AATCC Test Method 20-2007 Fiber Analysis: Qualitative Developed by AATCC Committee RAZA. Adopted as Tentative 1995; revised 1958, 1962, 1963, 1972, 1976, 1998, 1999, 2000, 2001, 2002, 2004, 2005; ceditotially revised and reatfirmed 1973, 1990, 1995; editorially revised 1974, 1977, 1982 (new title), 1983, 1984, 1988; reaffirmed 1985. Related to ISO 17781, 180 1833, and IWTO 68. 1. Purpose and Scope LI This test method describes physi- cal, chemical and microscopical tech- nigues for identifying textile fibers used ‘commercially in the United States. Fibers ‘may be examined in raw fiber form or taken from yarn oF fabri. 1.2 These test methods may be used 10 identify generic fiber types as defined by the Textile Fibers Products Identification Act and subsequent rules and regulations Of the Federal Trade Commission or ISO. 2076, Textiles man-made fibres-generic names. Quantitative methods for deter- ‘mining percentages in blends of fibers are covered by AATCC Test Method 20A, Fiber Analysis: Quantitative. 13 The test methods apply to fibers which are shown below grouped by ge- netic classifications: ces ea) mag ES “Sa i aa ; ; fren ibe & a See aan hut BERR any “Baan tezsiiny and rove =. = i = 2 be — rin (ina ypropyene nines Ea anaes oS = ea Es oO 38 TM 20-2007 2. Use and Limitations 2.1 This test method describes a num- ber of procedures—mieroscopical exami- nation, solubility in solvents, melting Point, refractive index, and micro-Fourier “Transform Infrared Spectroscopy”—whieh should be used in combination to identify 8 fiber type. For idertifying certain fibers some procedures will be found to be ‘more effective than others, 2.2 For example, microscopical exami- nation is particularly useful in eharacter- izing the natural fibers. It must be used with caution on man-made fibers since they are frequently produced in a number ‘of modifications which alter the longitu- inal oF cross-sectional appearance, In addition, man-made fibers may contain some or no delusterant or other additive particles. Filaments of a given type may vary in size or eross-sectional shape, In- dividual filaments may have two of more component sections of the same or differ- cent generic types. 2.3 Even natural fibers show a fairly wide variation in typical cross-section, [No specific specimen will look exactly like the pictures published. A sufficient number of fibers should be examined to cover the range of appearance in any specimen, 2.4 Successful identification of fibers depends upon experience and familiarity with the fibers. The identification of an unknown fiber is best made by compari- son with properly identified fibers used as reference standards. For this reason it is desirable to have available atleast one representative fiber sample from each ge- nerie class of fibers, which can be used fot comparative identification. 25 This test method provides means for identifying the generic classification of the common fiber types. In special ceases, a8 when dealing with fibers not de- scribed in this method or atempting 10 distinguish between produets of different suppliers of the same generic types, one ‘must consult standard texts on fiber iden- tification or technical bulletins issued by suppliers of man-made fibers. See refer ences Section 13. 8, Terminology 3.1 For definitions of technical terms, refer to the Glossary of AATCC Standard Terminology inthis TECHNICAL. MANUAL. 4, Satety Precautions NOTE: These safety precautions are for information purposes only. The pre- cautions are ancillary tothe testing proce- dures and are not intended to be al inclu- sive, [tis the user's responsibility 10 use safe and proper techniques in handling ‘materials in this test method, Manufac- turers MUST be consulted for specific details such as material safety data sheets tand other manufacturer's recommenda- tions. All OSHA. standards and rules must also be consulted and followed. 4.1 Good laboratory practices should be followed. Wear safety glasses in all laboratory areas. 42 All chemicals should be handled with care 43 In preparing, dispensing and han- dling the reagents outlined in Section 6, use chemical goggles or face shield, im- pervious gloves and an impervious apron, Concentrated acids should be handled only in an adequately ventilated labora- tory hood, CAUTION: Always add acid to water, 44 All poisonous and flammable re- agents should be mixed and handled only jn an adequately ventilated laboratory hood. CAUTION: Acetone and ethyl al- cohol are highly flammable and should be stored in the laboratory only in small containers away from heat, open lame and sparks. 4.5 An eyewash/sefety shower should be located nearby and an organic vapor respirator should be readily available for emergency use 4.6 Exposure to chemicals used in this procedure must be controlled at or below levels set by governmental authorities (e., Occupational Safety and Health Administration's [OSHA] _ permissible exposure limits [PEL] as found in 29 CER 1910-1000 of January 1, 1989). In addition, the American Conference of Governmental Industrial Hygienists (ACGIH) Threshold Limit Values (TLVs} comprised of time weighted averages CELV-TWA), short term exposure limits (TLV-STEL) and ceiling limits (TLV-C) are recommended as a general guide for air contaminant exposure which should be met (see 12.5). 5. Apparatus 5.1 Compound microscope with matched objectives and eye pieces to achieve magnifications of 100-500X and ‘equipped with a polarizer and analyzer 5.2 Glass slides and cover glasses. 53.3 Dissoction needles. 5.4 Scissors (small) and tweezers (fine) ‘AATCC Technical Manual2008 ae55 Croseseetioning device of one type soc as listed below. Msi Stainless steel plate, 2.54 x 7.62 x 0)0254 em (1 3.x 001 in) drilled Sain 009 ern (0.04 in) diameter hoes. Sot copper magnet wire AWG #34, Ghote em (0.0068 im) diameter 155.2 Microtome, hand (see 121). 36 Razor blades, shatp, thin, single edge or double edge with holder 7 Density gradient tube, glass ap- proximately 2.5 em (I in.) in diameter Fi ein (18 in.) long witha sealed bot- {am and 24/40 standard taper joint glass cap clsue af op avoid ae iekup or evaporation of solvents. Tiny Biss uphets of calbted density may fe used as density standards (se 12.2), $53 Melting point apparatus consisting ‘ofa heated block, temperature measuring device soch asa thermometer and means for controlling the rate of heating, and viewing the specimen at low magnifica- tion. The instrument should have a range oF 100-300°C oF more, and an accuracy of I degree over the entire range (se 123) 39 Micro-FTIR Instrument. 6, Reagents and Materials 6.1 Mounting Reagents. 6.1.1 Mineral oil, US.P. or other im- smersion fluid (see 12.4) 6.1.2 Collodion, solution of nitrocellu- ose (4 g/100 mL) in 1:3 aleohoVethy! ether 62 Bleaching Reagent. 62.1 Hydrosulfite-caustic solution. Dissolve 2 g sodium hydrosulfite and 2 2 sodium hydroxide in 100 mL of water. 63 Stining Reagents, 63.1 Zine chloro-iodide reagent. Dis solve 20 g of zine chloride in 10 mL oF ‘water. Add 2.1 g of potassium iodide and 0.1 g of iodine dissolved in 5 ml. of wa- ter. Add o leaf of iodine. 63.2 Acid phloroglucinol reagent. Dis solve 2 g of phloroglucinol in 100 mL of ‘water, Use with equal volume of concen= tated hydrochloric acid. 64 Refractive Index Immersion Lig ids. 6.4.1 Hexadecane (cetane) C. P. Grade, RI= 1.434, 6.42 Alpha chloronaphthalene, RI = 1.633 Poisonous. Avold inialing vapors. 64.3 Blends ofthe above. Assume that the reffactve index varies linearly by Yolume of ingredients For example, 0 take guid of R= 1.550 mix 42 parts by volume of hexadecane with 8 pars ty volume of alpha chloronaphthalene (Gee 2.4, 65x Stents 5.1 Acetic acid, glacial. Corosive Dotet eines oon shin 2 Acetone, reagent grade (Catton: tighy fammabig. ATCO Technical Manual’2008 6.5.3 Sodium hypochlorite solution, ‘5%, Home laundry bleach is satistactory 6.54 Hydrocblorie acid, concentrated reagent, 20%, Dilute 50 mL of concen- trated hydrochloric acid, 38%, to 95 mL ‘with distilled water 6.5.5 Formic acid, 85%. Corrosive. Do not get in eyes or on skin. 656 14-Dioxane. 6.5.7 m-Xylene, 6.5.8 Cyclohexanone. 6.59 Dimethylformamide. (Caution: if spilled on skin, wash off immediately.) 65.10 Sulfiric acid solution, $9.5 + 0.25% by weight, density 1/4929 + 0.0027 g pet ml. at 20°C. Weigh into a beaker $9.5 g of concentrated sulfuric acid (sp gr 1.84). Weigh into a 250 mL. Pyrex Erlenmeyer Nask 40.5 g of distilled water. Cautiously add the acid to the wa- ter switling and cooling in ice water or under a tap. Wear goggles! The solution becomes very hot and may boil and spat- ter ifnot cooled during mixing, After the solution has cooled to 20°C (68°F) adjust the density toa value between 1.4902 and 1.4956 g per mL. 6.5.1] Sulfuric acid solution, (70 + 1% by weight, density 1.6105 + 0.0116 g per mi at 20°C), Weigh 70 g of concentrated sulfuric acid (sp gr 1.84) and 30 g of Water and mix with the same precautions as in 6.5.10, After the solution has cooled 0 20°C (68°F) adjust the density to a value between 1.$989 and 1.6221 g per mL. 635.12 mCresol, reagent grade. Poi- sonous, Use in ventilated hood. 65.13 Hydrofluoric acid, 49% reagent agade. Very dangerous, Use goggles and hhood under suction. Do not iniale vapors or allow to contact skin. 7. Sampling 7.1 To obtain 9 representative sample for identification it is necessary to con- sider the following: TALL If the sample is loose fiber or ‘yar, it may contain one fiber only or it may be an intimate blend of two or more fibers. 7.1.2 A yam sample may be a ply or wrapped core blend of two or more yarn. ‘These yams in tum may be the same oF different and may themselves contain a blend of fibers 7.13 Woven and knitted fabries may be constructed of the same or different yarns in various combinations. The yarn ‘may contain one or more fiber types. “7.1.4 Different fiber types may be dyed to the same color. Contrarywise, the same fiber ype may appear in different colors in the finished article by mixing stock dyed or yam dyed materials or using fibers with modified dyeing character- 7.15 It is essential that the specimens scleoted represent the entire sample of raw fiber, yam or fabric under examine ation. 8, Specimen Preparation 8.1 In many cases the identity of an un- known fiber can be established without pretreatment. ‘8.2 When the presence of starch, wax, cil or other coating obscures the appeat= ance of the fiber, uy heating in warm to hot distilled water to remove the foreign matter, If this fails, try extracting with organic solvents, 0.5% hydrochloric acid for 0.5% sodium hydroxide. Some fibers such as nylon are damaged by acid and some such as azion, silk and wool, are damaged by caustic treatment (see 9.7) 83 To separate vegetable fiber bun- dles, treat with 0.5% sodium hydroxide solution, rinse well with water and dry 84 To strip dye from colored fibers, especially the cellulosic fibers, heat for 30min at SO°C with hydrosulfite caustic solution (see 6.2.1) 8, Procedure 9.1 The identification of fibers is usu- ally carried out by subjecting specimens to a variety of selected tests until enough information is obtained to make a satis- factory judument as (0 the generic class or specific type. The selection of tests and order in which they are performed can change depending on the knowledge already available and results of the pre- lirminary tests 9.2 Visual and Microscopical Exami- nation, 9.2.1 Examine the sample of material submitted for identification. Note form (loose fibers, yam, fabric, ote), color, f- ber length and fineness, uniformity of appearance and probable end-use. If the sample isa fabric, separate out yams by unraveling or cutting. If the fabric is woven, separate warp and filling ‘yams. If yams differ in colot, luster. size ‘or other apparent ways, make a physical jon of these yams for separate ‘identification. 9.2.2 The fibers may be identified using either light or scanning electron mieros- copy. If using transmitted light. mieros- copy, place a small quantity of the fibers fon a gas slide, tease fibers apart, mount swith a drop of mineral oi or other immet- sion fluid, cover with a coverslip and ex- amine under the microscope. 9.2.3 Observe the fiber characteristies as seen in traverse section and classi into four general classes. 9.2.4 Fibers with surface scales, These fare the animal hair fibers listed in Pur- pose and Scope (see .3). All of the kera- tin fibers listed except silk are included in this group. Continue detailed microscopi- cal examination including cross-section TM 20-2007 39‘examination (see 9.3). Compare with the characteristics in Table I, photographs in the appendix of this method, and known specimens of har fibers (See 12.6). Addi- tional confirmation of this class may be made by buming test (see 9.5); density {ce 9.6); and solubility (soe 9.7) 9.2. Fiters wth Cross Markings. These are the vexetable fibers other than cotton listed in 1-3. Continue detailed micro- scopical examination including cross- section examination (see 9.3), Compare ‘with characterises as given in Table Tl photographs and known specimens of ‘vegetable fibers. To distinguish linen and rami from hemp, observe the direction of rovation on drying (See 9.8). Ifthe fibers are light in eolor, stain with zine ehloro- jodide reagent and. with acid. phloro- alucinol as directed in 9.9. Additional Confirmation ofthis elass may be made by tests described in 9.4, 9.5, 9.6 and 97. 9.2.6 Convoluted Fibers. Tis class in- cludes cotton and tussah silk. The two are easily distinguished by cross-section (see 9.2), buming test (see 9.5) and solubility (see 9.7) or micro-FTIR (See Appendix ID, If fibers are light in color, they may be distinguished by staining’ with zine chloro-iodide reagent (see 9.9). 9.2.7 Other Fibers. This class includes all of the man-made fibers, Bombyx silk and asbestos. The latter wo can be ident- Tied by microscopical appearance include ing cross-section (see 9.3). Burning tests (see 9.5) and solubility tests (see 9:7) are especially significant for asbestos and are usefil in confirming the presence of sik The man-made fibers are best ident fied by micro-FTIR, solubility, melting point, refiactive indices and other optical Characteristics and density: properties Which relate to chemical nature rather than physical shape. Cross-sections may vary and staining tests can be misleading since modifications ofa generic type may diye difterently. Used with disrimination and in combination with other tests, cross-sections and dye tests may some- times be helpful in narrowing down the number of possibilities. Metallic fibers havea distinctive shiny appearance, but & shiny residue may not indicate a metallic fiber. Using a transmitted light micro- scope at $x, 10x and 20x magnification powers will not reveal difraction, inter- ference and gloss effects that can decep- tively appear to be metallic in nature, ‘Chemical (Colorimetric) and/or instru- mental (Atomic Absorption Spectropho- tometric) analyses should be performed to confirm their presence. 9.3. Microscopical Cross-Section Ex- amination, 9.3.1 Obtain a parallel bundle of fibers or yam. Thread 2 loop of copper wire through, one hole in the stainless. steel plate, Catch the bundle or yar in the {oop and pull i through the hole. Use suf 40 TM 20-2007 ‘Table |—Cheracteristies of Fibers with Scales on Surface Nol: The characteris cesignatd bya capil ter Xi stb that whic is espacly significant c Camel mere Alp Norse Llama Mohair Vieuna Wool Yok Lengua ices: Pronounced - Fein x Corea Torte x SSmoath edge = Senate Mel ‘eeurence: Usual present fs Seldom present == x Never present = Tie. Fragment ne Invergieg yo 2S Coninueus root ‘Siero Ror dana Under wot Overs Pigment Dike Sealy Granuse None Cross-Section Contour undo oval ee Ovaliocorgated © x Kidney edu contou: Ro ee ee ‘alte elongates x 0 5 2 Kéhoytodumboet =X Plgnentdtibton: ‘Unio | rok 5 5 ew = x = x entre S295 6 5 Eocene Ss oS fs 2424 Frneness (npn) Averege Range Number of sles per ‘oo yr - 5 oe x a Is mn bist 21023 18 1518S Wms) 9w40 Ses — 21028 — Is1014 —_ 181022 iO!o4 101090 G1025 191070 81650 Under Over Over bey — - 88 — 88 7 Garrat mears conic, nd retro sels in which fe vibe sole edge corolty ences he foe, ° Ibicale means overapping, ad etree In whic Pe sble scale edges overap ike ingles oot ang cover ely a pat ol the far cumiorence Te am wool used here a epresetcoting nel and rot capt wo “Te oniusraidemalaoeerarce cl caster Nbr while general etchant fee's wel snot start as come space fers such os cael ana ape. The evecae lamer cashmere toot as boedened in 200 based on a review of utc rescrch oan coming Asin capa nica Table Appearance of Fibers with Gross Markings or Swellings Longituinal Seti Linen Hemp Remie ato, lumen offer lametor nde oval over ver Cel ends ponted buntorforked unt. sharp polygen rounded poiygen elongated plan round or ol ineguar ireguar ficient fibers to pack the hole full, nec- essary, use some extra, readily identifi able other fiber to fill up the hole. 9.3.2 With a shagp razor blade make @ smooth cut on both sides ofthe plate, 933 Examine the section in air, o covered by a mounting fluid like mineral oil under a cover slip. Use transmitted Tight and useful magnification of 200- 'S00X. Compare with photographs in Ap- ‘AATCC Technical Manual2008 ceeentn oe wosssextosofknown bers ot Th te Hardy ype microtome is sec bow nseuegons withthe ste wecd en unde of bers of Sara ee hide the congue tothe slot ine po the bundle Adjust the qua too ea tut package. Ct of Ran sdes. Apply dop of collodion to te unt shows though desde and then a Op 1 einer side Lt diy thoroughly. Shice the eis colloaion and ir on bah oe ke plate ith ¢shasp Taso fine. 5s nach the auxiliary plunge, and wah te sew advance the embeded ough ine stout protides20- Aymabere the plate Add drop of cle He Tet ay about minor ua (eal off ellodion and embedded fr secin wha sharp rvor lad held ta angle wih ie slot Cut with tool arate he Remove the section, transfer toa dos side mount witha dp of nea Eforoe?immerson tld, ade covet Sip snd examine, Comnue W eu! see fis dserbed 93.5 unl good SS cecececons are obind. Exam fac and compre wo known cros-secons ut Refctve index, cL Place a sal sample ofthe er cna gasssice Immerse ina drop of thlorphulene and eta mitre (ot Sauivalen of retactive index 155. 42 Inet the poluize nthe sub- ape of he mlerscope to provide ight felond io the 612 oclek det, Rg te long tecnson of Ret ote face dncouor. Cloee the daphragm of Te rubnuge coodcat so a8 o pve Sl lanai 9.4.3 Focus carflyon he oulines of the ber With the fe adjustment ase the faust ust above the top ofthe tee the ter rouply 8 Wytinde, wile ike ens, I the refasive index Ue beri higher than the immersion Tigi, the fiber wil at lke 2 postive les A eight ine of tight wll move ito the middie of the ier the focus i fb te reftaaive nde of te bet iS vower than th inmersion qu, the Tigh wil fle out sth focus ised athe middle ofthe Re wl become ic Raper wl conan of te dee 944 The tet can be seen best with ‘ound fibers On fa abons it ay be Gaver ose movement a gt tae the Becks linea he oudlne ofthe fi = Me ement is in the same direction, ar the medium of higher fetactve Inv as eos 8 aed 45 Rotate the specimen 90° andre Peat the test. ae 9A Rott the specimen 45°, Insert tuaiyaer in the bey tbe or epee 1 prove essed polar, Obseve Ihe AATCC Technical Manual/2008 fiber appears very bright (strong biref gence), dim (weak birefringence) or dark (no birefringence). 9.4.7 Refer 10 Table IV for refractive index of fibers in the long and eross di- rection and an estimate of birefringence. Consider that the retardation depends on the thickness of the fiber specimen as well as the extent of drawing of a given specimen, Compare with known fibers of similar diameter for birefringence. 9.4.8 Select other immersion Tiguids snd repeat 9.4.1 through 9.4.5, As the re- figotive index of the liquid approaches that ofthe fiber, the outlines of the fiber become less distinct. Match the liquid to the fiber within 0.01 refractive index, 9.3 Burning Tes. 9.5.1 Take a small eft of fibers (held in tweezers) and place close to the side of a small flame. Note if the fibers melt or shrink from the flame. 9.5.2 Move the fibers into the ame, Nove whether the fibers will bum when held inthe flame. Remove from the flame very slowly and carefully, Note whether the fibers continue to bum outside of the flame. Make sure that the fiber was ig- nited before making this latter observa- tion, 9.5.3 Blow out the flame, if still bum- ing, and smell the smoke. Note the odor and examine the color and nature of any ash residue, 9.54 Compare the behavior observed with that listed in Table IIT and that of known reference fibers. Flame retardant ‘modifications of some fibers—cotion, rayon, acetate and modacrylic, for exam= ple—are available. Burning is retarded; ‘odor on burning and ash may be changed. Colored fibers—especially those colored by pigments—will retain color in the eol- red residue, 9.5.5 Odors of some burning fibers are quite ‘characteristic. The animal fibers and man-made protein fibers (azlon) have the ador of burning hair or feathers. The vegetable fibers and regenerated ceive lose (rayon) smell like burning. paper. The smell of burming rubber is @ familiar odor. Other man-made fibers—such as serylic, nylon and spandex—have char- acteristic odors which can be recognized With experience 9.6 Density 9.6.1 Prepare a density gradient col- ‘umn as follows. Clamp the density gradi- ent glass tube in a firm vertical stand. Pout into the tube 25 mL of tetrachloro- ethylene. Now prepare mixtures of xy lene and tetrachloroethylene by volume in descending order of percent terachlo- roethylene: 90/10, 80/20, 70/30, 60:40, 50/50, 40/60, 30/70, 20/80 and 10/90. Pour 25 mL. of each in order carefully down the side of the gradient tube, Fi- nally, put 25 mL of xylene on top. ‘Table ii—Reaction to Flame Shrinks From Flame Natural Fibers ox es yes 09 4 ‘aloes e ‘ seein mo v0 Man-Made Floors cyte es yes aceite on ay pahester ves yes ron ves yes dita ves es vial mosey ves ys vinjon nelate ys yes ass yes buy abet yes spandex ve ra rides yes ra ‘aon 0 ra ania 0 v8 solid "0 ra ns Coniues—Anpearanee Flame Burn Ash yes slowy ——_solblack teas yes siowy —_neguar black yes light greys ro 70 may Bacon ves yes ha black iregular shapec bead v8 yes hac black round bead ves yes hard grey round bead ves yes har tan bea ves ne ard black Iegular bead ro 0 roel bead "0 ro hard clear oad yes no iroguat mass yes yes thy back orgey yos yes bl black ieguiar beac yos yes none yes no nara alae oad bret no carbon TM 20-2007 41‘Table IN—Physical Properties of Fibers Refractive Index Tong Cross Natural Fibers asbesis (rysolle) 50.455 149 alos 15180 1504183 she 159 ist Weolandoterta 55-156. 185 Man-Made Fibers acca, secondary — Slee on = ——- : airy zn oe rmocacrlic 154 183 yon 66 158 182 Males Tags 18158 \ ; pat of 1.63 poetyene 158 131 were oa ete oe oe — = es — ares Tet ahap. Sickng pits 176. Density Melting Point Birefringence —giec—=—Degree C strong 2428 over 360 sang 151 one strong 11a none weak 115-30 none weak 12 250 weak ie 28 Weak negatve 1124.19 none = 12 softens a9 sang 138 ears 1400 one 190 none none 242s 850 S vars over 500 weak 130188" or 138 120 none 13 one strong Lions 213205 strong 12415 256-265, al 120 218 tense 1380 250-260, 133 282 song agoose 135 song Ogos 170 song 15 one = 0264.05 none weak negate 170 18 Si 120121 230 strong 126130 woaknegetve 134137 2300r “00 9.6.2 Take short fragments of dyed ref ‘erence fibers and te in a knot snipping off Toose ends. Bol for about 2 min in xylene solvent to remove moisture and air, Place in the column, After about a balf hour ‘they should come to rest atthe level rep- resenting their density, Calibrated glass spheres may be used fo determine the ac- tual density at various levels, 9.6.3 Prepare the unknown fiber in like ‘manner, place in the gradient column and note at what level it floats. Densities of f- bers are listed in Table IV 9.7 Solubility Test. 9.2.1 For tests at om temperature (20°C) place a small sample of the fibers Ina watch erystal, test tube or $0 mL bea- ker and cover with the test solvent (see TTable V), Use about 1 ml. of solvent per 10mg of fiber. 9.7.2 I the testis conducted at the boil- ing point of the solvent, first bring the solvent to boil in a beaker on an electric hotplate in a ventilated hood. Adjust the hot plate temperature to maintain slow boiling and keep watch so thatthe solvent does not boil dry. Drop fiber sample into the boiling solvent, 9.7.3 IF the testis conducted at some intermediate temperature, heat a beaker 42 TM 20-2007 ‘of water on a hot plate and adjust the tem: perature with a thermometer. Place the fi ber sample in the test solvent in a test tube and immerse in the heated water bath, 9.7.4 Note if the fiber dissolves com pletely, softens to a plastic mass or re- rains insoluble. Compare with data on fiber solubility in Table V. 9.7.5 Solubility can also be used as a test fo determine the presence of a metal ‘component in a fiber. On dissolving in ‘meta-cresol a shiny residue is evidence of «4 metal component 9.8 Drying Twist Test 9.8.1 Separate out a few parallel fibers. Dip in water and squoeze aif excess. Tap the end of the bundle to make separate fi bers flare out. Hold over a hot plate in ‘warm arto dry the fibers. Hold the fibers so that the free ends point toward the ob- server, Note the direction of twist as the fibers dry. Linen and ramie twist in a clockwise direction; hemp and jute cist ina counter clockwise direction 9.9 Stain Tests, 9.9.1 Place a few fibers on a micro- seopical slide. Apply a drop of zine cchloro-iodide reagent and cover with @ cover slip taking care to avoid bubbles. Examine the fibers for staining. Hemp, amie and cotton stain violet; linen stains brownish violet; jute stains brown. Many ‘other fibers stain shades of yellow brown including sik. 9.9.2 Warm a few fresh fibers on a mi- ceroscopical slide with a drop of acid phlorogucinol reagent. Woody fibers such as unbleached jute stain a deep ma- _Benta because of the presence of lignin, 9.10 Melting Point. 9.10.1 Fisher-Johns Apparatus, 9.10.2 Place a few fibers on the clean heating block. Cover with a cover slip. Tum the heat on and set the heating rate dial on 90 for fast heating. Observe the thermometer and the sample. When the temperature teaches 100°C, reduce the rate of heating, (If previous tests already indicate the fiber, the rate can be set at bout 10°C per min until 10-20°C below the expected melting point) Near the ‘melting point the rate should be reduced toabout 2°C per min. 9.10.3 Observe the fibers for evidence of softening. At the melting point, liquid begins to form which wets the cover stip. Fibers eventually merge and form a lig: bid mass. As the testis in progress itis sometimes helpful to press gently on the cover slip with twoozers to see if the fi- bers flatten under pressure. If this melting point is passed at a high heating rate, re= peat the test witha fresh sample. 9.10.4 Compare the melting point found with those listed in Table IV. 9.10.5 Kofler Hot Stage. 9.10.6 Place a few fibers on one of the small glass slides provided and cover with a cover slip. Place the slide on the stage of the microscope with the fibers over the central hole of the stage, Put the baffle and cover plate in place. 9.10.7 Insert the polarizing accessories in the optical path of the micrascope to provide crossed polars, The fibers should be visible if aligned diagonally to the di- rection of polarization. If fibers are not visible under these lighting conditions, remove the polarizing accessories and observe in ordinary transmitted light. 9.10.8 Set a high heating rate with the voltage regulator until the temperature reaches 100°C. Reduce the rate as the ex- pected melting point is approached as di- rected in 9.10.2. 9.10.9 Observe the fibers. As melting takes place there is a decrease in bireftin- gence: the fibers become dark. Read as melting point the temperature at which the fibers become completely dark. IP crossed polars are not used, observe melt- ing as deseribed in 9.10.2. 9.10.10 Compare the melting point found with those listed in Table LV. 9.11 Micro-FTIR, 9.11.1 Compare FTIR. spectra with FTIR spectra in Appendix IT or other li- brary sources (see Appendix II—Figs. 1-9) AATCC Technical Manuall2008 ——rceiation 68) pera) Tie (nats) | cela sic anor rand aon tation & nen oes rode riveic Table V—Solubiity of Fibers q 22 8 i. @ = = HeoE oo: UE TT S 5 i ts eo 3 5% % 1 ee if Fy toto od totot od boron i obo od gt fot oe | tot Pt sos tt a rot ot og rotod f hot ob | hot og 4 hot og 4 hot ot 4 I it sos 1 | s 1 tf fo 3 8 Lot i —-—o |, 33 eyelonexanone oe 3 3 Bi 2 3 2 ef 2 6 § 53.3 3 & & 10s 710) ‘® % & i % oo m 3 2 ss s § § tf tf Pe 4 Foro rr hors tot toro fotos voi | e Po Ny o$ 8 & $ if ft ¢ ror 4 oe oem tos 8 ft s tf tt i 8 8 $ & & & ios 6 | s 1 fo 5 roi ‘Solbe excepto one moder fbr characterized bylaw armatity and lid incase vile n rss-ecn, yor 6s sole, rjon 88s rs Soke at 200 wines past as, Novo uns ea 10, Report 10.1 Report the fiber type and, if more ‘than one type is present, where each is lo- cated. For example, the report could be woven fabric with nylon 6,6 warp and otton/rayon filling.” 11, Precision and Bias 11.1 A precision and bias statement is not applicable because data are not gener- ited by his method, 12. Notes 124 Available from SDL Atlas LLC, BISA Associste Lane, Charlote NC 23317; sek, 704329.0911; fax 704/329-0014; oma infoasaaes.om, 122 Available from Techne Ie. 743 Ales. ander Rel, Princeton NJ 08540" tel: 6097 452.9075, 12.3 Vasious commercial units are avail- able. One widely used by texte lahoratories 4s aailable from Fisher Scieatifi Co. at is ‘arious locations. A unit to fit the microscope Bie Kove miro ho sage supplied yA Prema Co, Vine and Thi Se, Philp 124 immersion liguids for reftactive index AATCC Technical Manval’2008 ‘measurements already bended and standard- ized are sold by RP Cargill Laborateries,Ce- dar Grave NJ 07009; te: 9732396633, 125 Available from Publications OFTice, ACGIH, “Kemper Woods Center, 1330 Kemper Meadow Dr, Cincinnati OH 45240; tel 51742-2020, 126 Reference samples, along wit interlab aus, of cashmere and woo, both seperate and ‘combined, are available from AATCC, P.O. Box 12015, Research Triangle. Park NC 27709; te: 919/849-8141; fax: 919/549-8933; ‘email: orders@astec ong, 18, References 131 The Testile Institue, Lennficaion of Tele Meterals, Sixth Eaton, C. Tnling & Co., London, 1970, 132 Federal Trade Commission, “Rules and Regulations Under the Textile Fiber Prod- ‘ets Identification “Act.” as amended. 1969, Washington, DC 20580, wwrw:fe go. 133 Heyn, AN. 1, Fiber Microscopy, A Text Book and Laboraiory Momvat, Inet- science, New York, 1954, Old, but good tech- Aigues and illustrations 134 Wildman A. B, The Microscopy of Aninal Textile Fibers, Wool Industries Re Search Association, Toridon, Leeds, England, 1954, 13.5 Appleyard, H. ML, Guide to he Ident Feation of Avira Fibers, same publisher 38 134, 1960. Both contain excellent descp- tions and photomicrographs, 13.6 Man-Made Fiber Producers Assocae tion, Man-Made Fiber Fact Book, New Yotk, 1970, Revised annually. List of current fibers made in United States, 13.7 Man-Made Textiles, Index to Mon Made Fibers of the World, Thtd Eition, Har lequin Press, Manchester 2, England, 1967. Lists about 3,000 man-made fibers by rade= ‘mark names and thei suppliers, 138 Linton, GF, Natal ond Mon-Made Tete Fibers, Duell, Sloan and Pearce. New ‘York, 1966. History and technology, espe- cially of natural fibers. 139 Potes, D. M. and Corban, B.P, Te les: Fibers’ 10 Fabric, Four Faiton, McGraw-Hill, New York, 1967. A textbook with section on fiber identification, 13.10 Chamot, E. ML, and Mason, C.W. Chemical Microscopy, Vol. 1 an Physical Methods, Third Edition, John Wiley & Sons, New York, 1950. A classical textbook with ‘various references fibers 13.1] TWTO Draft Test Method $8- “Quantitative Analysis of Blends of Wool with Specialty Fibers by Scanning Electon Microscope.” Describes method for dstin- {ishing between specialty animal fers and Wool and provides numerous efeences. TM 20-2007 43Longin View 590K Fig. 1—Cotton, not mercerized Cross-Section 500K wh Longiucinal View 00% Fig. 4—Hemp. 44 TM 20-2007 Appendix 1 Photomicrographs of Common Textile Fibers ‘Grose Seaton 500% Longtudinl iw 500% Longtudaa! View 500% Fig. 2—Cotton, mercerize. Fig. 3—Linen. Cross-Section 500% Longin View 590% Longtuieal View 800K Fig. Salute. Fig, 6—Ramie. [AATCC Technical Manval2008‘crass-Section 500K (ross-Section 500x (cress Seton 500% Longitudinal View 80% Lonotucinl iw 500% {Longhuainal View 500% Fig, 7—Sisal. Fig. @—Abaca. Fig. 9—Kenat. ‘cros- Section 500% Gros-Section 500% Cross-Section 500K Longiusnal View 500% Langnucinl Ww 500% “Longtucnal Ven s00% Fig. 10—Phormium. Fig. 11—Wool Fig. 12—Mtohair. AATCC Technical Manual’2008 TM 20-2007 45Longue! View 240K Longin! Vio 500% Longitudinal Viow 500% Fig. 13—Cashmere, Fig. 13A—SEM (Cashmere). Fig. 14—Camel halt. (ose Seaton 500K rose- Section 500% Cross-Section 118% Longitudinal ve Fig. 15—Alpaca. Fig. 16—Vieuna. Fig. 17—Horsehait. 46 TM 20-2007 ‘AATCC Technical Manual2008Longtuain! View 500% ‘ongiudna View 250K Fig. 22—Aoetate, secondary. Fig. 23—Triaestate, 2.6 denier (0.28 tex) per filament, dull luster. Fig, 21—Asbe AATCC Technical Manvall2008 TM 20-2007 47' Cross-Section 500% Fig, 24—Acrllc, reg. wet spun, sem-dul. Fig. 25—Acrylic, modified wet spun, 3.0 Fig. 26—Aeryli, solvent spun. denier (0.33 tex) per filament, semi-dull luster. rose-Secton 500K ‘ross-Sectin 100 ie Lonatna View 250% Lengtuain! view 100% Lengtuain! vw 250%. fic, two-component, 3.0 Fig. 28—Anidex, Fig. 28—Glass. ig. 27—Aerylic, denier (0.33 tex)’ per filament, semi-dull luster. 48 TM 20-2007 ‘AATCC Technical Manuell2008‘Cross-Section 100K NR FA A ee Longin! View 00x Lonotun! View 100% Fig. 30—Motallic, Fig. 31—Modacryic. Fig. 32—Modaeryic. cose Secon 50x Cross Sezton sox rose Seaton s00x Ie Longin! Vw 250% Longlinl View 500% Longlcial View 500% Fig. 33—Modacrylc, 3.0 denier (0.33 Fig. 34—Modacrylic with liquid inclusions. Fig. 35—tylon, bright. ex) per filament, dull luster. AATCC Technical Manual/2008 TM 20-2007 49Cross-Section 500K Fig. 36—Nylon, low modification ratio Fig. 37—tylon, high modification ratio trilobal, 15 denier (1.65 tex) per lobal, 18 denier (1.98 tex) per filament, filament, bright luster. semi-dull, (rose Sacton 500% Crose-Secton 500K Longitudinal Vw 500%. Longtinal View 500% Fig, 39—Polyethylene, low density Fig. 40—Polyethylene, medium density. 50 TM 20-2007 =e Longin! View 250% Fig. 38—Nytril, 2.0 denier (0.22 tex) per filament, dul luster. Cross-Section 00K Longiuinal Viw 500% Fig. 41—Polyethytene, high density. AATCC Technical Manual’2008500K se. High tenacity, AATCC Technical Manual’2008 TM 20-2007 51calsa uae: ES AVE 2 SS «A CRIN iy > on ee ‘9 LOR eo se TM 20-2007 AATCC Technical Manwal2008Grogs Seztion 500% (rose Sesion 500K hi Longitudinal View 250X Longin! View 250% Lonatuinl View 500% Flp, 54—Spandex, adhering filaments, 12 Fig. §5—Spandex, coarse mono- Fig. 58-—Fluorocarbion. ienier (1.32 tex) per filament, dul luster. filaments, 250 denier (27-50 tex) per filament, dul luster. (ose Sacton 600K bo) am Longitudinal View 500% Longitudinal Vw 600% Longin! Viow 600%. Fig, 57—Vinyon. Fig. 58—Aramid, round, high-tenacity Fig. 52—Aramid, FR staple fiber. filament. ‘AATCC Technical Manual2008 ‘TM 20-2007 53Crose-Secton 500K Longuainal vw 500% Fig. 60—Novoloid. rose Section 500% Lonotsinal View 500% Fig. 63—Vak. 54 TM 20-2007 rose Secon 1500 Longtusine! View 1500X Fig. 61—Permanently crimped tyocell fiber. Longitudinal Yew 1500% Fig. 63A—SEM of Yak. ‘tae Traneversa Grose Section 1800% Seaning Election Photomioropanh (10 on) Fig. 62—Unerimped tyocel fiber ‘AATCC Technical Manuall2008Appendix It Micro-Fourier Transform Infrared Spectra of Common Textile Fibers >| | re Fig, Poly(ethylene) Ultra High Molecular Weight ~ i i 4 al 1 4 Fig, 2—Poly(propyiene) Tye gesseRuncorseaszensne Fig. 5—Poly(m-phenyloneisophthalamide) AATCC Technical Manual2008 Fig. 6—Cotton TM 20-2007 55