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1Universidad Nacional de IngenieríaFacultad de Ingeniería Química y Textil

ÁREA ACAD!ICA DE IN"ENIER#A TE$TI%

%A&'RAT'RI' DE CIENCIA( DE %A( FI&RA()IT*++,A

)ERI'D' ACAD!IC' -.+/ 0 II

AATCC -.

AATCC TECHNICAL MANUALo Profesora:

Ing. Elsa Roca Meneses

o Realizado por:

FERNANDE RUE!TA" Lill#

Fec$a de realizaci%n de la pr&c'ica() *((*(+

Fec$a de en'rega del infor,e: (-*((*(+

LIMA PER/



1Fi1er Analysis2 Qualitative

+3 )ur4ose and (co4e(.( T$is 'es' ,e'$od descri0es p$#sical" c$e,ical and ,icroscopical 'ec$ni12es for iden'if#ing'e3'ile fi0ers 2sed co,,erciall# in '$e Uni'ed !'a'es. Fi0ers ,a# 0e e3a,ined in ra4 fi0er for,or 'a5en fro, #arn or fa0ric.(.) T$ese 'es' ,e'$ods ,a# 0e 2sed 'o iden'if# generic fi0er '#pes as defined 0# '$e Te3'ileFi0ers Prod2c's Iden'ifica'ion Ac' and s20se12en' r2les and reg2la'ions of '$e Federal TradeCo,,ission or I!6 )789" Te3'iles ,an,ade fi0resgeneric na,es. ;2an'i'a'i<e ,e'$ods forde'er,ining percen'ages in 0lends of fi0ers are co<ered 0# AATCC Tes' Me'$od )7A" Fi0er Anal#sis: ;2an'i'a'i<e.(.+ T$e 'es' ,e'$ods appl# 'o fi0ers 4$ic$ are s$o4n 0elo4 gro2ped 0# generic classifica'ions:

-3 Use and %imitations).( T$is 'es' ,e'$od descri0es a n2,0er of proced2res=,icroscopical e3a,ina'ion" sol20ili'#in sol<en's" ,el'ing poin'" refrac'i<e inde3" and ,icroFo2rier Transfor, Infrared !pec'roscop#=4$ic$ s$o2ld 0e 2sed in co,0ina'ion 'o iden'if# a fi0er '#pe. For iden'if#ing cer'ain fi0ersso,e proced2res 4ill 0e fo2nd 'o 0e ,ore effec'i<e '$an o'$ers.).) For e3a,ple" ,icroscopical e3a,ina'ion is par'ic2larl# 2sef2l in c$arac'erizing '$e na'2ralfi0ers. I' ,2s' 0e 2sed 4i'$ ca2'ion on ,an,ade fi0ers since '$e# are fre12en'l# prod2ced in an2,0er of ,odifica'ions 4$ic$ al'er '$e longi'2dinal or crosssec'ional appearance. In addi'ion",an,ade fi0ers ,a# con'ain so,e or no del2s'eran' or o'$er addi'i<e par'icles. Fila,en's of a



1gi<en '#pe ,a# <ar# in size or crosssec'ional s$ape. Indi<id2al fila,en's ,a# $a<e '4o or ,oreco,ponen' sec'ions of '$e sa,e or differen' generic '#pes.).+ E<en na'2ral fi0ers s$o4 a fairl# 4ide <aria'ion in '#pical crosssec'ion. No specificspeci,en 4ill loo5 e3ac'l# li5e '$e pic'2res p20lis$ed. A s2fficien' n2,0er of fi0ers s$o2ld 0ee3a,ined 'o co<er '$e range of appearance in an# speci,en.

).> !2ccessf2l iden'ifica'ion of fi0ers depends 2pon e3perience and fa,iliari'# 4i'$ '$e fi0ers.T$e iden'ifica'ion of an 2n5no4n fi0er is 0es' ,ade 0# co,parison 4i'$ properl# iden'ified fi0ers2sedas reference s'andards. For '$is reason i' is desira0le 'o $a<e a<aila0le a' leas' onerepresen'a'i<e fi0er sa,ple fro, eac$ generic class of fi0ers" 4$ic$ can 0e 2sed forco,para'i<e iden'ifica'ion.).? T$is 'es' ,e'$od pro<ides ,eans for iden'if#ing '$e generic classifica'ion of '$e co,,onfi0er '#pes. In special cases" as 4$en dealing 4i'$ fi0ers no' descri0ed in '$is ,e'$od ora''e,p'ing 'o dis'ing2is$ 0e'4een prod2c's of differen' s2ppliers of '$e sa,e generic '#pes" one,2s' cons2l' s'andard 'e3's on fi0er iden'ifica'ionor 'ec$nical 02lle'ins iss2ed 0# s2ppliers of ,an,ade fi0ers. !ee references !ec'ion (+./3 Terminology+.( For defini'ions of 'ec$nical 'er,s" refer 'o '$e Glossary of AATCC Standard Terminology in'$is TECHNICAL MANUAL.

53 (a6ety )recautionsN6TE: T$ese safe'# preca2'ions are for infor,a'ion p2rposes onl#. T$e preca2'ions areancillar# 'o '$e 'es'ing proced2res and are no' in'ended 'o 0e all incl2si<e. I' is '$e 2ser@sresponsi0ili'# 'o 2se safe and proper 'ec$ni12es in $andling ,a'erials in '$is 'es' ,e'$od.Man2fac'2rers MU!T 0e cons2l'ed for specific de'ails s2c$ as ,a'erial safe'# da'a s$ee's ando'$er ,an2fac'2rer@s reco,,enda'ions. All 6!HA s'andards and r2les ,2s' also 0e cons2l'edand follo4ed.>.( ood la0ora'or# prac'ices s$o2ld 0e follo4ed. Bear safe'# glasses in all la0ora'or# areas.>.) All c$e,icals s$o2ld 0e $andled 4i'$ care.>.+ In preparing" dispensing and $andling '$e reagen's o2'lined in !ec'ion 9" 2se c$e,icalgoggles or face s$ield" i,per<io2s glo<es and an i,per<io2s apron. Concen'ra'ed acids s$o2ld0e $andled onl# in an ade12a'el# <en'ila'ed la0ora'or# $ood. CAUTI6N: Al4a#s add acid 'o4a'er.

>.> All poisono2s and fla,,a0le reagen's s$o2ld 0e ,i3ed and $andled onl# in an ade12a'el#<en'ila'ed la0ora'or# $ood. CAUTI6N: Ace'one and e'$#l alco$ol are $ig$l# fla,,a0le ands$o2ld 0e s'ored in '$e la0ora'or# onl# in s,all con'ainers a4a# fro, $ea'" open fla,e andspar5s.>.? An e#e4as$*safe'# s$o4er s$o2ld 0e loca'ed near0# and an organic <apor respira'or s$o2ld0e readil# a<aila0le for e,ergenc# 2se.>.9 E3pos2re 'o c$e,icals 2sed in '$is proced2re ,2s' 0e con'rolled a' or 0elo4 le<els se' 0#go<ern,en'al a2'$ori'ies e.g." 6cc2pa'ional !afe'# and Heal'$ Ad,inis'ra'ion@s 6!HAper,issi0le e3pos2re li,i's PEL as fo2nd in )- CFR (-(7.(777 of an2ar# (" (-G-. Inaddi'ion" '$e A,erican Conference of o<ern,en'al Ind2s'rial H#gienis's ACIH T$res$oldLi,i' al2es TLs co,prised of 'i,e 4eig$'ed a<erages TLTBA" s$or' 'er, e3pos2reli,i's TL!TEL and ceiling li,i's TLC are reco,,ended as a general g2ide for aircon'a,inan' e3pos2re 4$ic$ s$o2ld 0e ,e' see ().(.

73 A44aratus 8see +-3-9?.( Co,po2nd ,icroscope 4i'$ ,a'c$ed o0Jec'i<es and e#e pieces 'o ac$ie<e ,agnifica'ions of(77?77K and e12ipped 4i'$ a polarizer and anal#zer.?.) lass slides and co<er glasses.?.+ Dissec'ion needles.?.> !cissors s,all and '4eezers fine.?.? Crosssec'ioning de<ice of one '#pe s2c$ as lis'ed 0elo4.?.?.( !'ainless s'eel pla'e" ).?> 8.9) 7.7)?> c, ( + 7.7( in. drilled 4i'$ 7.7- c, 7.7>in. dia,e'er $oles. !of' copper ,agne' 4ire AB +>" 7.7(9 c, 7.779+ in. dia,e'er.?.?.) Micro'o,e" $and.?.9 Razor 0lades" s$arp" '$in" single edge or do20le edge 4i'$ $older.?.8 Densi'# gradien' '20e" glass appro3i,a'el# ).? c, ( in. in dia,e'er and >? c, (G in. long4i'$ a sealed 0o''o, and a )>*>7 s'andard 'aper Join' glass cap clos2re a' 'op 'o a<oid ,ois'2re



1pic52p or e<apora'ion of sol<en's. Tin# glass sp$eres of cali0ra'ed densi'# ,a# 0e 2sed asdensi'# s'andards.?.G Mel'ing poin' appara'2s consis'ing of a $ea'ed 0loc5" 'e,pera'2re ,eas2ring de<ice s2c$ asa '$er,o,e'er and ,eans for con'rolling '$e ra'e of $ea'ing and <ie4ing '$e speci,en a' lo4,agnifica'ion. T$e ins'r2,en' s$o2ld $a<e a range of (77+77C or ,ore" and an acc2rac# of O

( degree o<er '$e en'ire range.?.- MicroFTIR Ins'r2,en'.:3 Reagents and !aterials 8see +-3-99.( Mo2n'ing Reagen's.9.(.( Mineral oil" U.!.P. or o'$er i,,ersion fl2id.9.(.) Collodion" sol2'ion of ni'rocell2lose > g*(77 ,Lin (:+ alco$ol*e'$#l e'$er.9.) leac$ing Reagen'.9.).( H#dros2lfi'eca2s'ic sol2'ion.Dissol<e ) g sodi2, $#dros2lfi'e and ) g sodi2, $#dro3ide in (77 ,L of 4a'er.9.+ !'aining Reagen's.9.+.( inc c$loroiodide reagen'. Dissol<e )7 g of zinc c$loride in (7 ,L of 4a'er. Add ).( g ofpo'assi2, iodide and 7.( g of iodine dissol<ed in ? ,L of 4a'er. Add a leaf of iodine.9.+.) Acid p$lorogl2cinol reagen'. Dissol<e ) g of p$lorogl2cinol in (77 ,L of 4a'er. Use 4i'$

e12al <ol2,e of concen'ra'ed $#droc$loric acid.9.> Refrac'i<e Inde3 I,,ersion Li12ids.9.>.( He3adecane ce'ane C. P. rade" RI Q (.>+>.9.>.) Alp$a c$loronap$'$alene" RI Q (.9++. Poisono2s. A<oid in$aling <apors.9.>.+ lends of '$e a0o<e. Ass2,e '$a' '$e refrac'i<e inde3 <aries linearl# 0# <ol2,e ofingredien's. For e3a,ple" 'o ,a5e a li12id of RI Q (.??7 ,i3 >) par's 0# <ol2,e of $e3adecane4i'$ ?G par's 0# <ol2,e of alp$a c$loronap$'$alene.9.? Fi0er !ol<en's.9.?.( Ace'ic acid" glacial. Corrosi<e. Do no' ge' in e#es or on s5in.9.?.) Ace'one" reagen' grade. Ca2'ion: $ig$l# fla,,a0le.9.?.+ !odi2, $#poc$lori'e sol2'ion" ?. Ho,e la2ndr# 0leac$ is sa'isfac'or#.9.?.> H#droc$loric acid" concen'ra'ed reagen'" )7. Dil2'e ?7 ,L of concen'ra'ed $#droc$loricacid" +G" 'o -? ,L 4i'$ dis'illed 4a'er. 9.?.? For,ic acid" G?. Corrosi<e. Do no' ge' in e#es

or on s5in.9.?.9 (">Dio3ane.9.?.8 mK#lene.9.?.G C#clo$e3anone.9.?.- Di,e'$#lfor,a,ide. Ca2'ion: if spilled on s5in" 4as$ off i,,edia'el#.9.?.(7 !2lf2ric acid sol2'ion" ?-.? O 7.)? 0# 4eig$'" densi'# (.>-)- O 7.77)8 g per ,L a' )7C.Beig$ in'o a 0ea5er ?-.? g of concen'ra'ed s2lf2ric acid sp gr (.G>. Beig$ in'o a )?7 ,LP#re3 Erlen,e#er flas5 >7.? g of dis'illed 4a'er. Ca2'io2sl# add the acid to the water s4irlingand cooling in ice 4a'er or 2nder a 'ap. Wear goggles! T$e sol2'ion 0eco,es <er# $o' and ,a#0oil and spa''er if no' cooled d2ring ,i3ing. Af'er '$e sol2'ion $as cooled 'o )7C 9GF adJ2s''$e densi'# 'o a <al2e 0e'4een (.>-7) and (.>-?9 g per ,L. 9.?.(( !2lf2ric acid sol2'ion" 87 O( 0# 4eig$'" densi'# (.9(7? O 7.7((9 g per ,L a' )7C. Beig$ 87 g of concen'ra'ed s2lf2ricacid sp gr (.G> and +7 g of 4a'er and ,i3 4i'$ '$e sa,e preca2'ions as in 9.?.(7. Af'er '$e

sol2'ion $as cooled 'o )7C 9GF adJ2s' '$e densi'# 'o a <al2e 0e'4een (.?-G- and (.9))( gper ,L. 9.?.() mCresol" reagen' grade. Poisono2s. Use in <en'ila'ed $ood. 9.?.(+ H#drofl2oricacid" >- reagen' grade. er# dangero2s. Use goggles and $ood 2nder s2c'ion. Do no' in$ale<apors or allo4 'o con'ac' s5in.;3 (am4ling8.( To o0'ain a represen'a'i<e sa,ple for iden'ifica'ion i' is necessar# 'o consider '$e follo4ing:8.(.( If '$e sa,ple is loose fi0er or #arn" i' ,a# con'ain one fi0er onl# or i' ,a# 0e an in'i,a'e0lend of '4o or ,ore fi0ers.8.(.) A #arn sa,ple ,a# 0e a pl# or 4rapped core 0lend of '4o or ,ore #arns. T$ese #arns in'2rn ,a# 0e '$e sa,e or differen' and ,a# '$e,sel<es con'ain a 0lend of fi0ers.8.(.+ Bo<en and 5ni''ed fa0rics ,a# 0e cons'r2c'ed of '$e sa,e or differen' #arns in <ario2sco,0ina'ions. T$e #arn ,a# con'ain one or ,ore fi0er '#pes.



18.(.> Differen' fi0er '#pes ,a# 0e d#ed 'o '$e sa,e color. Con'rar#4ise" '$e sa,e fi0er '#pe,a# appear in differen' colors in '$e finis$ed ar'icle 0# ,i3ing s'oc5 d#ed or #arn d#ed ,a'erialsor 2sing fi0ers 4i'$ ,odified d#eing c$arac'eris'ics.8.(.? I' is essen'ial '$a' '$e speci,ens selec'ed represen' '$e en'ire sa,ple of ra4 fi0er" #arn orfa0ric 2nder e3a,ina'ion.

<3 (4ecimen )re4arationG.( In ,an# cases '$e iden'i'# of an 2n5no4n fi0er can 0e es'a0lis$ed 4i'$o2' pre'rea',en'.G.) B$en '$e presence of s'arc$" 4a3" oil or o'$er coa'ing o0sc2res '$e appearance of '$e fi0er"'r# $ea'ing in 4ar, 'o $o' dis'illed 4a'er 'o re,o<e '$e foreign ,a''er. If '$is fails" 'r# e3'rac'ing4i'$ organic sol<en's" 7.? $#droc$loric acid or 7.? sodi2, $#dro3ide. !o,e fi0ers s2c$ asn#lon are da,aged 0# acid and so,e s2c$ as azlon" sil5 and 4ool" are da,aged 0# ca2s'ic'rea',en' see -.8. G.+ To separa'e <ege'a0le fi0er 02ndles" 'rea' 4i'$ 7.? sodi2, $#dro3ide sol2'ion" rinse 4ell4i'$ 4a'er and dr#.G.> To s'rip d#e fro, colored fi0ers" especiall# '$e cell2losic fi0ers" $ea' for +7 ,in a' ?7C 4i'$$#dros2lfi'e ca2s'ic sol2'ion see 9.).(.=3 )rocedure-.( T$e iden'ifica'ion of fi0ers is 2s2all# carried o2' 0# s20Jec'ing speci,ens 'o a <arie'# of

selec'ed 'es's 2n'il eno2g$ infor,a'ion is o0'ained 'o ,a5e a sa'isfac'or# J2dg,en' as 'o '$egeneric class or specific '#pe. T$e selec'ion of 'es's and order in 4$ic$ '$e# are perfor,ed canc$ange depending on '$e 5no4ledge alread# a<aila0le and res2l's of '$e preli,inar# 'es's.-.) is2al and Microscopical E3a,ina'ion.-.).( E3a,ine '$e sa,ple of ,a'erial s20,i''ed for iden'ifica'ion. No'e for, loose fi0ers" #arn"fa0ric" e'c." color" fi0er leng'$ and fineness" 2nifor,i'# of appearance and pro0a0le end2se. If T$e sa,ple is a fa0ric" separa'e o2' #arns 0# 2nra<eling or c2''ing. If '$e fa0ric is 4o<en"separa'e 4arp and filling #arns. If #arns differ in color" l2s'er" size or o'$er apparen' 4a#s" ,a5ea p$#sical separa'ion of '$ese #arns for separa'e iden'ifica'ion.-.).) T$e fi0ers ,a# 0e iden'ified 2sing ei'$er lig$' or scanning elec'ron ,icroscop#. If 2sing'rans,i''ed lig$' ,icroscop#" place a s,all 12an'i'# of '$e fi0ers on a glass slide" 'ease fi0ersapar'" ,o2n' 4i'$ a drop of ,ineral oil or o'$er i,,ersion fl2id" co<er 4i'$ a co<er slip ande3a,ine 2nder '$e ,icroscope.

-.).+ 60ser<e '$e fi0er c$arac'eris'ics as seen in 'ra<erse sec'ion and classif# in'o fo2r generalclasses.-.).> Fi0ers 4i'$ s2rface scales. T$ese are '$e ani,al $air fi0ers lis'ed in P2rpose and !copesee (.+. All of '$e 5era'in fi0ers lis'ed e3cep' sil5 are incl2ded in '$is gro2p. Con'in2e de'ailed,icroscopical e3a,ina'ion incl2ding crosssec'ion e3a,ina'ion see -.+. Co,pare 4i'$ '$ec$arac'eris'ics in Ta0le I" p$o'ograp$s in '$e appendi3 of '$is ,e'$od" and 5no4n speci,ens of$air fi0ers see ().+. Addi'ional confir,a'ion of '$is class ,a# 0e ,ade 0# 02rning 'es' see-.?S densi'# see -.9S and sol20ili'# see -.8. -.).? Fi0ers 4i'$ Cross Mar5ings. T$ese are '$e <ege'a0le fi0ers o'$er '$an co''on lis'ed in (.+.Con'in2e de'ailed ,icroscopical e3a,ina'ion incl2ding crosssec'ion e3a,ina'ion see -.+.Co,pare 4i'$ c$arac'eris'ics as gi<en in Ta0le II" p$o'ograp$s and 5no4n speci,ens of<ege'a0le fi0ers. To dis'ing2is$ linen and ra,ie fro, $e,p" o0ser<e '$e direc'ion of ro'a'ion ondr#ing see -.G. If '$e fi0ers are lig$' in color" s'ain 4i'$ zinc c$loroiodide reagen' and 4i'$ acid

p$lorogl2cinol as direc'ed in -.-. Addi'ional confir,a'ion of '$is class ,a# 0e ,ade 0# 'es'sdescri0ed in -.>" -.?" -.9 and -.8.-.).9 Con<ol2'ed Fi0ers. T$is class incl2des co''on and '2ssa$ sil5. T$e '4o are easil#dis'ing2is$ed 0# crosssec'ion see -.)" 02rning 'es' see -.? and sol20ili'# see -.8 or ,icroFTIR see Appendi3 II. If fi0ers are lig$' in color" '$e# ,a# 0e dis'ing2is$ed 0# s'aining 4i'$ zincc$loroiodide reagen' see -.-.-.).8 6'$er Fi0ers. T$is class incl2des all of '$e ,an,ade fi0ers" o,0#3 sil5 and as0es'os.T$e la''er '4o can 0e iden'ified 0# ,icroscopical appearance incl2ding crosssec'ion see -.+.2rning 'es's see -.? and sol20ili'# 'es's see -.8 are especiall# significan' for as0es'os andare 2sef2l in confir,ing '$e presence of sil5. T$e ,an,ade fi0ers are 0es' iden'ified 0# ,icroFTIR" sol20ili'#" ,el'ing poin'" refrac'i<e indices and o'$er op'ical c$arac'eris'ics and densi'#:proper'ies 4$ic$ rela'e 'o c$e,ical na'2re ra'$er '$an p$#sical s$ape. Crosssec'ions ,a# <ar#and s'aining 'es's can 0e ,isleading since ,odifica'ions of a generic '#pe ,a# d#e differen'l#.



1Used 4i'$ discri,ina'ion and in co,0ina'ion 4i'$ o'$er 'es's" crosssec'ions and d#e 'es's ,a#so,e'i,es 0e $elpf2l in narro4ing do4n '$e n2,0er of possi0ili'ies. Me'allic fi0ers $a<e adis'inc'i<e s$in# appearance" 02' a s$in# resid2e ,a# no' indica'e a ,e'allic fi0er. Using a'rans,i''ed lig$' ,icroscope a' ?3" (73 and )73 ,agnifica'ion po4ers 4ill no' re<eal diffrac'ion"in'erference and gloss effec's '$a' can decep'i<el# appear 'o 0e ,e'allic in na'2re. C$e,ical

colori,e'ric and*or ins'r2,en'al A'o,ic A0sorp'ion !pec'rop$o'o,e'ric anal#ses s$o2ld 0eperfor,ed 'o confir, '$eir presence.-.+ Microscopical Cross!ec'ion E3a,ina'ion.-.+.( 60'ain a parallel 02ndle of fi0ers or #arn. T$read a loop of copper 4ire '$ro2g$ one $ole in'$e s'ainless s'eel pla'e. Ca'c$ '$e 02ndle or #arn in '$e loop and p2ll i' '$ro2g$ '$e $ole. Uses2fficien' fi0ers 'o pac5 '$e $ole f2ll. If necessar#" 2se so,e e3'ra" readil# iden'ifia0le o'$er fi0er'o fill 2p '$e $ole.Ta1le I>C?aracteristics o6 Fi1ers @it? (cales on (ur6aceNo'e: T$e c$arac'eris'ic designa'ed 0# a capi'al le''er K in '$is 'a0le is '$a' 4$ic$ is especiall#significan'.



1

-.+.) Bi'$ a s$arp razor 0lade ,a5e a s,oo'$ c2' on 0o'$ sides of '$e pla'e.-.+.+ E3a,ine '$e sec'ion in air" or co<ered 0# a ,o2n'ing fl2id li5e ,ineral oil 2nder a co<erslip. Use 'rans,i''ed lig$' and 2sef2l ,agnifica'ion of )77 ?77K. Co,pare 4i'$ p$o'ograp$s in Appendi3 or crosssec'ions of 5no4n fi0ers.-.+.> If '$e Hard# '#pe ,icro'o,e is 2sed" follo4 ins'r2c'ions 4i'$ '$e ins'r2,en'. Inser' a 02ndleof fi0ers or #arn in'o '$e slo'. !lide '$e 'ong2e in'o '$e slo' 'o co,press '$e 02ndle. AdJ2s' '$e12an'i'# of fi0ers for a 'ig$' pac5age. C2' off 0o'$ sides. Appl# a drop of collodion 'o one c2'face" 4ai' 2n'il i' s$o4s '$ro2g$ on '$e o'$er side and '$en appl# a drop 'o '$e o'$er side. Le'dr# '$oro2g$l#. !lice off e3cess collodion and fi0er on 0o'$ sides of '$e pla'e 4i'$ a s$arp razor0lade. -.+.? A''ac$ '$e a23iliar# pl2nger" and 4i'$ '$e scre4 ad<ance '$e e,0edded '2f' '$ro2g$'$e slo' 2n'il i' pro'r2des )7 >7 , a0o<e '$e pla'e. Add a drop of collodion and le' dr# a0o2' ?,in or 2n'il fir,. !lice off collodion and e,0edded fi0er sec'ion 4i'$ a s$arp razor 0lade $eld a'a0o2' >?angle 4i'$ '$e slo'. C2' 4i'$ a single s'ro5e.-.+.9 Re,o<e '$e sec'ion" 'ransfer 'o a glass slide" ,o2n' 4i'$ a drop of ,ineral oil or o'$eri,,ersion li12id" add a co<er slip and e3a,ine. Con'in2e 'o c2' sec'ions as descri0ed in -.+.?2n'il good clear crosssec'ions are o0'ained. E3a,ine and co,pare 'o 5no4n crosssec'ions.-.> Refrac'i<e Inde3.-.>.( Place a s,all sa,ple of '$e fi0er on a glass slide. I,,erse in a drop of ac$loronap$'$alene and ce'ane ,i3'2re or e12i<alen' of refrac'i<e inde3 (.??.-.>.) Inser' '$e polarizer in'o '$e s20s'age of '$e ,icroscope 'o pro<ide lig$' polarized in '$e 9() o@cloc5 direc'ion. Align '$e long di,ension of a fi0er in '$e sa,e direc'ion. Close '$ediap$rag, of '$e s20s'age condenser so as 'o pro<ide a3ial ill2,ina'ion.-.>.+ Foc2s caref2ll# on '$e o2'lines of '$e fi0er. Bi'$ '$e fine adJ2s',en'" raise '$e foc2s 'o J2s'a0o<e '$e 'op of '$e fi0er. If '$e fi0er is ro2g$l# a c#linder" i' 4ill ac' li5e a lens. If '$e refrac'i<e

inde3 of '$e fi0er is higher '$an '$e i,,ersion li12id" '$e fi0er 4ill ac' li5e a posi'i<e lens. A0rig$' line of lig$' 4ill ,o<e in'o '$e ,iddle of '$e fi0er as '$e foc2s is raised. If '$e refrac'i<einde3 of '$e fi0er is lower '$an '$e i,,ersion li12id" '$e lig$' 4ill flare o2' as '$e foc2s is raisedand '$e ,iddle of '$e fi0er 4ill 0eco,e dar5er. Repea' 2n'il cer'ain of '$e direc'ion.-.>.> T$e 'es' can 0e seen 0es' 4i'$ ro2nd fi0ers. 6n fla' ri00ons i' ,a# 0e easier 'o see,o<e,en' of a 0rig$' line= '$e ec5e line=a' '$e o2'lines of '$e fi0er. Mo<e,en' is in '$esa,e direc'ion" 'o4ard '$e ,edi2, of $ig$er refrac'i<e inde3 as '$e foc2s is raised.-.>.? Ro'a'e '$e speci,en -7 and repea' '$e 'es'.-.>.9 Ro'a'e '$e speci,en >?. Inser' '$e anal#zer in '$e 0od# '20e or e#epiece 'o pro<idecrossed polars. 60ser<e if '$e fi0er appears <er# 0rig$' s'rong 0irefringence" di, 4ea50irefringence or dar5 no 0irefringence.-.>.8 Refer 'o Ta0le I for refrac'i<e inde3 of fi0ers in '$e long and cross direc'ion and anes'i,a'e of 0irefringence. Consider '$a' '$e re'arda'ion depends on '$e '$ic5ness of '$e fi0er



1speci,en as 4ell as '$e e3'en' of dra4ing of a gi<en speci,en. Co,pare 4i'$ 5no4n fi0ers ofsi,ilar dia,e'er for 0irefringence.-.>.G !elec' o'$er i,,ersion li12ids and repea' -.>.( '$ro2g$ -.>.?. As '$e refrac'i<e inde3 of'$e li12id approac$es '$a' of '$e fi0er" '$e o2'lines of '$e fi0er 0eco,e less dis'inc'. Ma'c$ '$eli12id 'o '$e fi0er 4i'$ing 7.7( refrac'i<e inde3.

-.? 2rning Tes'.-.?.( Ta5e a s,all '2f' of fi0ers $eld in '4eezers and place close 'o '$e side of a s,all fla,e.No'e if '$e fi0ers ,el' or s$rin5 fro, '$e fla,e.-.?.) Mo<e '$e fi0ers in'o '$e fla,e. No'e 4$e'$er '$e fi0ers 4ill 02rn 4$en $eld in '$e fla,e.Re,o<e fro, '$e fla,e <er# slo4l# and caref2ll#. No'e 4$e'$er '$e fi0ers con'in2e 'o 02rno2'side of '$e fla,e. Ma5e s2re '$a' '$e fi0er 4as igni'ed 0efore ,a5ing '$is la''er o0ser<a'ion.-.?.+ lo4 o2' '$e fla,e" if s'ill 02rning" and s,ell '$e s,o5e. No'e '$e odor and e3a,ine '$ecolor and na'2re of an# as$ resid2e.-.?.> Co,pare '$e 0e$a<ior o0ser<ed 4i'$ '$a' lis'ed in Ta0le III and '$a' of 5no4n referencefi0ers. Fla,e re'ardan' ,odifica'ions of so,e fi0ers=co''on" ra#on" ace'a'e and ,odacr#lic" fore3a,ple= are a<aila0le. 2rning is re'ardedS odor on 02rning and as$ ,a# 0e c$anged.Colored fi0ers=especiall# '$ose colored 0# pig,en's=4ill re'ain color in '$e colored resid2e.-.?.? 6dors of so,e 02rning fi0ers are 12i'e c$arac'eris'ic. T$e ani,al fi0ers and ,an,ade

pro'ein fi0ers azlon $a<e '$e odor of 02rning $air or fea'$ers. T$e <ege'a0le fi0ers andregenera'ed cell2lose ra#on s,ell li5e 02rning paper. T$e s,ell of 02rning r200er is a fa,iliar odor. 6'$er ,an,ade fi0ers=s2c$ as acr#lic" n#lon and spande3=$a<e c$arac'eris'ic odors4$ic$ can 0e recognized 4i'$ e3perience.-.9 Densi'#.-.9.( Prepare a densi'# gradien' col2,n as follo4s. Cla,p '$e densi'# gradien' glass '20e in afir, <er'ical s'and. Po2r in'o '$e '20e )? ,L of 'e'rac$loroe'$#lene. No4 prepare ,i3'2res of3#lene and 'e'rac$loroe'$#lene 0# <ol2,e in descending order of percen' 'e'rac$loroe'$#lene:-7*(7" G7*)7" 87*+7" 97*>7" ?7*?7" >7*97" +7*87" )7*G7 and (7*-7. Po2r )? ,L of eac$ in ordercaref2ll# do4n '$e side of '$e gradien' '20e. Finall#" p2' )? ,L of 3#lene on 'op. -.9.) Ta5e $or'frag,en's of d#ed reference fi0ers and 'ie in a 5no' snipping off loose ends. oil for a0o2' ) ,inin 3#lene



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1

sol<en' 'o re,o<e ,ois'2re and air. Place in '$e col2,n. Af'er a0o2' a $alf $o2r '$e# s$o2ldco,e 'o res' a' '$e le<el represen'ing '$eir densi'#. Cali0ra'ed glass sp$eres ,a# 0e 2sed 'ode'er,ine '$e ac'2al densi'# a' <ario2s le<els.-.9.+ Prepare '$e 2n5no4n fi0er in li5e ,anner" place in '$e gradien' col2,n and no'e a' 4$a'le<el i' floa's. Densi'ies of fi0ers are lis'ed in Ta0le I.-.8 !ol20ili'# Tes'.-.8.( For 'es's a' roo, 'e,pera'2re )7C place a s,all sa,ple of '$e fi0ers in a 4a'c$ cr#s'al"'es' '20e or ?7 ,L 0ea5er and co<er 4i'$ '$e 'es' sol<en' see Ta0le . Use a0o2' ( ,L ofsol<en' per (7 ,g of fi0er.-.8.) If '$e 'es' is cond2c'ed a' '$e 0oiling poin' of '$e sol<en'" firs' 0ring '$e sol<en' 'o a 0oil ina 0ea5er on an elec'ric $o' pla'e in a <en'ila'ed $ood. AdJ2s' '$e $o' pla'e 'e,pera'2re 'o,ain'ain slo4 0oiling and 5eep 4a'c$ so '$a' '$e sol<en' does no' 0oil dr#. Drop fi0er sa,plein'o '$e 0oiling sol<en'.

-.8.+ If '$e 'es' is cond2c'ed a' so,e in'er,edia'e 'e,pera'2re" $ea' a 0ea5er of 4a'er on a $o'pla'e and adJ2s' '$e 'e,pera'2re 4i'$ a '$er,o,e'er. Place '$e fi0er sa,ple in '$e 'es' sol<en'in a 'es' '20e and i,,erse in '$e $ea'ed 4a'er 0a'$.-.8.> No'e if '$e fi0er dissol<es co,ple'el#" sof'ens 'o a plas'ic ,ass or re,ains insol20le.Co,pare 4i'$ da'a on fi0er sol20ili'# in Ta0le .-.8.? !ol20ili'# can also 0e 2sed as a 'es' 'o de'er,ine '$e presence of a ,e'al co,ponen' in afi0er. 6n dissol<ing in ,e'acresol a s$in# resid2e is e<idence of a ,e'al co,ponen'.-.G Dr#ing T4is' Tes'.-.G.( !epara'e o2' a fe4 parallel fi0ers. Dip in 4a'er and s12eeze off e3cess. Tap '$e end of '$e02ndle 'o ,a5e separa'e fi0ers flare o2'. Hold o<er a $o' pla'e in 4ar, air 'o dr# '$e fi0ers. Hold'$e fi0ers so '$a' '$e free ends poin' 'o4ard '$e o0ser<er. No'e '$e direc'ion of '4is' as '$efi0ers dr#. Linen and ra,ie '4is' in a cloc54ise direc'ionS $e,p and J2'e '4is' in a co2n'ercloc54ise direc'ion.



1-.- !'ain Tes's.-.-.( Place a fe4 fi0ers on a ,icroscopical slide. Appl# a drop of zinc c$loroiodide reagen' ando<er 4i'$ a co<er slip 'a5ing care 'o a<oid 0200les. E3a,ine '$e fi0ers for s'aining. He,p" ra,ieand co''on s'ain <iole'S linen s'ains 0ro4nis$ <iole'S J2'e s'ains 0ro4n. Man# o'$er fi0ers s'ains$ades of #ello4 0ro4n incl2ding sil5.

-.-.) Bar, a fe4 fres$ fi0ers on a ,icroscopical slide 4i'$ a drop of acid p$lorog2cinol reagen'.Bood# fi0ers s2c$ as 2n0leac$ed J2'e s'ain a deep ,agen'a 0eca2se of '$e presence of lignin.-.(7 Mel'ing Poin'.-.(7.( Mel'ing Poin' Appara'2s.-.(7.) Place a fe4 fi0ers on '$e clean $ea'ing 0loc5. Co<er 4i'$ a co<er slip. T2rn '$e $ea' onand se' '$e $ea'ing ra'e for fas' $ea'ing. 60ser<e '$e '$er,o,e'er and '$e sa,ple. B$en '$e'e,pera'2re reac$es (77C" red2ce '$e ra'e of $ea'ing. If pre<io2s 'es's alread# indica'e '$efi0er" '$e ra'e can 0e se' a' a0o2' (7C per ,in 2n'il (7)7C 0elo4 '$e e3pec'ed ,el'ing poin'.Near '$e ,el'ing poin' '$e ra'e s$o2ld 0e red2ced 'o a0o2' )C per ,in.-.(7.+ 60ser<e '$e fi0ers for e<idence of sof'ening. A' '$e ,el'ing poin'" li12id 0egins 'o for,4$ic$ 4e's '$e co<er slip. Fi0ers e<en'2all# ,erge and for, a li12id ,ass. As '$e 'es' is inprogress i' is so,e'i,es $elpf2l 'o press gen'l# on '$e co<er slip 4i'$ '4eezers 'o see if '$efi0ers fla''en 2nder press2re. If '$is ,el'ing poin' is passed a' a $ig$ $ea'ing ra'e" repea' '$e 'es'

4i'$ a fres$ sa,ple.-.(7.> Co,pare '$e ,el'ing poin' fo2nd 4i'$ '$ose lis'ed in Ta0le I.-.(7.? Microscope Mo2n'ed Appara'2s.-.(7.9 Place a fe4 fi0ers on one of '$e s,all glass slides pro<ided and co<er 4i'$ a co<er slip.Place '$e slide on '$e s'age of '$e ,icroscope 4i'$ '$e fi0ers o<er '$e cen'ral $ole of '$e s'age.P2' '$e 0affle and co<er pla'e in place.-.(7.8 Inser' '$e polarizing accessories in '$e op'ical pa'$ of '$e ,icroscope 'o pro<ide crossedpolars. T$e fi0ers s$o2ld 0e <isi0le if aligned diagonall# 'o '$e direc'ion of polariza'ion. If fi0ersare no' <isi0le 2nder '$ese lig$'ing condi'ions" re,o<e '$e polarizing accessories and o0ser<e inordinar# 'rans,i''ed lig$'.-.(7.G !e' a $ig$ $ea'ing ra'e 4i'$ '$e <ol'age reg2la'or 2n'il '$e 'e,pera'2re reac$es (77C.Red2ce '$e ra'e as '$e e3pec'ed ,el'ing poin' is approac$ed as direc'ed in -.(7.).-.(7.- 60ser<e '$e fi0ers. As ,el'ing 'a5es place '$ere is a decrease in 0irefringenceS '$e fi0ers

0eco,e dar5. Read as ,el'ing poin' '$e 'e,pera'2re a' 4$ic$ '$e fi0ers 0eco,e co,ple'el#dar5. If crossed polars are no' 2sed" o0ser<e ,el'ing as descri0ed in -.(7.).-.(7.(7 Co,pare '$e ,el'ing poin' fo2nd 4i'$ '$ose lis'ed in Ta0le I.-.(( MicroFTIR.-.((.( Co,pare FTIR spec'ra 4i'$ FTIR spec'ra in Appendi3 II or o'$er li0rar# so2rces see Appendi3 II=Figs. (-.



1

+.3 Re4ort(7.( Repor' '$e fi0er '#pe and" if ,ore '$an one '#pe is presen'" 4$ere eac$ is loca'ed. Fore3a,ple" '$e repor' co2ld 0e 4o<en fa0ric 4i'$ n#lon 9"9 4arp and co''on*ra#on filling.V++3 )recision and &ias

((.( A precision and 0ias s'a'e,en' is no' applica0le 0eca2se da'a are no' genera'ed 0# '$is,e'$od.

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