Identification of Dyes on Textile Fibres ELLIS CLAYTON

The systematic proccclure involvccl in t,he identifictLtion of dyes on comniercial dyeings iind print.s appmently hns undergone very little change, so fa.r as can be ascert,ainetl from publishcd literature, since 1!)05-7, when Green3 and his collaborators4 introduced t-heir schemes of analysis for use in the examina.tioii of dyeings on d t o n and animal fibres. It is scarcely to be expected, of course, that any particiilar systcm of analy~is can retain its position for an un- limited period as a widely recognised standard system, without undergoing various niodifica- tions, but, the fact that the first systematic series of dye-identification Tables has been used with lit& alterat.ion for 30$years through- out the world, is a remarkable tribute to the efficiency of the work of the authors. During this period, however, a large number of new dyes have been introduced into commerce and some of them belong to dyeing groups which were unknown when Green's Tables were first published. Apart, however, from a few (a) acid- mordant dyes, other than anthrayuinonoid dyes, not containing azo groups, ( b ) polymethine dyes, ( c ) dioxazine and aryl-substituted fluorindene substantive dyes, i.e. members of two sub- groups of the oxazine and azine series respect- ively, (d ) ranges of dyes used for the specific purpose of dyeing cellulose acet,at,e ra.yon, and (e ) a few dischargeable dyes containing a thiazole ring, the actual chemical classes into which dyes have been divided, almost sintedye chemistry becnnieiiri exact scierice, have undergone very few changes in the last 30 years. It is well-known that, many of the dyes given in Green's Tables are niore or less obsolete, whilst certain dyes which formerly were used only in conjunction with mordants, are now available as acid dyes which contain the mordant. (metal) as a co-ordinated part of the dye complex, but in these and almost all other cases of new dyes of modified types, the charac- teristic chromophoric groupings, represented in the original Tables, still serve as the controlling and limiting factors in the design of new schemes of identification. The present position, therefore, seems to indicate that thc general tendency in dye-research work during t,he last two or three decades has been directed mainly towards im- provement in the properties of established dyes and to thc syntheses of allied chemiatl com- pounds of much great,er molecular complexity. The modern vat dyes, in particular, illustrate this tendency. Another aim has been direct,ed towards the conversion of insoluble dyes into soluble derivatives which yield colour effects having the same valuable inherent properties it8 the parent dyes. The conversion of leuco-vat

dyes into solublo siilpliiiric rs f vr ctcbriv;it iws, which can Isc applird to ;ill f i b ~ s in S I I C * ~ I i i \\';I>.

that t81iey yield dyeings equivalent. to t lw piircltit dyeings, is an out.ntnnding rrsiilt of this work.

Incident.ally, i t may be nobed thi1.t. tlic \ v d l - known method of introtlucing M U ~ I ' ~ I ~ I ~ O - ~ : ~ ~ I I I I ) S into higher aliphatic alcohols in ordcr t o iirodwc water-soluble products, 11;~s bcw ut ilisetl re- cently, in an indirect wity, t,o prodiiw vert ain t.ypes of wtter-soluble a m tlyes rsi i~~i;iI ly suit- able for cellulose acetate rayon. Thc Solawt. dyes of Imperial Cheniical Industrirs IAd. appear to be product,s of this t,yprx. Minor i i io ( l i - tications in chemical st,ruct,iires of \vcIl-Itno\\ I I dyes, therefore, have to be boriie in mind it1 i tny attempt t,o create new or niodified srhcmes of identification, but their influtvice on long- established analytical procedurc! is of little importa,nce, since no profoiind alt.erat ion in the characteristic chromophorie groupings is in- volved in most cases and the colour c:ffr:c:ts pro- duced with the modified dyes tire not t.o l)c regarded as offering much clifficwlty in plit(*itig them i n t,he correct. dyeing clnsses.

Perhaps the most important iittribute of iltly scheme of analysis is simplicity, and the uoconi- panying Tables are now presented in the hope t,hibt. they will~erveasa contribution tosuch atlesirablc goal. At theout,set,, i t should hestntecl tlitrt. t,hc?new Ta.bles have been built up on the lincs oripitlillly employed by Professor A. G. Green. Since the multiplication of test,irig reilgellts i n ;I try sc*licnir of analysis is undehxldc. only o i i c i i i i i i i i

reducing agcnt is reconiniciidrtl for twt in: t1yc.s on wool, etc. and celliilosic~ fibrw; t,liiH c*onsists of i t solution of Formowl cont iiining cdiylcric. glycol: in sonie wses of cotton tlyeiiigs it is necessary to usc it 3?k cmistic sotiii. solution, to which sniall amount,s of sodium hytlrc )sit1 phi t t' are added (luring testing. Only a vcry ftw rrdii- cible dyeings resist. alterittion when boilctl vigor- ously in the standard Fornioxul rea.pent for it maximum period of 2 tiiin. This r(bii.petit is termed Fonnosul G.

The following notes are int.cntled iminly to amplify t,he detu.ils given in t tie iic*t~onipiiny- ing Tables. I t has not, been vonsitlrreci udvisable t.o inclucle, unrlcr th t . ( h w i ( ~ i ~ I anti dyeing groups in the Tables, ttiv tiittiics of representative commercial dyes, except in ii feu. ca.ses where cx;tmples are needctl. The 'olviir I n d e d " should be consulted on this Iwi i i t ;IS ~vell as for individual rcact,ionn of dyes belonging to the various chemical pmi ) s .

Reagents-The chief reagents rtqtirc.rl in testing dyeings and prints on i l l1 kintls ot'iininiitl a.nd cellulosic fibres ttccordirig t.o t tie w l i t ~ i i e s presented in the acconipanying Tablcs mc-

May 1937 CLAYTON-“IDENTIl’ICATION OF DYES ON TEXTILE FIBRES” 179

(1 ) Dilute Ammonia (1 C.C. ammonia, sp. gr. 0.880, made up to 100 C.C. with water); (2) 5% Cawtic Soda Solution; ( 3 ) 5% Sodium Carbonate Sotution; (4) 5% Ammonium Chloride Solution; (5) 3% Hydrogen Peroxide; (6) Vat Dye Developer (8 g. ammonium chloride and 2 g. ammonium persulphate are dissolved in 100 C.C. cold water); (7) Formosul G (20 g. Formosul are dissolved in 75 C.C. hot water and diluted with 75 C.C. cold water and 50 g. ethylene glycol); (8) Ethylenediamine (the commercial product is colourless, has sp. gr. 0.97 and b.p. 117” C.; it is readily soluble in water and contains 60-70% of base); and (9) Developer 0 (1 g. ammonium persulphate and 0.5 g. ammonium dihydrogen phosphate are dissolved in 100 C.C. cold water).

Procedure-The tests are carried out in boiling tubes. About 2 in. of the dyeing, if in the form of yarn, or 4 sq. in. or less, if in the form of cloth, is sufficient material to use; a little more should be used, of course, if the sample is a parti-coloured print. It is inadvisable to use a large excess of any reagent.

IDENTIFICATION OF DYES O N WOOL AND SILK The chief classes of dyes which are most

likely to be present on wool fibres are ( a ) acid dyes and (b ) metallic dye-lakes produced by the use of acid-mordant dyes, dyes containing a co-ordinated metal, usually chromium, and a few true mordant dyes, Dyes used on a very much smaller scale are represented by members of the vat dye series, especially Indigo, and other members of the indigoid class, including also those dyes derived from the Indigosol, Soledon, etc. series, substantive and basic dyes. A few azoic dyes may be found occasionally on animal fibres. Acid and Substantive dyes are, perhaps, the most important dyes for silk, although mem- bers of all the classes used for wool may be found on this fibre.

Basic Dyes on Wool and Silk-These dyes are extracted readily either with boiling acetic acid or alcohol. Brilliant pinks are produced occasionally on both fibres with Rhodamines, and bright blues with Turquoise Blues. Triaryl- methane basic dyes which have been transferred to wool from cotton are reduced readily with Pormosul G and reversion to the original colour tones occurs on warming the rinsed patterns in Developer 0.

-4cid Dyes on Wool and Silk-No difficulty is experienced, as a rule, in detecting acid dyes on wool and silk. Most of the azo dyes of this class are reduced fairly readily to colourless compounds, although, in a few cases, the reduction product or products leave a yellow tint on the fibre; also, in some cases, the colour- less reduction products change to a pale yellow on treatment with weak hydrogen peroxide.

Anthraquinonoid acid dyeings are easily re- duced to various tints of yellow, reddish-orange,

A:,

etc. which revert t o the colour tones of the original dyeings on a,iring, or in presence of weak hydrogen peroxide.

Azine acid dyeings are reduced easily to colourless compounds, but revert to the original colour when placed in cold tap-water; the re- action liquids behave similarly.

Triarylmethane acid dyeings a,lso are de- colorised, but considerable variation in the degree of resistance to Formosul G is shown by different members of this group of dyes. Furthermore, variation in the ease with which the fully reduced dyeings are oxidised to the carbinol bases by mild oxidising agents,* intro- duces a somewhat complicated problem. As a rule, some of the exceptionally bright blues, greens, and violets are peculiarly prone to give difficulty in this respect, especially when ex- amined in artificial light. When dyes of this type, e.g. Patent Blues, are suspected, the method of examination adopted by the present author is as follows-The dyeing is boiled for &l min. in 5% sodium carbonate solution. The extract may be deeply or only faintly coloured. If the former condition prevails, a small amount of caustic alkali is added to the extract and the liquid boiled until it is either decolorised or acquires a very pale lilac, etc. tint. Glacial acetic acid is then added, drop by drop, until the original colour of the dye develops. If the sodium carbonate extract is only faintly coloured and the dyeing shows a diminution in colour intensity, it is usually found that either addition of a slight excess of ammonium chloride and boiling for a few seconds, or addition of acetic acid, develops the original colour of the dye.

Acid-mordant Dyes including Dyes contairhg a Co-ordinated Metal-A large number of the azo compounds in these groups are very resistant t.0 the action of Formosul C,; for ex- ample, most of t,he red and black “cIvon~e” dyeings can be distinguished from ordinary azo acid dyeings by this difference in behaviour. Preliminary boiling with 16% hydrochloric acid, however, breaks up the lakes of all azo metal- liferous dyes on wool, and, in most cases, there is sufficient of the metal-frec dye left on the sample, after rinsing well, to enable the analyst to detect easily t,he presence of the azo group. Similar tests hold good for metalliferous dyes on silk, although, in some cases, it may be necessary to use more highly concent,rated hytlrochloric acid than that recommended for uoo1 dyeings and to boil for a longer period. Thus, R Neolan Pink B dyeing on Tussah silk is extremely diffi- cult to reduce; boiling for 4 min. in 3096 hydro- chloric acid is necessary to eliminat,e the metal from the lake. A more satisfactory t,est is carried out as follows-The sample is warmed in ethyl- enediamine for & to 1 min., when a considerable portion of the dye is dissolved from the fibre

* After rednetion with Forinosul Ci the pattern Is washed well i n cold water and placed in Drvrloper’O. all leiico-compounds of triarylmethane acid dyes revert to the brivinal rolnur tonen of the dyeings and prints on gently warming the solution.

180 CLAYTON-“IDENTIFICATION OF DYES ON TEXTILE FIBRES’ .VaU 1937

without alteration in colour; on addition of a little sodium hydrosulphite, permanent decolorisation of the solution takes place almost immediately, especially on warming. The chromium lake of the triarylmethane mordant dye, Eriochrome Azurol B, behaves like an oxazine dye after reduction, i.e. the original colour tone is restored quickly on airing or by tap-water, although the reversion does not occur so rapidly, and the inten- sity of the restored colour is not so pronounced as in the case of an oxazine dye. This distinctive behaviour seems to indicate that the chromium in the molecule is present in the form of an 0-co- ordina,ted colour-bearing link, since the reduced non-chromed dyeing behaves like those obtained from ordinary triarylmethane dyes, i.e. mild oxidation with w c e n t oxygen is needed to develop the p-quinonoid coloured structure.

Substantive Dyu on Wool and Silk-Almost all substantive dyes on wool, whether after- treated or not, can be detected by boiling the dyeing in 5% sodium carbonate solution for about min. in presence of white cotton; the latter is stained readily, especially if allowed to remain in the cooling liquid, and little action occurs on boiling the stained cotton in 1% ammonia. Substantive dyeings on silk may be distinguished from acid dyeings in a similar manner, although in the cme of this fibre, it is best t o use 610% caustic soda solution. Even F’rimuline Red on silk, stains white cotton in this test. Some exceptions to this general test are the azo dyes of the Coomassie Navy Blue and Black, or Sulphoncyanine, types. These are generally applied to wool and silk from neutral or very slightly acid baths, but, although closely allied to substantive azo dyes in chemical structures, they stain white cotton in this test to a comparatively slight extent. Identification of dyeings of this type, however, may be achieved by boiling the wool dyeings in 1% caustic soda solution when a dull, yellowish colour resulk8 A somewhat similar effect, except that the fibre is not disintegrated, is obtained with both wool and silk dyeings on boiling with 50” Tw. sodium bisulphite. The possibility of the presence on wool of other dyes sensitive to the action of a mild alkaline reduc- ing agent, viz. wool in presence of boiling alkali, should be borne in mind in carrying out the foregoing test.

Vat Dyes 012 Wool and Silk-These are indicated by more or less pronounced colour changes on heating the samples in the standard reducing agent. I f excess of the latter is then removed and the pattern washed twice in nearly boiling water, the original colour tone of the aample is restored; the addition of a little 3% hydrogen peroxide to the last rinsing water facilitates this reversion. In many cases, the reducing solution obtained by heating the wool dyeing in 1% caustic soda solution is sufficiently strong to form the leuco-compounds of certain

vat dyes, especially those of the indigoid series, and use may be made of this action in the differentiation between various members of the vat dye classes. The leuco-compounds obtained by the caustic soda-wool method, quickly revert to the parent dyes; if, e.g. a few drops of a “vat” formed in this way are poured on to filter paper, the colour of the parent dye is produced almost immediately. Vat dyeings on wool produced via Indigosol, Soledon, etc. dyes, often contain chromium; traces of this metal may be present also in similar d o u r effects, either prints or dyeings, on silk or cotton.

The remarkable action of ethylenediamine on most classes of dyeings and prints affords a simple, hut excellent, means of removing them as solutions from the fibre for further examination. In suitable cases, dyes on wool and silk are cwiverted into their leuco- compounds, whilst in other cases, more or less complete dissolution and removal of the dye tak6 place. A detailed examination of this reagent as regards its behavioiir towards the various classes of textile dyeings and prints ia being made by the present author, as it seems probable that ethylenediamine may prove to be a valuable addition to the somewhat limited number of reagents at the disposal of the average dye chemist, whilst its possible future use for stripping dyes in large scale work is not to be ignored. Indigo, its halogeno-derivatives and many other indigoid dyes on wool are reduced to their leuco-compounds on standing for a short time a t room temperclture, and almost instantaneously on heating to nbout 60°-600 C . . in presence of ethylenediamine. A considerable amount of dye appears to be removed first by dissolution, RO that a comparatively strong vat is formed, but sufficient Imro-compound is invariably left on the fibre to give the usiial colour-reversion effect on oxidation. This reversion effect is seldom a rapid one when the oxygen in water is uRed to produce it (distinction from oxilzine dyes, etr.), but i4 farilitated by pouring the reaction mixtiire into Vat, Dye Developer.

Azoic Dyes on Wool and Silk-The presence of azoic dyes on wool and silk ia suspected when the results obtained in testing for the iisultl classes of dyes are negative. Hot ethylene- diamine extracts of the patterns are decolorised readily and permanently by sodium hydrosulphite (distinction from vat dyes). Most nzoic dytax on wool and xilk yield sliniy residues of the same intense colours as the original dyes on boiling patterns in 5% and 10% caustic soda solutions respectively (distinction from acid-mordant and mordant dyes), and most yellow dyeingx and prints change to orange or red rolours

IDENTIFICATION OF DYES ON CELLITLOSIC FIBRES Ba&c Dyes on Various C!elluIo&r F ibm-

The patterns are boiled first wit8h caustic nods

.Wau 1957 CLAYTON-“IDENTIFICATION OF DYES ON TEXTILE FIBRES” 181

solution; the dyes are then transferred to wool as originally suggested by Greens, but instead of using the “saline caustic soda” method, the fol- lowing procedure gives excellent results and there is no need to touch the pattern in the boiling tube until the dye has been transferred to wool and’its class determined. The sample is placed in a boiling tube, covered with I C.C. 5% caustic soda solution, and boiled for a few seconds 4 C.C. 5% ammonium chloride solution are then added and the whole boiled again. A piece of white wool is introduced next and the liquid allowed to cool; most of the dye is ‘(taken up” by the wool from the cooling liquid.

Substantive Dyes on Cellulosic Fibres-Bac- tically all dyes of this class, whether after- treated or not, are stripped to a considerable extent on boiling for min. in 5% caustic soda solution. (In a few cases the colour of the dyeing alters distinctly or much of the colour may be discharged). If a little white mercerised cot- ton is then added to the extract, a fair amount of dye is absorbed by the cotton from the cooling solution and this dye is not stripped by boiling 1 yo ammonia. The readiness with which stripping in 5% caustic soda solution takes place and the degree of stripping, as judged by the depth of colour of the solution, are important clues in helping the analyst to distinguish between straight dyeings and those which have been after-treated. Primuline, after-treated with bleaohing powder solution, and several coupled, and diazotised and developed dyeings are ex- amples of substantive dyeings which are only slightly affected by 5% boiling caustic soda solu- tion; some patterns change colour; others yield solutions differing in colour from the patterns, and white cotton is not, or only very slightly, stained in the cooling liquids. In cases where it is desired to prove conclusively that the dye present ix substantive to cellulose, a pattern is shaken for some time with a little cold ethylcne- dinminr, the roloured extract diluted with water, 11 hit,e cotton introduced, the solution heated to 80” C., 5 little common salt added, and the whole allowed to cool. The cotton is stained and the htain is not removed by boiling 1 yo ammonia.

During recent years a few substantive dyes which give straight shades of exceptional fast- ness to alkalis have been introduced. Amongst these, dyes giving pale blue dyeings are the most important,, e.g. Swius Supra Blue PFRL Rigan Sky Blue G, etc. Pale dyeings of these products on cotton and viscose rayon are not appreciably affected by boiling 5% caustic soda solution. They are stripped white, however, in about hr. by cold ethylenediamine. Rigan Sky Blue G dyeings change to red on boiling in Formosul G, but the colour reverts to the original colour tone in presence of alkali and tap-water. A dyeing of Sirius Supra Blue FFRL is decolorised on boiling in 1% caustic soda solution containing a little sodium hydrosulphite, but the white material de- velops the original colour tone on rinsing well in

tap-water. Apparently, dyes of this type belong to the dioxazine series. In some cases an azo group or an anthraquinonoid ring may also be present in members of this and related new classes of substantive dyes. As a rule most sub- stantive dyeings are decolorised readily by boil- ing Formosul G. Some members of the diazo- tised and developed series are best boiled in 5% caustic soda solution to which a little sodium hydrosulphite is added. This procedure also should be adopted with discharge and resist prints on cotton and rayon; a pattern containing both ground and illuminating dyes should be boiled in the reagent until decolorisation and/or colour changes ofeach portion have occurred; the pattern is then rinsed and placed in Vat Dye Developer. Vat dye discharges on diazotised and developed azo dyeings are detected readily in this way.

The possibility of the presence of a few diox- azine substantive dyes on viscose rayon dyeings should not be overlooked.

Sulphur Dye8 on Cellulosic Fibres-Patterns are boiled for & min. in 16% pure hydrochloric acid and the liquid cooled. A few chips of pure magnesium are added, the tube covered with filter paper saturated with lead acetate or mercuric chloride solution, the reaction allowed to continue for a few minutes and the test paper examined for the presence of lead sulphide or mercuric sulphide. The usual reduction test generally gives a nearly colourless product which reverts at once in presence of tap-water to the colour tone of the original dyeing (dis- tinction from most vat dyes). Dyeings of the Indocarbon Black type are not decolorised on boiling in 3” Tw. sodium hypochlorite solution, and they yield reddish solutions (which revert immediately to the original colour tone on diln- tion with water) on boiling with ethylenediamine. Ordinary Sulphur Black dyeings yield .greenish solutions when treated in the same way. Sub- stantive dyes containing thiazole rings, and also vat dyes Containing twlphur, evolve hydrogen mlphide when reduced with hydrochloric acid and magnesium as described above. Some of the brown sulphur dyes are exceedingly difficult to reduce, but they are distiiiguiuhed by their Renxi- tivity in presence of boiling dilute sodium hypochlorite.

dzoic Dyea on (’e.!lulosic Fibres-Most of these are reduced to colourless or yellow com- pounds by vigorous boiling in Formosul G , especially in presence of a little caustic soda. If no signs of reduction appear after boiling for 1-2 min., the sample is placed in boiling 5yo caustic soda solution to which a little sodium hydrosulphite is then added. All azoic dyeings, including the yellow dyes fkom Naphtol AS-G, are reduced completely by this method. A re- agent consisting of equal volumes of 10% caustic soda solution and the monoethyl ether of ethyl- ene glycol is recommended in place of 5% caustic soda solution when examining dyeing

182 CLAYTON-"IDENTIFICATION OF DYES ON TEXTILE FIBRES" Jlau 1937

on viscose rayon. Most azoic dyeings are quickly attacked by cold 60-70% ethylenediamine, and this method of testing is used in the Tables. If the intensely coloured solutions are diluted with water and boiled for a few seconds they become turbid owing to separation of finely divided pig- ments; in some cases, the suspensions exhibit fluorescent effects and all of them yield flocculent coloured precipitates on standing. Azoic dyes in warm ethylenediamine solution are readily re- duced on addition of a few drops of water and a little sodium hydrosulphite. The absolute identification of individual azoic dyeings and prints is rendered possible by an extension of the method described by Rowe and Levine.

Vat Dye8 on Cellulosic Fibrea-These generally give positive colour reactions on boiling in Formosul G, especially in presence of a little caustic soda; the original colour tones are restored either dowly or readily. The use of very hot rinsing water facilitates the change, whilst in some cases the addition of a few drops of hydrogen peroxide is effective. '(Vats" may be produced by heating the dyeings a t about 60" C, in 5% caustic soda solution to which a little sodium hydrosulphite is added; white cotton can be dyed in the vat, whilst the original colour is developed a t once if the contents of the tube are poured into an equal volume of Vat Dye Developer. Vat dyeings and prints may be distinguished quickly from azoic dyeings and prints by their negative or com- paratively slow reactivity (in most cases) in pres- ence of cold ethylenediamine.

Some specific reactions of individual vat dyeings have been published by Green and Franks, Budel, Vajols, Jones and Kilby7, and Herzoge.

ACTION OF ETHYLENEDIAMINE ON VARIOUS CUSSES OF DYEINGS AND PRINTS

References have been made previously to the uses of commercial ethylenediamine as a dye- t,esting reagent. It is of especial service in the rapid differentiation between vat and azoic dye- ings and prints on cellulosic fibres. Ethylenedia- mine is one of the most powerful solvents of dyes known, but hitherto its application in this direction appears to have been overlooked. It is now obtainable commercially a t a reasonable price. In addition to its solvent action, the com- mercial product also possesses reducing proper- ties, possibly owing to the presence of organic impurities. A t the same time, the reagent may develop a mild reducing system in conjunction with organic fibrous materials on account of its alkaline reaction and moderately high b.p. of 117" C. A few vat dyes, both on wool and cotton, yield leuco-compounds when treated for some time with the cold reagent, but most anthraquin- onoid dyes on cellulosic fibres are only slightly affected; these are removed, however, more or less completely, either by direct dissolution in

t.he reagent at or near its b.p., or i n solution as their leuco-derivatives, I n the l i i f k r case, SUE- cient leuco-compound is genrriilly left on t lie fibre to indicat,e the nature of t,hv dyeing by tlie usual re-oxidat,ion test. For exii.nlple. w 20" Caledon Jade Green XS dyeing on cotton loses much dye on boiling in t.he reagent for f to I niin. and the solution is the same colour as t,he dyeing. A medium dyeing of Caletlon Brilliant Purplc 2R is &ripped completely when treated in a. Yimilar manner. Some samples of cwniniercinl ethylenediamine appear to be slightly mow efi- cient than ot,hers in ttheir action on \ T i i t , dyes itnrl it is best, therefore, t,o ndd a litt,le glucnse to the reagent when testing for vat dycs on cotton. et,c. All vat dyeings and prints yield leuco-coitipoiinds readily when treated in this way.

One of the most import,a.nt properbies of the reagent is its power of dissolving from wool i d silk fibres some of the fast,est co-ordinated chromium lakes, e.g the chrorniuni lakes of Eriochrome Black T Supra, a.ll tlie h'ro1a.n dyes, etc. The first named dyeing is capnblc of wit.h- standing considerable boiling in 1606 hydro- chloric acid without any sign of dye being removed, but it. i R attacked rapidly by ethylcne- diamine; indeed, the action appears t.0 prcccdc the hydrolytic action of the reagent on the wool fibre. Also the cold reagent exerts a distinct action on dyeings of this type, especially on standing for some time.

Most rtienibers of other classes of tiyes a.re removed from different fibrous materials by t,he powerful solvent action of et.liylenediamine. The actions in all cases are extraordinarily rapid, whilst such fibres as wool and silk a.re gradiia.lIy disintegrated. Substantive dyeings on cotton and rayon are stripped readily, many of thrm in the cold; a dark shade of Primuliiie R . 4 is stripped by the boiling retigent, to a piiler yellow shade than the original Primuline dyeing. Basic dyes also are dissolved r e a d y and most sulphnr dyeings are stripped.

Another powerful solvent appa.rently obt.ainetl as a by-product, in the manufacture of et11ylcn~- diamine is known commercially as Tetriimine.* It is amixt,ureof condensed low nioleciilar \wiglit., a.lkylenediamines, and idao ront.nins imino- compounds, etc. It has3(r400/btiva,ila.blenitrogen which is slightly higher than t,he amount. in ethylenedia.mine. Its odoir resembles a mixt,urc of acetamide mid aldehyde ammonia. The init,ial b.p. is 178" C. Tetramine strips all v i~t dyeing8 on heating, including indant.hrone and its drrira- tives. A mixture of 3 part,R etliylenediiiriiine n r ~ l 1 part Tetramine acts in i L siiiiilar wa.y; iLzoi(* dyeings also are stripped re~lily. There is no need, however, to ut,ilise Tctriirninc i n dye testing. Basic-nwrda~t Oyes-The iiienibers oft his chss

are confined mainly to gidlocyiulinP deriv i1 t t v w , .

' l ' t i ~ r-iiniiwrvial ~ ~ t i t ~ l ~ ~ t ~ ~ ~ ~ l i ~ i ~ ~ i i ~ ~ ~ ! i u l i l 'r1.t n i l l i i l l , , m q I t i ~ ~ t i ~ ~ < l I n the t e x t were iiianufacturcd by Curbide and < ' : I ~ ~ I ~ I I I ctitmiic:iis C'ori)ornt ion.

~ ~~~

May 1037 CLAYTON-“IDENTIFICATION OF DYES ON TEXTILE FIBRES” 183

etc. They are not often found on wool and silk dyeings, but are of considerable importance in printing, especially calico printing. They are u w t l l y fixed as purple and blue chromium lakes. Their weakly acid solutions do not yield pre- cipitatcs with tannic acid, whilst their chromium hkcs on cotton are easily broken up by boiling 5?& hydrochloric. acid. If the acid solution is made slightly alkaline with concentrated am- monia, and any excess of the latter removed by addition of a little solid magnesium sulphate, it will be found that white wool is stained deeply in the cooling solution.

ill ixture Dye ings-Chroma togru phic A dqorpt ion Tests-An regards mixture dyeings, i.e. colour effects produced with two or more dyes, it is usually practicable to strip a fair amount of the dyes with boiling mild alkali, or other suitable reagent, and then to separate the individual dyes by means of the filter paper capillary test. During recent years, this and other adsorption methods have been developed, mainly in eonnexion with bio-chemistry, to such an extent that the latest practice in this work may prove to be of considerable use to the dye chemist in the separation and identification of dyes contained in dye mixtures or dyeings. The filter paper adsorption test i H too well-known, of course, to need nny description. The chromatographic adsorption method, which is said to be far more efficient than the older method, is carried out as follows-

Procedure-In making a chromatogran?, i.e. zones of separated colouring matters, advantage is taken of the differential adsorption which occurs when a solution of several dyes is allowed to drop on to a column of adsorbent, and the column rinsed (“developed”) with a pure solvent which may be the original or a different solvent. The adsorbent mixture undergoes innumerable elutionH and re-adsorptions from particle to particle, thereby causing the individual dyes to pass downwards at varying rates, through the adsorbent, so that distinct coloured zones, each corresponding to a constituent of the original mixture, are obtained. The subsequent

steps in the analysis consist in the isol- ation of the coloured constituents in the zones, either mechanically or by elutria-

:--- tion with the aid of selected solvents. --:-. The method was introduced by TswetP --: in attempting to solve problems con- ,< cerned with the functions of chlorophyll <-- in living plants. According to Zech-

meister14, one of the simplest forms of apparatus consists of a small tube containing the adsorbent (see Fig.); attached to this is a flask with suitable I! connections designed to enable tho dye

solution to be drawn through the adsorbent by slight suction or a srnall dropping funnel may be rtsed. A special type of aluminium oxide (Brock- niitnri’s) made by Merck, is considered to be the rno~t sutkfactory adsorbent for use generally in

chromatographic analysis. The tube is filled with a creamed mixture of this material and solvent, the latter being removed subsequently by slight suction, the column of adsorbent being kept covered with solvent during the analysis. Suitable solvents are water, ether, chloroforrn, petroleum, etc. whilst alcohol, pyridine, acetone, etc. may be used for elution, although the original solvent, to which a small quantity of another solvent has been added, is capable of breaking the adsorbent-adsorbate complex. The method is not restricted to the separation of coloured substances.

Ruggli and Jensenll used water and pyridine as solvents in the separation of dyes by activated aluminium oxide. The method was found to be far superior to Goppehroeder’s method of absorption by filter paper, and to fiactional dyeing methods. A large apparatus suitable for effecting separation of dyes in 1-2 hr., was used. These authors observed that, in many cases, a distinct connexion exists between adsorption, affinity towards cotton, and velocity of diffusion through gelatin. Water-soluble o-hydroxyazo dyes were found to be ndsorbed better than the corresponding p-isomerides.

The new Tables have been developed from the results obtained in the examination of a very large number of dyeings and p@ts, and may not yet be perfect. They will be extended later by the inclusion of Tables dealing with the identification of dyes on cellulose acetate fibres. It is hoped that the various new methods which have been advanced, as well as the schemes as a whole, may be helpful to those concerned with the identification of dyea on the fibre, and form a sound basis for further improvement and enlargement.

In Conclusion, the author desires to thank Professor F. M. Rowe for advice and assistance in arranging the matter in the Tables. DEPARTMENT OF DYEING

TECHNICAL COLLEGE BRADFORD

REFERENCES I Bude, Melliand Textilber., 1924, 6, 602. * Cook (Chm. and I d . , 1930,65,7%1) gives an account

with references of most of the work accomplished in this field.

Green, The Analyai.9 of Dyecrtufl.9, London: C. Griffln & Co. Ltd., 1916.

Green, Yeoman, and Jones, this Jour., 1906. 21, 236; Green, Yeoman, Jones, Stephens, and Haley, ad., 1907, 28, 252.

Green and Frank, ibid., 1910.26, 83. a Henog, Reactionstabelk der Kiipenfarbatofe, Basel,

Jones and Kilby, this JOUT.. 1925, 41, 127. Rowe and Dangerfield. ibid., 1936, 62, 55. Rowe and Levin, ibid., 1924, 40, 218.

1933.

l o The Colour Itauk. edited by F. M. Rowe, Bradford,

l1 Ruggli and Jensen, Helv. Chim. Acta, 1935, 18, 624;

Tewett. Bw. Dezltmch. Bot. ffea.. 1000, 24, 318, 884. Is Vajs, Mellinnd Textilber., 1027, 8, 01 1. I4 Zeohmeister, Annulen, 1934, 609, 209.

Sooiety of Dyers and Colourists, 1024.

1936, 19, 04.

TABL

E I

(RED D

YEX

NCS

AN

D PRINTS)

IDE

NT

IFIC

AT

ION

OF

DY

ES

ON

WO

OL

, S

ILK

, A

ND

RE

LA

TE

D

FIB

RE

S

-

The

dye

ing

or p

rint

is

boile

d fo

r 1-

2 m

in.

in d

ilut

e am

mon

ia (

cf.

Rea

gent

s, p

. 17

9).

in p

rese

nce

of w

hite

cot

ton.

The

sol

utio

n is

col

oure

d di

stin

ctly

. T

he c

otto

n is

not

sta

ined

-Aci

d Dy

e.

A f

resh

pa

tter

n is

boi

led

for

1-2

min

. in

Fo

mo

sul

G.

A li

ttle

dy

e is

ex

- tr

acte

d; t

he t

one

of

the

colo

ur

is

un-

alte

red-

X

nnth

cne

Dye

(Rho

ahm

ines

).

Som

e of

th

ese

e.g.

F

aat

dci

d

Vw

kt

A2R

. ar

e pa

rtly

di

scha

rged

, b

ut

re-

vert

, to o

rigi

nal

col-

ou

r to

nes

in

pres

- en

ce o

f 3O

;, hy

dro-

ge

n pe

roxi

de.

The

pa

tter

n is

dec

olor

- is

ed;

orig

i-

nal

colo

ur

is

rest

or-

ed b

y ta

p-

wa

ter

-

Azi

nc Dy

e.

tt

The

pat

tern

is

deco

l-

oris

ed; o

rigi

nal c

ol-

our

is r

esto

red

by

Dev

elop

er 0

- T

riar

ylm

etha

ne

Dye

.

"his

is

con

firm

ed

by b

oilin

g a

fres

h pa

tter

n fo

r 9 min.

in 5

% s

odiu

m car

- bo

nate

so

luti

on,

whe

n pa

rtia

l or

co

mpl

ete

deco

lori

- sa

tion

occ

urs ;

ori

- gi

nal

colo

ur i

s re

- st

ored

on

ad

ding

ex

cess

5%

am

mo-

ni

um c

hlor

ide solu-

tion

and

boi

ling

for

a fe

w seconds.

-

The

pat

tern

is

deco

l-

oris

ed p

erm

anen

tly

or

chan

ges

to p

ale

yello

w-A

m

Dye

.

Cer

tain

red

, sc

arle

t, an

d or

ange

sha

des,

e.

g. th

ose

prod

uced

by

Po&

. Su

pran

ol,

etc.

, dy

es,

areo

nly

sl

ight

ly a

ffec

ted

by

boil

ing

1% a

mm

o-

nia

and

are

re-

duce

d by

bo

iling

Fo

rmos

ul

G

firs

t to

com

para

tive

ly

sta

ble

y

ello

w

shad

-,

whi

ch

are

deco

lori

sed

only

by

vigo

rous

boi

ling

in

this

rea

gent

.

__

__

_

The

patt

ern

is c

hang

ed

t,o

yello

w

whi

ch.

re-

vert

s sl

ow-

ly .

to

the

ori

gin

al

colo

ur

in

wat

er

or

air - &

p

thra

quin

- on

oid Dye.

The

solu

tion

is

not,

or

only

ver

y sl

ight

ly, c

olou

red.

Th

e co

tton

is

not

stai

ned

(Mor

dant

, Ac

id-m

orh

t, o

r V

at

Dye),

or m

ay b

e st

aine

d (S

ubst

anti

ve Dye).

A f

resh

pa

t.te

rn is

boi

led

for

1-2

min

. in

For

mos

ul G

.

The

Dat

tern

is la

) dec

olor

ised

Der

- I Th

e pa

tter

n un

derg

oes a

dist

inct

or

sli

ght

colo

ur c

hang

e: o

rigi

nal

-1

m

inen

tly*

l- A

zo

Aci

d-m

or-

dan

t or

Azo

Sub

stan

tive

Dye ;

or

(a) i

s ch

ange

d to

yel

low

or

yello

wis

h-br

own,

whi

ch r

ever

ts

to o

rigi

nal

co

~o

ur*

* in

pr

es-

ence

of

3O,

hydr

ogen

pe

r-

Ant

hraq

uino

noid

ox

ide -

Mor

dant

Dye

; al

so C

ochi

neal

S

corl

el.

Tee

ts f

or a m

orda

nt

are

appl

ied.

A m

orda

nt i

s ' A

mor

dant

is

not

mes

ent-

or

esen

t-

(ajA

zoA

eid-

(a

j AZO

Subs

tan-

m

or

da

nt'

ti

ve D

ye.

Dye

? or

1 This

isc

on

h-

(b)

Ali

zar-

ed

by

boil

ing,

a in

R

e d

R

fres

h pa

tter

n in

and

Mar

- I

5% so

dium

car

- O

Ofl

R.

bona

te s

olut

ion

in

pras

enre

of

w

hite

co

tton

; 1

the

cott

on

is

stai

ned

dee

ply

colo

ur

is r

esto

red

mor

e or

-les

s re

adil

y by

air

, ts

p-w

-ate

r, o

r 30

, hy

drog

en

pcro

xide

- V

at D

ye.

Chr

omiu

m

may

be

pr

esen

t in

so

me

woo

l dy

eing

s pr

oduc

ed u

ia

Indi

goso

l, S

olet

lon,

et

c.,

dyes

. T

race

s m

ay b

e pr

esen

t in

cor

re-

spon

ding

silk

dye

ings

and

pri

nts.

A

va

t dy

eing

is

conf

irm

ed

by

heat

ing

a fr

eah

patt

ern

in e

thyl

- en

edia

min

e;

man

y dy

es

yiel

d le

uco-

com

poun

ds

at

abou

t 70

' C

.; ot

hers

are

cha

nged

in

colo

ur

on b

oilin

g; o

r are

part

ly or

com

- pl

etel

y st

ripp

ed.

Exc

ess

reag

ent

is r

emov

ed

and

Vat

D

ye

De-

ve

lope

r ad

ded

whe

re n

eces

sary

-O

rigi

n81

colo

ur

tone

is

re

- s t

ore

d .

ttC

f. f

ootn

ntr

niar

krd

in T

ahlr

111

.

SW

s 4

1)

Ba-

ic

red

clyr

s C

IU

woi

il an

d si

lk

give

de

eply

'M

nns

am a

cid-

mor

dant

dye

s 01

1 w

nrd

an

d si

ili.

part

iriil

arls

**

('w

liillr

aI S

varl

rt 0

11 t

in i

ii~Ir

daIi

t ir

not

rrst

on~d

to o

rigi

nal

roln

iired

sol

utio

ns o

n lm

iling

in

Lo,

aert

ir a

cid,

or

in a

lroh

ol.

the

reds

and

bla

cks,

arc

ver

y di

ffir

ult

to r

educ

r.

III

siw

h ('KQ(.P.

vh

ur

by

c~xi

dlsi

og n

gm

ta.

Tli

ry n

rn. i

drnt

iflr

d zq ii

idir

etrd

In T

able

VII

I.

Bas

ir a

zlnp

dye

%

the

patt

ern

is b

oilr

d fo

r t

inin

. in

16

% h

rdro

rhlo

rir

iu.id

. ri

nsri

l r.

g. S

afra

ii1nf

.s. R

hofl

ulin

e R

cdz,

etc

. ar

e ch

ange

d to

urr

rn h

y w

ell.

and

boile

d in

Fornimul

G.

wh

tii

~~

'rn

~a

nen

t cl

c~co

lori

s~~t

iol~

t.4

fw

(lyt

s cd

thr

suh

st;r

nIiw

~o

ncc

ntr

atcd

siilp

hiir

ir w

id.

Tri

aryl

met

hane

dye

s. e

.g.

Mag

mta

tx

kes

plac

r rr

adily

. A

ra

pid

test

is

LUI

fnlI

nws-

Tli

~~ d

yvit

ln i

? ar

t' H

xtd on u

1~

11

ait.

h ch

ronl

c.

arr

drro

lori

acil

hy F

orni

o$ul

G

but

the

orig

inal

col

our

i8 r

wto

rrd

heat

ed f

or +

min

. or

Irs

n in

etl

iylr

nrdi

aini

nr a

nd t

hrn

a lit

tlr

arid

-nio

rila

iit d

vi.in

g* h

y Ii

nilin

u on

ly h

? w

ti\r

. (t

xsur

n. (

Thr

y'sr

c se

ldom

fou

nd n

n u'

nid.

hut

art

' sn

diiim

hy

ilros

ulph

itc

addr

d to

thr

rlw

ply

rnlo

ur~v

l rxt

rwt:

w

hit(

, riit

t<m

. T

hv f

oriw

r st

ain

used

to

A

niot

lrm

tt*

i'xt

rnt

or1 l

iilk.

) pe

rman

rtlt

dtw

hrim

ticm

O

~I'

UT

B al

mos

t in

imr~

liat

rly.

(2

) The

pnl

yiiir

thir

rr t

insi

r dy

e.,

Ast

iap

hld

ne

FF

, is

,lc

tr(.

tr(l

as

indi

cate

d ii

i T

able

YII

I.

TAB

LE I

1

(OR

AN

GE

AN

D Y

ELLO

W D

YEI

NG

S A

ND

PRINTS)

IDE

NT

IFIC

AT

ION

O

F D

YE

S

ON

WO

OL

, S

ILK

, A

ND

R

EL

AT

ED

F

IBR

ES

__

_. _

__

_

-

The

dye

ing

or p

rint

is

boile

d fo

r 1-

2 m

in. i

n di

lute

am

mon

ia (

cf. R

eage

nts,

p.

179)

in p

reae

nce

of w

hite

cot

t,on.

chro

mem

or-I

O

ran

ge

(@

- da

nt.

nitr

oali

zari

n)

alum

in-

The

sol

utio

n is

col

oure

d di

stin

ctly

. The

cott

on i

s no

t st

aine

d-A

cid

Dye.

A f

reeh

p

atte

rn is

boi

led

for 1

-2m

in. i

n F

orm

osul

G.

' 1 T

he s

olut

ion

is n

ot, or o

nly

very

sli

ght.l

y, co

lour

ed. Th

e cotton is

not

sta

ined

(M

orda

nt, A

cid-

mor

d.nt

, or

V

at D

ye),

or

may

be

stai

ned

(Sub

stan

tive

Dye).

A f

reeh

pat

tern

is

boile

d fo

r 1-

2 m

in.

in F

orm

osul

G.

tern

w

ith

5

%

eodi

um

carb

onat

e an

d w

hite

cot

ton;

The

pat

te

rnis

no

alte

red-

Quino

line

Pel

low.

t'he

patt

ern

is d

ecol

orie

ed p

erm

anen

tly-

A

zo D

ye*;

(al

so N

apht

hol

Yeua

O S

).

Py~

awlo

ne Pe

Uow

Dye

ing

8 ar

e ei

ther

not

&ected,

or

are

chan

ged

to

dull

er

shad

es by

co

ld c

once

ntra

ted

hydr

o-

chlo

ric a

cid;

Ora

nge I

I dy

eing

s cha

nge

to re

d; a

nd

Nap

uhol

Yeu

aV S d

yein

gs

are

deco

lori

sed.

Dye

ings

of

the

Pda

r Ye

&w

type

are

dis

ting

uish

ed a

s fo

l-

Iow

a-A

pa

tter

n is

bo

iled

fo

r 2-3

min

. in

1%

am

mon

ia, a

nd

a li

ttle

20%

m

agne

sium

sul

phat

e so

luti

on a

dded

; w

hite

woo

l is

stained p

ale

yello

w o

n bo

iling

in t

he

solu

tion

for

1-2

min

. an

d

allo

win

g it

to

rem

ain

in t

he

cool

ing

liqu

id.

The

patt

ern

unde

rgoe

s a

slig

ht (

A) o

r di

stin

ct

(9) c

hang

e .in

col

our.

A

m

orda

nt

may

he

pr

esen

t.

Mor

dant

pre

sent

M

orda

nt a

bsen

t

The

p

atte

rn

unde

r-

goes

a p

rono

unce

d ch

ange

in

co

lour

w

hich

is

m

tow

d

by a

ir o

r V

at D

ye

Dev

elo

p e

r-Va

t

Chr

omiu

m

may

be

pres

ent

on

woo

l dy

eing

s (c

f.

also

th

e la

at c

olum

n of

T

able

I).

Dye

.

The

pat

tern

is d

ecol

oris

ed p

erm

an-

ently

-Azo

Dy

e (c

f. fo

otno

te

mar

ked

* in

Tab

le I).

A f

resh

pat

- te

rn i

s bo

iled

for

+ min.

wit

h 5%

so

dium

ca

rbon

ate

solu

tion

an

d

whi

te c

otto

n, a

nd a

llow

ed t

o co

ol

in t

he

liqu

id.

rhe

cott

on

is

not

stai

ned;

a

mor

dant

is

pm

nt

-

Aci

d-m

or-

d

ant

Dye

.

The

cot

ton

is s

t.ain

ed

deep

ly - S

ubst

an-

tive

Dye.

(Cop

per o

r ch

rom

ium

is

not

usu

ally

pre

a-

en

t in

y

ello

w

and

or

ange

su

b-

stan

tive

dye

ings

).

~~

* C

erta

in n

ltza

ted

azo

dves

, e.

g. I

ndia

n Y

ello

w

OT

Clt

roni

ne

Not

c-h

ic

oran

ge a

nd yellow

dyri

ng-8

of

the

arri

dine

cia

en

ue 0

cd

01

~U

y ored

In lr

atbe

r and

silk

dye

ing.

Tb

eg a

re re

duce

d ar

e at

rfpp

ed to

a co

nsid

crab

le r

xten

t b

y 5%

are

tic

arid

or by

d

v.

patte

rn8

chan

e to

dee

br

ight

red

whe

n tr

eate

d w

ith

con-

al

coho

l. C

old

conc

entr

ated

su

lphu

rir

arid

pi

rrr

fluo

rrec

ent

c&&

ed

hydr

ochl

or8

or su

lpR

uric

aci

d. o

r w

ith

5% c

anst

lc s

oda

(gre

en)

Rol

utio

nn w

ith

thrn

e dy

es:

(cf.

slw

Tnb

lc IX.)

solu

tion

.

The

sol

utio

n is

col

oure

d di

stin

ctly

. T

he c

ot.to

n is

not

sta

ined

- A

cid

Dye

. A

fre

sh p

atte

rn is

boi

led

for

1-2

min

. in

For

mos

ul G

.

The p

att

ern

ch

ange

s t,o

or

ange

- yel

- lo

w; o

rigi

nal

colo

ur

tone

is

rest

ored

by

3%

hydr

o-

gen

pero

xide

-A

nt

br a

- q

uin

onoi

d

Dye

.

The

sol

utio

n is

not

. or

onl

y v

ery

sli

ghtl

y, c

olou

red.

T

he c

otto

n is

not

sta

ined

(M

orda

nt,

Aci

d-m

orda

nt,

or V

at D

ye),

or

may

he

stai

ned

(Sub

stan

tive

Dye

). A

fre

sh p

atte

rn i

s bo

iled

for

1-2

min

. in

For

mos

ul G

.

The

pat

tern

is d

ecol

oris

ed.

Th

e p

att

ern

ch

ange

s to

r

e d

d i s

h -

brow

n;

iron

is

pre

se

nt

Ant

hraq

uin-

on

oid

Mor

d-

ant D

ye,

e.g

. Alizarin,

etc.

, on

iro

n m

orda

nt.

The

or

igin

al

colo

ur is

re-

st

or

ed

qu

ickl

y by

ta

p-w

ater

- *

Az

ine

, 0.

qZin

e. or

T

ha

azi

ne

Dye

.

Th

e p

att

ern

c

ha

ng

es

sl

ight

ly

or

unde

rgoe

s a

pron

ounc

ed

c o

1 o

u r

chan

ge;

the

orig

inal

col

- ou

r is

re-

sto

red

on

ai

ring

or

by

Vat

Dye

De-

v

elo

pe

r -

Vet

Dye.

C h

ro

miu

m

may

be

pres

- en

t on

woo

l dy

eing

s (c

f.

als

o

las

t co

lum

n

of

The

or

igin

al

colo

ur

is

rest

ored

by

Dev

elop

er

0 t-

Tri

eryh

eth

me

Xa

h th

ene

Dye

! e.

g.

Qal

ban.

DY e.

Thi

s IS

co

nfir

med

by

bo

iling

a f

resh

pat

tern

fo

r 4

min

. in

5%

so

dium

car

bona

te s

ol-

utio

n, w

hen

part

ial

or

com

plet

e de

colo

risa

- ti

on

occu

rs;

orig

inal

co

lour

is

rest

ored

on

ad

ding

excess

5”/.

am

mon

ium

ch

lori

de

solu

tion

an

d

boili

ng

for

a fe

w s

econ

ds?.

me p

at,t

ern

is

deco

lori

sed ;

orig

inal

col

- ou

r is

re

- st

ore

d

by

ta

p -

wat

er.

A

mor

dant

is

pre

se

nt

hF

ine

. or

T

bie

zin

e

Qal

lncy

anan

e.

be

,

eg

.

t C

f. fo

otno

te m

arke

d **

in

Tab

le IV,

,V

ote-

-Rae

ic

dyei

nas

arc

stri

pprd

to

a ro

nsid

erab

le e

xten

t on

* D

yein

86 o

f th

ese

clas

ses o

n w

oo1

are

usua

UY

rcd

urrd

by

hil

ing

ho

iling

in

50,;

ar

ctic

wid

or

alr

ullo

l. T

hry

are

iden

tifl

ed

as

for

1-2

min

. in

1%

ca

tist

ic s

oda

solu

tion

; re

vrrs

ion

to o

rigi

nal

indi

catc

d in

Tab

le S

. co

lour

tak

ps p

lace

in

pres

ence

of

tap-

wat

er.

rhe

patt

ern

is d

ecol

oris

ed p

er-

man

entl

y - Az

o

Dye

(cf.

fo

otno

te m

arke

d * i

n T

able

I).

A

fre

sh p

atte

rn i

s bo

iled

for

4 m

in.

wit

h 5%

so

dium

car

- bo

nate

so

luti

on

and

w

hite

co

tton

, and

allo

wed

to

coo

l in

th

e li

quid

.

[“ne

cot

ton

is

not,

or

only

s

lig

htl

y,

sta

ine

d;

a m

orda

nt

is

pre

sen

t-

Aci

d-m

ord-

an

t D

ye.

The

cot

ton

is

st

ai

ne

d

de

ep

ly-

Subs

tant

ive

Dye.

(CO

P-

pe

r

or

c

hro

miu

m

may

be

pre-

se

nt).

TA

BL

E IV

IDE

NT

IFIC

AT

ION

OF

DY

ES

ON

WO

OL

, S

ILK

, -f

iD R

EL

AT

ED

FIB

RE

S

(BLU

E D

YEI

NC

S A

ND

PR

INTS

) Slig

ht,

or d

isti

nct

colo

ur

chan

ge

oc

cu

rs

(pa

le

yello

w i

n s

ome

The

dye

ing

or p

rint

is

boile

d fo

r 1-

2 m

in. i

n di

lute

am

mon

ia (

cf. R

eage

nts,

p.

179)

. in

pres

ence

of

whi

te c

otto

n.

The

pat

tern

is

deco

lori

sed

pa

rtly

or

com

plet

ely;

The

sol

utio

n is

not

, or

onl

y ve

ry s

ligh

tly,

col

oure

d.

The

cot

ton

is n

ot s

tain

ed

(Mor

dmnt

, A

cidm

orda

nt, o

r V

at Dye

) or

may

be

stai

ned

(Sab

itu

rtiv

e Dy

e).

A f

resh

pat

tern

is b

oile

d fo

r 1-

2 m

in.

in F

orm

osul

0.

The

sol

utio

n is

col

oure

d di

stin

ctly

. T

he c

otto

n is

not

sta

ined

-Aci

d Dy

e.

A f

resh

pattern i

s bo

iled

for

1-2

min

. in

For

mos

ul G

. I

stor

ed b

y ai

r or

Vat

Dye

Dev

el-

oper

-Vat

Dye.

Chr

omiu

m

may

be

pr

esen

t on

w

ool

dyei

ngs

(cf.

als

o l

ast

c

ol

um

n o

f

Tab

le I

).

A d

isti

nct colour

chan

ge

occu

rs;

orig

inal

co

lour

to

ne i

s restored

gen

pero

nde-

A

nth

raq

uin

o-

no

id D

ye.

(The

c

olo

ur

chen

ge

may

be

yel

low

, re

ddis

h - o

rang

e,

yello

wis

h -br

own,

et

c.).

by 3%

hydr

o-

s t o

re

d b

y

tap-

wat

er.t

-j

A m

orda

nt is

p

rese

nt -

0xa.

zine

. or

T

h I

8 L i n

e

Dye

.

Th

e pa

tter

n is

dec

olor

ised

.

rhe

orig

inal

colour i

s re

- s

tore

d b

y

tap

- wat

er t

-A

z i

n e,

O

uzin

c or

T

hia

rin

e

Dye.

The

or

igin

al

colo

ur

is

rest

ore

d

by

D

evel

oper

O

**-

Tri

ary

l me

tha

ne

Thi

s ia c

onfi

rmed

by

boili

ng f

or 4 m

in.

in 6%

sodi

um car-

bona

te

solu

tion

, w

hen

part

ial

or

com

plet

e de

colo

ri-

sati

on o

ccu

rs; or

ig-

inal

d

ou

r i

s re

- stored

on

addi

ng

exce

m 5

%

amm

o-

nium

chl

orid

e so

lu-

tion

and

boi

ling

for

a fe

w s

econ

ds.

Dye

.

I'he

patt

erni

sdec

olor

ised

pe

rman

entl

y - A

zo

Dye. A

lso

cert

aind

yes

of t

he

azo

clam

whi

ch

are

dyed

be

st

from

ne

utra

l ba

ths,

e.

g.

Coo

mua

8ie

Nae

y B

lues

. D

yein

gs

of

thes

e on

w

ool

are

deco

lori

wd

(yel

low

ish)

on

boili

ng

in

1%

caus

tic

soda

so

luti

on,

bu

t si

lk d

ye-

ings

are

no

t af

fect

ed.

Dye

ings

on

both

fib

res

are

deco

lori

sedo

n bo

il-

ing

for

1-2

min

. in

60"

Tw

. sod

ium

bis

ulph

ite.

Lit

tle

if

any

a

lte

rati

on

oc

curs

;*

a m

orda

nt

is

pre

sen

t -

Ant

hraq

uin-

on

oid

hb

rd-

ant Dye.

__

~

The

pat

tern

is

dec

olo

rid

per

- m

anen

tly-A

zo

Dye

(cf. f

oot-

no

te m

arke

d *

in T

able

I).

A

freah

patt

ern

is

boile

d fo

r 4

min

. w

ith

8%

so

dium

ca

rbon

ate

solu

tion

and

whi

te

cott

on,

and

allo

wed

to

coo

l in

th

e liq

uid.

The

cott

on

is

not,

or

only

s

lig

htl

y,

stai

ned;

a

mor

dant

is

p

rese

nt -

Aci

d-m

ord-

8n

t Dye.

The

cott

on

is

stai

ned

deap

- ly

-~u

bst

an-

tiv

e Dye

or c

hrom

ium

m

ay b

e pre

s-

ent.

).

(Cop

per

and

l

t Cf. f

ootn

ote

mar

ked

* in

Tab

le 1

11.

A'&

-Bas

ic

dyei

ngs

are

stri

pped

to

a ro

nsid

rrab

le e

xten

t by

6

% a

ceti

c ac

id o

r by

alc

ohol

. T

hes

arc

iden

tifl

ed as

indi

cate

d in

T

able

XI.

Mn

B

lue

on c

hrom

ium

mor

dant

cha

nges

to

brow

n, h

ut

orig

inal

col

our

tone

is r

esto

red

on a

lrln

g.

** M

any

redu

ced

dyeings

of th

e tr

tmyl

met

hane

ac

id

g~

ou

p

espe

cial

ly t

hose

Of

the

Pate

nt B

lue

t,ype

, do

not

rev

ert

wil

y td

on

gina

l rm

lour

tone

s in

pre

senc

e of

ver

y di

lute

oxi

diai

og a

gent

s.

Mor

eove

r, s

o1ue

of

thew

dyc

inys

arc

uot

dec

olor

ised

on

boili

ug i

ll

5%

Bod

iuln

car

bona

te s

olut

ion.

T

he f

ollo

win

a pr

ored

ure

is r

ug-

gent

ed i

n su

ch c

ues-

The

dyei

ng is

boi

led

vigo

rous

ly f

or 1

-2 i

iiin.

in

5 c

.r.

5% s

odiu

m carbonate s

olut

ion.

the

dyei

ng is

the

u re

rnor

rd

from

th

e str

ongl

y or

Wea

kly

colo

lved

'wlu

tion

and

1 C

.C.

W T

w.

caus

tic

soda

add

ed t

o th

e la

tter

, , E

ithe

r de

colo

risa

t.ion

or

a pa

le

Lila

c..et

c. co

lour

res

ults

nft

rr b

oilin

g fo

r 1-

2 m

in.

Gla

cial

ace

tic

acid

1s

then

add

ed r

l~

p

by d

r(tp

uut

il t

.hu

sivl

uti(

~n is

aci

d, w

hen

it ch

ange

s to

tbe

orig

inal

col

oiir

ton

c of

the

dyei

ug.

The

who

le V

. th

e te

at ma? b

e ca

rrie

d o

ut

in p

rese

nce

of th

e fl

bre,

but

in

this

ca

se t

he A

nal

acid

sol

utio

n w

ill b

e tu

rbid

. tt -4

few

tria

ryln

ieth

ane

chro

me

dyes

, e.g

. the

Ch

Niu

N la

ke o

r Er

ioch

rom

e A

zuro

l B

, re

act

in t

his

way

, al

thou

gh t

.he

orig

inal

co

lour

ton

e is

res

tore

d le

as r

apid

ly a

nd i

s le

ss ln

tens

e th

an i

n th

e ca

se o

f an

oxa

zine

dpr

.

TA

BL

E V

ID

EN

TIF

ICA

TIO

X O

F D

YE

S O

N W

OO

L,

SIL

K,

AN

D R

EL

AT

ED

FIB

RE

S

(GR

EEN

DY

EIN

CS

AN

D P

RIN

TS)

tap-

wat

er*i

- A

i n e

, h

zin

e,

or

Th

iaz

ine

The

dye

ing

or p

rint

is

boile

d fo

r 1-

2 m

in. i

n di

lute

am

mon

ia (

cf. R

eage

nts,

p.

179)

. in

pre

senc

e of

whi

te c

otto

n.

$e.

Thl

s IS c

onfi

rmed

by

boil.

in

g for 4

min

. in

5%

so

diu

m c

arb

on

ate

The

sol

utio

n is

col

oure

d di

stin

ctly

. Th

e co

tton

is

not

stai

ned-

Aci

d b

e.

A f

resh

pat

tern

is

boile

d fo

r 1-

2 m

in. i

n F

orm

osul

G.

ton

e is

res

tore

d sl

owly

by

3%

hy

drog

en p

en

-

ide - A

nthr

a-

quin

onoi

d Dye.

A d

isti

nct

redd

ish

~ Th

e pa

tter

n is

dec

olor

ised

. , T

he p

atte

rn i

s co

lour

dev

elop

s:

deco

lori

sed

orig

inal

co

lour

_

_

I 1

perm

anen

tly

The

or

igin

al

The

or

igin

al

colo

ur

is I

-AZO

h

e.

do

ur

is r

e- 1

restored b

y D

evel

oper

I st

ore

d

bv

i O

t-T

riar

vhue

than

e

The

sol

utio

n is

not

, or

onl

y v

ery

sli

ghtl

y, c

olou

red.

Th

e co

tton

is

not

stai

ned

(Mordant,

Aci

d-m

orda

nt,

or Vat

Dye)

or

may

be

stai

ned

(Sub

stan

tive

Dye

). A

fre

sh p

atte

rn i

s bo

iled

for

1-2

min

. in

Form

osul

G.

T h

e

p a

t t e

r u

S

ligh

t, or

dis

tinc

t c

ha

ng

ea

to

1 co

lour

ch

ange

o

ra

ng

e o

r

occ

urs

(D

ale

brow

n: a

mor

d-

ant i

s p

res

en

t A

n thr

agui

no-

noid

M

orda

nt

he

. T

he c

olou

r of

th

e re

duce

d dy

eing

is

re

sto

red

sl

owly

on

airi

ng

or

rapi

dly

by

39/,

hydr

ogen

p

er

ox

ide

-

Cce

rule

in.

yello

w i

n'i

om

e ca

ses)

; or

igin

al

colour

is

re-

stor

ed b

y ai

r or

V

at

Dye

D

e-

relo

per - Va

t

Chr

omiu

m m

ay b

e pr

esen

t, on

woo

l d

ye

ing

s (c

f.

also

last

colu

mn

of T

able

I).

Dye

:

The

pat

tern

is

de-

colo

rise

d pa

rtly

or

com

plet

ely;

or

igin

al

colo

ur

is

rwto

red

by

ta

p -w

a t

er

. C

hrom

ium

is

pr

esen

t - O

x-

azin

e or

T

hi-

azin

e D

ye.

The

pat

tern

is

dem

lori

sed

per-

m

anen

tly-A

zo

Dye

* (c

f.

foot

note

mar

ked * i

nTab

le I).

A

fre

sh p

atte

rn i

s boiled

for

4 m

in.

wit

h 5%

sod

ium

car

- bo

nate

so

luti

on

and

w

hite

co

tton

, an

d al

low

ed t

o c

ool

-__

_

in t

he li

quid

.

The

co

tton

is

T

he

cott

on

is

not,

or o

nly

8 t

a i

n e

d

sli

gh

tly

d

ee

ply

- st

aine

d;

Suba

tant

he

mor

dant

1 D

ye

(Cop

- p

rea

ent - '

per

and

/ br

Aci

d - mo

r-

ch

rom

ium

da

nt D

ye.

1 may

bep

res-

'

fora

few

seco

nd

a.

, ~

ent)

. I

1 1

! I

~

"Cf.

fo

otno

te i

uark

ed *

iu T

able

111

.

boili

ng :

,"b

acet

ic a

cid

or h>

nlro

hol.

The

y ar

c id

nrtiR

t.d a

s in

- di

ratr

d in

Tab

le M

I.

t Cf.

foot

note

iiia

rked

**

in

Tab

le IV.

.V&

--Ra&

&

tndg

s ar

e st

ripp

ed t

o a

cona

idcx

nble

ex

tmt

by

* Kap

htho

l G

rew

B,

a ui

tmso

-con

ipou

nd,

beha

ves

rim

ilnr

ly;

it is

onl

y oc

casi

onal

ly

used

. A

pa

ttrr

n ch

ange

s to

pa

le t

irow

n rin

boi

ling

for

+ niiil.

in r

onrr

ntra

trd

Iiyd

rwhl

orie

ari

d.

TABLE

VI

IDE

NT

IFIC

AT

ION

OF

DY

ES

ON

WO

OL.

S

ILK

, A

ND

RE

LA

TE

D F

IBR

ES

(B

RO

WN

DY

EIN

CS

AN

D P

RIN

TS)

The

dye

ing

or p

rint

is

boile

d fo

r 1-

2 m

in. i

n di

lute

am

mon

ia (c

f. Reagents,

p. 1

79),

in p

rese

nce

of w

hite

cot

ton.

-

I

The

pat

tern

is d

ecol

oris

ed p

erm

anen

tly*-

Azo

Dye (cf. fo

otno

te

mar

ked

* in T

able

I).

A

fre

sh p

atte

rn i

s bo

iled

for

+ min

. w

ith

6y0

sodi

um c

arbd

nate

sol

utio

n an

d w

hite

cot

ton,

and

al

low

ed t

o co

ol in

the

liqu

id.

_.

The

cot

ton

is n

ot s

tain

ed;

a T

he c

otto

n is

eta

ined

dee

ply

mor

dant

is

pre

sen

tAci

d-

-Sub

stan

tive

Dye. (

Cop

per

mor

dant

Dye.

and/

or

chro

miu

m

may

be

p-

nt).

The

solu

tion

is c

olou

red

dist

inct

ly.

The

cot

ton

is n

ot s

tain

ed-A

cid

Dye

. A

fre

eh p

atte

rn is

boi

led

for

1-2 min. in

For

mos

ul G

.

The

pat

tern

is

deco

lori

sed

perm

anen

tly-

Azo

Dye;

or c

hang

es t

o a

pale

r sh

ade

whi

ch r

ever

ts t

ow-

orig

inal

col

our

tone

**

in

pres

ence

of

ho

t \'a

t D

ye

Dev

elop

x-A

nthr

qubm

id

Dye.

The

sol

utio

n is

not

, or

onl

y ve

ry s

light

ly,

colo

ured

. T

he c

otto

n is

not

sta

ined

(M

orda

nt, A

cid

mo

dan

t, or

Vat

Dye

) or m

ay b

e st

aine

d (S

ubsb

ntiv

e Dye).

A f

resh

pat

tern

is b

oile

d fo

r 1-

2 m

in.

in F

orm

osul

G.

The

pat

tern

is n

ot a

lter

ed;

a m

orda

nt i

s pr

eeen

t- h

thra

qu

bo

no

id k

hd-

ant Dye, e

.g. A

nthr

acen

e B

row

n; o

r C

utch

.

The

pa

tter

n ch

ange

s di

s-

tinc

tly

in colour; or

igin

al

colo

ur

is restored

by

Vat

Dye

Dev

elop

er-V

at

Dye

(cf.

also

last

col

umn

of T

able

I).

~ ~~

** T

he h

omog

enou

s,dy

e, A

lizar

in L

ight

Brown kL, ch

ange

s to

pale

yel

low

on

redn

ctio

n an

d th

e or

lgin

al c

olou

r to

ne d

evel

ops

on

oxid

atio

n. I

n th

e ew

e o

f ii m

ixtu

re t

he c

olou

r to

ne d

evel

oped

on

oxid

stlo

n m

ay b

e th

at o

f a

corn

pone

&.

Som

e dy

eing

s ch

ange

to

pale

r an

d ye

llow

er s

hade

s on

boi

ling

Arst

in 1

0% h

ydro

chlo

ric a

cid

and

then

in F

omos

ul G

and

rev

ert

part

ly to

orig

inal

col

our

ahen

tre

ated

with

3O;

hydr

ogen

per

- ox

ide,

e.g

. th

e br

own

chro

mlu

ni l

ake

froi

n ch

rom

otro

pic

acid

.

TAB

LE V

II

IDE

NT

WIC

AT

ION

OF

DY

ES

ON

\VOOL,

SIL

K.

AN

D R

EL

AT

ED

FIB

RE

S

(BLA

CK

S A

ND

GREYS)

The

dye

ing

or

prin

t is

boile

d fo

r 1-

3 m

in.

in d

ilut

e am

mon

ia (

cf. &

agen

ts,

p. 1

79).

in p

rese

nce

of w

hite

cot

ton.

of T

able

I).

The

solu

tion

is c

olou

red

dist

inct

ly.

The

cott

on i

s no

t st

aine

d-A

cid

Dye.

A f

resh

pat

tern

is

boile

d fo

r 1-

2 m

in.

in F

orm

osul

G.

wit

h w

ater

. C

hrom

ium

or

iron

is

pres

ent - L

ogw

ood

Bla

ck.

The

dye

ing

chan

ges

to b

row

n -N

apht

hazP

rin;

o

r is

ne

arly

cl

ecol

oris

rtl - In

di-

The

pat

tern

is d

ecol

oris

ed p

erm

anen

tly*-

A

zo Dy

e; o

r is

al

mos

t de

colo

rise

d.

but

reve

rts

to

orig

inal

co

lour

**

in

pres

ence

of

hot

Vat

Dye

Dev

elop

r-

Ant

hraq

uino

noid

Dye, e

g.

Ali

zari

n Light

Qre

y G

.

The

sol

utio

n is

not

, or

onl

y sl

ight

,ly, c

olou

red.

T

he c

ot,to

n is

not

sta

ined

(M

or

ht,

Aci

d-m

orda

nt,

or V

at D

ye)

or

may

be

stai

ned

(Sub

stan

tive

Dye).

4 f

resh

pat

tern

16

boiled

for

1-2

min

. in

For

mos

ul G

.

The

pat

tern

is

dec

olo

rid

per

man

ently

-Azo

Dy

e (c

f.

foot

note

mar

ked

* in

Tab

le I

).

A

fres

h pa

tter

n is

boiled f

or 4 in

in,

wit

h 5%

sodi

um c

arbo

nate

sol

utio

n an

d w

hite

cot

ton.

and

allo

wed

to

roo

1 in

th

e li

quid

. _-

The

cot

ton

is n

ot s

tain

ed;

a m

orda

nt i

s pr

esen

t-

Aci

d-m

orda

nt D

ye.

The

cot

ton

is s

tain

ed d

eepl

y --

Subs

tant

ive

Dye.

i

TA

BL

E

VII

I ID

ES

TIF

ICA

l'IO

~ (I

F D

YE

S O

K C

OT

TO

N ;

\NU

O

TH

ER

CE

LL

I'LO

SIC

F

IBR

E>

(R

ED

DY

EIN

CS

AN

D P

RIN

TS)

oure

d di

stin

ctly

an

d, a

fter

aci

di

The

dye

ing

or

pri

nt

is b

oile

d fo

r 1-

2 ni

in.

in d

ilut

e am

mon

ia (

cf. R

eage

nts,

p.

179)

. T

he s

olil

tion

is

not

arm

reci

ahlv

col

oure

d.

A x

mal

/ D

atte

rri

is b

oile

d fo

r a

few

sec

onds

in

1 C

.V.

>?,,

ciii

lsti

c so

da.s

olrl

tir,

n:

..._

____

-.

4 A B

asic

Dye

is n

ot p

rcsf

\

larg

e am

ount

of

dye

is s

trip

ped;

th

e so

luti

on i

s th

e fy

9g

wit

h ac

etic

ac

id

and

he

at

ing,

dy

es w

hite

w

ool -

Aci

c Dye.

(The

woo

dy

eing

is

ex

ai

nine

d as

de

sc

ribe

d in

Tab

lt 1)

.

sam

e co

lour

aa

tlie

pat

ter1

i.j-t

A

few d

rops

of

tann

ic

acid

sol

utio

n ar

e ad

ded

to t

he

wea

kly

acid

ifie

d so

lu-

' A'

~~

~~~~

~~~~

o

~~

~l

ia

~~

ti

on.

A c

olou

red

prec

ipit

ate is

obta

ined

-Bns

ic

Dye

. ~

Th

e d

ye

is t

rans

ferr

ed t

o w

ool

(cf.

p.

181)

an

d b

oile

d ~

~p

~f

~l

~~

~l

co

~~

ll

~~

~

~ sa

me

tls

that

of

th

e fo

r 1-

2 m

in.

in F

orm

osul

G.

.-I

dye

an

d d

oes

not

alte

r

Ver

y li

ttle

ch

ange

in

co

lour

-

Xan

then

e D

ye

(R

ho

da

tnin

e

Gro

up);

als

o th

e P

oJy-

m

eth

ine Dye, r

lstr

a-

phlo

xine

FF

. rh

e la

ttm

is f

a) u

ract

ic-

The

pa

pw

n is

deco

lori

sed

; or

igin

al

col-

ou

r is

re

- st

ore

d

by

t a

p-w

ater

- A

rine

Dye.

ally

un

affe

ect'e

d by

bo

ilin

g co

ncen

trat

ed

hydr

ochl

oric

aci

d, a

nd

(b

) th

e al

coho

lic

soh

- 1

tion

is

not

fluo

resc

ent,

w

hen

view

ed b

y

the

ca

rbo

n

arc

li

gh

t (d

isti

nc

tio

n

fro

m

Rho

dom

ine B).

I

The

pat

tern

is 1

deco

lori

sed;

or

igin

al

col-

, o

ur

is

re-

sto

red

h

yl

Dev

elop

er 0

-Tri

ary

l-

I m

eth

an

e1

appr

ecia

bly

duri

ng th

e te

st.

The

alk

alin

e so

l-

utio

n st

aim

whi

te c

ot-

ton

de

eply

,, T

he

wea

kly

acid

ifie

d so

lu-

tion

do

es n

ot

give

a

prec

ipit

ate

wit

h ta

n-

nic

acid

so

luti

on -

Sub

stan

tive

D

ye.

A

fres

h p

atte

rn is

hoi

led

in F

orni

osnl

G.

~ T

he p

atte

rn i

s (a) d

e-

colo

rise

d pe

rman

entl

y -A

t0

Dye:*

or (

b) is

I

redu

ced

to

a D

ale

I I

! ye

llow

- ~

hia

zo~

Za

zo

~ I I

1 I I

Dye,

e.g.

P

rim

ulitw

1

Red

**.

I

I I

I I

I

I I

.I

I I

I 1 ,

1 1

1

~t

.

Afr

esh

pat

tern

is h

oih

lio

r 1-

2 ni

in. i

n3

"~

cau

stic

si~

da

s~~

lilt

ioii

. \.w

y li

ttle

. if

any

. dy

e is

Bt,r

ippe

d-A

zoic

or

T

he c

aust

ic s

oda

~ V

at D

ye,

A

fres

h p

atte

rn i

s bo

iled

vig

or-

solu

tion

is

pale

' u

iisl

y fo

r 1-

2 ni

in. i

n F

orm

osu

l Gco

ntai

ning

vi

olet

.; a

mor

d-

! a

few

tlr

ops

700

~w

.

caus

tic

sod

a.

ant

(all

~I1

lin

i~l

1 Th

e p

att

ern

is

, T

he p

atte

rnid

- o

rch

oln

ium

) is

1 pa

rtly

o

r cu

m-

or

alte

red

in

shad

e;

pres

ent-

--A

nth-

pI

et,e

Iy d

ecol

or-

the

solu

tion

is

\wllo

w.

raq

uin

on

oid

e ,it

: t

h e

Mor

dant

D

ye,

e.g.

A

liz

ari

n

Red.

v an

d M

ar-

oo

m;

Tur

key

Red

, et

c.

chan

ge

is

per-

m

anen

t-A

zoic

D

ye.

Thi

s is

conf

irm

ed

bx

stee

ping

a

pat

tern

in

cold

et

hyle

nedi

amin

; io

rafe

amin

ute

s a

cons

ider

able

an

iou

nto

fdy

eis

extr

acte

d.

The

co

lour

ed e

xtra

ct,

is d

ivid

ed i

nto

two

port

ions

. A

lit

tle

sodi

um

hydr

osul

phit

e is

adde

d to

on

e po

rtio

n - P

er-

man

ent d

ecol

or .

isat

ion

occu

rs

in t

hec

old

oro

n

war

min

g.

The

ot

her

port

ion

is

dil

ute

d w

ith

w

ater

an

d b

oile

d -T

heli

quid

be

- co

mes

tu

rbid

an

d fl

akye

ggre

ga

teso

fcol

oure

d ,

pip

en

t se

ttle

'

out.

on st

andi

np.

!

blui

sh-r

ed.

etc.

; or

igi-

na

l co

lour

is

rest

ored

by

air

or

mor

e re

adil

y by

Vat

Dye

Dev

elop

er

(cf.

Rea

gent

s) - V

at

Dye.

Thi

s is

co

nfir

med

by

bo

ilin

g a

fres

h p

atte

rn

in

ethy

lene

diam

ine

cont

aini

ngal

ittl

e so

lid

gluc

ose.

T

he

leuc

o-

coin

poun

d is

pro

duce

d a

t on

ce a

nd

rev

ersi

on

to o

rig

ina

l co

lori

r oc

curs

on

ad

ding

a

port

ion

to a

few

c.c

V

at D

ye D

evel

oper

.

**C

onfir

med

by

rrdi

azot

ivin

g th

e re

duce

d dg

ring

and

det

elop

ing

with

S

Bas

ic t

oppi

ng d

yes

on s

ubst

anti

vr d

yein

g8 a

re r

emov

ed b

y bo

iling

glacial a

ceti

c ac

id.

t C

f. fo

otno

te m

arke

d t

in T

able

1x.

tt D

ccol

oris

atio

n oc

curs

in s

ome

case

s du

ring

the

init

ial

boili

ng

Als

o In

CB

SBS

of d

yein

g3 t

oppe

d w

ith

in c

amti

c so

da

solu

tion

. ba

sic

dyes

, th

e fln

al s

olut

ion

msy

onl

y be

slig

htly

col

oure

d.

Chr

orui

um o

r co

pper

may

be

pres

ent

in s

ome

dyei

ngs.

TAB

LE I

X

IDE

NT

IFIC

AT

ION

OF

DY

ES

ON

CO

TT

ON

AN

D O

TH

ER

CE

LL

UL

OSI

C F

IBR

ES

'

(OR

AN

GE

AN

D YELLOW

DY

EIN

CS

AN

D P

RIN

TS)

T

he d

yein

g or

pri

nt is

boi

led

for

1-2

min

. in

dil

ute

amm

onia

(cf

. Rea

gent

s, p

. 17

9).

The

sol

utio

n is

not

app

reci

ably

col

oure

d.

A s

mal

l pa

tter

n is

boi

led

for

a fe

w s

econ

ds i

n 1

C.C

. 5%

cau

stic

sod

a so

luti

on:

4 C

.C.

5OL

amm

oniu

m c

hlor

ide

solu

tion

are

then

add

ed,

and

t.he

who

le b

oile

d ag

ain

for

a fe

w s

econ

ds.

The

pat

tern

is n

ot a

ffec

ted-

Sulp

hur,

T

biuo

lc, h

ol

e-

u

o, A

zoic

, or

Vat

Dye.

X f

wsh

pat

tern

is

boile

d fo

r 4-

1 m

in.

or

long

er i

n F

orm

osul

G, c

onta

inin

g a

few

dr

ops

of 7

0" T

w. c

aust

ic s

oda.

rhe

patt

ern

is (

A)

part

ly d

ecol

oris

ed**

(S

ulph

ru o

r T

bhzo

+ sll

brt.n

tive Dye);

(B)

slig

htly

aff

ecte

dt o

r de

colo

rise

d (A

zoic

Dye

); or

(C) a

lter

ed d

isti

nctl

y in

co

lour

(V

at D

ye].

T

he o

rigi

nal c

olou

r to

ne is

res

tore

d on

(A

) (S

ulph

ur

Jlye

onl

y) a

nd

&

stor

ed

alm

ost

com

plet

ely

on (

C)

by m

ild

oxid

atio

n.

Th

e s

olu

tio

n i

s co

lou

red

d

is-

tinc

tlya

nd, a

fter

ac

idif

ying

w

ith

acet

ic a

cid

and

heat

ing,

dy

es

whi

te wool -

Aci

d Dye. (

The

w

ool

dyei

ng

is

exam

ined

as

de-

sc

ribe

d in

Tab

le

11).

c 'he

patt

ern

is

A l

arge

am

ount

of

dve

is s

triu

ued.

d

e c'o

lo

ris

e d

quic

kly-

A

ura-

m

ines

, T

hio-

@

vine

T, et

c.

Aur

amin

e dy

e-

ings

are

deco

lor-

is

ed a

t on

ce b

y cold 5

"/b c

aust

ic

soda

so

luti

on;

orig

inal

co

lour

is

re

stor

ed

on

addi

ng

exce

ss

5% a

inm

oniu

m

chlo

ride

so

lu-

tion

. D

ecol

or-

isat

ion

is

pr

- m

an

en

t o

n

boili

ng

in

5%

ca

ust

ic s

od

a

solu

tion

. rh

iofl

avin

e T

dye

. in

gs a

re n

ot a

f-

fect

ed

by

cold

5%

cau

stic

sod

a so

luti

on

, b

ut

are

deco

lori

sed

perm

anen

tly

on

boili

ng.

he

fina

l so

luti

on,

wh

iZ

is

yello

w,

is s

ligh

tly

acid

ifie

d w

ith

5%

acet

ic a

cid

and

a fe

w d

rops

of

tan

nic

acid

sol

utio

n ad

ded-

A

co

lou

d p

reci

pita

te is

for

med

o

n s

tand

ing-

Bas

ic

Dye

. T

he

dye

is t

rans

ferr

ed t

o w

ool

(cf.

p.

181

) and

boi

led

for

1-1

min

. in

For

mos

rtl G

. ~~

The

pat

tern

is u

n-

The

pat

tern

is

alte

red

-Ac&

de

colo

rise

d d

ine

Dye

. pe

rman

entl

y T

his

is c

onfi

rmed

-A

zo

Dye.

by

sp

otti

ng

a pa

tter

n w

ith

cold

co

nce

n-

trat

ed s

ulph

uric

ac

id.

A f

luor

- es

cent

so

luti

on

is ob

tain

ed.

__

__

$3

A B

.sic

Dpa

is n

ot p

rese

nt.

-4 fr

esh

patt

ern

is b

oile

d fo

r 1-

7min

. iii

SD,,

caus

tic

soda

sol

ucio

n.

A c

onsi

dera

ble

or s

mal

l am

ount

, of

dye

is s

trip

ped;

the

col

our

of t

he s

olu-

ti

on, w

hich

doe

s no

t al

ter !j

appr

eci-

ab

ly d

urin

g th

e te

st,

is t

he

sam

e in

m

ost

cwee

as

that

of

the

dyei

ng.

The

wea

kly

acid

ifie

d so

luti

on d

oes

not

give

a p

reci

pita

te w

ith

tann

ic

acid

sol

utio

n.

A m

orda

nt m

ay b

e pr

eaen

t-Su

bsta

ntiv

e or

A

cid-

m

orda

nt D

ye.

A f

resh

pat

tern

is

boile

d fo

r +I

m

in.

in 5

% c

aust

ic

soda

sol

utio

n to

whi

ch R

Zi

trle

solid

so

dium

hyd

rosu

lphi

te is

add

ed.

The

pat

tern

is (a) de

colo

rise

d pe

rman

- en

tly-A

zo

Dye:

or

(6

) is

o

nly

sl

ight

ly

affe

cted

-Thi

azol

e Dy

e.

A f

resh

pat

tern

is

boile

d w

ith

5%

ca

usti

c so

da s

olut

ion,

whi

te c

otto

n,

and

a li

ttle

sod

ium

chl

orid

e.

The

whi

te c

otto

n i

s

sta

ine

d

deep

ly - A

ZO

Su

bs

tan

tiv

e

DP

.

rhe

whi

te c

otto

n is

no

t st

aine

d;

a m

orda

nt

ie

pre

sen

t (a

) -A

zo

Ae

id-

mor

dant

Dye

* ;

or (

h)

Thi

azol

e S

ub

sta

nti

ve

D

ye (

a m

orda

nt

is n

ot p

rese

nt).

(A)

(B)

I (C

) h

pat

tern

is b

oile

d 1

A

pa

tte

rn

is

A

Vat

Dy

e is

fo

r 4

min

. in

di

uued

in l

iaui

d co

nfir

med

bv

l6qb

h

yd

ro-

chlo

ric

ac

id,

cool

ed

and

R

litt

le

inag

ne-

si

um

ad

de

d.

Hyd

roge

n so

l-

phid

e is

evo

lved

(a

) re

adilv

-

p&no

l, sq

uG

zed

li

ghtl

y,

laid

on

w

hit

e

fil

ter

pa

per

whi

ch

is

then

fol

ded,

and

pr

esse

d ei

ther

w

ith

a ho

t iro

nor

azai

nst

a st

eam

S

ulph

ur

"Dye

; py

pe.

Yel

low

- or

(6) l

as

read

i-

ly-T

h

ia z

o 1 e

S

ub

sta

nti

ve

D

ye.

stai

n on

pa

per

-Azo

ic

Dye.

Thi

s is

con

firm

ed

by h

eati

ng a

pat

- te

rn in

eth

ylen

e-

diam

ine,

di

vid-

in

g th

e co

lour

ed

extr

act

into

tw

o p

ort

ion

s a

nd

te

stin

g th

em a

s de

scri

bed

in t

he

the

ethy

lene

- di

amin

e te

st

(c

f.

la

st

c

olu

nin

o

f T

able

V

III,

an

d p.

182

).

TABL

E X

(VIO

LET

DY

EIN

CS

AN

D P

RIN

TS)

ID

EN

TIF

ICA

TIO

S O

F D

YE

S O

N C

OTT

OK

A

ND

OT

HE

R C

EL

LIJ

LO

SIC

F

IBR

ES

The

pat

tern

is

stri

pped

sl

ight

ly a

nd th

e co

lour

of

th

e so

luti

on

is o

f m

oder

ate

inte

nsit

y.

Whi

te

woo

l is

st

aine

d sl

ight

ly o

n st

andi

ng in

th

e co

olin

g so

luti

on.

The

ac

idif

ied

solu

tion

The

sol

utio

n is

colo

ured

dis

- ti

nctl

y an

d,

afte

r ac

idif

y-

in

g w

it

h

acet

ic

acid

an

d h

eati

ng,

dyes

w

hite

w

ool - A

cid

woo

l dy

eing

is

ex

amin

ed

as

desc

ribe

d in

Tab

leII

I).

Dye

. (T

he

' 9:

A h

ic

or B

uim

mor

dant

ye

is n

ot p

rese

nt. -4 fr

esli

patt

ern

is b

oile

d fo

r 1-

2 in

in.

in 5

yi

caus

tic

soda

sol

utio

n.

The

dye

ing

or p

rint

is

boi

led

for

1-2

inin

. in

dilu

te a

mm

onia

(cf

. Rea

gent

s, p

. 17

9).

Th

e so

luti

on is

no

t ap

prec

iabl

y co

lour

ed. A

8MII.

U p

atte

rn is

boi

led

for

a fe

w s

econ

ds i

n 1

C.C

. S

yo c

aust

ic s

oda

solu

tion

; 4

C.C

. 50

b am

mon

ium

chl

orid

e so

luti

on a

re th

en a

dded

, and

th

e w

hole

boi

led

agai

n fo

r a

few

sec

onds

. -

I The

pat

tern

is

stri

pped

to

a

grea

t ex

tent

, an

d t

he

solu

- ti

on is

col

oure

d de

eply

. A

fter

ac

idif

ying

the

sol

utio

n w

-ith

ac

etic

aci

d,

it y

ield

s a

col-

ou

red

prec

ipit

ate

wit

h ta

nnic

ac

id s

olut

ion-

Bas

ic

Dye.

The

dve

is t

rans

ferr

ed t

o w

ool

~ (c

f. "

p. 1

81)

and

boile

d fo

r 1-

2 ni

in.

in F

onno

sul

G.

The

pat

tern

is

deco

lori

sed;

or

igin

al c

ol-

ou

r is

re

- I

sto

red

b

y

-wat

er--

~

Zn

e D

ye.

i

The

pa

tter

n is

dec

olo

r-'

ised

: ori

gina

l

does

not

gi

ve a

pre

- ci

pita

te

wit

h ta

nnic

ac

id

solu

tion

, an

d ch

rom

ium

is in

the

ash

-Bas

ic-m

orda

nt

Dye

.

Thi

s is

co

nfir

med

by

bo

iling

the

sam

ule

for

colo

ur L re

- ,

sto

red

by

D

evel

oper

0 I

-Tri

aryl

- methane'

Dye.

- 1-

2 ru

in. i

n hy

dro-

ch

lori

c ac

id,

then

m

akin

g th

e so

luti

on

alka

line

wit

h co

ncen

- tr

ated

am

mon

ia

and

addi

ng

a li

ttle

so

lid

mag

nesi

um

sulp

hate

. W

hite

woo

l is

sta

ined

4 co

nsid

erab

le o

r,

smal

l am

ount

of

Ver

y li

ttle

, if

any

, dy

e is

str

ippe

d**-

Mor

dPnt

, Su

lphu

r, A

zoic

, or

Vat D

ye.

dye

is s

trip

ped

and

whi

te c

ot-

ton

is

stai

ned

deep

ly

in

the

cool

ing

solu

tion

- S

ubst

anti

ve

Dye

. A

fr

esh

patt

ern

is b

oile

d fo

r 1-

2 m

in.

in

For

mos

ul G

.

rhe

patt

ern

is d

e-

colo

rise

d pe

r-

ma

ne

n t

1 y *-

A

z

o,D

y e

(Chr

orm

um

or

copp

er m

ay b

e pf

esen

t, on

'

solu

tion

. 1

viol

et

suhs

tan-

de

eply

in

the

cool

ing

1 j ti

re d

yein

gs).

-4

pat

tern

is

boile

d fo

r ,

1-2

niin

. in

F

orm

o- 1

, S

lll

G.

I

The

pat

tern

is

deco

lor-

is

ed:

orig

inal

co

lour

is

re

stor

ed

by

tap

- w

ate

r-h

rin

e

Dye,

e.g.

Mod

ern

Vio

let,e

tc.

A f

resh

pat

tern

is

boile

d vi

goro

usly

fo

r 1-

2 m

in.,

or l

onge

r, i

n F

orm

osul

G c

onta

inin

g a

few

dro

ps 7

0" T

w.

caus

tic

soda

.

I T

he c

olou

r of

th

e ' T

he

pa

tte

rn ,

The

pat

tern

is d

e-

The

pat

.tern

an

d

patt

ern

is

not

! is

de

colo

r-

colo

rise

d;

orig

- so

luti

on c

hang

e al

tere

d - X

.n-

' is

edpe

rman

- in

al

colo

ur

is

to

a ye

llow

ish

acn

e Dye, e.

g. 1

shad

e, o

r t,h

ere

Ga

lle

in;

or

! Azoic

Dye.

wa

ter-

S

ul-

is

lit

tle

alte

ra-

chan

ges

to

a ph

ux D

ye.

tion-

Vat

Dye.

da

rke

r sh

ad

e I Th

is

is

con-

' A

pat

tern

is b

oile

d T

his

is c

onti

rmed

w

hich

re

vert

s fi

rme

d b

y

for$

min

.in 16?,

byth

eeth

ylen

e-

to th

e or

igin

al

stee

ping

a

hy

dro

ch

lori

c

diam

inet

est(

cf.

shad

e o

n a

irin

g'

patt

ern

in

acid

, coo

led

and

, la

st

colu

mn

of

-An&

raqu

in-

, co

ld

ethy

l.

a li

ttle

mag

ne- '

T

able

VII

I. a

nd

onoi

d M

or

bt

~ en

edia

min

e.

niu

m

ad

de

d.

1'.

182)

. D

ye.

A m

ord-

1 di

vidi

ng t

he

Hyd

roge

n su

l.

an

t,

usu

all

y ~

colo

ured

ex.

ph

idei

sevo

lved

ch

rom

ium

, is

tr

act

into

re

adil

y - Sul-

pres

ent

on b

oth

~ tw

o po

rtio

ns

phur

Dye

. cl

asse

s of

dy

e-'

an

d te

stin

g' A

p

att

ern

is

, in

gs.

1 th

em a

R d

e-

stri

pped

rea

dily

sc

ribe

dint

he

by

b

oil

ing

1 5t

h co

liii

iiii

e

thy

l~n

ed

ia- ,

en

t 1 y

t -

rest

ored

by

hot

, o

f T

ab

le

min

e.

I i V

III.

1 I I

t Ci.

foot

note

mxr

k~d t

in

Tab

le IS.

** C

f. fo

otno

te m

arke

d in

Tah

lr X

I.

5 C'

f. fo

otno

w iu

arkr

d s i

n T

al~l

t. \

111.

+

A

liear

iii 01

1 ir

on m

orda

nt g

ives

a v

iole

t so

luti

oncb

angi

ng to

an

oran

ge c

olou

r; f

inal

ly.

the

patt

ern

is d

ecol

orie

ed.

\%hi

t,. w

tttw

Is

not

sta

ined

011 b

oilin

g a

uar

iip

li~ i

ii 5°

'o r

awti

c so

dn s

olut

ion.

TA

BL

E X

I ID

EN

TIF

ICA

TIO

N O

F D

YE

S O

N C

OT

TO

K A

ND

OT

HE

R C

EL

LV

LO

SIC

FIB

RE

S

(BL

UE

DY

EIN

CS

AN

D PRINTS)

The

dye

ing

or

prin

t is

boi

led

for

1-2

Inin

. in

dilu

te a

mm

onia

(cf

. Rea

gent

s. p

. 17

9).

__

~

__

~

~ -_

Th

e s

olu

tio

n

is c

olo

ure

d

dist

inct

ly a

nd,

afte

r ac

idif

y-

in

g w

it

h

acet

ic

acid

an

d he

atin

g,

dyes

w

hite

w

ool - Ac

id

woo

l dy

emg

is

exam

ined

as

desc

ribe

d in

Tab

le I

V).

Dye.

(The

The

sol

utio

n is

not

app

reci

ably

col

oure

d.

A a

mdl

sam

ple

is b

oile

d fo

r a

few

sec

onds

in 1

C.C

. 57

4 ca

usti

c so

da s

olut

ion;

4

C.C

. 5%

am

mon

ium

chl

orid

e so

luti

on a

re th

en a

dded

, and

th

e w

hole

boi

led

agai

n fo

r a

few

sec

onds

.

k de

eply

col

oure

d so

luti

on

is o

btai

ned.

T

he

wea

kly

acid

ifie

d so

luti

on y

ield

s a

prec

ipit

ate

wit

h ta

nnic

aci

d so

lutio

n-B

asic

Dye.

The

d

ye

is t

rans

ferr

ed t

o w

ool

(cf.

p.

181)

an

d bo

iled

for

1-2

min

. in

For

mos

ul G

.

L'he

pat

tern

is

deco

lori

sed;

o

ri

gi

na

l

colo

ur is

re-

sto

red

b

y

tap-

wat

er-

Az+

. O

X-

az

ine

or

T

hia

zin

e

Dy e.

l'he

patt

ern

is

deco

lori

sed;

o

ri

gi

na

l

colo

ur i

s re

- st

ore

d

by

D

evel

oper

0

-Tri

aryl

- m

et h

a n

e

Dye.

Th

e

patt

ern

chan

ges

to

pink

or

red

firs

t a

nd

th

en

be

-

com

esco

lour

le

as; r

eddi

sh

colo

ur i

s re

- st

ore

d

by

ta

p-w

ater

-

Safr

anin

e-

azo

Dye

.

Str

ippi

ng o

ccur

s to

a

med

ium

ext

ent a

nd

wh

ite

wo

ol

is

stai

ned

slig

htly

on

stan

ding

in

th

e 1 X

con

side

rabl

e co

olin

g so

luti

on.

~ o

r si

n a I

1 T

he a

cidi

fied

sol

u-

amou

nt

of

$ A

Bas

ic o

r B

asic

-mor

dant

Dye

is n

ot p

rese

nt.

A f

resh

pat

tern

is b

oile

d fo

r 1-

2 m

in.

in SO,;

caus

tic

soda

sol

utio

n.

tion

doe

s no

t yi

eld

dye

is s

trip

- a

prec

ipit

ate

-with

ta

nnic

ac

id

solu

- ti

on;

chro

miu

m i

s pr

esen

t in

th

e as

h -B

asic

-mor

dan

t

Thi

s is

conf

imrn

ed b

y bo

ilin

g a

patt

ern

for

1-2

min

. in

506

hydr

ochl

oric

ac

id,

then

m

akin

g th

e so

luti

on

alka

line

w

ith

conc

ent r

ated

am

mon

ia a

nd e

dd-

ing

a

litt

le

solid

m

agne

sium

su

l-

phat

e.

Whi

te w

ool

is

stai

ned

deep

ly

in t

he c

oolin

g so

lrr-

ti

on.

Dye.

p?

* a

id

whi

te c

otto

n is

st

aine

d de

eply

in t

he

cool

ing

solu

- t i

on - S

ub-

sta

nti

ve

fres

h pa

tter

n is

boi

led

for

1-2

min

. in

F

orin

osul

G.

Dye

: A

rhe

patt

ern

is

deco

lori

sed

perm

anen

tly

-AZ

O

Dye

.

Ver

y li

ttle

, if

any,

dy

e is

st

ripp

ed-M

orda

nt,

Sul

phur

, A

zoic

, or

Vat

Dye.

A f

resh

pat

tern

is b

oile

d vi

goro

usly

for

1-2

ini

n.,

or lo

nger

, in

For

mos

ul G

con

tain

ing

a fe

w d

rops

of

70"

Tw

. ca

usti

c so

da.

The

pat

tern

is '

Lit

tle,

if

any,

de

colo

rise

d;

. o

ri

gi

na

l

co

lou

r is

re

stor

ed

on

expo

sure

to

ai

;-Su

lphu

r Dye.

This is

con

firm

- ed

by

boili

ng

rnan

ge

oc-

curs

. A

lum

- in

ium

or

ch

roru

ium

is

pre

sen

t-

Ant

hraq

uin-

on

oid

Mor-

da

nt D

ye.

a pa

tter

n fo

; 4

rnin

. in

16

% ,h

ydro

- ch

lori

c ac

id,

cool

ing

and

ad

din

g

a 1 i

ttle

mag

nes

ium

. Hyd

ro-

gen

sulp

hide

is

ex

-olv

ed

lead

i 1 v.

' X p

atte

rn

is

boile

d , fo

r I-

? m

in.

in

, The

pa

tter

n is

de

. I

colo

rise

d :

orig

inal

For

mos

ul G

.

The

dye

ing

is

colo

ur

is

rest

ored

1 '

str

ipp

ed

q

I I ic

kly

by

by

ta

p-w

ate

r-

1

ened

iam

ine.

I

Oxa

zine

Dye

. bo

iling

eth

yl

rhe

patt

ern

is

dec

olo

rkd

t pe

rman

entl

y -

Az

oic

Dye.

C'hihis

is c

onfi

rm-

ed

ing

a by pa

tter

n st

eep-

inco

ldet

hyl-

en

e di

aiiii

ne.

divi

ding

the

ro

lour

ed e

x-

tra

ct

into

tw

o po

rtio

ns

and

test

ing

them

as

des-

cr

ibed

in th

e 7t

h co

lum

n o

f T

ab

le

VII

I.

The

pat

tern

and

solu

tion

ar

e ye

llow

ish

in

sh

ad

e,

or

litt

le

alte

ra-

tion

oc

curs

-V

at

Dye

. rh

is is

co

nfi

rm-

ed

by

the

eth

yle

ne

-

dian

iine

tes

t (c

f. l

ast

col-

umn of

Tab

le

VII

I,

an

d

p. 1

82).

__ _

____

_-__

~

- ~ ~

-_

_

~ _

_-

~ _

__

__

~._

__

_~

~._

- -_

__

t

Cf.

foot

not

(% um

kcd

t i

ri

'L'tt

bir

IS.

5 (.f

, fo

otno

te m

arke

d 5 i

n T

able

VII

L

Afe

wst

aig

ht p

ale

blue

. vio

let,

etc

.dge

ings

onco

ttou

an~1

vi6c

wer

avon

, C.U

. tho

se o

lrtn

ini,d

wit

h Si

rius

Sup

ra l

llue

FF

RL

Hiy

an Sky

B

lue

G,e

t4..

are

scar

cely

aff

rete

d IJS

ho

iliog

5",,

caus

tic

pods

sol

utio

n.

A d

yein

g of

thi

' B

r~t-

nani

t~d pr

oduc

t ia

dec

olor

ised

oo

boili

ng

in b";

calr

stir

sod

m so

luti

on C

onta

inin

g a

littl

e so

diun

l hy

dro6

uil1

hite

. but

rew

rts

to

the

orig

inal

rol

our

trm

. in

Iir

ewnc

i' of

tap-

wat

er-D

ioxa

zine

d

ye

Rig

an Sky

Blu

e G

dy

ring

a ch

ange

to

rvd

OII

I,

ollin

y irr

Forniosul

(;: th

vy a

rc i

lrc.

olor

i*rd

by

boili

ng

:>'',,

ca

usti

c sod

a B

olut

irrn

con

tain

ing

sodi

um I

wdr

oeul

phit

e. h

ut d

o ri

ot r

cvrr

t tu

the

oriu

inal

vol

our

tonv

a in

~w

srn

rr tui o

xidi

siri

g ag

vnts

.

TABL

E X

I1

IDE

hTIF

IC.1

TIO

S O

F D

YE

S OX C

OT

TO

S A

KD

OT

HE

R C

EL

L1

LO

SIC

F

IBR

ES

(G

RE

EN

DY

EIN

CS

AN

D P

RIN

TS)

obta

ined

. The

wee

kly

acid

ifie

d '

solu

tion

yie

lds

a pr

ecip

itat

e w

ith

tann

ic

acid

sol

utio

n-

Bas

ic

Dye

. T

he d

ye

is

tran

sfer

redt

owoo

l (c

f.~

. 181)

The

dye

ing

or p

rin

t is

boi

led

for

1-2

min

. in

dil

ute

amm

onia

(cf

. Rea

gent

s, p

. 17

9).

stri

pped

sli

ght-

ly

. T

anni

c ac

id

solu

tion

do

es

not

caus

e p

w-

1

The

sol

utio

n is

co

lonr

ed d

is-

tinc

tly

and,

af

ter

acid

ify-

i

ng

wi

th

ac

etic

ac

id

and

heat

ing,

dy

es

whi

te

woo

l - A

cid

Dye

. (T

he

w

ool

dyei

ng

is

exam

ined

as

desc

ribe

d in

Tab

le I

V).

The

sol

utio

n is

not

app

reci

ably

col

oure

d.

.A s

md

l pa

tter

n is

Im

iled

for

a fe

w s

econ

ds i

n 1

C.C

. .iv

b re

nsti

c bo

da s

olk

itlo

ll;

4 C

.C.

50,b

am

mon

ium

chl

orid

e so

luti

on a

re th

en a

dded

, and

the

who

le b

oile

d ag

ain

for

a fe

w s

econ

ds.

and

boile

d fo

r 1-

2 &

n.

in

For

mos

ul G

.

The

pat

tern

is

deco

lori

sed;

or

igin

al c

ol-

ou

r is

re

- st

ored

by

ta

p-w

ater

- A

zin

e,

Ox-

a

zin

e,

or

Tb

iaz

ine

Dye.

I

rhe

patt

ern

is

deco

lori

sed;

or

igin

al c

ol-

ou

r is

re

- st

ore

d

by

D

evel

oper

0

-Tri

ar

yl-

me

th

an

e

Dye

.

5 A %

sic

or B

aric

lmor

durt

Dye

is

not

pres

ent.

A f

resh

pat

tern

is

boile

d fo

r 1-

2 In

in.

in J

O/b

caus

tic

soda

sol

utio

n.

cip

ita

tid

n;

ch

rom

ium

is

' pr

esen

t in

th

e a

s h-Ba

s i c

- m

orda

nt Dye.

rhis

is

conf

irm

ed

by

boil

ing

a p

att

ern

fo

r 1-

2 m

in.

in 5

%

hy

dro

ch

lori

c

acid

, the

n ni

ak-

ing

the

solu

tion

al

kal

ine

wit

h

con

cen

tra

t e

d

amm

onia

an

d ad

ding

a

litt

le

soli

d

mag

ne-

si

um

sulp

hate

. W

hite

w

ool

is

A c

onsi

dera

ble

Ver

y li

ttle

, if

any.

dye

is s

trip

ped*

-Mor

dant

, S

ulph

ur,

Azo

ic,

or V

at Dye

. - .

or

sm

all

1

amou

nt

uf ~

stai

ned

deep

ly

in

the

cool

ing

solu

tion

. A

pa

tter

n is

de-

co

lori

sed

o

n

1 bo

ilin

ginF

orm

- os

nl G

; or

igin

al

co

lou

r is

re

- st

ored

by

tap

- ,

wat

er - h

-

dye

is s

trip

- '

pe

d a

nd

w

hite

cot

ton

1

A f

resh

pat

tern

is b

oile

d vi

goro

usly

for

1-2

niin

., o

r lo

nger

, in

For

mos

ul G

and

a

few

dro

ps o

f 70

' T

w. c

aust

ic s

oda.

is

sta

ine

d

~

deep

ly in

the

cool

ing

solu

- ti

on -Su

b-

sta

nti

ve

Dye.

Sfr

eshp

atte

rn ,

is b

oile

d fo

r 1-

2 m

in.

in '

For

mos

ul G

. , T

he p

atte

rn i

s de

colo

rise

d;

orig

inal

col

- o

ur

is

re-

stor

edon

ex-

~o

sure

to

air

-SU

lp h

ur

Dye

. T

his

is

co

n.

, fir

me

d

by

b

oil

ine

a

rhe

patt

ern

is

deco

lori

sed.

pe

rman

entl

y -A

zo

Dye

: o

r ch

ange

s to

ye

llow

- T

hi8

ZO

kO

Dy

e M

ixiu

re.

Th

e

co

lou

r ch

ange

s to

a

b r

o w

n i

s h

shad

e; o

rig-

in

al

colo

ur

is

rest

ored

on

ai

ring

. A

m

orda

nt

(chr

om i u

ni

or

nick

el)

is

pre

sen

t -

'

patt

zrn-

for

A

n t h

r a

- 4

min

. in

q

uin

on

oid

16

% h

ytk

o-,

Mo

rd

an

t ch

lori

c ac

id.

Dye

, e.

5.

rool

ing

and

A 1

z 2

u r

I 71

a

dd

ing

a

Gre

enP

,ora

li

ttle

mag

ne-

Xa

n t

h e

n e

si

um. H

ydro

- D

y e ,

e . g .

gen

sulp

hitl

e ,

C'o

prul

cin.

is e

vcih

ed.

rhe

c

olo

ur

1 The

patt

ern

is 'T

hepa

tter

ncha

nges

ch

ange

s to

' de

colo

rise

dt ,

to

r e

dd

i s h

- r

ed

dis

h-

1

brow

n; o

rig-

in

al

colo

ur

isre

stor

edby

ac

tive

o

ry-

pen.

Chr

oni-

iu

ni i

s p

m-

en

t- A

nthr

a-

qu

ino

no

id

Aci

d - m

or-

dan

t D

ye,

e.g.

A1i

:ari

n V

irid

inr .

perm

anen

tly

oran

ge, g

reen

ish-

-A

zoic

Dye

. ve

llow

or

blac

k,

Chi

s is

co

n-

ori

ssca

rcel

yaf

- fi

rme

d b

y

fect

ed-V

at Dye.

.ste

epin

g a

pat,

tern

in

'(C

'ule

rlon

Jad

e G

reen

co

ld

ethy

l- '

ened

iam

ine,

I ch

erry

-red

whe

n t

o

divi

ding

the

he

ated

in

For

m-

rolo

urrd

cx

- ~

osu

l C:

to w

hich

tr

act

into

1 a

litt

le

sodi

um

two

port

ions

hi

sulp

hite

ha

s an

d te

stin

g be

en a

dded

.).

them

afi

tle

- ! vat.

dy

eing

s ar

e sv

rib

ed

in

I co

rlfi

rrne

dbyt

he

the

7th

col.

; et

hyle

nedi

amin

e un

inof

Tab

Ie 1

test

(c

f.

last

V

III.

co

lum

n of

Tab

le

1 V

III.

andp

.182

).

Z C

f. f

ootn

ote

inat

krd

Z in

'ra

bk

VII

I.

TABL

E XI

11

IDE

KT

IFIC

AT

IOK

O

F D

YE

S O

h' C

OT

TO

X A

ND

OT

HE

R C

EL

LU

LO

SIC

FIB

RE

S

(BRO

WN D

YEI

NC

S A

ND

PR

INTS

)

The

dye

ing

or

prin

t is

boi

led

for

1-2

nun.

in

dilu

te a

mm

onia

(cf

. Rea

pent

s. p

. 17

9).

The

solu

tion

is col.

oure

d di

stin

ctly

en

d, a

fter

aci

di-

fyin

g w

ith

acet

ic

acid

and

hea

ting

. dy

es w

hite

woo

l -A

cid

D

a.

(me w

ool

dye-

in

g is

exa

min

ed

as

desc

ribe

d in

T

able

VI)

.

The

sol

utio

n is

not

app

reci

ably

col

oure

d.

A

sam

ple

is b

oile

d fo

r a

fern

sec

onds

In

1 C

.C.

5yo

caua

tic

soda

sol

utio

n:

4 C

.C. 50

,; am

mon

ium

chl

orid

e so

luti

on a

re t

hen ad

ded.

and

the

who

le b

oile

d ag

ain

for

a fe

w s

econ

ds.

Che

so

luti

on i

s co

l-

oure

d de

eply

, an

d .

.-

afte

r ac

idif

yin

g

wit

h ac

etic

ac

id,

A

cons

ider

able

or

V

ery

litt

le, i

f an

y, d

ye is

str

ippe

d*-M

ord.

nt,

Sulp

hur,

Azo

ic, o

r V

at D

ye.

yiel

ds

a co

lour

ed,

smal

l am

ount

of

p

mip

itat

e w

ith

, dy

e is

str

ippe

d an

d

tann

icac

idso

lutio

n -B

ark

be.

T

he

stai

ned

dw

dv

in

9 A

Bu

ic Dye

is n

ot

pres

ent..

-4

fre

sh p

atte

rn i

s bo

iled

for

1-2

min

. in

Sqo

cau

stic

sod

a so

luti

on.

.-

~.

-__

__

~

~.

Whi

te

cott

on

i8 ~

A f

resh

pat

tern

is b

oile

d vi

goro

usly

for

1-2

min

., or

long

er, i

n Fo

rtno

sill

G c

onta

inin

g a

few

dro

ps o

f 70

' T

w.

caus

tic

soda

. dy

e is

tr

am

fe

d '

the

cool

inn

s&tio

n

The

pa

tter

n is

de

- ----'

co

lori

d

perm

an-

The

pa

tter

n is

de

- I

entl

y - A

zo

Dye

, co

lori

sed

perm

an-

'

e.g

. R

istt

ka

rck

en

tly-

AZ

o D

ye.

Bro

wn.

(C

oppe

r or

chro

m-

iuni

may

be

pres

- en

t).

ora

ng

e

co

lou

r;

fibr

e is

dul

l yel

low

; a

mor

dant

(ch

rom

- iu

m,

iron

an

d/or

al

umin

ium

) is p

m-

en

t-A

du

a

uin-

onoi

d M

arl

an

t Dye,

e.g.

br

owns

de

rive

d fr

om -

4li:-

a

ritr

, A

1i:

ari

n

Ora

ttge,

et

c.

wit

h m

ixtu

res

of a

bove

m

orda

nts.

__

- .

-~

~

The

colo

ur

chan

ges

Lit

tle

, if

a

ny

, T

he

patt

ern

is

to

yello

w,

etc.

or

chan

geoc

curs

;a

de

co

lori

sed

t m

ay b

edec

olor

ieed

; m

orda

nt

(chr

o-

prni

anen

tly-

or

igin

al

colo

ur

is

miu

m o

r co

pper

A

zoic

Dye.

rest

ored

on

ex-

or b

oth)

is p

m-

Thi

s is

co

nfin

ied

, Thi

s is

con

firm

ed b

y I

boil

ing

a pa

tter

n '

for 4

min

. in

16?

, I

hydr

ochl

oric

ac

id,

, ro

olin

g an

d ad

ding

a

litt

le m

egne

sium

. H

ydro

gen

sulp

hide

is

wol

ved.

IS.

sent

- (a

)Ant

hzo-

ce

ne

Brm

m o

r (b

) Cu

fck;

(a)

is

utri

pped

by

5%

hy

dro

ch

lori

c

acid

, b

ut

(6) i

s on

ly s

ligh

tly

af-

fect

ed.

by

stee

ping

ca

patt

ern

in c

old

ethy

lene

diam

ine.

di

vidi

ngth

erol

- ou

rmi

extr

act

into

t.w

o po

r-

tion

s an

d te

st-

ing

th

em

a

s

indi

cate

d in

the

7t

h ro

luni

n of

T

abla

\-IT

T.

Cf.

foo

tnot

r m

arke

d *

in T

ablr

SI.

$ C

f. fo

otiin

tr m

arke

d S

in T

ablr

VII

J.

The

pat

tern

is

not.

appr

ecia

bly

af-

fect

ed;

or

it

ch

an

ge

s to

a

pale

r or y

ello

a-

ish

sh

ad

e-

Vat

Dye

. T

his

is c

onfi

nuet

l hy

the

eth

ylen

e-

dia

min

e t

.eR

t (r

f.

last

co

l-

umn

of

Tab

le

TII

I.an

dp.1

82).

TA

BL

E X

IV

IDE

ST

IFIC

AT

IOS

OF

DY

ES

OK

CO

TT

OS

-4X

D O

TH

ER

CE

LL

CL

OSI

C F

IBR

ES

(B

LA

CK

AN

D G

RE

Y D

YE

ING

S A

ND

PR

INT

S)

e0i-

q w

ith

acet

ic a

cid

and

he

ati

ng

, d

ye

s w

hit

e w

ool -

The

dye

ing or p

rint

is

boile

d fo

r 1-

2 ni

in.

in d

ilut

e am

mon

ia (

cf. R

eage

nts,

p.

179)

.

The

so

luti

on

is

The

clo

lutio

n is

$

A Buic Dy

e or

Log

woo

d is

not

pre

sent

. A

fre

sh s

ampl

e is

boi

led

for

1-2

min

. in

so,

cau

stic

sod

a so

luti

on.

co

lo

d

and,

af

ter

acid

ifyi

ng

wit

hace

tica

cid,

ferr

rd

to

wo

ol

(cf.

p.

181)

and

bo

iled

for

1 niin

. in

Formosul

G.

Hy

dro

gen

su

l-

phid

eise

rolv

ed

read

ily - S

u1-

phur

D

ye.

Thi

sisc

onfi

rmed

The

pa

tter

n is

d

ec

olo

ri s

ed

: or

igin

al

colo

ur

is

rest

ored

by

ta

p - w

a t.

e r -

Azi

nc Dye

, e.g

. M

ethy

lene

Qre

y.

(Bla

ck

dyei

ngs

of

basi

c dy

es

, ar

e ao

met

imes

I

mix

t.ure

s.)

Hy

dro

ge

n

sul-

ph

ide

is

not

I ev

olve

d - A

ni-

1ine

Bla

ck.

I T

he

c

ol

ou

r

__

re

d a

nd

:-

chro

miu

m o

r ir

on i

s pp

es-

ent

in

the

p a

t t e

rn-

Lo

gw

oo

d.

The

pat

tern

w

hen

boile

d in

5%hy

dro-

ch

lori

c ac

id,

give

s a

red

so

lu t.

i o n

, ch

angi

ng t

o

v

i o

lo

t

on

ad

din

g

8 t.

a n n

o u

s

c.11

lo

r i d

e.

\ co

nsid

erab

le

or

sma

ll

amou

nt

of

dye

is s

trip

- p

ed

a

nd

w

hite

cot

ton

is

sta

ine

d

deep

ly in

the

cool

ing

soh

- ti

on - S

ub-

at

an

ti

re

D

ye

. A

p

att

ern

is

bo

iled

for

1- 2

min

. in

FO

ITIlO

sUl G

.

Ver

y li

ttle

, if

any

, dy

e is

str

ippe

d-M

orda

nt,

Sul

phur

, A

roic

, V

at.

01'

Phc

nyla

zoni

um

(rl?

din

e B

lack

) Dye.

A f

resh

pat

tern

is

boile

d vi

goro

usly

for

1-2

m

in.,

or l

onge

r. i

n F

orm

osul

G c

onta

inin

g a

few

dro

ps of 7

0' T

w.

caus

tic

soda

. -

-

-

.- _

_

The

col

our

chan

ges

to a

brow

nish

! L

ittl

e.

if a

nv

. T

he

oa

tte

rn i

s L

ittl

e ch

ange

oc-

, The

pat

tern

is

deco

lori

sed

perm

anen

tly

i -A

ZO Dy

e.

chan

ge o

ccur

s;

chro

miu

m

is

pres

ent - A

n-

tbra

qu

ino

uo

id

Mor

dant

Dye,

B.R

. A

liza

rin

de

co

lnri

sed

t cu

m.

altK

ough

pe

rman

entl

y-

the

so

1 u t

io n

Azo

ic

Dye

. m

ay b

e oo

lour

ed

slig

htly

- V

at

by s

teep

ing

a,

Dy?

patt

ern

in c

old

I Thi

s is

co

nfir

med

C

'Gni

ne

Bla

ck.

et h

yle

ne

dia

- by

thee

tliy

lene

- m

ine,

di

vidi

ng '

dia

nii

ne

te

st

~ th

e ro

lour

ed e

x-

(cf.

las

t co

lum

n tr

act

into

tw

o of

Tab

le

VII

I,

' p

ort

ion

s a

nd

an

d 1'.

189)

. te

stin

g th

em as

' de

scri

bed

in t

he

ith

rol

unin

in

Thi

s is

con

firr

ned

I T

ahle

\-ITT.

t Cf.

foo

tiio

tt.

inar

krd t

In T

ahle

IS.

5 Cf. f

ootn

ote

iiutr

lit.d

3 in

Tab

le Y

III

N&

--.uL

Urr

iu

Bla

ck

wv

OC

C~S

IOM

U~ b

e fo

und

oil

Iir

iuts

. *

Iiic

loca

rhou

B

larl

in

uith

atai

id t

he

acti

on of

IwU

iug

dUuk

so

diui

ii I

iypr

hlor

itr so

lutii

iii: i

wlia

lly t

hey

clll

nge

to p

ale

rlat

e-

It c

hang

ea to

brow

n ou

boh

oy i

n Fo

riiio

sul

G, b

ut th

e or

igin

al

wlo

ur la

res

tore

d b

y ar

tlvr

oxy

urii

. C

hroi

iiiu

tii

16 p

rtw

iit.

blue

.