r- - - _OD'SQ_' ~- _"--

(HI!MISfRY Sf' _ u r f 5'y[ LA BlUS Of' A [fCW'R COUiRSE ADAPrED FOR USE I,N TfXTI,lf ILAIJO,RATO "£S

THE METHODS

BEING THE SYLLABUS OF A LECTURE COURSE ADAPTED FOR USE IN

TEXTILE LABORATORIES ~_,..-

;/'"

/'

BY

FREDERIC DANNERTH, PH.D.

Cou sulti l Industrial 'he nist

(formerly of the Dejm-tmellt of Chemistry and Dyemg

._- __ / ............ ' ,....

LIBRtl.R

JOHN

& SONS

LONDON: CHAPMAN & HALL, LIMITED

PRE

wnen t e rea cr las it In the following pages an attempt has been made to systematize approved methods of textile-chemical analysis which are at present only to be found in widely distributed and expensive special works and journals. These methods have for some time formed the syllabus of the author's lecture courses in textile chemistry. They therefore make no claim to completeness, although care has been taken to emphasize the essential points in each case. The student will do well to use some standard manual of chemical analysis such as "Newth" in conjunction with the present volume.

The author hopes that our now prosperous textile manufacturers and merchants may soon realize that accurate methods are not only interesting but necessary in these days of keen competition. At the same time this little volume is intended to be a source of information and ready reference for the textile chemist. To add to the readier understanding of calculations, practical examples

iv

PREI·ACE

to cover the field of chemical and physical analysis of the textile fibers, yarns and fabrics. Dyestuffs, mordants, and finishing materials are treated of not as raw materials

but as substances encountered on the finished goods.

FREDERIC DANNERI'LL

204 WALNUT PLACE, I)HILADELPHIA, Autumn, 1908.

-





'RHR~'RPNrH~
~ .-~ -
---~-~---
IN the preparation of this book the following publi-
cations were consulted:

P. BEAN: The Chemistry and Practise of Sizing and Finishing,
London. 1905, 1906.
BOWMAN: The \Voo! Fibre, Mancheste-r. rRRS·
Cnoss and BEVAN: Ct:llulosc. London. I p,() 5-' fI)OS·
P. IhmRMANN: Textil-chcmische Unte rsuc-hurursmcthoden. Ik-rl i 11, tr)07·
J. HEHZFELD: Die Tec-hnische Pruefung rlc-r ( ;arne unci ( ;(,\\,(·1/(:.
Vienna. 18()o.
r T .()1.'HNr.:l~· C;;:tllrlif'n lIphl'r r li • \Vnll(, (; rur-n lli'n' IRol
J. M. MATTHEWS: The Textile Fibres. N('\\' York. 11)07·
\V. MASSOT: Kurze Anlcitung zur Appn-tur Analyse. 'Berlin, I()CO.
H. SILBEl~:V1A~N': Die Seide. Dresden. rSCJS.
'T'"vt,! 11 r'C!,.rlll'·'; 7., .it ,n" H"r!i"
r, "1" rot. ... r .. ,. .1 r 1 ,. ' , r
'\.J •. L'U,~"'·" '\.-11<;1111;-" Ll-,,'-" ;"'I' .IL 1".·1"", 1 I 'n . ..,1 11 ';.lIl' ". .. Il, I v
EditIon,
v. HOEHNEr.: Microsr-opie ck-r tr-rhnisr-h vc-rwcnrh-tcn Fas{'l"stofTc'. Bcrl i 11.
H)OS·
A r r ,.:~,: r:,.,,.,~,..., .• rl·· • .1 {I,.",,,,; ... ;\ "" I ' ...... Ph;1. ,l.l ,I " ,"',.,
. J i
. . .
\1. I..J!ml{Gu~Vl\"';:': \ ncrmscnc lC('nl1mogH.' ner \,eSlnnnSl.l<ts(·rn. v WI! na.
H>9c.
The Journal of the Society of Chcmir-nl Industry. r .ondon.
The J ournal of the Society of Dyers and Colorists. :
.
The ((Tables for the Idi-ntifirntion of Dyestufr:.; Oil tlu- Filx-r," hy Arthur !
r' ,'. ., . r ,. " • r
1:"<';11 ,I. II >llll;!., '''lll II oll'lII" <1 Il",I 111 i r u .I(1l1lllili 11 1111; ,1'" 1'"1)' III I ,~I·1.1 .
1 .... , • • •
,Ul\! \A)JOrJ!'l.'"i, fllay Ol~ (TlIl"'U!H'Cj In lIH' Y('arr/(Jol( lor \ OlOrI<;IS a rill
"T"", , I ')'I"SIUI'(';
r rycrs C'Il!ll'( I oy 1"""1. /\.. IV1('Ii';. on anmuu 1I1)(,I"S, XCi<:J5, ,
page 47· lJyeslUlls on vcgctanre nners, 11)077 page olC).
;
:
v i



, '
... LIBR

"l"' .....

' ....... __ .......... _.-_.,

PART I

QUALITATIVE NALYSIS.

Reactions of-

PAGE

Wool an rair ers .

Natural silk fi bers " . . . . . . . . IS

Jute and hemp fibers " ".. 19

Cotton, flax, and ramie fibers. " . . . . . . . . . . . . . . . . . . . . . . . . 21

Imitation silk fibers ' " " "'" . 27

Detection of-

Rosin, mineral, and vegetable oil, in textiles .. " .

Mordants on wool. " " " .

on silk" " " . " .

PART II

29
30
-':2
34
36
1
1:
:i4
45 '1".
47 I
48
48
50
50 Sizings on cotton , " .

Finishing materials in textiles " " .

Ana YSIS 0

Wool-cotton fabric " .

Wool-silk fabric '" .

Cotton-silk fabric . " - .

Cotton-silk-wool fabric ' .

Silk-imitation silk fabric .. _ .

Waterproof fabric , .

Anal sis of-

Textile fibers , " - .. '" , . 56

Raw vegetable fibers _ _

Raw v/ool fibers _ .

57 59

Ra'l' silk fibers " .........•.......

vii

, 'j

H

Vlll

CONTENTS

Determjnation of-

The" boiling-off" loss of raw silk .

The" washing-out" loss of raw silk ' .

The" shrinkage" of raw wools .

Moisture in textiles .

Mineral matter in textiles " : .

Oil and gl ease in textiles .

At senic in textiles .

"{IT ' hti , 'lk.t: b .

vvelg tmg In 51 La nes .

Fjnishing in cotton fabrics , , .

Determination of

72 72

81

Tensile strength , _ . . 82

Humidity. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86

Specific gravity. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 87

The fastness of dyes on the fiber ... , . . . . . . . . . . .. . . . . . . 89

MATERIALS, PROCESSES, AND PRODUCTS,

Cotton bleaching , ..

. Turkey-red dyeing .

Anilin-black dyeing .

Mercerization .

Carbonization .

97 J06

114 117 119

ApPENDICES

SteIger and Gruenberg'S Table " .. 125

Areometry . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 123

Yarn counts ' ' .. , . . . . . .. 126

PART IV

GLOSSARY ............•..............•.................• , /3 r

13I

..................... , . . . . . . .. 136

-; a








t---
, -
PART I METHODS OF TEXTILE

INTRODUCTION

THE word" analysis" as used at the present dayincludes all the processes and operations made use of by chemists

In or er to etermine t e constituent parts 0 any compound, or to enable them to identify the substance. The

1 su bstanccs used

b

of a wet reaction. In the following is given a list of the

reazents which will be re uired for the wet reactions·

they should be made up as indicated in order to obtain the best results.

IO% Caustic potash. .... Dissolve 10 grams of potassium hydroxide in 50 c.c, of water, cool and make up to a total

vo

100 C.C.

1% Caustic potash .... Dilute the above solution I :ro, i.e. to 10 cubic centimeters of the 10% solution add 90 c.c.

of water.

40% Hydrochloric add. The concentrated chemically pure add. Specific

TEXTILE CHEMISTRY

10% Hydrochloric acid .Mix 25 C.c. of the above concentrated acid with

r% Hydrochloric acid .Dilute the 10% acid I to 10.

10% Sulphuric acid ...• Dilute the above solution I to 10.

100% N'iiric acid ...•.• The concentrated chemically pure acid. Specific o B .

Calcium hypochlor£te ... A clear solution having a specific gravity of

chloride of lime with water in a mortar.

,

Cross and Bevan prepare this reagent as follows: 2 grams of copper

of a 10% solution of sodium hydroxide. Wash the precipitate

glycerol. Preserve in stoppered bottles, and when desired for use wash

taining about 5% of copper and a relatively small amount of ammonia

copper turnings in tall cylindrical vessels, and the whole is cooled down to

o to 5

mixture copper an ammonia

The solutions so obtained are only stable at low tern

suitable precautions must be observed when using the same.

necessary to dissolve it. An additional 10 grams of mercury is

water. As copious fumes of the red oxide of nitrogen are evolved,

s of sodium

hydroxide are dissolved in roo c.c. of boiling

water. PbO 2N aOH = N

INTRODUCTION

5

Liebermann's reagent ... One gram of Magenta (Fuchsin or Rosanilin) crystals is dissolved in roo c.c. of water. To this is added ammonium hydroxide until the

solution is just decolorized.

Loewe's reagent ....••.. An alkaline copper-glycerol solution.

,10 grams of copper sulphate crystals are dissolved in 100 c.c. of water.

To this are added 5 C.c. of glycelOl and a solution of sodillIlI

hydroxide until the precipitate at first fOImed is just redissolved.

Richardson's reagent .... An ammoniacal solution of nickel oxide.

25 grams of nickel sulphate crystals are dissolved in 300 c.c. of bOllmg water and precipitated with a slight excess of a 10% solution of

sodIum hydroxIde. The preCIpItate IS carefully filtered and washed,

then nnsed mto a 250 c.c. flask contaimng 125 c.c. of ammonia (sp. gr. = 0.88). The whole is now made up to 250 c.c. with water.

Elsner's reagent A solutIOn of baSIC ZInC chlonde.

roo grams of dry zinc chloride and 4 grams of zinc oxide are mixed with

85 c.c, of water.

H oehnel' s reagent Solution I) One gram of potassium iodide

dissolved in 100 c.c. of water, and iodine added in excess.

Solution II) Twenty cubic centimeters of glycerol are mixed with 10 e.c. of water. To this cold

solution are added 30 c.c. of concentrated sulphuric acid.

The fiber is. first treated with solution I, the excess

of reagent is removed with filter paper, and after one or t;vo minutes solution II is applied.

Nickel's reagent A solution of hydrazin sulphate in water.

Zinc-chloride-iodine solution. One gram of iodine crystals, 5 grams of potassium iodide, and 30 grams of zinc

chloride are dissolved in IS grams of water.

Nitroprusside solution. A 2 % solution of sodium nitroprusside in water

The salt may be prepared as follows: A small quantity of potassium ferrocyanide crystals is boiled with strong nitric acid; finally dilute with '.vater and neutralize the free acid 'with sodium carbonate.

The salt is obtained in the form of deep-red crystals.

Test Solutions for Lignin. I) Phloroglucol in IO% alcoholic solution.

Dilute with an equal volume of 10% hydrochloric acid before using. 2) AniIin sulphate

or hydrochloride in saturated solution. 3)

Indol in 5% solution.

6

METHODS OF TEXTILE CHEMISTRY

sulphuric acid. Adamkiewicz's test may also be carried out as given under the reactions

Fucbsin-bisuipliite solution. One gram of Fuchsin is dissolved in rooo c.c. of distilled water. Sulphurous acid is now led into this solution (or a few drops of liquid

, , ,

,

The following arrangement ers IS upon

their chemical composition. Although this classification

materially different from the usual arrangement. Such classification reminds us that the fibers are chemical

extremely complicated.

Mulberrv silk. Jute.

Tussah silk. Hemp.

\Vool. Mohair.

Cotton. Lustre-

Flax. celluloses:

Fibers

from the

Bromelia. Coiro

.

Horse.

Vegetab. silk.

•



INTROD DeTION 7

/'1 ..... " .. .,. .... " ...... ~ .... 1 -h1-. ,.,.,... ,,"' ..... 4·.,; ..... ; ..... ,... ,..."1,..,1-,,,,. 11".,.,.,... ... .1·; ... ;
,-,.I.\,UU.L .I.. .L J.J.IJ'-'J.." '-v ......... ' o • .. "" ..... 1JJ..L........ \.L>""".J. ..
nbers) 0
GROUP 2, Animal fibers containinz no sulphur (silks)
~ ~
r« ''\T. • 1... 1 .c:t. .1.. c., 1.. rl ~ ,1.. 10 0
........-Auur j. v ~5\"'I.a,u.l.\;.. .Ll.U~.L'::' VV,l.J.l.\.,.l..L.L _.[" loU 1.1..1.'- U
reaction (Iignocclluloscs).
rr "R o UP 11 V ('O'pt::l,hl~ tih('r~ which do not .... esnond to

. LJ J.
" 1 • . 0 I, .11 .1 .\
LUl: llbllll1 1 l:UL Ll Vll ~ L.l Ut; I....Cll U1U;:'\;;:') 0
GROUP So ArtificIal fibers or pseudo-silks (lustre-
rplln 1 nc,(>c,l
-/


























_ ..... _._-_---
"_._
-- .. WOOL AND HAIR FIBERS.

The chief analytical differences between these fibers lie in their physical properties. These will therefore be

the fiber seems to melt and then slowly decomposes with evolution of gases. These have a characteristic "empyreumatic" odor, resembling that of burning horn, due to

e mou will owing to the ammonia vapors, a paper moistened with lead acetate solution will be turned black owing to the vapors of hydrogen sulphide which

ride be subjected to dry distillation in a vacuum at a temperature of 3000 C., a bad-smelling liquid, consisting of ammonia water and various sulphur compounds, distills over. The off include e

8

L . __ .. .2 L .... L ...

WOOL AND HAIR FIBERS

SuI hur rna be detected: First b heatin the fiber

with sodium carbonate and sodium nitrate in a combus-

tion tube. The product of the reaction is dissolved in hydrochloric acid and the clear solution tested with barium chloride. A white precipitate of barium sulphate

sulphide is produced. Third, by heating the fiber with metallic sodium in a combustion tube, sodium sulphide is formed. Extract the product of the reaction with water

Nitrogen may be detected by heating in a strong tube with metallic sodium whereby sodium cyanide is formed. Boil with a small uantit of ferrous suI )hate and ferric

Carbon may be observed as before mentioned, if the fiber be strongly heated in a combustion tube .

.

WET REACTIONS. Wool and other fibers obtained from the mammalia arc insoluble in water, alcohol, ether, petro-

Ieum benzin, coal-tar benzene, carbon tetrachloride, etc.

This fact is of value in removing the impurities from the fiber as the mineral matter is soluble in water and the fatty matters can be readily removed by these organic

tion dissolves the fibers on boiling. If cold dilute sulphuric

9

10 METHODS OF TEXTILE CHEMISTRY

acid be added to this solution a precipitate, containing more

white and lustrous, and acquires a "silk scroop."

cold .ro% solution docs not affect the fiber to any marked

·Calcium hydroxide in saturated solution removes most

phuric acid, If ed to dry on the

fiber, will rot the same. A warm 10% solution hardly

affects cr in strength. By s treatment, however,

the latter acquires an increased affinity for the acid dyes.

solution and dried at 1000 the fiber is hardly affected,

Picric acid in saturated aqueous solution dyes woof,

Nitrous acid apparently diazotizes the amino groups of

used to impart a silk" scroop" to the fiber and to render

1

reactions. (1) \\1'001 moistened with Millon's

red coloration. (2) If wool be boiled with a I 00/;; solu-

hydroxide solution be added, a violet coloration will be

"VOOL AND HAIR FIBERS

II

glacial acetic acid, cooling, and then adding concentrated

sulphuric acid, a violet coloration is produced, and the

solution fluoresces Adamkicwicz's reaction). The usc of

a mixture of 1 oxalic acid and concentrated suI huric acid

in which the rrotcid is then boiled h

so

owins b

o isc ~ s reaction. e ] er IS trcate 111 a test t u e

with I C.c. of water, a few drops of Molisch's reagent, and I C.C. of concentrated sulphuric acid. Solution takes place' slowly, and a brown coloration is observed. \T cgetable fibers dissolve immediately with a violet coloration.

Furfurol reaction. If wool be heated with a dilute solution of sugar acidified with sulphuric acid, a red coloration is obtained.

Coloring matters. All the fibers of this group have a decided affinity for substantive, acid, and basic dyes. Alizarin and a few other coloring matters will only adhere aft cr a metallic oxide (like Cr20:J) has been fixed upon the f bcr.

The physical properties upon which depends the valuation of wool and hair fibers arc:

12 METHODS OF TEXTILE CHEMISTRY
I. Elasticity. 6. Uniformity in diameter.
2. Color. 7· Crimpinesg.
" Lustre. 8. Fineness (diameter).
".
4· Length. 9· Tensile strength.
5· Softness. ro. Serrations per inch. The microscopic examination of a fiber is generally sufficient for its identification, and should therefore form

a part of every complete investigation.

GROUP l(a). \VOOLS.1

This class includes. the woo of the Merino" sheep of Spain, Silesia, and Australia as well as the Rambouillet

ranee.

nest gra

very

between

orm-

The

or scales of irregular shape, the appearance of which

sha ed scales seem to over la one another each one

r ng lame r,

length, and serrations is approximate and is therefore not absolute and

mvaria e.

2 The terms, Merino, Lincoln, and Southdown are used in the United States to indicate certain rades of wool rather than the breed.

iiilLX. Ii

. "".,-

GROUP I

I

b cylinder or medullary portion, sometimes called the pith

of the fiber, is absent or invisible. The epidermal scales

small part of their length.

This class includes Lincoln Leicester and Cotswold

wool and represents the diametrical opposite of the fore-

,

o per cm. 00 0 I400 per Inc 1 . idcrmal scales horn and attached

Wool mediu . .ni.

This class of wool is produced by the sheep of South-

down, the Cheviot Hills, Shropshire, Hampshire, Oxfordshire, and Dorsetshirc. It stands midway between the

Diameter: 0.020 mm. (0.0008 inch).

Length: 7 to 20 cm. (3 to 8 inches).

GROUP I(b). I-IAIRS.

1-£ airs of Goats.

Mohair is obtained in Turkey from the Angora goat.

I4 METHODS OF TEXTILE CHEMISTRY

Diameter: 0.025 mm. (0.0010 inch).

on y WI Ig

maznifvin 0' powers if at all. They are regular and encircle

o " b

the whole hair. In most cases the pith is absent, although

it is sometimes seen in the form of a canal 0

Less important goat hairs arc obtained from the alpaca, vicuna and llama of South America, and from the Cashmere and the Thibet goats of China and India.

sense to all South American goat hairs. The common varieties are brown and black. Cashmere is used in the manufacture of the famous "Cashmere shawls." The

Hairs of Other Mcmmals.

Camel hair is obtained from Russia, Syria, and China.

..

o ,

things, in the manufacture of the" jaeger normal fabrics."

Diameter: 0.015 to 0.075 mm.

Length: 5 to 10 cm.

Cow hair is obtained from Siberia Amcri

is short and irregular in diameter; black, white, or red in color. Under the microscope the hair-root can frequently

GROUP I

tail is about 65 cm. and that from the mane about 45 em,

Diameter: 0.090 to 0.250 mm.

The hairs from the dog, cat, rabbit, and squirrel are

also used to a limited extent in the textile and related

industries (in the manufacture of hats, etc.).

In true hair the scales are firmly attached to the cortical

length, and only reveal themselves under the microscope as fine irregular transverse lines on the surface, and by

o e ce S 0 e 1 rous su s ance sows a air y IStinct medullary axis. The shaft, or medulla, is usually firm and straight, and the scales are horny and dense.

In wool fiber the scales are attached much less firml 1 and

their free margin is more prominent, being frequently notched in a more or less irregular manner. The serra-

NOTE. - Some misleading terms used in trade are:

Cheviot shirting: a fabric made totally of cotton.

. .

Cashmere: a fabric: made of merino wool.

Alpaca cloth: a worsted fabric. Vicuna: a worsted fabric. Thibet: a worsted fabric.

JROUP

This group comprises t wo classes of silks; the one

uct of the insect Bombyx mori, while the most important

15

16 METHODS OF TEXTILE CHEMISTRY

uct

'"

some cases in its recognition, but the chemical reactions

are almost identical for all the members of this group.

Dry reactions.

of suI hur in silk is a characteristic difference from wool.

On heating silk in a dry tube an empyreumatic odor is

notice .

Wet reactions.

All varieties of silk have the same ph y-

The pure silk fiber is not affected by any of the ordinary

organic so vents.

on the fiber has a decidedly tendering action. A com-

mon form of this chemical action is the effect of perspIr-

a Ion on Sl s prepare

On acidifying this solution a precipitate is obtained.

Sulphuric acid, if concentrated, dissolves silk almost

Immerse

considerably and loses most of its lustre.

Hydrochloric acid, cold-

y.

solution dissolves the fiber in 2 minutes.

GROUP II

+ur uro reacuon, en gIves par ICU-

lars of this test: "If some cane sugar be dissolved in the not too dilute solution of a orotcid and the liquid be then

cautiousl oured u oon some stronz suI ihuric acid so as

to avoid admixture of the two liquids, a fine violet colora-

"

an equal volume of water for usc.

o

or one

solutions and shows various colors on developing with different phenols C'diazo " reaction).

b

removes the silk gum from raw silk completely, After

being thus" boiled off " the fiber presents its characicris-

Loewe': .. ; rea

thick solution. Distinction from wool

and lustre-

cellulose. )

Elsner's reagent dissolves silk in one min utc.

Raw silk is rather dull in appearance, due to the coverin t of sericin' which is always to be found surroundinz

the fiber. It might be added that this encrusting matter increases the strength of the fiber considerably. Most of the

I7

I8 METHODS OF TEXTILE CHEMISTRY

silk obtained from Japan, China, Italy, and France is of a silvery 'white appearance, but there is also a large anrount

of the ,. yellow " silk produced in Italy and China. The

golden yellow coloring matter is contained in the gum and may be removed by "boiling off. " Under the microscope the silk fiber appears wbite, or yellowish white and lus-

trous. The thread is seen to consist of two distinct fibrils, between 'which is the sericin. The aver age dianrctcr is

0.or8 mm.

Wild Silk.

The raw silk varies in color from light buff to dark broJ,vn. This coloring matter is distributed through

'the fiber, "'Nhile in the case of cultivated silk the color

is contained in the gum and may therefore be removed

by boiling off. In the case of tussah silk the fiber must be thoroughly boiled off and then bleached 'with

sodium peroxide. O\ving to its large diameter(o.050 lnm.)

wild silk is much stronger than the cultivated variety. Under the microscope the fiber is seen to be very broad,

while the cross-section appears wedge shaped. (Distinc-

tion from cultivated silk.) I.JongitudinaI striations running obliquely across the fiber are plainly visible. Irregularly occurring coarser striations due to bundles of circular

threads may also be noticed. The sericin cannot readily be distinguished from the fibroin;' The narrow side of

the fiber appears dark gray with pink or light green spots,

while the broad side is Irregular in thickness, the thinner

parts appearing bluish 'white or light brown.

The most important varieties of wild silk are:

1 The actual fiber-substance.

India from Anthcrca mylitta

pa e green. Fagara: - Obtained in China from Attacus Atlas.

Muga: - Obtained in Japan from Anthcrca assama.

False tussah: - Obtained in northern China from Antherea pernyi (dark brown).

GROUP III.

Of the fibers which respond to the '41igni n test" (i. ('., contain ligno-cellulose) jute and hemp are the most irnortant representatives. They arc both basi fibers, but

Reagent.

Anilin sul hate.

Iodine-sulphuric acid (Hoch-

Zinc-chloride-iodide sol.

c

Yellow.

Yellow.

Phloroglucol + H'Cl, Hydrochloric acid. Basic dyestuffs.

Intense crimson. Yellow.

,strong affinitv.

---"-_ ..... _- -"-_._-----_._ ... " .. __ .

Pith· bl'OWI1. V(·IIClw.

Lit th- ;1 nill it v ,

Jute (Corchorus ca.psulnrisr,

Chromic acid followed by sulphuric acid: bl u« coloration.

H ydrazin sulphate: pale yellow. Concentrated hydrochloric acid changes this color to orange.

P henylhydrazin hydrochloride: pale yellow colora! ion

'9

no nodes are visible.

20 METHODS OF TEXTILE CHEMISTRY

. cresco e: e ce s possess a pecu iar ap

due to irregular thickening of the cell walls. The interior (lumen) appears at some places quite large and at others

not wider than a single line. Not all commercial samples

show thi however. The cell wall a

the cell wall in width. The varying thickness of the walls

of the fiber.

Length: maximum = 3.5 meters.

Diameter: 0.010 to 0.030 mm. Color: . ale ellow to brown.

Lustre: silk .

Hem-p (Cannabis sativa).

Schweitzer's reagent swells the fiber irregularly and finally dissolves it, leaving only the parenchymous

Issue.

Microscope: The forked ends of this fiber serve to dis-

tinguish it from flax. The cells arc irregular in shape, at

times fiat, and then again cylindrical. The inner canal r 11 broad diminishin in width toward the

end of the fiber. The cell walls arc much less regular than in the case of flax. The forked ends of the fiber ter-

Diameter: 0.or6 to 0.025 mm. Color: light buff.

The less important fibers of group III are:

Bromelia.

Sou th America.

Bromelia karatas.

. .

Coiro

New Zealand.

Pita.

Raphia taetigcru. Aga ve rigida.

Crotolaria june-ca.

therefore preferably designated as: Ncw Zealand fiber, Sunn fiber, Manila fiber) etc., reserving the term hemp for the fiber obtained from cannabis sativa.

these fibers is by the use of the microscope. They are composed of nearly pure cellulose and therefore do not

respon 0 C 19n1n rcac .ion; on lC 0 er ran lCY give a pure blue color when subjected to Hoehncl's "iodine-suI huric acid" test. Other reactions character-

istic of cellulose are zivcn below:

1. Sodium hydroxide in concentrated aqueous solution

22 METHODS OF TEXTILE CHEMISTRY

if applied in the presence of air (see mercerized cotton).

removal of the waxy matter which encrusts the cotton fiber. In concentrations of 12% under 10 atmospheres pressure

caustic so a 1SS0 yes a out 50 0 0 cotton.

2. Sui huric acid. Cellulose (c.g. filter paper) dipped

in concentrated sulphuric acid for a moment, then thor-

product is waterproof and much stronger than the original

o

iodine solution. Dilute sulphuric acid, if allowed to dry

on the fiber, causes disintegration and the formation of

hydrated cellulose. (Application in carbonization.)

. H idrochloric acid. Dilute solutions if allowed to

dry on the fiber will weaken it considerably, while con-

4. Nitric acid (sp. gr. = 1.4). Bleached cotton steeped

o shows a contraction of 24% and an increase in tensile

dizes cellulose to oxalic acid, 'while the less concentrated acid converts it into ox -cellulose. This latter substance

may be recognized by its great affinity for the basic dye-

"

s. Nitric acid and sulphuric acid. On treating cellu-

pounds are obtained (collodion, pyroxylin). The nature

of the pro uct depends on the proportion of the two adds

used, the temperature and the duration of the reaction.

6. I-I dro uoric acid. This rea ent converts cotton

and flax as well as ramie into a transparent, tough, flexible,

T

7. Non-volatile organic acids (oxalic, tartaric, citric).

removed, the crystallization of the acid causes rupture of the cell walls, which manifests itself by the brittleness

o t e er.

8. Zinc chloride. In concentrated solutions this reagent rcadil dissolves cellulose. Cotton must be previously

"boiled off" with caustic soda.

9. Thymol reaction. Cellulose treated with sulphuric

assumes a violet coloration.

over. On adding aniline and

I 1. Catcium hypochloriie, or "bleaching po\vder" in

convert

into oxv-

prepared will dissolve cellulose readily. Raw cotton must be previously "boiled off" with caustic soda in order

to remove t1C waxy an the fibers.

olorin r matters. N one of the fibers of this group

possess great affinity for aqueous solutions of dyestuffs, the only exception to this being the substantive colors

24 METHODS OF TEXTILE CHEMISTRY

(benzidines and diamines). These" salt colors," or " direct colors " as they are sometimes called, produce moderately

fast shades on the vegetable fibers.

I4. Dry reactions. If the fibers be heated to I 50° C.

decomposition takes place. When burnt in the Bunsen flame a sweet odor is given off and a very small

amount of ash remains. Cellulose is a carbohydrate consisting of the elements carbon, hydrogen a nd oxygen

Cotton (Go ssypium)

The physical properties upon which depend the valua-

tion of cotton are:

Length of staple; uniformity in length of staple; ten

sile strength; color; diameter of the fIber.

The characteristic varieties of cotton .are:

1. G. barbadense. Including American Sea Islands

cotton, which is strong, lustrous, fine, of uniform diameter and white in color; Egyptian (white in color); Peruvian

(white in color).

2. G. herbaceum, Including India cotton (surat), which

is white, and of uneven diameter; Egyptian (makko), strong, long, and buff colored.

3. G. hirsutu111,. Including American Uplands cotton (peeler) which is classed jnto short staple and long staple

4. G. arboreum or religiosum. Including Chinese (nankin) which is short, harsh, and buff colored.

5. G. peruvianum. Including Peruvian (red), and Brazilian (vvhite) . These cottons are strong, "'{vviry, and

harsh.

The tables on the following page show the relative

values for diameter, length, etc., of the several varieties.

Diameter in Relative Length in
Breaking Color.
Strength.
Egyptian ..... , .. , .. 0.or7 7·5
...................
Indian ............. 0.025 IO
Sea Island .......... 0.009 8
.
,.,
.....................
Brazilian ................... 0.oI8 3·5 White.
Upland ....... , .. , .. 0.oI9 2·5 \Vhite. M icrosco pe : Under the microscope, cotton as a seed overed with a thin

trated sulphuric acid. The lumen or inner canal contains

air, or as 1 pressed firmly together, so that the lumen disappears

which has been twisted around its axis many times,

Flax (Linu1n usitatissi1num).1

Of the numerous tests which have been repeatedly

o b

only a few are worthy of mention.

app lea e on y 0 containing no sizing). If the dry fibers be immersed in olive oil and then pressed between blotting paper, cotton

remains opaque while linen becomes transparent.

st. First remove the size from the sam le

place for about one-half minute in concentrated sulphuric

1 The term linen should be limited to the yarns and fabrics made

2

26 ::\IETHODS OF TEXTILE CHEMISTRY

Wash 'well, place in dilute ammonia water and then dry.

By this treatment the cotton is turned into a gelatinous

mass and mav be removed by 'washing and rubbing. The

J

success of this test is dependent on the complete renroval

of the size and upon the time of immersion in the acid.

Sclnoeitzcr's solution causes flax to swell up strongly; the fiber does not, h01fileVCr, dissolve completely .

Microscope: Under 'the microscope the fiber appears

rcO"ular with a lumen which is in some cases not WIder

Co

than a line. The end is pointed. The characteristics

of the fiber are the dislocations or nodes which occar at

rather regular intervals. These sometimes take the form

of pronounced lines extending across the fiber at an angle of from 60 to 90 degrees. There is no cuticle.

Diameter: 0.05 mm. to 0.20 mm.

Length: 20 to 100 em. This of itself often serves to

distinguish the fiber from cotton, the maximum length, of

which is 5 ern.

Color: yellowish 'white to gray, but it may be bleached

a pure white with potassium permanganate, chloride of

li b ti" bI I' , ":Pi bI h d f b .

lIIlC, eryIe grasseac I.ICeac CI cr 1S lustrous and can often be mistaken for silk at a rough

glance.

Ramie (boehmeria tenacissima).

,J! icroscope: The interior canal occupies about two-

thirds of the whole diameter. Very often lines may be noticed extending through the individual cells and a gran-

ular protoplasm is seen. The cell walls arc regularly thickened so that the lumen is usually uniform. The

extremes have thick-walled, round ends and striated lumen.

Length: 5 to 100 em. Diameter: 0.25 to 0.110 mm. (characteristic). The purified fiber is qu ii"e white, lustrous,




GROUP V 27
generally tubular . form, with bast cells about 8 centi-
In
I
lYlptprc. in lpnath 'T'hP fihPr ic. lpc.c. pl~c.tir' th'.ln UTA"l lpc.c.
'W~ _ b . - ~ ---- ~-, - - ~-.-.- ........ '-'-, --
flexible than cotton, and more lustrous than flax.
The chemical reactions are those of pure cellulose. Lig-
nin C.PPrrlC:: t{) hP pntlrphr !=lhc::pnt in thp T!=lrr1ip fihPr
~ "-~~ . 1 '
,
t
GROUP V.
II
At this time there are as many as five varieties of imita- 1
I
I,
tion or " pseudo-silks" manufactured on a commercial
scale. Those of Chardonnet, Lehner and du Vivier are
made from nitrates of cellulose; Pauly silk is made from I
Schweitzer's solution of cellulose, and Stearns silk (Vis- .~
'Ii
case) . made from cellulose thiocarbonate. All these
IS
nrrvlllrtc. nAc.c.pc.c. -;} rlic.tinrthr rrlpt~lli(' 111drp !=lnt1 thP nr()n_ 1
.r- - - ~- w_ .r- ~--~-~ - - "./ - w - .L .f" ,
1
I
erty of being affected by water. On moistening these $
fibers a gain in elasticity and a loss in tensile strength is ,
n"t;,..p'.l 'hlp
........... v ........... ""..., __
The diameter . according to Massot from 0.028
vanes
mm. to O.O.i" mm., the coarser numbers being sold as
"~rtifiri~ 1 hf"\rc.p'h~ir "
__ w • ________ ~_ ._
The specific gravity varies from 1.50 to 1.53, but in no
case falls as low as that of natural silk (1.:~o to 1. 40). .:1
'T'hp 'Vplnli'71P fp1!Jsilp ~f'Vp'YI.ath. nf c::pvpr!=ll v!=lriptipc:: ic:::. alvpn 1
~ ·0 0 'i
below:
;i

1IJ"....,,,,, Tensile Strength. Relative strength
. \ till berrnarm) .
Wet. Dry. j
"
Chardonnet ................ ,
2.2 12 50
Lehner ..... " ............. 1.1) 17 68
du Vivier .......... : ....... 2.0 15 24
Pauly (Glanzstoff) .......... 3.2 I9 - \
Stearns (Viscose) ........... 3·5 21 -
Mulberry silk .............. _- _ 100 l
TU~5;ah !=:ilk -- - I26
......... , ,
l' ODS OF TEXTILE CHEMISTRY

he valuation of lustre-cellulose the following points

should be considered: Tensile strength of the dry yarn;

~ . arn' diameter' uniformi t .

~ v

di arneter; brilliancy; softness; elasticity .

.

t tenvtam are dissol~red in concentrated sulphuric acid. If pyroxy-

Ii n silks arc immerse In t IS reagen , ey assume an intense blue color due to the presence of nitro groups. d Paul r silk are not made from nitrated

cellulose and therefore do not give this reaction.

cellulose but .does not dissolve it even on boiling. (Dis-

tinction rom na ura Sl c.

Loeuie's reagent does not dissolve lustre-cellulose even

on heating. (Distinction from natural silk, quantitative r tion.

Iodine-sulphuric acid colors lustre-cellulose a blue.

Coloring matters, even the basic dyestuffs, arc readily

. .

remove rom eir aq u 0

lustre-cellulose, particularly Chardonnet silk. This great

affinity of lustre-cellulose for the dyestuff makes it necessarv to observe zreat care when d ein this material.

Dry test. Lustre-celluloses when held in the Bunsen flame ignite with a flash like that observed in the case of

Al icroscope. When examined under the microscope

t ese ers appear WIt eep ongitu Ina striations an

distinct air bubbles. Examined in a ray of olarized

light, they show double refraction.

silk be treated in separate beakers with Fehling's solu- .

on a wa er- a 0 rive 0

placed in a test-tube with I c.c. of acetic 0.5 c.c. of concentrated sulphuric acid, when a

DETECTION OF OILS IN TEXTILES 29

tion, Chardonnet silk, owing to its reducing action, 'will

Pauly and Viscose silk the liquid will remain blue. Now prepare a reagent consisting of 20 g. zinc chloride, 2 g. potassium iodide, o. I g. iodine and 15 c. c. water. If Pauly

and Viscose silk be then treated 'with this reazent and

its blue-green color while the Pauly silk quickly loses its color on washing.

Detection of Oils in Textiles.

a stiffening in lining fabrics. For these purposes the oil is diluted with some easily volatile solvent so that it may be

am

the fabric is extracted with petroleum benzin or coaltar benzene in a Soxhlet apparatus for about 30 minutes.

2. Mineral oils. These oils are at times found on woolen yarns and fabrics, having been used as a lubricant

be encountered alone some vcaetablc oil beinz

admixed. In all cases their presence should be the cause

(

30 :METHODS OF TEXTILE CHEMISTRY

for complaint, for it is extremely difficult to remove them from the goods by the ordinary scouring methods. For their detection the sample is extracted with low-boiling

Iigroin (previously redistilled to remove tarry matter) .

The residue left jn the flask after evaporating the solvent

is boiled with a solution of alcoholic caustic potash. It is

necessary to use alcoholic potash solution, as an aqueous

solution readily emulsifies mineral 011. If mineral oils are present in the fabric they will be seen as small globules on the surface of the potash solution, for, being hydrocarbons, they are" unsaponifiable."

3. Vegetable oils. "Non-drying oils" or fats are found in all woolen fabrics to a greater or less extent, having been used for spinning the yarns,' To prove that the oil

contained in a particular sarnple of goods is purely of

vegetable origin It should be extracted and saponIfied

with alcoholic potash solution. The result of this treat-

ment should be a soap completely soluble in distilled

water.

Detection of Mordants on the Fiber.

Every finished article may contain dyes, mordants, sizes, and finishing materials in addition to the fiber of which it is constructed. The assistants used in the dyebath, such as tartar or glauber salt, do not come into

consideration at all; "turkey reds," however, will be found

to contain both the oil and the mordant (alumina). Fin-

ishing IuateriaIs may as a rule be removed from the fiber

by simple boiling with water; while the mordants, being

m~re firmly fixed, are obtained after ignition of the fiber or on extraction of the fiber with various solvents.

1 In the spinning of worsted yarns on the " French System " no wool

oil is used. )

ION OF MORDA The ignition method is often found to be preferable

as the dyestuffs are thereby destroyed. All the nonvolatile inorganic constituents are found in the ash, and

ble before and after ignition.

o phosphates .

.

oxide are insoluble, and if present the ash rnust be [used in a silver crucible 'with potassium hydroxide. This is

sulphide passed through the mixture. Pb.Cu.Sb.Sn are

water; (2) treating with 2% sodium carbonate sol ution; treatin with OJ ace ic i

extracts are united, acidified and tested with ferric chloride, which gives the black" ink" reaction.

eic acid com ounds of alumina or some simil. r

metal) are decomposed with boiling dilute hydroch lorir:

. .

an exammed. portance in the

Iron compounds will be found with 10 wood. In this case

32 ~IETHODS OF TEXTILE CHEMISTRY

any color reactions so that the iron must be removed by

treatment yrith 5% hydrochloric acid, after vlhich the test

with potassium ferricyanide may be applied.

Till compounds are looked for in the ash as gIven

ave •

. Another method for examining dark colored fabrics con-

sists in immersing the sample in a solution of bleaching

powder of 1° Be, whereby the dyestuffs are destroyed. If necessary the solution may be made of 2° Be, or it may be heated slightly, or it may be acidified "with acetic acid. The appearance of the bleached fiber thus obtained will at times suggest the presence of chromium and iron. If it be white, aluminium or tin may be present. Confirm aluminium by dyeing in an alizarin bath.

Detection oj Weighting on Silks.

The \\ eighting nraterials used for silk are either volatile

(that is, organic) or non-volatile (inorganic) , so that the

determinations rnust be made accordingly. The volatile

matter is removed from the fiber by means of various

solvents, while the mineral matter is looked for in the ash.

Colored silks may contain antimony, zinc, aluminium, tin, phosphoric, silicic, or tannic acid; glue, oil, glucose, cane sugar, starch, dextrin, glycerol, or gum arabic.

Black silks may contain chromium, zinc, aluminium, tin, iron, lead, phosphoric or silicic acids, prussian blue, and organic matters.

1. Glue and tannic acids (if not combined with iron

or tin) are soluble in water at 60° C. Both may be present.

Tannin in aqueous solution gives a dark coloration or

test (cone.

DETECTION OF \VEIGHTING ON SILKS 33

precipitate with ferric chloride. Glue, if in solution alone, is precipitated by dilute solutions of tannic acid. If basic

extracted may be determined. Fatty acids are due to and oils used in the brizhtenin

cold water.

Cane sugar is recognized (after inversion 'with dilute

tannic aci , and phosphoric acid are warm 5% hydrochloric acid. 6. The ash may contain silica, tin, aluminium, and

Mix the powdered ash with fluorspar and cone. sulphuric acid. Warm gently and detect the escaping silicon

the 'whole 'with '\"'1 ater of it.

Add ammonium molybdate to a portion. A

inous precipitate indicates aluminium.

Detection of Sizing 011, a Fabric.

The sample is boiled with water for about tw in order to remove stiffening materials, soluble sa earthy matter. Filter the extract.

tests:

Chlorides. A small portion of the solution i:

fied with nitric acid. If silver nitrate be added t white precipitate of silver chloride will be obtainec chlorides usually present are those of zinc and mag

Sulphates. To a small portion of the soluti hydrochloric acid and barium chloride. A white tate indicates a suI hate. The suI hates usuall

are those of magnesium (Epsom salt) and

(G auber sa t .

Glue, gelatin, dextrin, and gum are precipitate the concentrated filtrate on the addition of Glue if present will give a precipitate with tann Dextrine is detected when the filtrate is exam the polariscope; it is dextro-rotary. Gums are

added to the almost neutral solution. A small quantity of hye acid is then added before testing with ammonium molybdate.

itate with the usual

DETECTION OF SIZING ON A FABRIC 35

testing with Fehling's solution.

Glycerol. - If the concentrated filtrate be heated with

II. The RESIDUE may contain starch, mineral matter or fats, etc.

Starch rna be readil detected by the blue color which

it gives with dilute solutions of iodine.

Mineral matter. Gypsum (calcium sulphate), Blanc fixe (barium sulphate) and China clay (aluminium sili-

ca e are teste

analysis.

Fats and Colophony. - An original sample of the fabric

.

a pre-

1 per 1

is prepared by steeping 10 grams of ground malt in 1000 c.c. of water at 60 to 6 0 C. The fabric is immersed in

thoroughly washed in order to free it from the dissolved starch. Within the last two years a special preparation of malt has appeared in commerce under the name of

" diastafor." This can be used in a concentration of one

gram per hundred cubic centimeters of water.

-

~ o

.r"'

;:::

<J) 0 ::i+> o

a:

H

t:: o

.~

.....

r'l<

o

if]

Z o

H

~

~

IU

>

o

I I

:;:: :l 00;:::

u

u

Q) III o o

-

!Il ctI ~ <Il ~.~ a

I

.. a o C)

....

C)

ffl OJ

OJ >

'0 u

o <Ilq::

(/)

I o o

- ~

aj

tl E

aj 0

u:

I=: o

.~

-

Q)

be

'--'

u

I

.....

0.

.....

(,)

~ 0.

~

o

.5

...,

C1l

..-.

"_

-

-

o 5;i

.~

o

~ o

...

+-'

.2

o Vl

C!.l

.5

'0 o

-

Z

.......

I:Q

ill til c

g

-

u

I Q) ;..., c,

;..., o

I

;:l eo

o .......

.~

. _

s

.....

[J).

o

'0

o ...,

. E 8.

Q)

.:: o

._

'7'

I .......

6 0

..... Q)

5' ()

.S "'=

...

'0

lfJ

....... .....

c:;

::J

S

S

::l .0

....

'0

....

...

• • C':!

Cl) r.tl

.E ~

CD ....

0.0

C)

E

..... Co!

~ C)

o

40 METHODS OF TEXTILE CHEMISTRY

Survey of Finishing Materials used for Textiles.

I. FOR STIFFENING. -, The starch of wheat, potato,

rice, corn, and sago; flour, dextrin, glue, gelatin, glucose,

gum arabic, gum tragacanth, gum tragasol, Iceland moss,

Irish moss.

2. FOR SOFTENING. - Turkey red oj), 'soaps, tallow,

stearin, paraffin, olive oil, Japan JNax, spermaceti.

3. HYGROSCOPIC li\.1:GENTS. l\mmonium chloride, mag-

nesium chloride, zinc chloride, calcium chloride, glycerol,

glucose, cane sugar.

4. FOR FILLING. - Kaolin (or China clay, an hydrated silicate of alumina), gypsum (calcium sulphate), talc (magnesium silicate), whiting (calcium carbonate), blanc fixe (barium sulphate).

5. COLORED WEIGHTING AGENTS. - Ultramarine (a mixture of sodium-aluminium silicate with polysulphides of soda), prussian blue Fe4 (FeC6N 6)3' smalt (finely powdered cobalt silicate), ochre (a mixture of silica, clay, and hydrated oxide of iron), indigo carmin (soluble sulphate of indigo) ..

6. ILLOMINATING AGENTS. Copper, brass, silver and

aluminium in a finely powdered condition; powdered

metallic sulphides.

7. FOR WATERPROOFING.-Aluminium, magnesium and

lead soaps, gelatin, tannin, paraffin, caoutchouc, ceresin

(purified ozokerite) , waxes and oils, beeswax.

8. FOR FIREPROOFING. - Sodium tungstate, sodium

biborate, sodium silicate, ammonjum pbospba.te.

9. ANTISEPTIC AGENTS. - Salicylic acid, carbolic acid, formic acid, boric acid, borax, camphor.

-

~~ ..
r: "
,
, ,
j

---I

, ---I


i,
,

, ;;1
1
l
PA R'T' TT 11
jl
I
i
1
l - PART II

MIXED FABRICS IN GENERAL.

FABRICS are made in a variety of grades or qualities in

b

the grade of a fabric for this reason only. This is par-

ticularly true in America, where the fabrics must at the

facturer is compelled to bend the quality to the price

b

by chemicals called filling materials.

b

A person who

tain a fine worsted fiber in the 'warp and a much cheaper

. .. .. .

woo or soy yarn or mg. n ia inon con ams no flax at all; it is made of combed cotton yarns. "Linen

mesh" underwear has been produced solely from cotton

Goods made of linen and cotton can be finished with a

en again zlancc a eared

"' ..

, I

I J

'j

I I

44

:METHODS OF TEXTILE CHEMISTRY

to be identical were offered at 50 cents and $1.25 per vard. The analysis showed that the first contained 50% ~ottonl ,,,hIle the second contained 25% of the 'vegetable

fiber. These are but a few of the nlany examples of

falsification, or rather substitution, which serve as illustrations at this point. One flagrant abuse of a term has been 05seryed in recent years in the case of "merino."

This name was originally applied only to the vv'ool obtained

from sheep bearing the same name. It is one of the finest wools at the disposal of the textile industry. After a while the term merino was applied to mixtures of "vool and

cotton containing from 5 to SoCX) cotton, and now to avoid

buy In ourrygoo s stores pure merIno un erwear" which contains cotton only. The "~vvooly" effect is ob-

tained by napping or "raising" the fabric. There are three different ways in which fibers may be mixed in a fabric so that by the use of onc or more of the::;e, various

effects may be obtained.

I. The rQ7J) fibers are mixed before spinning. Underwear fabrics made of "merino yarns," and certain umbrella cloths containing silk and coHon, will serve to

illu~trate this rnethod.

2. Two" single" yarns are twisted together. This may often be noticed in cheap suitings, where a black shoddy yarn is twisted with a fine yvvhite cotton yarn, producing

what is kno'\vn as a "pepper and salt" effect. In better-

class goods this same effect is obtained with silk and worsted yarns.

3. Tuft) d~tJer(!;nt fibers are used in warp and filling.

Cotton or linen being stronger is generally chosen for the

\varp, while wool, worsted, or silk is used fo~ the filling.

1

4S

we have urnbrel

ana YSIS 0 weig rtcc a rics t ic sizing an hnishing materials should in all cases be previously removed by boiling with hydrochloric acid (2 or 3(iD for 10 minutes. T'hc iron weighting on silks can thus be totally removed provided it docs not form more than 2So/c of the sample.

ANALYSIS OF A \VOOL-COTTON ABRIe.

cotton in Schweitzer's solution; (4) aration of the \varp and filling Method I. The fabric is boiled for about IS minutes in a 5~~'1 solution of caustic potash. The residue, which is cotton, IS washed well to remove the alkali, then dried

EXAMPLE:

\Veight of the sample (air-dry) . . . Weight of the sample (after treating)

Loss (-wool). . . . . . . . . Percentage of wool . . . . . Percentage of cotton. . . . .

5 ·.V grams 2.27

3.05

57·3 ..P·7

NOTE. - Owing to the fact that cotton is slightly attacked by this treatment, an amount e ual to % of the weight of the cotton found

= 2.I~ and

cotton

is added and a corresponding amount subtracted from the wool figure;

wool

46 1fETHODS OF TEXTILE CHEMISTRY

ill ethod 11. Finishing materials are first removed from the sample by boiling in r% solution of hydrochloric

acid followed by rinsing in a solution of sodium carbonate (0.5 g. per liter). The sample is now immersed in 80%

sulphuric acid for r 2 hours. It is finally washed well in 50% alcohol and filtered off, using alcohol for 'wash-

ina the residue. The vlcight after drying in the air

b represents wool.

...lIethod III. This method finds very limited application because of the diffirll11-y with 'which ordinary cotton

dissolves in the ammoniacal solution of cupric oxide.

The insoluble residue left after treatment represents wooL

J.11 ethod IV. The mechanical analysis of fabrics is in many cases quite as satisfactory as the separation of the fibers by chemical rneans. For this rnethod it is

however essential that the yarns be made wholly of one

fiber- the \varp may for instance be of cotton and the filljng

totally of 'wool. The sample is cut exactly parallel to

the warp and filling, vveighed, picked apart, and the warp and the filling threads weighed separately.

Meiluui V. Pinagel has devised the follo1Aring modi'

fication of the caustic soda method. The analysis

requires about 5 hours: (r) remove all grease by ex-

traction wi th a volatile sol ven t; (2) remove finishing materials by treatment vlith hot 2% hydrochloric acid for

r 5 minu.tcs. Wash thoroughly with distilled water, dry in a weighing bottle at I 10° C. and weigh; (3) remove

the wool by boiling in a 2% caustic soda solution for 15 minutes, occasionally adding ·vVater to replace the loss by

evaporation. Rinse the remainIng cotton in water, hydrochloric acid and distilled water, Dry and weigh. The

following constants are used for the calculations,

XAMPLE:

Weight a ry sam ple after egreasmg ... __ .. ... _

Weight of sample after NaOH boil. - .. - 5. 2437 g.

Add 3 - 5% - . - . -. - . - - . - . - .. - . _ .. - . - o. 183$

Dry cotton - _ - 5.4272

Add 8.5% 0.4613

Normal cotton 5.888S

Wool removed by NaOH 4. 13I8

Add r% - _ __ .. o. 04I3

Dry woo I . . . . . . . - . . .. - . . . . .. - - - 4. I 73 I

Add 17% - - . - . - ....•................. ~Z09_±

9·559° g.

4.1318

Normal wool .. _ _. _ .. _ 4.8825

NOTE. - In the United States the amount of moisture in "normal" wool is usually taken as I5% instead of 17%. (Compare page 68.)

, I

I ,

ANALYSIS OF A SILK-WOOL F ABRIe.

Method I. Treat the sample with dilute hydrochloric acid and then with sodium carbonate, in order to remove finishing materials, etc. Dry and weigh. A concentrated solution of h drochloric acid 0 is now heated

to 500 C. and into this the sample is dipped for 2 or 3

minutes. B~ this treatment the wool is hardly affected,

while the sil: is dissolved. Dilute with water, and filter.

Ij

The weight of the dried residue represents the amount

of wool present.

Method I I. The silk is dissolved by immersion in an ammoniacal nickel hydroxide solution for 5 minutes at 20° C. (Richardson). It will usually be found that the

~. I

'iiI\liW S 7111

8 IvlETHODS OF TEXTILE CHEMISTRY

this is the case the mixture of hydroxide and ammonia should be thoroughly shaken before using. After boiling the sample in this turbid liquid for 5 minutes it is re-

moved rinsed and then thorouzhl washed with I (XI

hydroxide. The residue of wool is then rinsed again, dried, and weighed.

Method III. The silk is dissolved in a boiling solu-

b

fected. The residue (wool) is finally well washed with

r% hydrochloric acid, washed with water, dried and wei hed.

Method 1. The previously weighed sample is immersed in Loewe's alkaline-copper-glycerol solution at a ternperature of 50° C. for IS minutes. The residue of rattan

is then rinsed dried and wei shed.

ANALYSIS OF A WOOL-SILK-COTTON FABRIC.

b. Remove finishing materials and dyestuffs by boiling in 3 % hydrochloric acid for ten minutes. ,

.\NALYSIS OF .\ \\f()OL-SILK.-COTTON FABRIC 49

c. Remove the silk with ammoniacal nickel hydroxide

il II

b

the amount of each constituent may be determined. The

final residue of cotton will in both cases be found to be

Method I I (von Remonti, a. Weigh out 4 samples of

b. Boil 3 of the samples in a 3o/c! solution of hydrochloric

c. Rinse well in order to rC1110VC all the acid (residue b .

d. Two of the samples obtained by the above opera-

to remove any wool. Wash well with water. (residue J).

tion is boiled for 15 minutes with s?1o caustic soda in order

lese are

The first loss represents finishing material; the second

cotton.

o wa b~

for com aring the value of such fabrics. The two chief

JYIETHODS OF TEXTILE CHEMISTRY

alb lose (imitation-silk) may be analyzed by treatment with

Loewe's reagent. Genuine or mulberry silk disso vcs in this

. . .

cellulose is not affected. The residue left after treating a

weighed sample will therefore represent ustre-ce u ose.

INATION OF WATERPROOF CLOTHS.

The incrcasinz number of so-called "raincloths," for

which the claim is made that they resist the penetration

articles for which waterproof fabrics arc demanded arc raincoats and umbrella covers. Three other articles

paring fabrics in order to make them water-resistant, arc:

1. Impregnation with metallic salts.

2.

4·

solution by means of Schweitzer's

cloth.

rcssing 0

ock of wax. By another in benzin and the fabric

EXAMINATION OF WATERPROOF CLOTHS 5 I

The second

imitation leather, etc. The fabric is passed between

dress goods.

U 1 of this class of fabrics we have ossamer cloth mackin-

II

I

tosh cloth, bathing caps, etc.

b

solution of Cll ric oxide which dissolves the cotton on

the surface to a slight extent. A passage between hot

1;

ro ers comp .es e opera Ion. The determinations to be made in the examination of

4·

2. The weight of the fabric per square yard.

3. The amount of matter soluble in 3% hydrochloric

6. The waterproof value.

1. Wool is separated from cotton by the usual method

o

1 If a solution of cellulose in Schweitzer's reagent is used in place of

.. .. .... ..

is obtained.

then represents the amount of wool present. Wool is separated from silk by immersing the sample in concen-

5~ :METHODS OF TEXTILE CHEMISTRY

er cent is added to the weight of the

The difference between this and rooo

trated hvdroc one aci 'or 3 minu es a 50 ., were y

'" '"

the silk is dissolved. Linen is separated from si k by treatinz with an alkaline glycerol-copper solution, whercbv

b •

inc qua ny whilst the lower grade cloths consist of wool and cotton all cotton. The" e er and salt" effects often ob-

worsted yarn with a white thread of cotton, worsted, or silk. The term" gloria" is generally limited to fabrics

ous ualitv of these umbrella cloths is due more to the

wca \'C than to any finishing materials. However, in the case of heavily weighted silk covers, the loading

proof.

2. The weight of the fabric may be determined by

0.02949,

The factor 0.0295 is sufficiently accurate for technical work. It is derived as follows:

3. By treatment with a 3% solution of hydrochloric

acid for I minutes an soa s which rna c r i

ATERPROOF CLOTHS 53

I ram = o.

I sq. meter = 1550 square inches.

I sq. yar = I296 square inches. I296

o

1550

be decomposed and the inorganic matter 'will to a large

4. cas w IC 1 remain In

and drying the residue of the previous determination ar e soluble in ether and can ther cfare be cstilIlated by

5. The ash is determined by igniting a 'vveighed sam-

extracting the sample in a Soxhlet apparatus.

plc in a porcelain crucible until all the organic matter

has been oxidized or burnt off. The weight of the residue represents non-volatile mineral matter.

6. The waterproof value of the fabric may be determined by the following method, which has given good

results:

A sample about two and one half inches square is

:1

.~

stretched across the mouth of an ordinary thistle tube/ takjng care tbat tbe sample contains no selvage, as tbis

is generally more pervious than the fabric proper. Fasten

the sample securely by means of a string around the neck

of the tube so that the face of the goods will be toward

1 If the diameter of the mouth of the thistle tube is 3 em., the area of cloth exposed to the water will be: 3 X 3 X 0.7854 = 7.06 sq. em.

54

METHODS OF TEXTILE CHEMISTRY

the inside, i.e., toward the water. The thistle tube filled

with distilled water at 20° C. is supported by a clarnp

above a graduated cylinder, and the amount of water passing through in 5 hours and in 10 hours is measured in cubic centimeters. A fabric which allows no water to pass through in 10 hours is considered first class. An-

other point which may be observed is the time which

elapses before the appearance of the first drop on the

outer surface.

The examination of rubbercoated cloths includes several special tests which are given below.

7. The percentage of "rubber and coating materials"

is determined by immersing the goods in solvent naphtha.

or carbon disulphide for several hours in order to soften

the coating; this is then removed by scraping with a blunt knife edge and the last particles removed by treatment with boiling carbon disulphide for 30 minutes. By weighing the sample before and after treatment, the loss,

i.e., the percentage of coating material, may be deter-

mined. A sample five inches square should be used

for the test.

8. The tensile strength of the fabric is determined before and a/tell' the coating has been removed, as the coating of rubber is vcr y often depended upon

to cover up a poor piece of cloth. For this test the

ordinary cloth testing machines of Schopper or Kohl may

be used. 9· The drying test should give some idea of how a rubber cloth will wear when subjected to high temperatures. For this purpose the sample is placed in a dry-

jng oven heated to 50° C. for 5 hours and then

allowed to lie in the air again for one hour. The" feel"

~ ... ------------------------ .... ---------------------

of the cloth at the end of this test will show whether it has

10. A qualitative test for the mineral matter is sometimes desired and may then be carried out according to

which may be encountered are: sulphur; sulphides of sodium, lead, and antimony; oxides of magnesium and

stances may be detected by careful incineration in a porcelain crucible. Sulphur is determined quantitatively

nitric acid.' The sulphuric acid so obtained is determined

Warp and filling: worsted yarn, Weight per square yard:

Breakin strain:

in. Ion

and 2 in. wide).

Matter soluble in 3% ncr.

Ash (mineral matter) :

Water oroof value: After

water were visible on the outside of the fabric IS minutes after startinz the test.

56 METHODS OF TEXTILE CHEMISTRY

ANALYSIS OF TEXTILE FIBERS.

ining into the chemical constitution of cellulose but have come to no final conclusions. Cellulose forms the essential constituent of all vegetable fibers and belongs to the

Per cent

Car bo n .. - ........•................ - ..... - - - .. - . - ... 44· 4

Hydrogen _ . __ _ . __ .. . _ . .. _ 6 _ :2

Oxygen - - 49.4

proteid containing one or more ammo groups. average composition is:

Per cent

Carbon .. _ .... _ .....•.. _ ....•...•..•.•...... e. e' •• e •• 51.0

, , ,

Mulder, Silbermann, Vignon, and Richardson have at different times observed interesting reactions of the silk fiber and seem to agree that it is a proteid possessing the

Carbon - - .•......................... - . - 48 . 5

Hydrogen - . - ..•. - - . - _ - _ - - . - - - 6. 5

Nitrogen _ ......•............... __ __ . _ .. I9.0

Oxygen __ . _ . _. _ ..... . _ . .. .26_ 0

ANAL YSIS OF TEXTILE FIBERS

57

!

I;

All of the investigators have proposed formulae for the silk-fibroin but the a roximate em irical formula seems

ANALYSIS OF RAW VEGETABLE FIBERS.

For the proximate analysis of these fibers Cross and others have proposed the following determinations:

3. "Boiling-off" loss.

4. "Hydrolysis" loss.

5. "Mercerization" loss. 6.

1. A 5-gram sample of the fiber is dried in an oven at I 10° C. until its weight is constant. The loss in weight is calculated as per cent of the original sample.

e en a e organic rna er IS comp e e y OXI ize .

It will be found to be low in true celluloses (cotton) and high in the pectocelluloses (raw flax), while the lignocelluloses (jute) occupy an intermediate position.

tion of the fiber.

4. This is carried out in order to estimate the effect

58 METHODS OF TEXTILE CHEMISTRY

of bleaching, scouring, and frequent washing of the fiber. It is determined by boiling the sample in I% sodium hydroxide for one hour, whereby the fiber is hydrolyzed.

5. The fiber is placed in a 30% solution of potassium h droxide for one hour at a tern erature not exceedin

and finally dried. By this treatment the acid-soluble impurities are removed without affecting the fiber materially.

8. This is of course the most important determination, for, after all, the cellulose is the .most valued constituent of the fiber. Boil for minutes in a I solution of

weighed.

9. The fiber obtained by purification with acid (7) is analyzed in the ordinary combustion oven or in the wet way by means of chromium trioxide (CrOj) and sulphuric acid. In the latter case the mixture of carbon monoxide and dioxide is obtained and measured in the

" - "
r


.... T T .... r r+r rv '""'"" ........ 'l"Y7 'l"T T r-.,..... T I"'r..
.n...I.'in.L 1. ..::l.l..:::l Vl.' .L"-~VV 'IV VV.l.J J';J
The analysis of raw cotton shows approximately:
Per cent I
Cellulose •....... _ . _ ..... ____ . __ .. _ . __ - ___ - __ - 87.0 to 9I.0
Water ..... _ .. _ . _ . _ . __ . _____ . _ . _ ... _ . _ .... __ . _ 7.0 to 8.0
Fat and wax. . o r:: to 0.4-
T ~11111ar matter o .o c to 0 '7
I ~ .
A<:.h (") T ') to T '7
.
The analysis of raw flax shows approximately:
I
Per cent
Cellulose ......... _ .......................... 71.0 to 83.0
water ............... .. .. .. .. . .. .. .. .. .. . .. .. .. .. ................ b.O to II. 0
Fat and wax .................................................................. 0.5 to 2.-1-
I intercellular matter ..................... ............ :2.5 to 9·5
Ash ... .. .. " .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .............. 0.5 to 5.0 ANALYSIS OF RAW WOOL.

I. Moisture.

2. Grease.

3. Matter soluble in water.

4. Matter insoluble in water (sand and earth).

rylng a 105 • In a s ream 0 ry y rogen.

2. The grease is preferably determined before steeping the sample in water, as otherwise some of the fatty matter is removed. The weighed sam pIe is extracted

,

~

,

NOTE. - If it is desired to estimate the amount of alkaline oleates present, this may be done by shaking up the ethereal extract with water in a separatory funnel.

60 METHODS OF TEXTILE CHEMISTRY

and earth.

4. The insoluble mineral matter removed in the prc-

VIOUS operation IS .

and weighed.

5. The wool finally obtained is dried and weighed.

The following figures will give some idea of the pcr-

100

IS 22

30 21

Low Grade. High Grade.

Per cent

Moisture " .

23

12

rease .

Matter solu ble in water .

Matter insoluble in water .

"Wool fiber .

7

21

6

43

Method of Maercker and Schulz, r. Determine moisture by drying in a stream of h dro en

2. Determine wool-fa

afterward shaking extract with water in order to remove oleates. Separate the two solutions, evaporate the ether to dryness and weigh the fatty resid uc. Evaporate the

distilled

ANALYSIS OF RAW S LK .

61

found in the previous determination. weight represents the alkaline oleates.

The combined Finally

dried, well shaken and then teased out by hand over a large sheet of paper in order to remove dirt, sand, etc. It is then again dried and su bsequentl y weighed.

6. Sand and dirt are determined by difference.

" I

ANALYSIS OF RAW SILK.

OWIng to the great value of SIlk ($4 to $7 per pound)

and the fact that shipments from China and Japan are at times found to be adulterated with large quantities of fat, the examination of this material is very desirable.

The commercial value of such an examination 'will be

easily realized when it is stated that one lot which was examined contained 9% of fat in place of the 1% usually

found in natural silk.

Although Mulder was the first chemist to investigate the nature of raw silk his methods and results have been given a rather low rating by Silbermann. The latter

investigator has spent much time in the chemical study

of the silk fiber, a subject in which he is unquestionably the leading authority. A typical analysis of a white mul-

berry silk by this author is given on the following

Per Cent

ater ...........................•......•...•..•.. ~. ==

Salts .......................•.....••....•..•..••. " 0.30

a.1{ at. . . . .................•................

Seric in. . _ . _ - - . . . . . . 22 • 0 I

Fibroin .................................•........•. 76.20

an be determined in the raw silk accord-

ing to-th-~>"~sual method of drying a weighed sample at 10 0 C. to constant weight.

2. The salts soluble in water may be determined by

~-,-.",:...-

steeping a weighed portion of the dried sample in

30 nu es.

in warm water, dried at roSo C. and

present.

and extracted in a Soxhlet apparatus with ethyl-ether or with C. P. benzene for about hours. The solven .

the flask is evaporated by means of a current of warm air on a steam bath and the residue weighed in the flask.

etween s and the original

weight of the flask will represent the amount of wax and

4· The silk residue from (2) is now "boiled off" in a

soap per liter of distilled water. After boiling for one

The amount which the silk loses in weight represents silk gum (sericin).

! ;

b

in Italian silk to 84 in Japan silk.

SILK.

I !

, I ~ ,

..

grams of perfectly neutral olive oil soap per liter of dis-

ti e water.

this weizht and that of the

silk shows the

"boiling-off" loss.

Boiled-off silk dried at IISo . . . . . . . . . . . . . . . .. 38.9 grams

9.8 X 100

= 20.1 urn.

(Crefeld Conditioning House, Average Values for 1906.)

23.6 24·0 LOS 1.20
18.86 20.0 r. 27 I. 30
25·5 1. 4 1. 5
........ .. .. .. . .. . 4 . . . ~ .. .. .. . .
22·5 0·43 0.50
.. .. .. .. .. .. . .
China .. .................................... 20·43 24.0 2.2S 4.80
Canton ... ............................ . . 2 .28 24.0 2. 8 2. 0 1 These figures are those usually used in calculations and represent

6 J\fETHODS OF TEXTILE CHEMISTRY

DETERMINATION OF THE "WASHING-OUT" Loss OF RAW SILK.

Crefeld Method. A weighed sample of raw silk is ath of distilled wa

................................

.. .. ..

1. I X roo

o·

DETERMINATION OF THE "SHRINKAGE" OF RAW WOOL.

By the" shrinkage" of raw wool is meant its loss in weight after passing through the usual processes of scouring. An experienced wool sorter acquires a rather accurate idea of this loss by examination of the fleeces. The approximation should come within one or two per

45 X 50 = 6!.

40 5

To find the percentage of shrinkage of a wool:

Rule: Subtract the weight of the scoured wool from the weight of the raw wool. Divide the remainder by the weight of the raw wool and multiply by 100.

SHRINKAGE OF RAW WOOL

EXAMPLE: If I28 pounds of raw stock yield 60 pounds

(r28- 60) X IOO = 53.1% (or a yield of 46.9%).

128 To find the cost of wool at a given shrinkage:

u e : . 'LV'L e t e cost per poun the' woo ~n

grease" by the yield stated in per cent.

EXAMPLE: If a wool in grease costs 2 4 cents per pound

and shrinks 40%, what is the cost of the scoured wool?

24

roo - 40 = 60% yield. 60 = 0.40.

The scoured wool costs 40 cents per pound.

In the table belo¥l are given a fe\v "shrinkage" values

of "domestic " wools.

WASHED WOOLS.

Price
lirade. Cost. Y ietd. "Clea.n. "
Cents. Per cent. Cents.
XXX. . · . . . . . . . · . · . . . · . · . · .. ... 3-+ 64 53
XX. . . · . . . . · . · . . . . · . · . · .. ... 30 45 00
X. . . . . · . . . . · .. · . . . . · . · . · .. . . 34 46 73 ERRATA.

Page 64, bne 11 from bottom should lend.

Other things being equal, the money value of two wools offered at the same price will be proportional to the yield after scouring. Thus if a wool which shrinks 50% ( - yield of 50%) costs -15 cents raw,

tho v::tlue of f~ similar wool which sb rinks 40% ( = yield of 60%)

would be

45 X 60

--- = 5-1- cents.

the

e appara us rcq uirc

heated air

DETERMINATION OF :NIOISTURE IN TEXTILES 67

2. sea es sensi ive 0 o. I gram rm y xe

to the oven in such a position that one extreme end of the beam is exactly over the centre of the oven and from which is suspended a reel or cage containing the sample.

.111

i .' I .' .. 1

"

\ I

, "i

'I i

3. One reel and one cage mentioned above, the former for tops and yarns and the latter for wool, noils, and loose material.

i

1

The following data are taken from the pamphlet of the Bradford Conditioning House and may therefore with propriety be quoted as the

The samples are drawn, in the case of tops, from the centre, middle, and outside of the ball and are weighed immediately. The sample should weigh about 500 grams

rom c a ance. e ime requIre

to expel all the moisture will vary with the quality, age, and condition of the tops. The heating in the oven is continued until the sam Ie ceases to lose weight and

68 METHODS OF TEXTILE CHEMISTRY

Weich f l"'d"

elg to woo air- ry ....•..........•....•.. 512 grams

Weight of wool "bone-dry" __ _ .. _ 420 grams

After years of observation it has been found that the various fibers contain an amount of moisture which is

sentative of the amount of moisture which a perfectly dry sample will take up: (Bradford constants).

Cotton yarns __ . _ _ . . . . . . . . • • . . . .. 8 ~%

Silk yarns •....................................•... I I %

Linen yarns .............••.. _ ...•.................. 12 %

a regain loIS

r6% of 420 grams = 67.2 of " normal wool."

wooL The essential part of the conditioning is the determination of the amount of "absolutely dry wool"

EXAMPLE: How much "bone-dry" wool in a 1000- pound lot which gave the above test?

DETERMINATION OF MINERAL MATTER 69

How much" normal wool" in a tcoo-pound lot which gave the above test?

x = 95I.

Ii

rs 0 e a 0 U 13 / c , whether 13 or 15 or the European standard of I8t~

be chosen as the American standard is quite immaterial as the price of worsted tops or of any other textile material is regulated in all cases by the amount of "bone dry" material which the seller knows or estimates the

........................ .).

Top combed in oil I 2.8

Top combed in oil. ............•...........•......... I 2.0

Top combed in oil 11.3

Tops direct from comber __ __ _. 9- 2

DETERMINATION OF MINERAL MATTER IN TEXTILES

the determination a 5 gram sample should be cut up in small pieces and placed in a weighed porcelain crucible. Heat with a good Bunsen flame until all the black, carbonaceous matter disappears. After allowing to cool in a

70 METHODS OF TEXTILE CHEMISTRY

desiccator the crucible is reweighed. The matter remaining

in the crucible is the ash and is calculated to percentage.

EXAMPLE:

Crucible (after drying and cooling)............... 5. 5643 grams

Crucible (with sample of fabric) ..........•...... 10.4653 "

1, j.

}

Fabric (air dry)................................ 4. 9010 "

[ ' f \

! •

I

!

, .

t

Crucible (with ash).. .. . .. . . .. . . . . . .. . .. .. . . . ... 5· 9644 "

Ash (after deducting weight of cruc.) . _ .. _ . . . . . . .. 0.4001 " 0.4001 X roo

Percentage of ash = 8.16%

4·90IO

In certain cases it is interesting to know the moisture content of the sample, and so the following preliminary weighings are made:

f

Weight of sample air-dry ...................•......... 4.9010 grams \Veight of sample after drying in an oven at IOSo C for

one hour 4 4000

Loss ( - moisture) ... .....• __ .•. _ ....•. _ •... _ . . .• O. 50I 0

Percentage of moisture . . _ .. _ . _ __ . _ • IO. 2%

The complete report of this analysis would then read:

N arne of fabric: fireproof cloth.

Moisture ....•..•.•.. _ . . . • . . . . . . . . . . . . . . . . . . . . •• 10.2%

Non-volatile matter (ash) . .................• _ 8. r6%

Volatile matter (fibers, etc.) _ 8r.64%

IOO.OO%

The estimation of the mineral matter is of especial importance in the examination of such fabrics as:

Waterproof raincloths (aluminium, magnesium, and metallic oxides).

J."Vindo"<ll shade cloths (Hollands) (prussian blue, ultra-

,

,

4

marine, ochre and other pigments).

Bookbinders' cloths (gypsum and dye-lakes).

Fireproof cloths (sodium-biboratc, -silicate, -tungs-

state; phosphates).

Hea.vily wejghted silks (tin, jron, etc).

I

Si n cloths calcium acetate, alum

etc. )

gypsum, etc.)

to the

f

yarns spun In 01 an

fabrics. A wei hed sam

es on laced

in a Soxhlet extractor which is connected with a weighed

in order to drive off the solvent after which the weizht

oil in the air-dry fabric may be readily calculated. In

the case of tops it is convenient to weigh out a sample of

weighed sample represents.

EXAMPLE:

A sample of tops was found to contain moisture ....••. I3.2%

Hence fiber + rease = _ ' 86. 8

rams

rease .

"

After extraction the flask + grease weighed ' 28.3490 grams

The flask wei hed _ _ .. _ . _ . _ _. 2 • 6 I 0 "

Therefore grease weighed .. _. ' .... _. _ . . . . . . . . . . . 0.3880 "

72 METHODS OF TEXTILE CHEMISTRY

DETERMINATION OF ARSENIC IN TEXTILES.l

is of little importance. The third and most common source of the arsenic found on woolen goods are the " sheep di ps " applied to sheep for the cure of the scab disease. Thus IOOO grams of a wool flannel were found to contain 5 milligrams of arsenious oxide.

EXAMINATION OF WEIGHTED SILKS.

The weighting on a black silk may vary from zero to 250%. The values of 300 and 400% sometimes mentioned

weighting number, for example, 80%, is given with

reference to the weight of the raw silk (this latter weight is

b b

pounds. From this we see that a "weighting of 80% "

may actually represent a silk containing I05 pounds of

1 For further information on this subject see: Arsenic in papers and fabrics, by J. K. Haywood, Bulletin 86, Bureau of Chemistry, U. S. Department of Agriculture. Also: Textil chemise he U ntersuchungen, Paul Heermann, Berlin, I903.

The data

EXAMINATION OF WEIGHTED SILKS 73

ing = 80%,

EXAMPLE: If the weight of the raw silk = 60 pounds

To find the weight of the finished goods,

60

60 - (60 X 0.25) = 45 (pounds).

To find the percentage of fibroin in the finished goods,

1 !

To find the percentage of weighting in the finished goods,

1

1

The proximate analysis of weighted silks includes a

determination of Prussian blue, silica, tin and phosphoric

acid. See: Luehrig, Chemiker Ztg., I902, 87, page T039;

also Gnehm & Brenzigcr, Faerber Ztg., 1897, page I.

In the 0 ni ted States the weighting on silk is indicated by stating the "ounces of weighting" which have been

added to each pound of raw silk. As the " charge," or quantity of weighting material which the silk has taken up,

varies slightly the dyer states it within certain limits. Thus

it has become a trade custom to allow a variation of two

, b b'

it is understood that r6 ounces of raw silk have been loaded

until the weight has reached approximately 32 ounces.

74 11ETHODS OF TEXTILE CHEMISTRY

. h . . k "(J1 b e a"

Such a \velg ting IS nown as 100/0 a OV p r.

recapitulate:

To

Orizinal lveight of the raw silk. , .. ,. 16 ounces.

o

Weizht of the boiled-off silk .... , . .. 12 ounces.

o

\\Teight of the loaded silk ..... "... 32 ounces.

32 ounces therefore represents an incre.as.c of IOO% above

16 ounces.

The results of the chemical analysis. wj]] show the

amount of actual silk fiber present. From this the amount of 'weighting is calculated by difference and

reported in " ounces per pound." This can be done

\vith the aid of the table prepared by Matthews:

Per cent Weighting, Ounces.! Per cent Weighting. Ounces.'

0-13 12/q 142-158 30/32
13-29 14/16 158-I74 32/34
29-45 16/r8 174-I9° ~~~~~
.11:' .• f.'T T 'X'I ",..... Tr. ...... ,., ..... f..
;.J -r '7 - J'-".' ~1'
6r-77 20/22 206-222 38/40
77-93 22/.24 222-238 40/42
93-r09 24/26 238-254 42/44
r09-125 26/28 2~4-270 44/46
I25-r42 28/30 270-286 46/48 To illustrate the use of the table:

A commercial sample of silk was dried at 1050 C. and

then weighed 0.45 grams. The weighting was removed, the remaining fibroin was dried at 1050 C. and found to \-veigh 0.31 grams.

Weighted silk = 0.45 grams Fibroin

= o.3I grams

V'feIg tmg

- 0.14 grams

0·3I 1 See page 73.

= 45% weighting.

DETERMINATION OF THE WEIGHTING IN SILK.

From the table we see that this corresponds to 18/20 ounces (or an average of 19 ounces). These 19 ounces of weighted silk represent 16 ounces of "raw" (un-

contain

2. Treat in a platinum dish with 100 c.c. of a So/t) solution of hydrofluosilicic acid and agitate frequently during one hour at ordinary temperatures.

.., Decant the solution and treat the sam le with

"

~ .

arge

sample represents the weighting. The action of the fluorine acids on silk is inconsiderable and may therefore be neglected.

rymg

Difference

= L0208 g. = 48.00% weighting.

6 METHODS OF TEXTILE CHEMISTRY

If the "boiling-off" loss be taken at 20% we have the

x = 88.9.

r68_9

which means that the silk has been weighted 68.9%

Moyret's Method. 1. Water. Dry a ten gram sample

1

15% indicates the presence of hygroscopic substances.

2. Substances soluble in water. Boil with distilled

water. Glycerol, sugar and epsom salt will be dissolved.

3. Substances soluble in petroleum ether. Treat a dried sample with the solvent and examine the residue

a ter evaporation, ats an 01 s WI C 1SS0 vc .

4. Substances soluble in h drochloric acid. Treat for

15 minutes in a bath of 5% hydrochloric acid at 40° C. Aluminium, chromium and iron mordants will be dissolved.

bonate. Tannins, etc.

). I n a porce ain

crucible.

Koenig's Method. 1. Water.

Dry at 1250 C. to C011-

100 grams of water.

sodium hydroxide.. The sodium ferrocyanide obtained

I

:~.

WEI HTING ON SILK

tate and oxidize with a drop or two of nitric acid.

I gram of Fe20g = 1.5 grams of prussian blue.

Calculate as catechu-tannate of tin.

The total ir

oxide.

The remaining iron is calculated to tannate.

the solvent action of h drofluoric acid on silicic acid and

is therefore suitable only for the tin-phosphate-silicate weighting.

1. Place about 2 grams of the silk sample in distilled

solution

acid for IS minutes at 60° C.

'. Without washinz lace the silk in a % solution

of hydrochloric acid at So to 60° C. for 10 minutes.

for one hour in order to remove any sericin which may be

6. Wash. in a r% solution of sodium carbonate for

. Rinse well in hot distilled water.

8. Dry and weigh.

table for the calculation of the

METH

The substance obtaine is practically pure fibroin.

ure

b

method is based u on 1(· ehldahl's observation that nitro-

decomposed with concentrated sulphuric acid and after-

b

substances include glue, ammonium salts, amino dye-

stuffs, and silk gum. It should be remarked that the sue-

I. An air-dry sample of the silk (about 2 grams) is

hours with a 3o/cl solution of

which may be in the silk.

10 minutes at 60° C. to remove soluble salts.

6. Rinse thoroughly and dry.

7. Determination: The silk obtained at the end of the above treatment is treated 'with 30 to 50 c.c. of sulpho-

Specially prepared by Kahlbaum.

'VEIGHTING ON SILK

pale yellow remaining. Heat for one-half hour longer to insure the completion of the reaction.

8. After allowing to cool the contents of the flask are

distillation. N O\v add caustic soda solution very carefully (to avoid any loss of ammonia). Connect the flask with a condenser and conduct the distillate into a receiver

mixture in the flask is boiled for about one hour, after which time the residue in the flask is tested for ammonia by means of litmus paper.

mal

rgure 0 m .rogen.

I c.c. of normal sulphuric acid used = 0.017 g. NH3 (ammonia) =0.OI4 g. N (nitrogen) =0.°7638 pure fibroin ..

9·

24.00

fibroin = _ .

the nitrogen content of pure fibroin = _ . _

then one gram of nitrogen is equal to _ . _

and 0_ OI4 gram of nitrogen is equal to .. _

For example:

weight of the original sample _ .. _. 1.0000

18-33%

5 - 45 5 grams fibroin

0_°7638" "

gram

;,. - ',) = -4 2

add II% formoisture ... __ .•. _._. . . 0.5354

hence weighting above par = I - 0_ 535..J. X 100 = 86.77%

0-5354

"

80 11ETHODS OF TEXTILE CHEMISTRY

Nitrogen Method' (alternative estimation). Tlie pure fibroin is placed in a 200 c.c. round-bottom flask, and

treated with 30 c.c. concentrated sulphuric acid. A small

amount of anhydrous copper sulphate is then added and the whole heated for about 5 hours. The end of the

reaction is shown by the solution turning green. Remove the heat and add potassium permanganate until a deep gr een color is obtained. i\Jter alIe'wing to cool

add water carefully. Allow to cool again and pour

the whole into a copper distilling flask, using plenty of

water In transferring it. Add excess of caustic soda) distill off the ammonia and absorb in U tubes with

standard acid.

The percentage of "charge" is usually stated with reference to raw silk containing I 1% of moisture. For exam-

pIe a charge of 40% above par means that 100 grams of raw silk yielded 140 grams of weighted silk. The

amount of bast or gum in raw silk varies within several

per cent, so that it is advantageous to know which variety has been used in the sample. In the table below arc

given the average values which are usually accepted:

Italian (yellow) o •••••••••••••••••••••• 0 • - ••• - - __ ••• 24%

Japan 0 •• 0 ••• 0 •••••••••••••• _ •••• _ •••••• 20

China (white) - - ...• - .. _ - - .. 0 •••• 0 ••••• 24

Canton ....•...... 0 ••••••••••••••••••••••••••• _ ••••• 24

Chappe. . . . . . . . . . . • . . . . . . . . . . . . . • . . . . . . . . . . . . . . . . . .. 4

If Japan silk had been used in the example given above, the fibroin figure would then be multiplied by ~·3· instead ~

1 For other methods of determining nitrogen see U. S. Dept. of Agriculture, Bureau of Chemistry, Bulletin 107. For Steiger and Grucn-

berg's table for the calcul~tion of the \veighting sec Appendix 1.

lure and

DETERMINATION OF THE FINISHING MATERIALS IN A COTTON FABRIC .

. ove 1 a .ool

1. The percentage of filling materials. A weighed sample of the fabric is boiled consecutively in distilled caustic soda solution and I h drochloric

vith

fer-

o

of absolutely dry fiber present. Add 8% to obtain the

" normal" air-dry weight.

2. The percentage of moisture in the air-dry fabric

icty are

by extraction in the Soxhlet apparatus.

4. The percentage of starch, etc., is determined by difference as shown below:

O> ••••• - •••••••••••••••••

'a s, C c.. . . . . . . . . . . . 5 0 ••••••••••••••••••••••••

Starch, etc.. .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5%

The qualitative test for mineral matter in the fabric

) J

cad

dium. The insoluble portion may consist of China clay, barytes, gypsum, chalk, talc, lime or aluminium soaps. These latter compounds will of course be decomposed

82 METHODS OF TEXTILE CHEMISTRY

or less extent. Among these processes may be mentioned,

1. The dyeing of aniline black. In the drying and atures and a

2. The dyeing of "mixed goods" with sulphur colors.

Sodium sulphide has an injurious action on animal fibers; an excess should therefore be avoided. The dyeing should also be done at the lowest possible temperature.

with a consequent weakening of the fiber.

4. The production of mercerized cotton. If properly carried out this process increases the tensile strength of the material, but care must be taken that the temperature of the liquor does not rise above 6 0 or 0° F.

on the wool. Here again the temperature must be kept low and the immersion extended over not more than 5

DETERMINATION OF TENSILE STRENGTH 8

ots.

b render the wool non-shrinkable, concentrated liquors

must also be avoided.

- l ~

tensile strenzth on cominz in contact with water tensile

strength determinations of the dry and moist material

obtained by impregnating with solutions of metallic salts

which sometimes corrode the fiber' raincloths umbrella-

contained in the yarn at the time

cloths and rubber-coated cloths should therefore be

examine

b

the yarn so that it may be used for 'weaving without dan-

ger of breaking. The elasticity of the yarn depends on

of size on the arn and the er-

cing cs e . 9· Shoddy yarns. The carbonization of the vegetable

fiber invariably affects the tensile strength of the wool

fiber, even though the acid and soda have been thoroughly

removed.

10. Bleached coiton yarn and fabrICS. 'The action of chloride of lime is in no case without its injurious

effects on the fiber. In order to ascertain the relative

loss in tensile strength and so observe the "tendering" action the raw and the bleached coHon should be tested.

The determinations are made with specially designed

apparatus made for testing fibers, yarns, and fabrics. It

is encouraging to note that governmental contracts for the ddivcry of yarns and fabrics arc now in almost all cases

84 METHODS OF TEXTILE CHEMISTRY

based on a definite strength of materials, so that in this case also we will soon observe the" survival of the fittest."

Tensile strength is defined as the resistance which a solid body offers to being pulled apart. It is proportional to the area of the cross-section and independent of

return to their former shape after deformat.ion. The elongation which a thread suffers is -

Proportional to the pulling force exerted;

Proportional to the length of the thread; and

Inversely proportional to the cross-section area of the thread.

The coefficient of elasticity is a fraction which expresses

the increase in len zth suffered b ieee of the material

than for yarns. In the following table arc given extreme

NOTE. - Tensile strength testing apparatus is manufactured by Louis Schopper (Leipzig), Max Kohl (Chemnitz), Henry Bacr (Zuerich), Tarnogrocki (Essen). For the testing of fibers the machine built bv A. S. Mackenzie (Philadelphia) yields excellent results. It is the orilv one which has come into extended usc. ~

DETERMINATION OF TENSILE STRENGTH 8

values which have been observed, the numbers indicating

Cotton from 30 (Up and) to 40 (Egyptian)

that the results 0

inter-

Silk from 35 (boiled-off) to 45 (raw)

Jutc from 30 (bleached) to 50 (raw)

to make a complete

in order

preted, c. g. :

N arne of fabric.

Weight per square yard in ounces.

,

P;l"lJ'"' r>. ..... ,.. ;'Y\l"'h (.(,11;,..,rr\

..L .L",,,"-oJ 1-''-'''' ......... '-'.L.L \ .L ......... .L.LbJ •

Ends per inch (warp).

Breaking strain in pounds.

NOTE.-The length of the sample between the jaws of the two vises should be 5 inchps and the wid1h I inch Knitted fnbrics ma.y he cut in

widths corresponding to ten wales.

Yarns and fi bers arc reported as follows:

Name of the fiber.

Diameter of the fiber.

Tensile strengt.h of the fiber. Elasticity of the yarn or fLber.

Size (or count) of the yarn.

Breaking strain of the yarn.

The tensile strength of yarns of the same material will

vary with the "count" of the yarn, the length of the

-

86 METHODS OF TEXTILE CHEMISTRY

,.

" staple" of the constituent fibers, and the "twist per

inch ". applied in spinning. The following table showing the results of tests with carded cotton yarn is of interest

I I

!

at trus point:

I,

Ii ,

I'

tIl~

o lJ')

Average number of fibers
in cross-section 'of yarn .. I20 100 110 roo 74 60
::,tren~tn ot eacn 110er In J46 I46
, graIns ................. 140 140 150 150
, Calculated strength of yarn
in pounds .............. 200 160 184 ]117 127 10.,
Actual strength of yarn in
pounds ................ 50 36 46 .H 2R 24
;
! DETERMIN ATION OF HUMIDITY. This determination is of especial importance in the snin-

'.

~. A-

ning, winding, carding, and weaving of cotton and in the

., . '"'' . ,..,....-., ,.

oxicanon or ageIng or anum OlaCK. 1 ne amount or moisture contained in the air can be ascertained bv means

- .- .. ~~ ~ .• -.- ,_ -~ ~~ - --.1 cr ~ .---~-~, -~-- ~~~--- -~---

manly used being known as a wet and dry bulb hygrometer.

The wet bulb consists of a thermometer, around the bulb {)f "iUhlr h 1 c "i~Tr~ nnf'ri {)np pn r1 ()f ~ "i1iTlr 1,.. 'T'hp ()thpl'" pnrl

T.t'

of the wick dips into a small bottle of distilled water.

If the air is very warm and dry the water on this bulb

will evaporate quickly with the result that a lower tem-

.~ ......:1. 4-,..l 'T'1 ..l t.n· ..1 .•

}'1,....La.l..U.U ... .l;:) U.LU1\...Gl.!l..\...oU. .J. He Ul.j UUJ.l..I 1;::' a.ll. Ul.U1lli::UY

thermometer suspended within a few inches of the wet

bulb. The temperature on the drv hn Ih is rear] ann then

.L .,/

from a table is ascertained the amount of moisture which

DETERMINATION OF SPECIFIC GRAVITY 87

the air is capable of holding at this temperature. By

means of the same tab e we can ascertain how ill uch moisture the air is capable of holding at the temperature

The figure corresponding to the wet thermometer is

known as the absolute humidity (A).

cxpresse In pcrcen age. or exarnp e:

The dry thermometer indicates 77° F. and the "vet

At 77° F. the air is capable of holding 10 grains of water

per cubic foot.

per cubic foot, and

5·9

10

DETERMINATION OF SPECIFIC GRAVITY.

A. In the d ehouse it is often necessar to determine

the strength of a bath of a tannin extract or of some acid by

meter is used. As its name indicates, this instrument is

used to ascertain the density and therefore the concentration of the liquid. The common forms of densimeter are

noticed that Twaddell's scale bears a direct relation to the

c

1 See Appendix.

88 METHODS OF TEXTILE CHEMISTRY

the specific gravity I and 2 into 200 parts or dee (168° Tw X 5) + rooo ----------= r.84

Con version:

orne ye s abo It) b a e v

of silk could be calculated from the specific gra vi sample. Although this application is of no v. s ecific ravit of fibers rna in some cases forn for judging the quality of a fiber. A good examp is furnished by imitation silk or lustre-cellulos should possess a density very near to that of cotu

For obtaining the following data an ordinary l;

peci c gravity 0 a samp e 0 pure coa zene (Db).

Weight of the fiber in air (use from 0.5 to I grs Weizht of the fiber in the benzene Wb),

Wa W_aWb X Db = the specific gravity of the S~ The average values obtained by Vignon and c

given below:

F

Raw silk - - _ __ I. 3 °

Boiled-off silk. _ _ . .. . _ _ .• _ .

Wool __ _ . _ .. _ _ _ .. __ .

.... _ -- ----- _.

Lustre-cellulose _ _ ......•. _ .. __ .. _. _.

Linen. . _ . _ __ . _ . _ . _ _ . __ .

Hem p. . . _ . _ _ . _ . . __ . _ . . . _ . _ . . . . . . _ . . . . . _ _ . _ .

Jute. . . . . - . - .. _ - _ __ _ .. _ _ .

Ramie. . . . . _ . _ .. _ . _ .. _ . _ __ _ .. _ . __ . _ .

DETERMINATION OF FASTNESS

DETERMINATION OF THE FASTNESS OF DYED FABRICS.

The tests which will receive consideration at this point include fastness to

.

air

fulling

.

spongIng

aci S

greenmg

s oving

hot-pressing

soda

boiling-off

peroxides

washing.

crocking

sa mu

in IO% ammonia solution. Dry without rinsing. In lace of ammonia a 10 soda solution rna be used.

Wool. - Immerse the sample in a 20% solution of soda crystals. Squeeze and dry without rinsing.

size. They are then covered with

> I::> ,

If a standard sample be exposed at the same time under

the same conditions the relative fastness of the two colors

can readily be observed. If only the fastness to light is to be tested the experiment must be carried out under

a g ass cover. sample to the

exposIng e action of dust and

jecting the sample to the action of light, and exposing it

to the action of the air, dust, and rain at the same time.

Acid. Cotton. I. Spot the sample with dilute hy-

In e boiled off. In this operation the goods are treated in a

90

:METHODS OF TEXTILE CHEMISTRY

drochloric acid containing roo c.c. of the (sp. gr. = 1. r8)

.

act per I er. 2. S ot the sam Ie with a 50% solution of acetic acid .

• Allow the acid to act for 10 minutes.

Wool, Spot the sample with dilute hydrochloric acid

containing 300 c.c. 0 e

, llow the acid to act for 2 hours.

Boiling-off or degum1ning. Silk is sometimes dyed

boiling soap solution containing r 5 grams of soap per liter, for two hours.

t orine. 0 on.

hour in a solution of chloride of lime. Two experiments

should be carried out, one with a r? Be and another with

jected to an after-chloring, so that the test is of especial

im ortance in this case.

Carbonizing. Wool. Treat the sample with sul-

y In e

Neutralize with dilute soda

Rinse, dry, and examine. In order to observe

b

subjected it is advisable to sew the sample with a few

threads of cotton.

Crocking, Wool. This test may be carried out by

b

w hi te surface.

Finishing. The varied nature of the finishing processes

As one example we might take the following: aste containin 20 rams of otato

DETERMINATION OF FASTNESS

Ii

The

e samp e 0 yarn IS white cotton, then thor-

milling IS used, so that In this case the test should be

Cotton. In this case the test is carried out by rubbing in a solution of soft soap or by immersing in a 1%

lution (IS g. soda ash per liter). In all cases the yarn should be plaited with white wool and white cotton.

black on cotton. The natural test is to subject the sample to the action of air, light, and weather and observe the

and 500 grams of water. The sample is immersed in this for IO minutes, rinsed thoroughly with distilled water, dried, and examined.

Hot-pressing. Cotton. The sample is ironed with

an iron which has been well heated and the change of color js noted.

~IETHODS OF TEXTILE CHEMISTRY

Itt use ay b

more the time of exposure should be noted.

Perspiration. The sample of cloth should be sus-

any chanze which has taken place. The laboratory test

"" b

is carried out with a solution containing 50 grams of 50%

acetic acid and 100 grams of sodium chloride per liter.

The fabric

two fibers (satins and other mixed fabrics) sometimes contain threads of mercerized cotton in the wca vc. This dyed yarn must be able to withstand the subscq uent

operations of degumming and bleaching to which the

silk is sub iected. As the bleachinc 0 eration is now

generally carried out with peroxides it is important to know what action these chemicals have on the coloring matters.

ags, urn re a covers with dyestuffs capable The sample is

of resisting the action of this sewed to a ieee of white wool

DETERMINATION OF FASTNESS 93

n. an t en ne. ter repeating t IS 5 times t e

_es are compared with the standard.

x-rrzing, This test is best carried out by placing

.55 through the actual steaming operation in the ,_ A small piece of undyed fabric should be simul-

r IS

'vvool yarn and white cotton yarn. These should

of sulphur dioxide may be generated by burning

laited with white

L yarn and boiled for one-half hour in a solution of

led or become paler.

c mp I

cotton and immersed Lsh (20 g. per liter).

~et dust. Wool and silk. - A milk of lime is pre-

ter. The sample is spotted with this mixture, then

a.z her. This has already been discussed under

s hing. Cotton. - The sample is treated with a o ra containin 2 rams neutral soa cr liter for

alf hour. Two experiments are carried out, one at

94 1o.IETHODS OF TEXTILE CHEMISTRY

60° c. and the other at 1000 C. The changc in shade

of the sample is noticed.

Wool, - The sample is treated with a solution con-

taining 2 grams soap and 0.5 g. soda ash per liter for 15

minutes. The change in shade is noted.

In carrying out the tests above outlined it must be rcnlembered that the term "fastness" is in every case

• present time no instruments vvhich enable us to draw

meant to be "relative fastness." There arc up to the

absolute comparisons between two dyestuffs on the fiber. Of all properties, the fastness to light is probably the most

important, so that this should be detcrmined in every

case, while the other tests may be applied as the necessity for the same rna y arise.

•