annual Engineer Fiber Selection and the Texas Food & Fibers Commission for their System Conference," 17- 19 April 2000, Cotton Inc., Cary, NC, pp. 99-121 (2000), financial suppo". 7. Hequet, E, Abidi. N., and Ethridge, D., Processing Sticky Cotton: Effect of Stickiness of Yarn Quality, Submitted to Literature Cited the Textile Res. J, 75(5), 402-410 (2005). 1. Frydrych. R .. Hequet, E., and Cornuejols, G., A High 8. Miller, W. B., Peralta, E .. Ellis, D. R., and Perkins, Jr, H. H., Speed Instrument for sticki ness Measurement, in "Proc. Stickiness Potential of Individual Insect Honeydew Carbohy 22"" International Cotton Conference," 3--5 March 1994, drates on Cotton Lint. Textile Res. J. 64(6), 344 -350 (1994). International Textile Manufacturers Federation, Bremen. 9. Sisma, S., and Schenek, A. Bremen Honeydew Test - New Gennany. pp. 83-91. 1994. Method for Testing the Stickiness Tendency of Cotton. 2. Frydrych, R.. and Hequet, E., Standardization Proposal: Mi/liand TeX/ilberiehle 13, 593--595 (1984). The Thennodetector and its Methodology, in "Proc. Inter 10. Strolz, H. M .. ITMF Cotton Contamination Survey 2001, national Comm. Cotton Testing Methods," Zurich. Swit in "Proc. 26'" International Cotton Conference", Intema zerland, International Textile Manufacturers Federation tional Textile Manufacturers Federation, Bremen, 13-16 Bremen, Gennany, pp. 97-102, 1998. Marcb, pp. 35-39. 2002. 3. Hendrix. D. L. , Wei, Y-A., and Leggett, I. E. Homopteran II. Watson, M. D. An Overview of Cotton Stickiness. In. honeydew sugar composition is determined by both the "?roc. International Cotton Conference," 1-4 March 2000, insect and plant species. Compo Biochem. and Physiol. International Textile Manufacturers Federation, Faserinsti 1018(1/2),23--27 (1992). tut, Bremen, Germany, 2000.