LA BO R A T O R Y G U I D E

IN DU ST R IA L C H EMIST RY

BY R ALLEN ROGE S, PH . D.

I STR CTOR IN INDUSTRIAL CHEH ISTRY PRATT INSTITU TE OOKL N U , , B R YN ; I EHB EE AKERICAN CHEMICAL SOCIETY; SOCIETY OF CH MCAL INDUSTRY; AHE RICAN LEATH ER CHEMI STS ASSOCIATION

N E W Y O R K D N O T R N D C MP N Y . V A N S A O A

E ' 23 MURRAY AND 1 908 27 WA RR N Srs . o ri ht 1 08 C py g , 9

D AN N TRAND MP Y BY . V OS CO AN

The filimflon Pre ss N w ood Mass . FACT S WHICH SHOULD BE REMEMBERED

l Do r igh t and you will be succe ssfu . k wh i h i for u n d do i with smil c o . Do th e tas s se t be e y , a t a e

im r r Do not be a t e se ve . ’ Do not use your ne igh bor s standa rd solution for accurate de te r i m nations .

D n rr w r o ot bo o appa atus . Ke e our de sk and a aratus cle an if ou h o e to obta in satis p y pp , y p r facto y re sults . Alwa h ow l d n e in o r de sk and use th e m wh e n ys ave a t e an spo g y u , r h d you le a ve fo t e ay .

- ill r dr d h e fl r Glass ware w b e ak if oppe to t oo . r old u i Ne ve r touch a mach ine until you a e t h ow to se t .

Ne ve r run a mach in e with out oil .

Le ave your mach ine or ke ttle in be tte r condition th an you foun d it .

PREFACE

IN the average course of chemistry as taught in our tech nical sch ools there is little or no attempt made to bring h the student in close touch wit manufacturing conditions . h ff is x ffi n T is state of a airs e ceedingly di cult to u derstand, when we consider the large amount of time devoted to prac i tical work in some of our engineer ng courses . Th e factory is surely no less fertile a depar tment of this

industrial era than the railroad or the foundry . For in the manufacturing plant there is more need of techno-practical (if such a term may be used) trained men than in any other

branch of industry . Unquestionably it is necessary to have

z a and organi ation for the m nipulation of power, machinery,

so as labor, to obtain the maximum of production with the

But minimum of expenditure or depreciation of plant . in

s th e addition , it is highly es ential that we understand chemi se cal principles upon which these industries are ba d . T h e is object of this book, therefore, to acquaint the

s student of chemistry with a few commercial proces es, by introducing practical methods of handling materials on a large scale ; the care and use of machinery ; the cost of raw material ; transportation ; wage system ; the handling of men

and shop discipline . The subjce t -matter of this book presupposes a certain knowledge of chemistry ; and purposely leaves many of the ut minor details to be worked o by the student . Great lee way is also given to the instructor in order that he may e xe r

vii viii PREF ACE

i A h s . cise own originality few suggestions, however , may

not to be out of place, and may serve as a guide those engaged

in this important branch of teaching. The first chapter has been introduced in order to insure that the student understands the use and value of the various

for methods employed taking the density of liquids, and the

tests given should be conducted by each individual . a The work in the second chapter, de ling with inorganic preparations is best conducted on the foremansh ip system which is carried out at Pratt Institute as follows : One man is assigned as foreman of the chemical works and has as h is i T h assistants three or more of h s classmates . e work which he is given may be the manufacture of bar ium chlorid for

He example . first has his men make an analysis of witherite to determine the percentage content of barium and also test

‘ f In the strength o the hydrochloric acid . orde r that the work may be more commercial he is told to estimate the

of . cost producing lbs , it being understood that all weighings are made in grams . The necessary quantity of

is h mineral then weig ed , crushed and treated with the diluted acid in the kettle as described under that prep aration . During such a preparation as th e one cited it will be u necessary to remove impurities, this being reg lated by analytical tests .

Chapter three is devoted to the dyeing of textile fibers . Here it will be advantageous to have all tests mounted with an names of color, method employed , and y other data written under each skein . In the fourth chapter the preparations given have bee n se lected with the view of manufacturing commercial products rather than following the usual custom of making su s an to i H e organic b t ces llustrate typical organic groups. er PREF ACE ix

it has been found advisable to have the student save a

- of h h e 4 dram sample each compound , w ich seals and

I th e th e l - on . n s mounts cardboard ca e of coa tar colors,

- the student should make dye tests with the same , mounting

th . e skeins and color on the same card In order, also, to illustrate the use of his colors in the manufacture of lakes h e

on should prepare dry and pulp colors , mounting them card h - board toget er with rub outs in glue and Japan . h h In the c apters devoted to soap, paint , leat er and paper the work outlined comes again under the h ead of foremanship method and should be conducted along the same line as

re S on for inor ganic chemicals . The foreman should be held p sible for the quality as well as quantity of the output from h is plant ; he should see that a"machinery is left in perfect

condition , and that his factory is clean . The advantages gained by this foremanship system are

e - s lf evident , giving the student more confidence in his own

ability than by any other possible means . As we are only beginning to se e the first faint light of dawn

- of l in this all important branch education , the author wi l

e of be gratified , inde d , if this book proves to be any service to those who are attempting to solve the great prob u l E all lem of Ind stria ducation , and espe ci y the teaching of

Industrial Chemistry . s h i In conclu ion , the author desires to express s appre c ia tion of the kindness and courtesy shown to h im by his man y friends for the many valuable suggestions which have so h im been helpful to in the preparation of this volume . AL LEN ROGERS. P ATT I STITUT R N E .

B roo l n Se te mbe r 1 k y , p , 9 08 .

TABLE OF CONT ENT S

PREFACE GENERAL PROCESSES

INORGANIC PREPARATIONS

DYEING OF T EX TILE FIB ERS

COMM CIAL O A IC COMPOU DS COAL-TA COLO AND ER RG N N , R RS

SYNTHETIC O ILS

PIGMENTS AND LAKE S

D I S VA ISH S PAI TS A D STAI S R ER , RN E , N N N

SOAP AND ALLIED PRODUCTS

LEATHER MANUFACTURE

O F B P P P P WO D I ER, UL AND A ER

USEFUL DATA

CHAPT ER I

GENERAL PROCESSES

Lixi iati n W hl 000 I v o . . eigh out roug y 5 grams of crude h as salt, which been ground to a fairly fine powder in the A 0 mill . gitate with 3 liters of water in a kettle or receptacle h as provided with an arbor. When all soluble matter dis

or to a . solved , run into kettle tanks and allow st nd until clear

06 su e rn ate nt Next draw the p solution , wash the residue a sever l times with fresh water, or until a test portion shows f only minute traces o chlorides in solution . This process demonstrates the method employed in extracting soluble substances from products containing varying amounts of soluble and insoluble matter.

2 ntan e ou Eva orati n S o s o . . p p In the warmer climates ’ h advantage is taken of the sun s eat to produce evaporation .

al c This may so be accomplished in cooler lo alities , only less

sun . on rapidly, by the and wind To dem strate this process th e solution obtained above is placed in Shallow pans ex sun e va o posed to the and wind in the open air, the rate of p

r ration being noted f om day to day . To obtain the best r esults , the pans should be large , the depth of the liquid not over two inches, and should be arranged in such a manner as to be easily covered in case of rain . Eva oration b Dir c A li n f H at 3 p y e t pp catio o e . This is e e d method not us d very extensively, but where it is mploye

a B there are two general methods in use , ( ) y bringing th e flame in contact with the bottom of the pan ; (6) By pass LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

ing the heated gases or flame over the top of th e liquid to be

evaporated . The first may be easily illustrated in the laboratory by placing a copper or iron kettle directly over h th e charcoal fire or gas flame . T is will shortly bring th e

to liquid to a quiet boil , which may then be regulated suit

T h e the required condition . second form can only be

so not l reproduced on a fairly large scale , that it is advisab e

to try to introduce such a process into laboratory work . A li n f H t Eva oration b Indire ct catio o e a . 4 . p y pp This

FIG — K le T h e u . 1 te a e e tt . t a r . S m Jac k t S t

e te r n C u r lin ton N o . P so , B g , . J .

of o out means evap ration may be carried by various methods .

T h e one h of w ich is most widely employed is by means steam ,

- or in which case a steam jacketed kettle , tank with steam coils is used , but usually the former . In conducting an evap

in th e oration by this means place your solution kettle , and T h open the drip to the outer jacket . e object of this is to

th e th e drain kettle , allow first condensation to escape and to

- prevent bumping . The exhaust valve is Opened , the inlet GENERAL PROCESSES 3

h valve given a half turn , and t en slowly opened until a good

T h e supply of dry steam issues from the drip . drip is then closed and th e inlet of steam regulated to secure th e proper

h h not too heat for evaporation . T is s ould be strong as it

th e not will cause solution to boil over the sides, and too of weak as this would consume an excessive amount time .

The best condition is a quiet boil, which as the concentra

S TILL CONDENS ER

P n T k FIG . acuu a o as B u r r 2 . a . V m h m h d, roo n N Y B kly , . . tion continues may be regulated by slowly cutting dowh the to h steam . This is necessary prevent the formation of a ard cake which would be produced if the heat were continued th e or same , increased during the operation .

E n in c va o atio Va uo. f 5 . p r The di ferent forms of appa ratus used for vacuum evaporation vary much in their con struction but all depend nevertheless on reduced pressu re . The necessary equipment for a plant to demonstrate this 4 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

of - process consists a vacuum pump (dry system) , a pan , con T h denser and receiver . e pump may be of any form al th ough one taking up a small Space and power driven is

Th e of preferable . pan consists a globular copper or iron - - h vessel with steam jacket, water gage, man ole , minometer,

thermometer, peep glasses, and discharging valve . A “ ” catch-all is introduced between the pan and condenser to hold back any liquid carried over mechan ically by the

GO e r i steam . The condenser is a tin lined pp coil and s

surrounded by running water . The receiver should be con n e cte d with the bottom of the condenser and also provided

- with water gage . In con ducting the process the liquid should be introduced l until the pan is about half fu l . The manhole is then l covered , and the pump started . The steam shou d be slowly introduced into th e jacket and so regulated that a h quiet boil is obtained . T is can be seen through the peep

W is holes . hen the operation is complete , the pressure

of - al slowly reduced by means an exhaust v ve , and the con

. tents removed . through the discharge 6 r talliza ion T h C s . e . y t process of crystallization may be demonstrated in connection with evaporation . Thus if a solution is evaporated until small crystals begin to appear on the surface and is then run into tanks and allowed to cool it will be noticed that well -de fine d crystals sh ortly begin to collect on the bottom and sides of the vat ; th e size of which will depend Upon the nature of the substance and also upon of the rate evaporation . Thus if evaporation takes place rapidly small crystals are produced , while the Slower the evaporation the larger the crystals . One of the best salts to use for illustrating this process is

h h on sodium sulphate , w ic slow evaporation yields a large

- n d crop of well de fi e crystals . GENERAL PROCESSES 5

Very good crystallizing vats may be made by having an

- oak barrel cut in the middle , or small wash tubs may be of used for the purpose . Tanks porcelain, stoneware , glass or enamel may also be obtained .

T n s FIG Se tt in a . . 3 . l g k

Le a n n i ti . l 7 . v g o To il ustrate this process , the substa ce is mixed with water and ground in the wet condition . From the mill it passes into a series of settling tanks arran ged in A d battery . The heaviest material is deposited in an thus

as h becomes finer it reac es the last tank . Such a plant can be readily Obtained by securing several ice -cream packers and arranging th em so that A is about two inch es h igh er " than A and so on down the line having an overflow from T h tank to tank . e coarse particles are then returned to the mill and the process continued until all of the substance is in a very fine state of division . 8 . Filtr ti n e of con a o . On of the simplest forms filters sists of a wooden frame of four flat sticks over which is h ung either cotton or woolen cloth in such a manner as to form a bag . The filtrate may be turbid at first but soon becomes clear when the first portion may be returned to the filter .

F l ati n . Pre s ure i tr o A n 9 s . convenie t and rapid form of 6 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

filtration is by means of pressure . This may be applied by h eith er of two met ods . h h The first met od is one in w ich a vacuum is employed , h th h th e air being t us exhausted from e receiver . T is may be demonstrated in the laboratory by means of the laboratory size of suction filter wh ich is made of stoneware and can be obtained from any dealer in chemical appara

tus . The most satisfactory filter is made by spreading a piece of cotton over the

e o p rforated plate , p uring over th is about one -h alf

s inch of a bestos fiber, and h then anot er piece of cloth . Such a filter will retain the

finest of precipitates . A second form of pres sur e filtration is carried out by m Of th e filte r pre ss Fi t IG . ac u u e r Fil r F . . A te 4 V m l , o Wt l'l IS I th e Be d E aust C u l largely used n ; B , xh ; , O t e t .

industries, especially where h the insoluble portion is the essential product . T ese presses vary much in construction although all are based

th e A ll s upon same principle . sma press can be ecured h whic will answer for purpose of instruction . The press consists of a strong iron frame in wh ich a number of filter

E Of a cells are supported . ach cell is made up two flat met l

T h e plates , separated by a hollow distance frame . liquid holding th e insoluble matter in suspension enters th e frame h h t roug openings in the side . The solid matter is retained in the filter cloth while the pressure forces the liquid through

LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY GENERAL PROCESSES 9

By constructing a bridge of fire -clay at the front of the muffle h the c arge may be introduced and worked as desired . One of the simplest examples of calcination is the preparation of i s . red oxid , which given under the head of pigments 1 2 Sublimation a . . In this process the subst nce passes from a solid to a vapor and then to a solid without passing

through the intermediate liquid stage , and may be most readily represented by heating crude naphthalene in an s iron kettle over a low flame or , better , on a bestos . The naphthalene vaporizes and may be condensed by placing a cone over the top of the kettle leaving a very small opening

in the top for escaping gas es . The cone may be made of

sheet iron or even of heavy cardboard . A piece of muslin or filter paper may al so be stretched over the kettle which serves as a filter and retains any liquid which might be ofl given . 1 Distillation — 3 . . There are many forms of apparatus l employed for fractional distil ation , but the one which is most available is the French column still ; which can be obtained from any copper maker. These stills may be heated - s - by steam coil , steam jacket or by open fire according to the ll nature of the product being disti ed . I De n sit — B 4 . y . y density or specific gravity of a liquid is meant its relative weight as compared to the weight of an al equ volume of water at a definite temperature . The determination of specific gravity is one of the most frequent ope rations in chemical work . For all practical purposes a the test may be m de with the hydrometer, but for very exact results the pyknometer or specific gravity bottle is employed .

c se Three systems of hydrometer s ales are in common u , besides a great many special ones intended for obtaining a n is particular substa ce in a liquid ; the principle , however, I o LABORA TOR Y GUIDE OF INDUSTRIAL CHEMISTR Y

. l of the same in each These instruments are usua ly glass,

having a bulb weighted at the lower end , and drawn out at U the pper end to a long slender tube carrying a scale . The graduations on the scale being at the top and read down at ward , the largest number being the bottom, except in one — ’ instance that of Baume s scale for liquids lighter than is water, where it the reverse . When the hydrometer is placed in a liquid it sinks sufli cie ntly to displace a volume equal in weight to the weight of

the instrument and floats in an upright position .

1 Th e Di S cific ravit H m — . re ct e G d e e 5 p y y ro t r . This in strument is so constructed that the reading of th e scale shows the density of a liquid as compared with water at ° n 1 5 C . The point to which it si ks in pure water is marked

These hydrometers as usually employed are in a se t of four . The first spindle is graduated from . 700 to and

for is liquids lighter than water , the being at the bottom ; while the remainder of the se t are for liquids h eavier than water, with the smaller number at the top starting with

Practical use is made of the density of solutions for deter f mining th e weight o a given volume .

M 1 000 . . easure c c of water and take its Specific gravity .

M 1 000 ultiply the specific gravity by . Now pour the water into a weighted flask and after a h t e . second weighing, record the weight of water Con cluMsion ? . al 1 0 easure 1 000 c . c of a s t solution ( per cent) and take

1 000 its specific gravity, multiply the specific gravity by , How weigh the salt solution . does it correspond with the theory ? Conclusion ?

R s l epeat the experiment with caustic soda solution , u GEN ERAL PROCESSES I I

al fut ic acid , hydrochloric acid , nitric acid , ammonia, cohol

and benzine or naphtha. ’ e ll H dr me te r i I Twadd s o . hi s 6. y T s also a direct read se t ing in strument . The consists of a se ries of Spindles ° (usually six) having graduations from 0 to The read ° ° 1 . as 0 e s ing for water at 5 5 is taken and each ris p . gr . i s al as al s recorded on the c e one addition division . Thus ° s . 1 0 Twaddell becomes p gr . The density by this ° w 1 0 T . means is recorded as for instances . Twaddell readings are readily converted into specific gravity in the following manner :

M a . 00 ultiply the re ding by 5 and add to the product . ° s 1 Tw . s . . Thu , 5 p gr

1 ( 5 X . 00 5) In the reverse order specific gravity may be converted into

’ ° . 1 . 1 0 s . . 0 Tw . Twaddell Thus, 5 p gr becomes 3

00 . 5 3 0)

is That , from the specific gravity subtract and v 00 di ide by . 5 . This is the most convenient hydrometer for factory or i use . s d i laboratory It , however, not adapte to l quids lighter than water .

Take the density of water with the Twaddell hydrometer . Take the density of the salt solution use d in the former experiment . C l a culate its specific gravity . How does this agree with the former readings ? ’ 1 B m - . au é s H dr m r 7 y o e te . This is a very unscientific is l e It instrument , but large y us d in technical work . s read B mé ings have no very direct relation to specific gravity . au dissolved 1 5 parts of pure salt in 8 5 parts of pure water at 1 2 LABORA TORY GUIDE OF INDUSTRIAL CHEMIS TRY

J ° a 1 2 . 5 C. The point to which his instrument s nk was marked 1 5 ; the point to which it sank in pure water was marked 0 . The distance between these points was divided into fifteen equal par ts . This produced an instrument for liquids heavier than water .

n in For liquids lighter tha water, the point to which the strument sank in a 1 0 per cent solution of salt was marked

0 an 1 0 , and that to which it s k in water was marked , the distan ce between these points was divided into ten equal parts , and this graduation continued the entire length of the ° 0 of Spindle . The thus being at the bottom the stem , the lighter the gravity of the liquid tested , the greater numerically is the reading of the scale . For instance , a liquid reading

0 B6 0 B6 7 is of less density than one at 5 , which in turn is lighter than water at 1 0 B6.

To further complicate matters , the instrument makers appear to have become confused and produced instruments with erroneous scales . A test made several years ago dis - f f s o . clo ed thirty four di ferent scales, none which were correct The conversion of American Standard Baume readings to specific gravity is usually accomplished by reference to as tables, but may be worked out follows

Sp. gr . (for liquids heavier than water at ° 1 5 C. )

Sp . gr . (for liquids lighter than water at ° 1 7 . 5 C There is still another form of Baume which is in quite

use so- al Baumé common , the c led rational scale instrument ’ ° 66 (Kolb s) which indicates zero in pure water at 1 5 C. and ° r . 1 . in sulfuric acid of sp. g at 5 C al Take th e density of water, s t solution, caustic soda solu GENERAL PROCESSES 1 3

tion , sulfuric acid , hydrochloric acid , nitric acid , ammonia, alcohol, naphtha . H w By conversion determine their specific gravity . o doe s this agree with the first set of expe riments in density ? kn m t Th e P o e e . 1 8 . y r This consists of a small bottle , having ground into its neck a capillary tube enlarged at its upper end to form a reservoir which is closed by a stopper .

The bottle is filled with the liquid to be tested , and the W stopper loosely inserted . hen the bottle and contents have reached the normal temperature the excess of liquids in the reservoir is removed by means of filter paper until the lever of the liquid reaches the mark thereon . Th e stopper is tightly

inserted , and after cleaning and drying is then weighed . The density of the liquid is ascertained by the following

Weight Of bottle and liquid weight Of bottle Weight of bottle and water weight of bottle

Weight Of liquid Weigh t of equal volume of water

D etermine the specific gravity of salt solution , caustic soda, c sulfuric acid , hydrochlori acid , and alcohol . 1 W h al B l n c i e s a a e . 9 . tp This s a special form of balance f or determining the density of liquids . A glass plummet of known weight and volume is suspended from the beam by a

fine platinum wire , and is submerged in the liquid to be T h tested . e weight which the plummet loses is the weight

of the liquid displaced . By using a set of riders this loss can d be etermined , and when recorded gives the specific gravity

of the liquid .

Determine the specific gravity of a salt solution , caustic

soda solution , sulfuric acid , hydrochloric acid , and alcohol . In all dete rmination of density the question of tempera I 4 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

l r be ture is an important factor, and a l cor ections should made accordingly . Wh en using the Twaddell hydrometer ° a 1 T w . for commercial purposes, however, the ddition of ° ° a 20 . 60 ffi for e ch F above will su ce .

REFERENCES

f h m r r l h rk l n d ri l . n r Ne w o ut i e s o In us t a C e ist F a k Ha l T o . Y O y p , 0 1 9 7 . ’ h m l r illi r k n Fe rdinan d Wagne r s C e ical T e ch no ogy . Si W am C oo s a d r rk . 1 0 Fish e Ne w Yo , 9 4 . h l d k of ndu rial r an h m r l r . i n oo I . ad e a Ha B st O g ic C e ist y S. P . S t P

de l h ia 1 06. p , 9

Books on Te ch nical and Analytical Ch e mistry — . 6 l L . n e . n d n l F nd il . d Lo o 1 0 Anima a ts a O s o s . . E A s 1 8 v , 9 7 9 3 h d l h i l Gill . 0 A. . ila e a 1 . il Ana is . H P O ys p , 9 3 mi l T e h n lo an d Anal i of il F nd x l 2 o . Ch e ca c o gy ys s O s, ats a Wa e s . v s

L ndon 1 . L wk wi h . o 0 . e o tsc J , 9 4 r l r n An l A . . All n . 6 l h il d l h mme cia a ic a i . H P Co O s s e o s . a e ia g y v p , - 0 1 896 1 9 7 .

h mi l An l f r n A l r h l d I . A . ai i a e l h 1 . C e ca a sis o o . . B P ia 06 y p , 9 k r n i An l r . Ne w r 1 a c i A . B . P e Y 0 1 O a s s . scott o . g y , 9 h r Th illm n . P n ine e rin e mi . S a a on E o B . E C st s . t st a . 1 0 . g g y , , 9 5 i h l l r l F nk owe and . . l m n uan ta i e e mic Ana i . Q t t v C a ys s a C s J B Co e a . d n n 1 . Lo o , 906

i i e h l An r ant tat e mi R F . k u i . r ius Ne w o . C ca al s s C. . e se n Y 1 0 Q v y , 9 3 T - k f x l n . r . e t b o uan it i e An l i . Ne w k oo t at a s s . C. O se Yo 1 08 Q v y J , 9

ol e ric An l i . Fr h 0 um t a s s ancis utton . Ph ilade l ia 1 V y S p , 9 4 .

1 6 LABORA TOR Y GUIDE OF INDUSTRIAL CHEMISTRY

mate the necessary quantity of sodium carbonate , sodium bicarbonate and sulfuric acid . The student should also be l and required to estimate the theoretica yield , cost per pound h is of finished product, taking into account the question of freight , labor, interest on investment , wear and tear of ma an d of chinery, containers, besides that his raw materials .

Example l s . B 1 000 b of auxite at c . per lb - l . of 3 000 bs Soda ash at I i c . l 2 0 bs . 2 3 3 of Sodium bicarbonate at c .

l 2 1 884 bs . of Sulfuric acid at c .

l s Of 1 1 b . 6 0 . 1 00 l s 9 4 Incoming freight at per b .

. Y . . N. f o b ,

l . 6 s . 2 b 6 1 00 . 0 b . O . 4 9 of utgoing freight at c per f ,

1 . Containers at 5 c per 1 00 lbs . .

A 20 s ddition of per cent for labor, intere t, wear

and tear, etc . Total cost

l cents per b.

2 1 Antimon -Potassi m Tartrate . y u . H ,O . Dissolve 1 000 grams of cream of tartar in 1 5 liters of boil

ing water and slowly add 800 grams antimony oxid . When all h as dissolved filter the hot solution and evaporate to point A al al . of cryst lization llow to cool , separate the cryst s and

again evaporate the mother liquor for further yield .

This salt is known commercially as Tartar Emetic .

Estimate cost per pound . INORGANIC PREPARA TIONS 1 7

Ammonium Sulfate . 22 . Determine the amount of ammonium hydroxid and sul

2000 N furic acid necessary to produce grams of ( SO, as follows :

H SO : 2 NH 2000 : x ( I ) (N ,) 2 4 , H x . N amt of 3

Take the specific gr avity of your ammonia and refer to the f H table to find the per cent o N ,

x

use . amt . of ammonium hydroxid to per cent : H SO 2000 : ( 2) (NH,) 2 SO, z , y

H S . y amt . Of , O,

Take specific gravity and refer to table as for ammonia . Now mix the sulfuric acid with about ten times its volume E of water and slowly add the ammonia . vaporate to obtain

crystals . n Estimate cost per pou d .

l rid . B l H 2 Barium Ch o aC 2 O . 3 . ( ,, z ) To estimate the necessary quantity of material for the production of 5000 grams of barium chlorid the following

method should be employed .

— l 2 H Ba 00 0 : x Ba O : . Calculation . C 2 , 5

Ba x amt . of necessary .

As the barium is derived from the mineral witherite the percentage content should be determined by analysis and from this the quantity of mineral determined thus :

as

amt . of witherite . per cent of Ba

BaCl,2 H,O 2 HCl 5000 : y H l y amt . C 1 8 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

By taking the specific gravity of the acid and referring to table the percentage strength is obtaine d when

y Of amt acid required . per cent of HCl

is d The mineral ground , place in a suitable vessel, and

1 0 liters of water added . The hydrochloric acid is then d slowly intro uced , and the solution brought to boiling ; about 200 gr ams of powe rde d witherite is added to pre cipi mi so to tate the iron and alu nium, and the lution evaporated ° d e . Tw . an z 5 5 filtered , allow d to crystalli e The mother liquor being concentrated for a further yield .

Estimate cost per pound . rr Ammo m te 24 . Fe ous niu Sulfa .

6 H,O) . Dissolve 1 400 grams of ferrous sulfate and 664 gr ams

2000 . . s of ammonium sulfate in c c of water eparately, ° l heatin g to 60 C. Fi ter if necessary and mix the two solu 6 l u tions , concentrate, add 3 grams of su f ric acid and

r z R allow to c ystalli e . emove the crystals from the mother l dr al n and iquor, y in the centrifug machi e, evaporate the

mother liquor for more crystals .

Test for pur ity and estimate the cost per pound . 2 L ad Ace tate P e H . 5 . . ( b 3 ,O) In order to manufacture 2000 grams of lead acetate it will first be necessary to make an analysis of the litharge and acetic acid and from the percentage composition determine

the quantity of each to be employed .

Re action — P H H . h O 2 C,, ,Oz ,O

26 Le ad Ni . trate . This compoun d may be prepare d in th e same manner as r e commended for the acetate . INORGA NIC PREPARA TIONS 1 9

d l H . 2 Ma ne sium Ch lori . MC 6 O 7 . g ( g , z ) Having determined the per cent of magnesium in mag i ne s te , and the strength of hydrochloric acid , estimate the quantity of each necessary to produce 4000 grams of the salt . Mix the magnesite with an equal quantity, by weight, of water, slowly add the acid and heat on the steam bath until the action ceases . If acid in reaction make neutral with D l magnesite . igest for an hour and filter while sti l hot . Evaporate the filtrate on the steam bath to a density of ° Tw . 60 . and allow to cool The crystals are removed and

al separated from the mother liquor in the centrifug machine .

The liquor being evaporated for further yield . EMstimate the cost per pound . agnesium chlorid is very deliquescent, and should be placed in a bottle as soon as removed from the centrifugal machine . i m Dich r te 28 Potass u oma . .

D 1 0 issolve 3 5 grams of potassium carbonate in 1 500 c . c . Add of . 200 water this solution slowly to 4 grams of lime, ll l l and a . S let stand until of the ime is slaked tir we l , evap ° 1 0 C . orate to dryness, and heat to 5 until thoroughly pow

ix 2 00 dered . Mwith 7 grams of powdered chromite and heat in a reverberatory furnace with oxidizing flame at a bright t red heat for 3 to 4 hours ; cool the mass, pulverize , and ex ract with 9000 c . c . of water . Concentrate until crystals begin to form and then add a hot concentrated solution of potassium chr o sulfate , to precipitate the calcium from the calcium

mate . To the yellow filtrate of potassium chromate , add

sulfuric acid , diluted with twice its volume of water, until

. Off a strongly acid , and let the liquid cool Filter the cryst l

t e line precipitate , redissolve the mass in hot water, and E crystallize . vaporate the mother liquor for further yield , 20 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

which, however, may be contaminated with potassium sul fate . m m e 2 Potassiu Ch ro at . 9 . This salt is prepared from potassium dichromate and potas sium carbonate according to the following reaction :

K,CO, 2 KzCr O4 CO2 Therefore estimate the quantity of each necessary to produce

2000 grams . m Pe rman n te 0 Potassiu a . 3 . ga Ignite a quantity of powdered pyrolusite at a red heat on an iron plate to burn out any carbonaceous matter it may

D 8 0 1 200 . . contain . issolve 4 grams of caustic potash in c c

Of 20 otassIum h water, stir in 4 grams of p c lorate and heat

20 until dissolved . Th en mix in 7 grams of the ignited to h pyrolusite, evaporate a smooth , t ick paste , and heat

a . to redness in an iron crucible , adding sm ll portions at a time When thoroughly hard let the crucible cool and break out the mass with a chisel . Then boil with a large excess of of i water, passing a stream carbon dioxid into the boil ng solution to convert any hydroxid into carbonate . The green liquid passes over into a violet solution of potassium F permanganate , and a dense brown precipitate forms . ilter through asbestos or glass wool and evaporate the filtrate - t A to until needle like crys als appear on the surface . llow cool . Separate the crystals and evaporate the mother liquor for further yield .

1 Potassium Sodi m Tartrate H . 3 . u . 4 zO) The preparation of this compound is based upon the reaction 2 KHC H O Na CO H , , , , , 3 ,O

2 K H H Nac; ,O, 4 ,O CO,. Therefore estimate the quantity of cream of tartar and soda INORGANIC PREPARA TIONS 2 1 ash necessary to produce 3000 grams and work out a method of preparation . — 2 A h O . Soda s . N 3 . a , Prepare a saturated brine solution by dissolving 880 grams ° 1 C. of salt in 3000 c .c . of water at 5 To this brine add

1 . S . r . . 1 0 s 000 c . c of ammonia ( p g 9 ) and pa s in carbon di oxid so long as the gas is absorbed and a precipitate is

r e formed . Ca e should be taken to keep the vess l cool and to use a large delivery tube in order to prevent clogging. The precipitate produced is sodium bicarbonate and should be filtered by suction and washed with a little cold water to remove adhering salt . It is then dried and heated strongly (do not fuse ) to convert the bicarbonate to the car bonate . The liquor may be heated with milk of lime to recover the ammonia .

H d o n Ph s h at HP -1 Disodi r e o e . Na O 2 33 . um y g p ( q ,

H,O) . Into a lead -lined tank or porcelain dish introduce 5000 grams of bone -ash and mix with it 3 880 grams of sulfur ic m acid (Sp . gr . The ixing is conducted in the open

l ixivi a . L air or hood . Stir well and l ow to stand over night ate the mass with twice its volume of water and boil by blow

OE o ing in steam . Filter the s luble portion and wash the E fil residue se veral times with fresh water . vaporate the l trate and washing to a convenient bulk , and neutra ize the boiling solution with a concentrated solution of 2 750 grams - h ofl of soda as . Filter the precipitate of calcium carbonate and evaporate the filtrate until the solution h as a density of ° ° s 2 5 T . at 60 F . The crystals which eparate on cooling sh ould be dried in the centrifugal and bottle d as soon as

Re act on possible . i i m Bi lfite H Sod u su . Na SO . 3 4 . ( a) 22 LABORA TORY GUIDE OF INDUSTRIAL CH EMISTR Y

This compound is usually placed on the market as a liquid containing per cent of the salt . It is prepared by pass ing sulfur dioxid into a solution of sodium car bonate until S completely saturated . The Oz may be easily obtained by l l a burning su fur in a sma l furn ce , made by boring a hole muflle as in an ordinary , and drawing the g by suction through the soda solution, which may be placed in flasks or small casks . Therefore have the student estimate the quantity of soda ash e , water, and sulfur to produc grams of the product, also estimate cost per pound and write reactions . Zin c Sulfate H . . Zn SO O . 3 5 . ( , 7 z ) Having determined the strength of the sulfuric acid and n zi c oxid , estimate the quantity necessary to produce 5000 grams of zinc sulfate and work out the method of procedure . a s The foregoing s lts repre ent a few typical preparations, and it is left to the instructor to make the list as complete as he sees fit REFERENCES

f ri li L . d n Sul u c acid and Alka Ge o . un e Lon o 1 06 . g , 9 . ’ r h m r d r r mi . h il l Rich te s Ino anic C e ist E a F. S th P ade h 1 . ia 06 g y g p , 9 . r l f r ni h e m r rr n P inci e Ino a c C ist Ha . o e s 1 06 s o . C . p g y y J , 9 f r h m r ilh e lm T h e Principle s o Ino ganic C e ist y . W Ostwald and r d n 1 Ale xande Findle . Lon o 0 . y , 9 4

T i m r . D i d . r re a t se on Ch e ist I . I . . He n e Ne w Yo k 1 0 y , 9 7 .

utline of Inor anic Ch e mistr . F A h d lk r Gouc an . A . a e . O s g y . . J W Ne w York 0 , 1 9 5 .

’ CHAPT ER III

DYEING OF TEXTILE FIBERS

6 of - 3 . Dyeing is the process precipitating coloring matter d upon or within the substance of a bo y by chemical action .

or The solution may be neutral , acid , alkaline according to

' f the d e s ufl o t . the nature of the material, and y employed f ff . are O 3 7 There two general classes dyestu s , namely th natural and artificial . Owing to e lar ge number of coal

e e h tar colors on the market , however , and the as with w ich

al t e they are applied , the natur colors have been steadily placed until to-day logwood is practically the only one which f is O any importance in the trade .

8 th e al - 3 . For practical reasons co tar colors are divided generally into the following groups : A 1 . cid dyes . B 2 . asic dyes .

D th e cos 11 . 3 . yes of group i Su stan t ne s . 4 . b dye

5 . Mordant dyes .

6. Developed dyes .

7 . Spirit colors . Acid D e s — 3 9 . y . These colors are chiefly used for wool

e xce dying, but they are also applied to silk, and with few p tions the dyeing takes place in an acid bath . They are only

th e of little interest for cotton , but , on other hand , they are of f h great importance or jute . T e commercial dyestuffs con

Of l a s in sist the a k li or lime alts of the color acid . Thus, the

23 24 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

o as case of wool dyeing, the wo l acts a base , combining with

the color acid to form an insoluble compound . B c D 0 asi e s . s m 4 . y The e colors are chiefly used for or L danted cotton . arge quantities are also consumed in silk fe w dyeing, and a considerable amount of a brands is use d f . x or for wool They are also e tensively used jute dyeing .

B al asic dyes are the s ts of colorless bases, that is, the color

does not appe ar until the salt is formed . The commercial

f al dyestu fs are usually s ts of acetic , oxalic , nitric, sulfuric ,

or hydrochloric acid , and most of them are soluble in water .

In the process of dyeing these compounds decompose , setting

constitu free the acid , while the base combines with the acid

th e ent of the animal fiber, or with acid mordant in the case of vegetable fiber , thus producing the color on the fabric .

1 D e s of th e Eosin Grou 4 . y p. In the textile industry

se and o l the colors are used for wool silk , als to a sma l ex

h i flu re e in tent ou cotton . T ey are der ved from o sc by the

a io l . h h ct n of ha ogens To t is group belong eosin , eryt rosin , l i Al - ff h o ox n . l p , rose bengal, and uranin of these dye stu s se - pos ss a yellowish green fluorescence .

2 n i D e Substa t ve s . 4 . y These are very largely consumed for dyeing cotton and unions ; they are also used for wool “ ” to and silk . They are sometimes called direct dyes owing

the fact that they dye cotton direct without mordanting. To rimulin this group belong the benzidine dyes, p , congo, diamin , benzo and immedial colors . Mordant D e s 43 . y . They comprise a great variety of

- coloring matters, both natural and artificial , which are dyed M of on all fibers by the aid of metallic mordants . any these dyes are polygenetic , and they possess the property of form

x ing insoluble color lakes with metallic o ids . The usual method employed is to mordant the goods before passing i - c nto the dye bath , which usually ontains nothing but the 13mm: OE TEXTILE FIB ERS 5 5

and color . In a few cases the mordant color are introduced W l “ ff into the same bath . hi e in the process known as stu ” ing the goods are first run in the color and subse quently in

the mordan t . D l d D e ve o e e s . U 44 . p y nder this heading are included ff two di erent methods of developing, viz (a) The production of dyestuffs from substances which

e l poss ss no dyeing qua ity themselves, but which can be changed into dye stufls by a chemical reaction taking place n h o t e fiber . (b) The production of new products by further develop

in ff SO as h h g dyestu s to c ange t eir shade and properties . The first of th ese processes is represe nted by the produc

T h e c tion of anilin black . second by the pro ess of diazo i i t z n . g, both of which will be taken up later on S irit olo s — C . 45 . p r These dyes are insoluble in water,

s but soluble in alcohol . They are ometimes used for dyeing silk , and when dissolved in acetone for printing silk and

als . cotton, o for making colored varnish G n r l In r ction s for D e in 6 e e a st u . 4 . y g In conducting dye -tests it will prove advan tageous to make up the solutions as follows :

N ff 1 0 atural dyestu s and tannins . per cent solution Coal-tar colors 1 per cent solution Acids 1 0 per cent solution Salts 1 0 per cent solution Soap 1 per cent solution

P se is rovide your lf with a reel, a convenient form of which

As represented in the illustration . all tests are conducted

of is on the weight the material , it necessary to determine the number of yards required to give a skein of definite weight . The following list , however, may prove useful 26 LAB ORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

German kn itting worsted . 20 yds . weigh 5 grams

- d 1 2 2 . 200 s . 0 m Cotton yarn, ply y weigh gra s

60 . S . 2 pun silk , single thread yds weigh 5 grams

By noting the example given below a clear idea may be gained as to the use of the solutions mentioned and the reason for having the skeins of definite weight.

FIG —T in R h . . e st e e . ar e Kn s . a Pate rson N 7 g l C l H pp, , . J.

E m l — P - xa e . 47 . p repare a dye bath with 2 per cent of 2 congo red , per cent of sodium carbonate , and 20 per cent ’ G six I o- of of lauber s salt, using gram skeins cotton yarn ,

for . R boil half an hour emove, rinse and dry .

: 6 r Thus X g ams .

2 60 per cent of grams is grams.

20 60 1 2 per cent of grams is grams . AS is the congo red a one per cent solution , it will require

1 20 c . c . As the sodium carbonate is a ten per cent solution it will

1 2 . require c c . D YEING OF TEX TILE F IBERS 2 7

’ And as the Glauber s salt is a ten per cent solution it will

1 2 . require 0 c . c 8 - 4 . The dye tests are best made in porcelain beakers, n placed in brine to secure a u iform temperature . The skein

and th e o is suspended on a glass rod , p sition changed at least

once in five minutes during the time of dyeing . ar e On completing the tests the skeins hung up to dry ,

l : twisted , and mounted as fo lows P 49 . lace each end of the skein over the two middle fingers,

n h - twist u til tig t , then bring the right hand loop under the w wrist and up through the loop in the left . No holding the

k a l two loops stretch the s eins out straight , and l ow to curl r together . In this manner a ve y tight and even skein is the

result . These skeins should then be mounted on cardboard

by sewing through from the back , catching down the threads on the under side in such a way that it does not Show from

the front . W l ll 0 oo . 5 . In the study of dyes and dyeing we wi first

a ma e take up the natural mord nt colors, which y be us d for

wool . One of the oldest and most important dyes for wool is o ‘ logw od or campeachy wood , which is the wood of a larch a W M and tree growing abund ntly in the est Indies, exico ,

parts of Central America . It is imported in logs weighing

00 . oo s about 4 lbs The fresh w d is colorles , or nearly so ,

se and contains a glucoside , compo d of hematoxylin and

sugar . It is cut into chips or rasped . These chips are then digested with hot water when the solution on evaporation

gives the logwood extract of the market . Formerly for wool dyeing the chips were allowed to oxi

h is d in th e dize before extraction , but now t is accomplishe o as hi s lution and the product is known hematein , w ch o th r as c mes on e ma ke t e ither paste or powder . 28 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

Logwood is a mordant color, by which we mean that the color is only produced by bringing it in contact with some l meta . In this way a combination takes place with the formation of an insoluble lake . . 1 l 5 . In the first bath we wil boil two skeins of wool with 1 0 per cent logwood extract (on the weight of the fiber) for one half hour . The slight brownish color produced on the wool is of no al as v ue it is not fast to washing, and consequently would h as fi be removed . It , however, enough af nity for the color ing principle of logwood to absorb sufficient of it to produce a good color when afterwards mordanted .

2 h as 5 . To Show that the logwood been absorbed by the wool we will boil one of these skeins in a solution of 5 per cent of ferrous sulfate and 1 per cent of copper sulfate as i for half an hour . In this c e copper hemat te and ferrous

x hematite are formed , the latter being probably o idized to ferric hematite by the air . This experiment simply shows the power of wool to absorb c m colors, but does not represent the actual pro ess e ploy ed in dyeing .

wo is To dye wool with log od or other mordant color, it first mordanted and after wards introduced into the dye ll bath . To mordant wool with meta ic mordants it is boiled m d with solution of alum , or potassiu dichromate with a e dition of acids, whos function will be discusse d later . m The wool acts chemically upon the salts, deco posing an d x i s them , fi ing the alum num or chromium o that it can

n not be washed out , bei g in such a form that it combines readily with the logwood and similar colors to form the de sired lakes .

5 3 . To demonstrate the process of mordanting we will boil three 5 -gram skeins of wool for half an hour in a solution

30 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

directly with the logwood without oxidation . Cream of and ff tartar, tartaric , lactic acid have the same e ect as oxalic

acid . Besides influencing the composition of the body absorbed

ll for by the wool, assistants are used with meta ic mordants the following purposes : T ( 1 ) o prevent superficial and uneven mordanting. For o example , wo l decomposes alum so rapidly that in mor

danting in large quantities, where portions of the material are more exposed for a time to the action of the mordanting h liquid than ot er portions, some parts of the wool will take up the aluminium more rapidly than others and stripes or h F spots will appear w en dyeing . urther the mordant is be to liable to superficially attached the wool , and the color ff lake subsequently formed will rub o . The addition of

of bitarfrate th e sulfuric acid , oxalic acid , potassium to mordant bath prevents the alum from decomposing so rapidly

and aids to produce even the fast colors .

2 T o e Sul ( ) caus more of a mordant to be taken up . furic acid added to potassium dichromate by liberating

th e to h chromic acid , causes wool combine wit a larger h portion of t e mordant . Wool takes up chromic acid from potassium dichromate to a certain extent

K Cr O K Cr r z z 7 z O, C o3 .

5 7 . To demonstrate the above methods of dyeing we will mordant two skeins of worsted with 3 per cent potassium

2 200 . . t dichromate and per cent oxalic acid in c c of wa er, boiling half an hour . We will then boil one of the skeins with 8 per cent of

for hematein paste half an hour . Following with the second

as t ~ skein an exhaust test . That is o se e how much color re s in h e main t bath . DYEING OF TEXTILE FIBERS 3 1

8 We as 5 . will then mordant two more skeins above with 3 per cent of dich romate of potassium and I i per cent of

1 and 8 sulfuric acid , boiling % hours, dye with per cent of n hematein paste for one hour, ru ning the second skein as an exhaust test . M - 5 9 . ordant two 5 gram skeins with 3 per cent of

z ta 1 and l per cent cream of rtar, boiling 5 hours and dye with 8 pe r cent of hematein paste for an hour. 60 B is n . esides the methods given above there a other

process known as the single bath method , in which the dye

and mordant are applied in the same bath . The color lake is formed and Slowly absorbed by the wool after the manner

o h as : of a direct dye . The meth d two disadvantages first , part of the color lake is liable to be fixed only superficially

on of is the fiber, second part the dye precipitated in the

for bath and lost . It is, however, largely used both cotton of w and wool, especially in the case cheap dyes like log ood , in which the cost of the dye is not great compared with the

time and cost of labor in dyeing. 61 . To illustrate this method we will dye a skein of woolen

r h 1 0 wo e r ya n wit per cent log od , 3 p cent ferrous sulfate ,

on 1 per cent oxalic acid in 200 c . c . of water for e and one

half hours . The methods described for logwood apply to other mor

or is ff x dant colors , that dyestu s which are invariably fi ed

upon the fiber in the form of metallic lakes, with a color

which may be diff erent from that of the coloring principle .

They are very important dyes , being characterized by great

fastness to washing, light and other agencies .

62 f al-tar . O the co colors the acid dyes are used to a great of h for extent on wool , both on account their c eapness and

the reason that they are eas ily applied . The process of dyeing on animal fibers is to be regarded as ID 3 2 LABORA TORY GU E OF INDUSTRIAL CHEMISTRY

or a salt or lake formation , in which the wool silk acts the

th e of part of the base , while color acid plays the part the W acid . ith the exception of picric acid , the acid colors are l l a sold as salts , mostly a ka i s lts, but a few in the form of

lime salts . T h e c 63 . general method of pro edure is to prepare a bath . ’ of 1 0 per cent of Glauber s salt (sodium sulfate) and 4 per ff cent of sulfuric acid with the necessary amount of dyestu . After the material is entered the temperature is raised to boilin g and the dyeing finish ed by boiling three -fourths of an hour . 6 - 4 . For purposes of demonstration we will dye a 5 gram

e of 1 skein of wool with s veral the following colors , using per cent of dyestuff

(a) Fast red (j) Acid magenta (all brands) (b) Patent bl ue (g) Acid violet (all brands) s 12 (c) Scarlet 6 R . crystal ( ) Orange (all brands) d h S i . ( ) Naphthol yellow . ( ) Nap thol brown 0

e 2 R N h ( ) Scarlet . (j) apht ol black D .

All other acid colors .

6 Silk — is 5 . . This the fibrous substance which the silk worm spins to form its cocoon . Silk resembles wool in many respects . The numerous kinds of silk may be divided into two classes artificially reared and wild silk . The prin ciple species of silk-worms feed on the leaves of th e white

C th e mulberry , and is reared in hina, Japan , India, Italy, to U south of France , Greece , and a slight extent in the nited h S . A t e tates In sia the worms are reared in Open air , but in Europe this is done in sheds . The eggs are placed on ° d th e 1 8 C shelves, an temperature of the room raised from ° 2 C 1 to 5 in 2 days, when the eggs hatch , the caterpillars and are removed to another room , feed on the leaves of the D YEING OF TEX TILE F IBERS 33

white mulberry . They grow rapidly , changing their skin

At 0 every 4 to 6 days . the end of 3 to 33 days the mature

worms creep into birch twigs or bundles of broom or heather,

where they spin themselves into cocoons . The spinning

lasts 3 days , generally, but in order to be more sure that e all of the worms have ceas d spinning , 5 days are allowed

to elapse before the cocoons are collected . Some of the e finest having been s lected for breeding the rest are killed , either by exposing them in stoves to a temperature of 60 °

C or f 1 . 75 for 3 hours, by steaming them or 0 minutes Before the silk is spun it is found in the worm as two

liquids, one a clear, colorless liquid , the other colorless or ll ye ow, which are both secreted from two glands, one on of each side the head , communicating with a capillary orifice

in the head . The silk liquid solidifies on coming in con

tact with the air, forming a uniform double fiber, which in

2 some places may be seen separated into filaments . ff o . The cocoons having been sorted , the silk is reeled

A con fter removing the outer portion of the cocoon , which of h sists of a loose tangle t reads, a number of cocoons are to th e placed in warm water soften gum, and the ends of the fibers from 4 to 1 8 cocoons are collected and reeled off as one

thread . The length of the fiber in a single cocoon varies from 1 000 to 4000 yards . 66 O an zine o off . rg or warp silk is comp sed of the reeled

fibers of a number of cocoons . Tram or weft silk contains a smaller number of fibers . The outer portions of the cocoons

. C are used in the manufacture of silk ocoons pierced , or otherwise defective and the in nermost layers of the cocoon

for . are used spun silk These are fermented with water, boiled with soda, washed , dried , combed , carded , and Spun . 6 8 0 7 . The count of Spun silk is the number of hanks of 4 yards to the pound . The size of raw silk is measured by 34 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

1 000 A the weight of yards in drams avoirdupois. pound of

1 dram silk contains yards . S 68 . ilk is hygroscopic , and absorbs moisture from the

to to 0 air . It can be made absorb up 3 per cent of water without feeling damp . The legal quantity of water in silk is 1 0 per cent and it is sold on that basis , the moisture in each purchase being determined by conditioning . Silk is very strong ; it is elastic and can be stretched one-seventh of its length without breaking . 6 S o al 9 . ilk behaves like w ol toward metallic s ts used for

m e al d mordants . It deco pos s the s ts even in col solution . It likewise acts in a similar man ner toward coloring matters

h as aflinit in general , but less y for acid colors, and a greater affinity for basic colors . 0 f 7 . The luster o silk is increased after dyeing by treat

h a ment wit acids ; by this means it acquires a peculi r feel,

a and emits a peculi r crackling sound when compressed . h T e scrou . p feel, as it is called , is frequently desired Tar taric acid gives the best results .

1 7 . The absorptive power of silk is taken advantage of in the weighing of the fiber, which is accomplished by

al . means of tannic acid , iron and other s ts The dyeing of silk is usually accomplished with mordant colors , but for demonstration we will dye a few samples in an acid bath , and some in a neutral bath .

2 For of i 7 . the acid bath make a solution sulfuric ac d

1 0 200 . . . 1 grams in c c of water To this add per cent of dye , ° ° 86 ai 20 C enter the silk at and r se to 3 F . ontinue dyeing until the bath is nearly exhausted . The dyestuff for this bath may be

a S 6 R l . c R . ( ) carlet cryst ( ) Bril iant orange O . G b a h h l d N t o S. A B ( ) p yellow ( ) cid magenta 4 . D YEING OF TEX TILE FIBERS 35

73 . In place of sulfuric acid employ acetic acid , using

R v c G . (2 ) Methyl iolet (all brands) ( ) Janus yellow . ll d l (b) Safranin (a brands) ( ) Diani orange G . pat .

P th e 1 0 7 4 . repare bath with per cent olive oil soap ,

2 of add 1 l broken with per cent acetic acid , per cent of co or,

k to 1 80 F . enter a skein lu ewarmand Slowly raise , rinse well

e r and scroup with 5 p cent solution of tartaric acid .

l . c M . B B (a) Safranin F . F extra ( ) ethylene b ue . .

M 1 B - P N. . B (b) hosphin ethyl violet 7 .

ble Fibe rs e Ve e ta . 7 5 . g The bas s of all vegetable fibers is to be found in cellulose , a compound belonging to a class of naturally occurring substances known as carbohydrates .

1 These fibe rs may be divided into two classes . ( ) Seed hairs ; that is fibers attached to the se ed of plants as the i . C s common thistle , dandelion , and cotton otton the only of al fiber this kind of commerci importance . Each fiber is

- compose d of a single cell . They vary from one fourth to

2 B : two inches in length . ( ) ast fibers fibers from the stem as or leaves of plants jute , flax, etc . The fibers may be 6 h m . co quite long , in some cases upward to feet T ey are pound fibers being composed of bundles of cells cemented h together . The cells or ultimate fibers are quite s ort . About 30 kinds of vegetable fibers are used in th e United

S . tates, not all of them , however, as textile fibers The most important are cotton, flax (linen) , hemp , jute , and c hina grass .

- Cotton . e 7 6. Cotton is enclos d in a 3 to 5 valved

or capsule boll, which bursts when ripe . It is picked by hand and ginned to remove seeds and coarse impurities like

. is leaves , from the seed hairs or lint The cotton packed in bales weighing from 300 to 500 pounds . 36 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

i its . C s 7 7 otton graded chiefly by length of fiber, though and its freedom from dust, color, leaves, seeds, seed particles are also considered . The longer fibers are smaller in diam

hr eter, are silkier, and can be spun into finer t eads than the coarser . 8 i ur s . Se h 7 . O cotton of two types a Island cotton as the longest and finest staple , and commands the highest price

is of any commercial cotton . It grown only on the islands S C a and along the coast of outh arolina and Florid , and to a ulf M limite d extent along the G of exico . It is less than one of per cent our crop . - as The remaining ninety nine per cent ,known the American U h as an d is a i h pland , a larger staple of a better qu l ty than t e

E a and E a ast Indi n other growths, except the gypti n , which comes between American Upland and Se a Island in quality and price . Pr tie f tton o e r Co . . s o as 7 9 p Dilute mineral acids ,

u s lfuric , or hydrochloric , have little action on cellulose , unless allowed to dry upon it ; as the fiber dries and the acid

th e l f e f . becomes mor concentrated , cel ulose is a ected Fibers e compos d of cellulose like cotton or linen , become weaker or h packe d to a powder under suc conditions . The degree to which this change occurs depends on the temperature at h i h w ich the dry ng takes place , and upon the strengt of the acid . The destruction of vegetable fibers by the action of mineral

is for acid at an elevated temperature called carbonization , th e s - is rea on that the powder hydro cellulose usually black, W o is r so . or nea ly , and it was thought to be carbon o l not destroyed by carbonization . C h and ellulose as weak acid basic properties, and will B absorb acids or alkalies from very dilute solutions . eyond al on this , dilute solutions of caustic kalies have no action

F H 38 LABORA TOR Y GUIDE O INDUSTRIAL C EMISTR Y

i 1 s 00 s . in which about gram of odium carbonate to 5 c c . When thoroughly wet they are placed in clean water until

needed . P - 2 repare a dye bath with per cent of color (direct dye) ,

’ ’ of an d 20 of G 2 per cent sodium carbonate , per cent lauber s

o I o- s salt (s dium sulfate) , using six gram skein , boil for half

R . an hour . emove , rinse and dry d e stufls List of a few direct y for tests on cotton .

B ur e in Congo red 4 R . enzo p p r Primulin Dianil red D Benzo orange R . ianil brown O x B B . Benzo green . . y diamin brown 3 G N.

R Ox . W . F Diamin black . O . y diamin black J .

R . Diazo brown G .

8 - rarn of 3 . Dye six 5 g skeins wool in the same way, with out the sodium carbonate . If we examine the two solutions after dyeing cotton and

h : wool wit a direct color, we find

1 h as - . The wool exhausted the dye bath ; that is, it h as ff withdrawn almost all dyestu from solution . h h 2 . as The cotton not ex austed the bath , but has left a th e considerable portion of dye unabsorbed . The experiment illustrates the characteristic difference between animal and vegetable fibers in their be h avior toward direct dyes . The object in adding salt to the dye -bath is to cause a decrease in the solubility of the dye , and thereby cause more of it to go on to the fiber . Hard water should not be used for dyeing as it caused a precipitate of the dye as magnesium and calcium salts with a consequent loss . When cotton yar n dyed with a direct color is boiled in D FEING OF TEX TILE F IBERS 3 9

water, part of the color will be removed or stripped from the

fiber . 8 P 4 . lait a skein of the dyed cotton with undyed cotton and boil it for 1 5 minutes .

8 th e 5 . Do the same with wool , using undyed woolen yarn . Th ese tests sh ow that cotton is more easily stripped than

I th e . t wool also shows in case of cotton , that the undyed cotton takes the color away from th e oth er and eventually they would become of the same color .

8 6 to . It we subject the dyed yarn the action of warm — water and soap that is, imitate the action of washing If the solution becomes colored . white material is present

i. e . to it also becomes colored , , the color is said blend . P h lait a skein of the dyed cotton wit undyed cotton , make f ° 2 s 200 . . o 60 C . a solution of gram of soap in c c water, heat to

for 1 0 I Introduce the plaited skein and work minutes . t is

h out t en rinsed in cold water, wrung and dried . 8 7 . Test the dyeing of wool in the same way and note results in each case .

88 If for . a skein is placed in direct sunlight several days All ff the color will fade . dyes are e ected by light , but vary in their resistance toward it .

for t Dyes are also treated fas ness to acid . This test represents their resistance to acids in the air and pe rspira tion . I of 89 . ntroduce a skein dyed yarn into a 2 5 per cent f solution o acetic acid and work for 5 minutes . Wring h . N . out , wash and dry ote any c ange in color A nother test is for fastness to alkalies . 0 I of 9 . ntroduce a skein yarn into a 1 pe r cent solution of

d h . so ium carbonate and work for 5 minutes . Note any c ange s The above li ts are members of a class of dyes , known as ll direct cotton colors , or substantive cotton colors , which wi 40 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

dye cotton , wool, or any other fiber without the aid of other substances .

1 Mmoriza i n e t o . 80 9 . Dissolve grams of caustic soda

. d 00 . an in 4 c c of water allow the solution to cool . Cut a piece of unblMeached cotton cloth about 6 inch es long 2 . and inches wide easure it carefully, wet, squeeze , and h t en immerse it for 5 minutes in the above solution , remove , R How was h and dry . emeasure . much has it shrunk ? What pe r cent ? 2 -off 9 . Immerse 4 boiled skeins of cotton yarn in the

O above solution , work carefully for 5 minutes, remove , wash with water, then with water containing a little acetic acid , di and dry . Are they in any way fle re nt from ordinary cotton ?

93 . Dye a skein of your mercerized cotton with l per cent

mine blue and 1 0 2 xa 00 . O per cent sodium sulfate in c . c I 1 . s x ? of water , boiling 5 minutes the bath e hausted This dye is a direct cotton color .

94 . Dye an unmercerized skein in the same way . Which skein takes up the more dye Which is darker ?

9 5 . Work two skeins of mercerized cotton 3 0 minutes in

2 . 2 pe r cMent tannic acid in 00 c . c cold water . 6. e i 9 ordant two unmerceriz d ske ns in the same way. D . e 9 7 y one of each , mercerized and unmercerized , in a

2 . separate bath of l per cent methyl violet in 00 c c . of water ° h 0 C. w 20 . t e ? at 5 , orking minutes Is bath exhausted Which skein takes up the more dye ? The depth of color

depends upon the amount of tannic acid taken up . Which takes up the more tannic acid 8 9 . Dye a skein of mercerized cotton with 1 pe r cent of °

. 0 . . me th yle ne blue in 200 c c . water at 5 C working 1 5 minutes

n . W 99 . Dye an u mercerized skein in the same way hat difle re nce do you se e ? D YEING OF TEX TILE FIBERS 4:

Both of these dyes are basic colors . That is, they are s salts of color ba es, direct dyes for wool , but not for a a an cotton , and are dyed on cotton with t nnic cid mord t,

or mordants of acid nature .

1 00 M To- . ordant five gram skeins of cotton yarn with 5

00 . . 1 per cent of sumach in 4 c c of water , boiling for 5 min “ ” utes , or until wetted out, and allowed to stand one

hour .

1 0 1 one h as as . Dye skein , which been mordanted above

2 with each of the following, using per cent of the — ° ff e 1 20 1 0 . dyestu , temp rature 4 F

(a) Auramin (c) Malachite green (all brands) d M R (b) Safran in T extra . ( ) ethyl violet .

1 62 M 1 0 - . ordant five gram skeins of cotton yarn with 5 as per cent of cutch in 400 c . c . of water in the same manner

above . 1 0 c h as a as 3 . Dye one skein whi h been mord nted above

1 with each of the following, using per cent of the

dyestuff .

c Ma (a) Auramin . ( ) al chite green (all brands) d M R b . ( ) Safranin T extra. ( ) ethyl violet

These tests illustrate some of the numerous sources of

tannic acid as applied in dyeing and printing. The examples given under tannic acid mordants serve to illustrate a large class of basic colors which are applied to cotton , and as they all act in practically the same manner it will not be necessary to give more along this line , except to include a list for those desiring to make a more exhaustive study of the subject . A few other basic colors 42 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

(a) Rhodamin (all brands) (f ) Magenta B c B (b) rilliant green ryst (g) Janus red .

' (c) Cotton gr een (h) Janus yellow

d Ne w a I N ( ) f st blue ( ) aphthol blue R . T . (e ) Phosphin (i) Bismarck brown

Diazotizin d De ve o in 1 0 an l . W 4 . g p g hen goods dyed

rimulin with p , and many other direct colors , are treated with a solution of nitrous acid , and then with a developer, new dyes are produced with new properties . They are in insoluble water, and valuable on account of being fast to i . s z washing The process called diazoti ing and developing. Direct cotton colors and bodies wh ich can be diazotized h H t e N . and developed contain group 2 They are related to ammonia in which one atom of hydrogen h as been replaced of as Wh by a complex group atoms anilin . en these substances are treated with nitrous acid , the two com bine to form a diazonium salt :

C 1 NH HC1 HNO C H N : N 1 2 C H 0 . J 5 2 2 o s 2 Anilin hydrochlorid Phe nyl diazonium chlorid or for any of these compounds

RNHzHCl HNO2 RN : NCl

u for un Diazonium compo nds are , the most part , very stable , and even explosive in the solid state . s When a diazonium alt is treated with phenol , or an aro matic amine under proper conditions, the two combine

e o . For directly and a stabl comp und is formed example,

C H N : NCl C H OH C H N : N-C H OH HCl O S o s , , , , Diazonium chlorid Phenol azoxy benzene

This is the kind of action which takes place when a diaz h otize d fabric is treated wit a developer . The developer G OF X D YEIN TE TILE FIBERS 43 combines with the diazonium compound to form a more stable body, which is a new dye . Some diazo colors :

(a) Sulphin (e ) Dianil black

b Oxamine ( ) violet (f ) Dianil ogene sky blue N.

c Oxamine B . G . O x . O . . ( ) blue (g) y diamin ogene T pat . (d) Dianil brown (h ) Primulin

1 0 D e 1 0 - of ff 5 . y five gram skeins boiled o cotton yarn rimulin 0 al with 4 per cent p , 3 per cent of s t and 5 pe r cent

00 . . of sodium carbonate in 4 c c of water ; heat, enter the yarn

0 . W and boil 3 minutes ork from time to time . Is the bath exhausted ?

1 0 a o th e 6. Di z tize four of dyed skeins in a bath of 3 per 200 cent of sodium nitrite , and per cent dilute hydrochloric acid in 400 c . c . of water . Free nitrous acid is liberated accord ing to the reaction :

1 = NaNO, HC NaCl HNO,

h Enter t e yarn and work ten minutes . The diazotized

imulin is n pr very u stable , and must be developed as soon as possible . 1 0 H 7 . ang one skein of the yarn , after diazotizing and

1 0 before developing in the sunshine for minutes, and then

a develop as in ( ) below . 1 De e H 08 v lo in . l . p g ave ready the fo lowing baths, enter

1 0 one skein in each , work cold minutes, wash and dry . (2 ) 1 per cent be ta-naphthol and 1 per cent sodium hydroxid in 200 c . c . water . (b) 1 per cent of resorcin and 2 per cent sodium hydroxid

2 . . in 00 c c of water . (c) 2 per cent alpha naphthol and 4 per cent sodium car

o i 200 . b nate n c .c water . 44 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

ff The preceding experiment shows that di erent developers, acting upon diazotized pr imulin produce difie re nt dyes of o l different colors . It als shows that ight decomposes diaz

i d rimulin and ts ot ze p , preven it from uniting with the

developer. 1 0 Mordants of Me tallic Tannate s 9 . . Insoluble metallic s r tannates pos ess an att action for basic colors, equal to if

not greater than tannic acid . The prese nce of the metal aids in the decomposition by reason of a portion neutralizing the

- liberated acid of the coloring matter, and it is probable that a very insoluble tann ate of the metal and the color base is

produced . The process of converting tann ic ac id into in is ll soluble metallic salts termed fixing, and is usua y carried

a n . S out fter mordanting with ta nic acid alts of antimony,

e as iron and sometimes tin are us d fixing agents . Antimony tannate is colorless and gives the brightest

and fastest colors . For this purpose tartar emetic is usually K SbO C H O O . employed , ( , , G) l 1 1 0 B I - . oil three o gram skeins of cotton yarn with 5 per

00 . . cent of tannic acid dissolved in 5 c c of water, until the i s d . At cotton thoroughly wette out least 1 5 minutes . A llow the solution to cool an hour, working the yarn from

time to time . Tannic acid is absorbe d more readily by cotton

ze from a cold solution . Squee well and proceed as below .

1 . as . Skein No. Dye directed below

S o 2 . N . 1 0 kein Fix with antimony, by working minutes m 2 00 . . in a bath of per cent tartar e etic in 4 c c water.

. 1 0 Skein No 3 . Fix with iron by working minutes in a bath of 5 per cent copperas and 3 per cent calcium car bonate in 400 c . c . water .

1 1 1 P - 1 . repare three dye baths with per cent mal achite E r 200 . . g een in c c . of water nter a skein in each bath , raise ° h e 6 C. and a fo t temperature to 5 , keep t this temperature r

46 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

and without rinsing by a strong solution of oxalic acid .

l and . Wash we l, dry

se n Grea spots, oils, paints, var ishes, and tar may be removed by washing or rubbin g with a cloth saturated with l either naphtha, benzene , ether, ch oroform, carbon disnl fid hl m , carbon tetrac orid , turpentine , or com on kerosene . Those who desire to make a more exhaustive study of this subject should refer to the literature published by the various - A coal tar color companies . brief outline, however, will be not given here in case such literature is available . Th ulfur D e stuffs on Co on 1 1 e S . 3 . y tt The colors be longing to this group are absorbed by cotton in a bath con lfi taining sodium su d . The bath is prepare d by boiling a solution containing 2 1 0 of ff 2 d from to per cent dyestu , to 3 per cent of so ium

1 0 sulfid 1 0 20 carbonate , 5 to per cent of sodium , and to ’

G . per cent of sodium chlorid , or lauber s salt The fiber is entered into the boiling bath and worked until finished , - h about one and one fourth ours . l It is very essential that , after dyeing, the cotton shou d be thoroughly washed before dryin g.

xam le — mme dial black 1 E s . I o lfid p 5 per cent, s dium su

- ’ 1 0 e r G s al 2 . per cent , soda ash 5 p cent, lauber s t 0 per cent

’ Imme dia l e llow sulfid e r y 5 per cent sodium 5 p cent ,

-ash G 5 I mme dial soda 5 per cent, lauber salt 5 per cent .

Dark blue 20 sulfid 20 - per cent, sodium per cent , soda ash ’ K 1 0 20 . at e I d R per cent, Glauber s salt per cent ig n n igo 2 .

- L . 1 0 sulfid 20 ash extra per cent, sodium per cent , soda ’ 6 al K b 0 ati e n lack T . per cent, Glauber s s t 5 per cent . g

sulfid 1 d - 8 extra per cent, sodium 5 per cent , so a ash ’ G 60 per cent, lauber s salt per cent . 1 1 Va n — . t Colors o Co ton an d W ool im 4 t . The most o ff p rtant dyestu of this class is Indigo, which is produced D YEING OF TEX TILE F IBERS 47 upon the fiber by first treating with an alkalin solution of r Indigo white , which , on oxidation in the air, is reconve ted “ ” into the blue . The term vat applies to the vessel em ployed for dissolving the Indigo and also to the solution it of self, which may be prepared by the aid various reducing agents .

1 1 h e Zin c Lime Vat 5 . T

L . 2 . M. 1 0 grams of Indigo . G powder or 5 gr paste 1 0 grams of zinc dust

30 grams of quick lime .

°

. 0 Mix the zinc dust with 1 50 c c . of water at 5 C ; add the T h Indigo and then the lime with constant stirring . e whole f or 6 h . is left to stand ours , but is stirred from time to time The reduction is complete when a drop of th e solution placed on a sheet of glass runs off as a yellow liquid which

- v oxidizes in the air in the course of forty fi e to fifty seconds .

n h 00 . . The reduced solutio is t en diluted with 5 c c of water, and the cotton fiber dyed in it by th oroughly soaking . It is

h out re t en wrung , and dried in the air ; the process being l pe ate d unti th e requisite shade is obtained . 1 Th lfa f n 1 e Su e o I o Vat . B 6. t r y following the same direction as above this bath may be prepared by using I M E 0 L . . 1 grams ndigo . . powder f 50 grams ferrous sul ate .

60 grams lime .

1 1 Th e H drosu lfite Vat 7 . y (for cotton) . This vat is

on of H S O based the property hydrosulfurous acid z z , of forming with Indigo a colorless double compound which is oxidi soluble in alkalies , and is decomposed by the weakest dation ; Indigo blue being thereby liberated . For practical use the sodium salt of hydrosulfurous acid

on Na,S,O, is prepared by allowing zinc dust to act sodium 48 LABORA TOR Y GUIDE OF INDUSTRIAL CH EMISTR Y

i s b sulfite in a tightly closed ves el , the mixture being kept

stirred and cooled . The reaction is usually complete within

h drosulfite t 4 or 5 hours . The y solu ion is rendered slightly al al l k in with milk of ime in order to diminish its instability , as ll and is then ready for use . The procedure is fo ows i fi 1 00 parts of sodium b su te solution Tw .

2 2 e of 5 parts of cold water, and in the cours half an hour h 3 2parts of zinc dust stirred into t is solution .

to is t The whole , which is stirred from time time , left o stand for 4 or 5 hours, and then mixed with

1 1 h parts of lime slaked in

3 0 parts of water .

A is fter allowing the sediment to settle , the clear solution 6° T w decanted , and 7 parts caustic soda solution 3 . added .

h drosulfite S The y solution is now ready for use . hould — ° 1 20 Tw . stand at 9 , and kept in a tight bottle in a dark room . 1 1 8 Pre aration of D e Vat . p y

1 0 grams of Indigo are mixed with 3 0 grams of hot water ; to this mixture 8 ° T w 6 . 5 grams caustic soda 7 are added , and the ° to 0 whole well stirred ; after heating 5 C . ° 2 0 h drosulfi w 5 grams of y te solution 20 T . are added ° and the temperature kept at 50 C.

of and In the course the reduction which takes place , is al which tested in the usu way with a sheet of glass, more h drosulfite al y solution is added in sever portions . The reduced Indigo ough t to run off the sheet of glass as a yellow

x to liquid , which o idized in twenty thirty seconds . The cotton fiber is then dyed in the same manner as in dicate d of in the case the zinc vat . D YEING OF TEX TILE FIBERS 49

fi 1 1 Th e H drosul te Vat . 9 . y (for wool) The process

e al s m is ess nti ly the same , only the use of caustic oda ust be replaced by milk of lime in sufficient amount to produce an

alkalin reaction . T k -r d u on n — - 1 20 ur e e Cotto . r i . y p The name turkey e d s ap al plied to the color produced upon cotton by the aid of izarin ,

e alumina, lim , and fatty acid compounds . This fatty acid compound known as Turkey-red oil is prepared by treating Oil Oil olive or castor with concentrated sulfuric acid , usually i e 1 0 O l. Se e 3 parts of acid being add d to , parts of (

The acid is slowly poured into the oil with constant stirring, and the whole then let to. stan d un til a sample of the product

is is found to dissolve completely in water, whereupon it poured into water and washed with a solution of sodium chlorid until free from sulfuric acid . During the process of mixing the temperature should not ° be allowed to rise above 40 C. Sometimes the last trace of acid is neutralized with ammonia . The production of a good Turkey-red upon cotton can only h ow be attained by practise ; the directions given should , ll ll if . ever, yield fairly good results carefu y fo owed

1 2 1 l in — I - C e ar . F o . g ree the cotton fiber ( gram skeins)

s . from grea e , etc , by boiling in a weak solution of sodium carbonate ; wring out thoroughly . 1 2 2 Oilin W con . g . ithout drying, enter into a bath taming 1 0 grams Turkey-red oil 90 grams water

W dr and work until thoroughly soaked . ring out and y in ° - 0 —0 h ot air cupboard at 4 5 C.

R . epeat this Operation twice ,drying between each immersion 1 2 Alumina Mordan t — W 3 . . ork the fiber through a bath ° — ° 0 0 C. of aluminium acetate 9 Tw . ; wring out and dry at 4 5 so LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

Repeat this treatment . ’ lk in E h ath con tainin 1 2 Ch a . e b 4 . g nter t cotton into a g

6 grams Of chalk and 1 liter of water

— ° l w 0 0 C. S at 3 4 tir we l for about half an hour, and then ash thoroughly in clean water . It is unnecessary to dry the cotton before dyeing . 2 D e in — h f 1 . S t e f 1 5 . y g tir dyestu ( 5 per cent alizarin — ° W paste) into th e water and enter th e skein at 20 2 5 C. ork

h for 20 nu the skeins at t is temperature about mi tes , and then heat up SO that in about half an hour th e tempe rature ° K h for h e 60 C. rises to eep at t is point about an hour, t n wring well and dry .

2 te amin for one 1 6 S . S . g team the dried cotton hour at a pressure of 1 5 pounds or for 2 hours without pressure ; then wash well . Bri h t nin 1 2 . e B al 7 g g . righten the dyed materi in a closed k of apparatus at a pressure Of 5 pounds . Wor in a solution

1 of 4 . 5 grams of soap in liter water ; leave the cotton in it

1 0 for minutes and wash well .

1 2 olors P odu c d Dire c l n Fi Oxida 8 . C r e t y upo th e be r by ion — A h r t . e nilin black, the typical memb r of t is g oup , is produced directly on the cotton fiber by the oxidation of two o ffi to anilin , and the following meth ds will su ce indicate the manner in which dye stufls Of this kind are forme d : n I . O e bath black The bath should contain

5 per cent anilin 1 2 per cent hydrochloric acid 6 per cent dichromate of soda

e r 5 p cent copper sulfate . The cotton should be entered into the bath and worked D YEIN G OF TEX TILE FIBERS 5 1 for one hour ; then the bath should be r aise d to boiling h during anot er hour, and the fiber worked at this tempera h ture for another alf hour ; wash and dry . I b I . Oxidation lack

1 26 grams anilin hydrochlorid are dissolved in

00 . . 3 c c of water, and mixed with 40 grams ch lorate of soda

1 0 T 5 grams acetate Of alumina w. grams ammonium chlorid 3 grams COppe r sulfate i and the whole made up to one l ter . s The fiber is thoroughly impregnated in this olution , wrung out and dried . ° It is then worked for half an hour at 60 C. in a bath con taming per cent bichromate of soda 5 per cent anilin h ydroch lorid

. 2 Tw per cent sulfuric acid .

and then washed and dried .

REFERENCES

T h e Li e r r bli h d b Me iste r Lucius an d B r t atu e pu s e y uning .

Farbe n brike n orm Fre de rick Ba e r Co . Fa v , y 81 d h l rik n Ba isc e Ani in an d Soda Fab e .

ll l r m n Casse a Co o Co pa y . Kalle and m n Co pa y .

Be rlin Anilin ork W s .

He ll r nd M rz e a e .

D e in and li ri co . London 1 . Ca P ntin A Sansone . 8 y g g . , 9 7

T h e ri i f T e x il F r R h ll ondon n n o F . o w L P t e b i . t a cs C. . S t e . 1 g , 897 .

olor in n Ro r mon nd n 1 0 2 C o e De i . b B W s n e e au t . Lo o . v g ts , 9

rin i le f D e i r r c . F . e w o k 1 . P s o n G . S. a s N Y 0 p y g p , 9 3 T x ile r rr h r e it a e ws . e w k 1 . t Fibe s . . Me t M t Y J N o , 904 CHAPT ER IV

MMERCIAL ORGANIC COMPOUND - CO S, COAL TAR OLORS AND SYNTHETI C , C OILS

d form HI 1 2 Io o . 9 . (C ,)

2 5 grams potassium iodid

5 grams acetone .

2 00 . Dissolve 5 grams of potassium iodid in 5 c c . of water

of . h and add 5 grams acetone To this mixture add , throug n a drop funnel with consta t shaking , a dilute solution of h l sodium hypoc lorite as long as a precipitate forms . Al ow off to . u the precipitate settle Decant the liq id , wash with “ water two or three times, filter , drain thoroughly, dry on

filter paper, and recrystallize from alcohol . The solution of sodium hypochlorite used in this e xpe ri all ment, may be made by precipitating the calcium in a solution of bleaching powder by a solution of sodium car

' A sli h t ot bonate . g excess of sodium carbonate will n inter

fere with the reaction .

Re action

I H H I H 1 I st . C ,COC , 3 , C ,COC , 3 H

2d . H I H1 2 C ,COC , 2 C ,

h l d 1 H l . 0 Ace t l C ori . C COC 3 . y ( s )

1 00 grams glacial acetic acid h 80 grams phosphorus tric lorid .

To 1 00 grams of glacial acetic acid contained in a 2 50 c . c . 5 2

COMMERCIAL ORGANIC COMPOUNDS 5 5

. n w ether, the distillation is stopped The receiver o contains

to h a h and in addition et er, lco ol , water sulfurous acid . The liquid is poured into a large separating funnel and a — small quantity (3 0 40 c . c . ) of dilute caustic soda added and l h A wel s aken . fter settling, the caustic soda solution is

off a Of drawn below , and about the same qu ntity a strong of a solution common s lt added , and the process of shaking

Off . and drawing repeated The ether , which is now free

of a from sulfurous acid and from most the lcohol , still con tains water . It is therefore poured into a large dry distilling of a flask and some pieces solid c lcium chlorid ad ded . It is allowed to stand loosely corke d over night . The distilling flask is now attach ed to a long condenser and heated on th e

. can water bath The ether , which distils , be freed from traces of alcohol and water by metallic sodium . A few very thin slices Of sodium are dropped into the receiver and th e w h vessel closed with a cork, through hic an open calcium chlorid tube is inserted . When th e action ceases the ether is decanted and distilled ° on th e water bath at a constant temperature of 3 5 C.

Re actions

C H OH C H SO H H O z B , , , , C H SO H C H 0 H C H 0 C H , , , , 5 , 5 , , — S . r . ro e rtie s . C . . P p olorless , mobile liquid ; b p p g ° 7 20 at burns with a luminous flame ; not miscible

1 a h with water ; 9 parts of water dissolve p rt Of et er, and 3 5 parts of ether dissolve 1 part Of water at the ordinary tem

r at pe ure . 1 2 l f rm a CHCl h o o o . 3 . C r (Trichlorometh ne) ( ,)

200 grams bleaching powder (fresh )

800 c . c . water

40 grams (50 c . c . ) acetone . 56 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

s is A lar ge round fla k (four liters) fitted with a cork, i through wh ch a bent tube passes , connecting the flask with a long condenser and receiver . The flask is placed upon a large sand bath . Grind the bleaching powder into a paste

and s with 400 c . c . of water rinse it into the fla k with the Add and remaining 400 c . c . the acetone attach the flask to H the condenser. eat cautiously until a reaction sets in , R which is indicated by the frothing of the liquid . emove the flame for a time , until the reaction has moderated ; finally boil the contents until no more chloroform distils . This is easily determined by collecting the distillate in a test -tube

v and obser ing if any drops of heavy liquid are prese nt . The distillate is shaken with dilute caustic soda solution in a se parating funnel and the lower layer of chloroform run in to A a distilling flas k . few pie ces of solid calcium chlorid are added and left until the liquid is clear, when it is distilled from th e water bath with the thermometer inserted into the

Y 0 neck of the flask . ield about 4 grams . The bleaching powder acts as though it consisted of a u d compo nd of calcium hy roxid and chlorin , and the process probably occurs in two stages .

Re actions

- - 1 . CH COCH C1 CH CO CCI H 3 , 3 , 3 , 3 cl.

H ~ 2 . 2 C 3 CO (CH,

Pro e rtie s . C s s p olorle s liquid po sessing a sweet smell, 1 b . p . 6 Sp. gr; at very slightly soluble in -inflamm water ; non able .

Re action 1 . . Heat a few drops with double its volume of methyl alcoholic potash . On the addition of water a o P clear s lution is obtained . otassium formate and chlorid being formed . H l C C , 4 KOH 3 KCl HCOO K 2 COMMERCIAL ORGANIC COMPOUNDS 5 7

B - 2 . on ring into a test tube two drops of chloroform , e l l drop of an i in and 1 c . c . of alcoho ic potash and warm in the N l of fume cupboard . ote the intolerable smel phenyl car

carbamin bamin ( reaction) ,

HCl C H NH KOH C H NC K l C , 6 5 ,+ 3 , , + 3 C +3 H,O

1 Am "Ace tate . 33 . y

A a distilling flask is attached to condenser and receiver . T he flask is provided with separatory funnel as in the prep A of f aration of ether . mixture equal parts o amyl alcohol and

1 . e sulfuric acid ( 00 c c . of each) is pour d into the flask which ° i Oil- 1 0 C s . then heated in the bath to 4 , and kept at this tem A pe r ature . mixture of equal volume of glacial acetic acid l l . and ac oh o 200 . a amyl ( c c of e ch) is now added , drop by drop, from the tap funnel at the speed at which the liquid W all distils . hen the mixture has been added , the distillate is shaken with a solution of sodium carbonate in a separatory of funnel ,until the upper layer amyl acetate no longer reddens

is n blue litmus paper . It agai shaken with a concentrated

f 1 o 00 1 00 . solution calcium chlorid ( grams in c c . water) ; after removing the solution Of calcium chlorid th e amyl acetate is allowed to stan d over fused calcium ch lorid for

1 2 hours and then distilled . The portion passing over — ° 1 0 1 C. between 4 5 5 being very pure amyl acetate .

Re action

C H OH CH COOH H 5 ,, , ,O

This compound is use d very extensively as a solvent for

un - g cotton and in the manufacture of varnish .

1 Ni ro e nzol H t b . C N0 3 4 . ( 6 5 ,)

200 grams of benzol

2 0 S . 4 grams of nitric acid , p gr . 60 S 3 grams of sulfuric acid , p . gr . 58 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

The nitric acid is added in small portions at a time to

1 . . the sulfuric acid contained in a 000 c c . flask During this l Operation the flask is we l cooled under the tap . The mix ture is transferred to a tap funnel and added slowly to the benzol contained in a two liter flask . The flask is well shaken after each addition and the temperature not allowed ° all of h 2 C. n as to rise above 5 u til nearly the acid been added . A wide glass tube is now attached by a cork to the flask s forming an air conden er, and the mixture heated on the ° - for 60 C . water bath an hour at being frequently shaken . The contents of the flask are poured into about two liters of h to water w en the nitrobenzol settles the bottom , which of It can be removed by means a separatory funnel . is

then wash ed several times with water . The nitrobenzol is next r un into a distilling flask fitted with a th ermometer — and connected with a long glass tube about 8 1 0 mm . in

. l diameter, forming an air condenser The Oil is distil ed

over a free flame . At a first water and benzol p ss over , then the temperature ° h n h rises rapidly to over 200 C . w e the receiver is c anged ° b l 20 —20 and the nitro e n zol co lected at 4 7 C.

r —L - ro e tie s . P p ight yellow liquid , with a smell Of bitter ° . . 2 . . . 1 almonds ; b p 06 m p Sp gr . at 5 Nitrobe nzol comes on the market as ( 1 ) light or pure

. 20 S . . . 2 nitrobenzol, b p 5 p gr and ( ) heavy i l l z n troto uo e s b 2 1 0 S . nitroben ol (containing ) , . p . p h ” “ gr . The terms lig t and heavy apply to the

to th e b . oiling point only , not specific gravities

s e — P n fo U . ure itrobenzol is used r the manufacture of

n H n anilin , benzidi , and in perfumery . eavy itrobenzol th of is used in e manufacture magenta .

Re action HNO C H N , , , O, COMMERCIAL ORGANIC COMPOUNDS 59

n — C H NH 1 An ili . 3 5 . ,, 5 2

200 grams of nitrobenzol 2 40 grams of iron powder

c 20 grams of hydrochloric a id .

h 20 . . a a The iron , toget er with 3 c c Of w ter is pl ced in a large — s flask Of 2 3 liters capacity and well shaken . The fla k is warmed sligh tly and a few drops of nitrobenzol added . Then the acid is poured into the flask and the remainder of

FI f G . C or e n n T u . A an e r i e a be in l w u 9 , g at g st m ; B , pass g be o s rface of

i u i F as D on e n se r E Re c e i r l q d ; C , l k ; , C d ; , ve .

the nitrobenzol is introduced in small portions at a time . After each addition the flask is thoroughly shaken and cooled under the tap . The addition of nitrobenzol is so regu lated as to keep the temperature about 80 When the re action is finished (sh own by no further rise in tempe rature on sh aking) th e contents of th e flask are distilled with steam Fi l ( g . 9 ) till the distil ate is no longer milky . The distillate is i a ff transferred to a separatory funnel and the n lin drawn O . The water is now saturated with salt and the Oil which rises to the top is added to the first portion and the whole distilled . 60 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTR Y

A little water passes over at first and is separately collected ; th en anilin passes over at

r ie s . e ro e t C . P p olorless oil with a p culiar smell ; b p .

Sp. gr . “ ” At Commercial pure anilin is tested by distillation . least 90 pe r cent by volume should distil at It should give a clear solution with hydrochloric acid ; a yellow color

indicates the presence of nitrobenzol . “ ” Anilin for Re d for the manufacture of magenta) — n 2 2 e r - — 0 is a mixture of a ilin (3 4 p cent) , ortho toluidin (3 5 5

- — 1 2 . s per cent) , and para toluidin ( 4 4 per cent) It re ults from “ ” the reduction of heavy nitrobenzol . It should boil be ° tween 1 90 and and have a specific gravity of ° to at 1 5 C. —A l i Use . ni in is used for making a large number of ts sub

stitution l as for products as we l quinolin,indulin ,magenta , ani

- z azo i lin blue , diazo ben ene salts (for dyes) , and an lin black .

Re action

C H NO 6 HCI= C H NH e , , ,+3 Fe + , , ,+ 3 Fe l,

i c ic Ac d . 1 6. Pi r 3 .

20 grams phenol

20 grams sulfuric acid (conc . )

1 00 grams nitric acid .

° H n - eat together o a water bath to about 1 00 C. a mixture f o 20 grams phenol and 20 grams conc . sulfuric acid until

complete solution takes place . Dilute with twice the volume

of water and transfer to a separatory funnel . Now add this

raduall car e ull constant s h a kin mixture g y , f y , and with g , to

1 00 W r grams of cone . nitric acid . a m the mixture on a water to bath until the red color changes yellow ,then pour into a liter of w fi te r ofl c rstals n a h ater, l the y , drai thoroughly, w sh wit

62 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

H l 1 8 Be n zo l Ch lorid . C COC 3 . y ( o s )

5 0 grams benzoic acid e ntach lorid 90 grams phosphorous p .

a 00 . w Treat 50 grams benzoic cid in a dry 5 c c . flask ith 90 grams Of finely pulverized ph osph orous pe ntach lorid under h two h the ood . The are s aken well together, upon which an energetic action takes place with th e evolution of hydro

th e of th e chloric acid ; in order to prevent cracking flask ,

not an or place it on a wooden block and on y stone porcelain .

A a d fter standing for a time , it is twice fraction te , using a D long wide air condenser . etermine the boiling point .

Re action

C H COOH PCl C H COCI POCl HCl O B 5 G S ,

1 Fl r c in 3 9 . u o e s e .

3 0 grams ph thalic anhydrid 44 grams resorcinol h 1 4 grams zinc c lorid .

The materials are ground togeth er in a mortar and heated ° - h 1 For h in an oil bat to 80 C. t is purpose a nickel crucible

A as th e h may be used . S soon temperature as reached ° h 1 80 C. 1 a l n , 4 grams Of zinc c lorid are added gradu l y duri g

1 0 A minutes, the melt being stirred with a glass rod . fter th e zinc chlorid has been added th e temperature is raised to ° 1 h 2 0 C. t e a s , and kept at this temperature until m s becomes

w h T h e solid (one to t o ours) . cold melt is broken out of th e or n crucible with a chisel k ife , powdered , and dissolved l A h a . a in di ute c ustic soda fter filtering , hydroc loric cid is

h fluore sce in h added , w ich precipitates the ; t is is filtered ,

T h e i washed and dried . crude substances are treated w th h t e e . alcohol (boiling) , and residu after filtering is dried COMMERCIAL ORGANIC COMPOUNDS 63

Re action

2 2 H,O

One -third of the solution obtained by treatment with to - caustic soda is evaporated dryness, and a dye test made

5 . 6 with it on wool and silk as given under tests N0 3 and 73 .

1 0 Eosin 4 . .

1 5 grams fluore sce in 33 grams bromin

60 grams alcohol .

T e fluore sce in a 60 h is pl ced in a flask , grams of . alcohol l added , and the bromin dropped in slowly from a sma l h a . W sep ratory funnel en half the bromin has been added , th e dibromid which is formed is in solution ; but on further

f h e addition o bromin t e tetrabromid s parates out . After

for two is s standing hours the precipitate filtered , wa hed

a h first with lco ol , then with water, and converted into the

i a sodium salt by mix ng it with a little hot water, c refully neutralizing with caustic soda (avoiding an excess of this

on - reagent) and evaporating to dryness the water bath .

r r E - P ope tie s . osin forms bluish red crystals or a brown ish -re d - powder, dissolving in water with a bluish red color.

Re action :

H Br B . 1 . r 4 2 4 H 2 a H 2 . 2 . N O ,O

n Dye a skein of worsted a d silk as under tests Nos . 63 and 73 . 1 1 Dim th l A ilin e . 4 . y n

1 50 grams anilin 50 grams anilin hydroch lorid h 1 50 grams met yl alcohol .

T h e mixture is h eated in a closed iron retort for 7 to 8 64 LABORA TORY GUIDE OF IN DUSTRIAL CHEMISTRY

° hours to 230 the product then made alkalin with th H e . NaO , distilled with steam , and oil separated It is dr ied over solid caustic potash and the fraction boiling at °— ° 1 90 200 is collected . ° r s M . 1 2 e . . Prope ti obile liquid ; b p 9 C.

Re action :

1i H 2 c11 0 11 2 c , ,N , ,

Anilin hydrochlorid is made by dissolving the anilin in hydrochloric acid and evaporating to the point of crystalliza tion . Trade name , anilin salt . l B 1 Me h l Vio e t . 45 . t y . T .

NHCH 3 8 75 grams of sodium chlorid 5 0 grams of copper sulfate ' C N

The salt and copper sulfate (finely powdered) are well

0 mixed together in a mortar, and a solution of 4 grams of

h 1 0 . . p enol in c c of water added , and the whole stirred well . T h e dimethyl anilin is now added and the mixture trans ferred to a round flask and heated on the water -bath for

8 out hours , at 5 The product is poured into a porcelain

In basin and allowed to cool . order to free it from phenol

to and salt , it is broken up and added gradually three liters

to h h of water (boiling) w ic has been added milk Of lime , pre

0 a 2 f C O 00 . o A pared from 4 grams Of and c . c water . fter h no x eating until more lumps are present , the mi ture is

to of allowed settle , and the clear solution salt and calcium

d nt phenate e ca e re d .

x h The residue of copper o id , met yl violet and calcium

s a a . sulfate is wa hed ag in by decantation , and fin lly filtered COMMERCIAL ORGANIC COMPOUNDS 65

In order to get rid of the copper oxid the precipitate is l boiled with dilute su furic acid , and sodium sulfate (free

from chlorid) added to precipitate the dye , which is filtered di and washed . The precipitated violet is subsequently s solved in water aMnd re pre cipitate d with salt . r e rtie s . P op ethyl violet is a glistening greenish powder,

dissolving In water with a violet color .

Dyes Silk and wool violet ; cotton , after mordanting with — d . o . 6 1 1 tannin an tartar emetic Tests N s 3 73 and 0 .

Re actions

( 1 ) O CH,O C H N11C11 H O (2) 2 , , , C , O, C0 11

2

(3) HCI -Cl

1 Fa Gre n 0 dinitro r or in 6. st e so e s c 4 ( ) .

O

40 grams of resorcinol

n 90 grams of co e . hydrochloric acid

1 of 5 grams sodium nitrite .

NOH

1 The resorcinol is dissolved in 600 c . c . of water and the

200 hydrochloric acid added , together with grams of common i ° . s 0 . salt Ice is added till the temperature C , and into this r solution , which is sti red mechanically, the sodium nitrite i 200 . . s e dissolved in c c of water allow d to flow very slowly, the temperature not being allowed to rise above This takes about half an hour . When all of the nitrite h as been ad A ded , the liquid should show a faint acid reaction . fter s - tanding for one hour, the brownish yellow precipitate is 66 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTR Y

h filtered , was ed with ice cold water , and the paste dried on a porous plate .

R e action :

211NO H O H , , C, , H (NO ) 20 2

- Pro e rtie s . G h o t . p rayish brown powder, soluble in water o D Dyes iron mordanted cotton r wool green . ye a skein of f 1 1 0 or . cotton and worsted . Test cotton

1 N h h l Ye llo a w S. 47 . p t o 2SO,K,)

1 00 grams a-naphthol

400 grams conc . sulfuric acid

200 grams conc . nitric acid .

The sulfuric acid is warmed in a round bottom flask to ° 1 00 a- C . and the finely powdered naphthol added gradually . ° h The temperature is now raised to 1 20 C . and kept at t is

x point for 3 or 4 hours . The sulfonation mi ture is then

00 . AS poured into 6 c . c . of water and stirred mechanically ° soon as the temperature is about 30 the nitric acid is added

- th e very slowly drop by drop through a tap funnel , tempera ture not being allowed to rise over The din itron aph th ol

i w h sulfonic ac d , hic separates out after standing, is filtered h i at the pump , was ed with saturated salt solut on till free P from acid , and mixed with boiling water . otassium car

a bonate is now added till an alkaline re ction is obtained , and , l after cooling the precipitated potassium sa t , filtered and dried on a porous plate . 4 - D r r n . P ope tie s . Ora ge yellow powder yes wool and - h silk yellow from an acid bat . Dye a skein of worsted and

6 . silk as under tests No. 3 and 73

Re action :

1I 11 2 HNO H SO C,, ,O + ,+ , , COMMERCIAL ORGANIC COMPOUNDS 67

- Acid 1 P su lfanilic . 48 .

200 grams anilin

2 2 . 0 grams conc sulfuric acid .

The anilin is stirred into the acid contained in a shallow h C H porcelain dis , and the acid sulfate thus obtained ( , , N is heated in an oven till the temperature reaches ° 20 5 C . This must take four hours . The oven is kept at

ix this temperature for s hours more . The product is broken up and dissolved in h ot water with the addition of 80 grams

a of caustic soda (alkalin re ction must be obtained) . The solution of sodium sulfanilate is boiled for a few minutes

l a h with a ittle anim l charcoal and filtered ot . On acidifying h with ydrochloric acid (congo paper must be turned blue) , th e sulfanilic acid crystallizes out ; after standing over night it is filtered at th e pump and dried at

r r e s P ope ti . Sulfanilic acid crystallizes form water in large colorless plates containing one molecule of water of a h h is s l crystalliz tion , w ic , however, ea ily driven Ofl. Su fan ilic th e - acid is used largely in preparation of azo dyes .

Re action :

C H NH H SO ,, 5 z , , H,O I 1 Oran e I . 49 . g

SOsNa N : N

grams of P-sulfanilic acid grams Of sodium nitrite

- grams of B naphthol .

The sulfanilic acid is dissolved in water by careful addi 68 LABORA TORY GUIDE OF INDUSTRIAL CH EMISTRY

tion of caustic soda solution . Ice is added till the tempera ° f is C. o one ture 5 , the volume the whole being about liter ;

con e . 60 c . c . of hydrochloric acid are poured in , and then the sodium nitrite dissolved in a small quantity of water added

r slowly . Tests are made from time to time with sta ch iodid

paper, and a slightly blue coloration should be obtained when h - all of the nitrite as been added . The diazo compound

separates out in fine white needles . The B—naphthol is dissolved by heating it with a solution

0 . of 9 grams of caustic soda in 3 c . c Of water, and the sodium

20 naphtholate solution thus formed is poured into 3 c . c . of cold water and cooled if necessary to about This solu tion is stirred and the diazo-compound (in suspension) run

th e h - in gradually . When w ole of the diazo compound h as

h al been added , the mass should S ow a weak alk in reaction .

for The mass is stirred an hour longer, when nearly the

of - l whole the coloring matter wil have separated out . A to little salt solution is added aid in the precipitation , until

a test on filter paper shows only a pink orange rim .

D e y a skein of worsted and silk as under tests Nos. 63 and 73 .

Re actions

2 NaNO 2 11cl = SC H ( ) , O, , ,N 2N

2 a l 2 H N C ,O .

2 2N C H a S Na H N : C H H ON O C N O . ( ) l o , , , , 10 ,

Ac i id e tan l . C H NHC H O ( o s 2 , )

200 grams of an ilin

1 0 Of 5 grams glacial acetic acid .

anilin and acetic acid are mixed in a round bottom

D 7 0 LABORA TORY GUIDE OF IN USTRIAL CH EMISTR Y

— P-nitrace tan ilid Use . is used for the preparation of

- - p nitran ilin and p amidoace tanilid .

Re action :

NH NO H + O3 , ,O

1 2 P-nitranilin 5 . .

200 of -n itrac nili grams p e ta d .

i s 00 . The acetyl compound boiled with 5 c . c of dilute sul furic acid (25 pe r cent) in a round bottom flask connected h s h T h wit a reflux conden er until the w ole dissolves . e clear

re ci i solution is poured into a beaker, and the free base p p tate d a al by adding dilute caustic soda solution till lk ine .

A -nitr anilin is l e fter cooling, the p fi tered , recrystalliz d from

h ot e on o . water, and dri d a p rous plate — Y r e rtie s . P o . . p ellow needles or prisms ; m p , dis

in 1 2 0 not h solves 5 parts of water at volatil wit steam .

— P-nitranilin Use . is used in the production of azo

- dyes, and also for the preparation of its diazo compound , h — which, by combination wit Bnaphthol on the fiber, yields ili paranitr an n red . Dye a skein of cotton as given under

o 6 1 08 . N s . 1 0 1 0 tests 5 , and

Re actions

( 1 ) 2 H,SO, H ,SO, 2 CN,COOH . (2 ) 2 NaOH 2

Na SO 2 H , , 20 .

1 An h ra uinon t e . 5 3 . q

20 grams anthracene 240 grams glacial acetic ac id

0 4 grams chromium trioxid dissolved in 30 water,

1 0 . . acid a dd then 5 c c glacial acetic e d . COMMERCIAL ORGANIC COMPOUNDS 7 :

The anthracene is dissolved in th e acetic acid by boiling them togeth er in a round bottom flask (one liter) with upright h condenser over wire gauze . The solution of c romium - h trioxid is then dropped in from a tap funnel , pus ed into

th e to . p end Of the condenser , while the liquid is kept cooling h The Operation s ould last about one hour . The solution I t . t o becomes a deep green is allowed cool , and is poured into water (one liter) which precipitates the anthraquinone in

A one the form of a brown powder . fter standing for hour it is l h l h ot filtered through a large folded fi ter , was ed with a litt e water, then with warm dilute caustic soda, and again with water . It may be purified by sublimation .

r e Y : . . Pro e ti s . p ellow needles m p , sublimes at

b . p . insoluble in water, soluble in acetic acid , l ess soluble in benzin .

2 2 2 2 02 . H 30 C. .

Anth r a n Acid 1 uino ni . H 5 4 . q e Sulfo c (C, ,

SO3 H) 1 00 grams anthraquinone

1 00 grams fuming sulfuric acid .

The finely powdered anth raquinone is added to the sul furie acid and th e mixture heated gradually on th e Oil ° bath till a temperature of 1 60 is obtained . The mixture is

h ot 2 th e slowly and carefully poured into water ( liters) ,

for h solution boiled some time , and the unchanged ant ra

O h quinone filtered ff at t e pump . The filtrate is neutralized h wit caustic soda and allowed to cool, when the greater part

of the sodium anthraquinone sulfonate crystallizes out . “ h so- A of (T is is the called silver salt . second crop crys th tals may be Obtained by further concentration of e filtrate,

but is apt to be contaminated with sodium sulfate .

Pr r ope tie s . The sodium salt crystallizes from water 7 2 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

al with one molecule of water of cryst lization , having the formula On melting with caustic soda l it is converted into a izarin . OH a

’ 1 Alizan n 5 5 . . OH fl

1 00 grams sodium anthraquinone sulfonate 3 00 grams caustic soda

1 8 grams potassium chlorate . f 00 . o The caustic soda is dissolved in 3 c c . water in an autoclave and th e sodium anthraquinone sulfonate stirred

T h h 1 00 . . in . e potassium c lorate is dissolved in c c of water

(hot) and thoroughly mixed with the mass . The lid of the autoclave is then fixed on and the whole heated for 20 hours to After cooling the melt is ex tracted with boiling water several times, and the solution acidified with hydrochloric acid .

The alizarin which separates out is filtered at the pump , r washed with water, p essed on a porous plate and dried at

Pr e rt e s Y o i . p ellow powder, slightly soluble in boiling

e d . water, can be sublimed to long r needles Dyes cotton ,

- mordanted with alumina, scarlet red ; with tin, bluish red ; h wit iron , violet ; with chromium , brown . Re action

H K l 3 9 NaO 2 C O, 3

ONa Na 2 K l H ( ) , ,SO, C 6 ,O .

1 60 Me h le n Bl . t e ue y .

N(CH,) C1 CoMMER IA O c L RGA N IC COMPOUNDS 73

48 grams dimethyl anilin

1 3 0 grams conc . hydrochloric acid grams sodium nitrite 40 grams zinc dust 1 00 grams sodium thiosulfate 50 grams potassium dichromate 1 06 grams sulfuric acid

1 6 grams neutral sodium chromate .

Twenty-four grams of dimethyl anilin are dissolved in a of mixture of 80 c . c . water and 1 30 grams of concentrated and hydrochloric acid , the solution cooled with ice to 1 2

h r This is stirred mec anically, and a solution of g ams of sodium nitrite run in slowly (delivery tube unde rneath th e h surface of the liquid) , taking care t at the temperature does not rise above The nitroso compound is reduced

0 of l by adding about 4 grams zinc dust careful y , and the reduction is complete when the solution is of a clear red

sufli i n color . The amount of zinc added must be c e t to neu tr alize the hydrochloric acid , so that congo paper is no longer turned blue . The solution is now diluted with water to f . 2 o 1 000 c c . and a solution of 4 grams dimethyl anilin in the exact quantity of hydrochloric acid necessary to form the

20 . . hydrochlorid (about c c ) added , and then a solution of of h 1 00 grams sodium t iosulfate in a little water . The mixture is oxidized by adding a concentrated solution of 50 grams of potassium dichromate and boiling for two

1 0 6 u . of hours ; grams of s lfuric acid diluted with 200 c c . h t e SO . water are now added , and solution boiled to expel , The le ucO-methylene blue is oxidized by addin g 1 6 grams of neutral sodium chromate dissolved in a little water, and the resulting dye is precipitated by adding salt . The base is to filtered , dissolved in a little boiling water which a little 74 LA BORATORY GUIDE OF INDUSTRIAL CHEMISTRY

hydrochloric acid has been added , and the hydrochlorid

precipitated by common salt , filtered and dried on a porous

plate . D - r e rtie s . P op ark green or red brown bronzy powder,

. D easily soluble in water, forming a blue solution yes tannin

D e mord anted cotton blue . y a skein Of cotton as under test

NO . 1 1 0 .

Re action

NC H NH o ” " O CH NC H NH ( 1 ) (CH3) 2 6 4 2 s z s l ( 3) 2 3 3 2

~ H H O . S SO3 Z H H - H H H 2 CH3) 2NC3 3 N 28 SO 3 CG N(C 3) 2 0 2 ( ) ( ‘5

H 2 H . CH ) 2NC0 3 ,O ( 3 \ S SO , H H NC6 ,N(C 3) / 2 CH NC H Hcl O (3) ( 3I2 0 3 \ s -SO , N

H H C H N CH 1 " " H C ) 2NC6 3 O a ( 3) 2C l ,SO,. ( S < > S

1 n d lin 1 I u . 6 . (Spirit soluble)

2 50 grams of an ilin

60 of grams anilin hydrochlorid .

2 of on The anilin is mixed with 4 grams c e . hydrochloric

of acid in a round bottom flask , and a solution grams

of T h e sodium nitrite in a little water added . mixture is ° 0 — 0 allowed to stand over night , and is then warmed to 4 5 in order to complete th e conversion of th e diazoamidO-ben

- zol into amido azobenzol .

S of now ixty grams anilin hydrochlorid are added , and Oil- the mixture heated in an bath , the temperature being gradually raised to 1 7 5 and kept at th is point for four COMMERCIAL ORGANIC COMPOUNDS 75

hours . The melt is poure d into water and acidified with hl e hydroc oric acid . The indulin is filt red from th e solu ° of 0 tion anilin hydrochlorid , dried at 7 and ground .

r B h - P o e rtie s . p luis black powder, insoluble in water,

- soluble in alcohol with blue violet color . Dyes blue wh en dissolved in aceton (prepared from acetic acid and glycerin) , etc . , and printed on cotton . This indulin is a mixture Of the following bases

C,H,HN

1H H / C C, ,N NHC,H,

C,H,HN

CIHC,11,N

CoHs

1 2 lin Indu . 6 . (Water soluble)

50 grams indulin (spirit soluble)

00 cone . 3 grams sulfuric acid .

Fifty grams of indulin are dissolved in 3 00 grams 76 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY furie acid and the mixture heated on the water -bath till a sample is soluble in dilute alkali .

The mixture is poured into water , the sulfonated dye

filtered , washed , transferred to a porcelain evaporating dish an d neutralized with caustic soda solution . The solu tion of the sodium salt is now evaporated to dryness and powdered .

B - Pro e rtie s . p ronzy or blue black powder, soluble in

- water with bluish violet color . Dyes wool and silk blue from

- an acid bath . This substance is a mixture of the sodium salts of the

- various spirit soluble indulins . Dye a skein of worsted and — 6 . silk as in test N0 . 3 73 Primu lin 1 . C 63 . hief constituent

s s / c \ C H C \< / , , N 40 grams p-toluidin

S SO,Na 28 grams sulfur H H C C . C , ,< > N NH, The substances are well mixed together and heated in a - h casserole in an oil bat . The temperature is slowly raised to l e su fureted hydrogen is evolved , and the mass b comes yellow . The reaction is finished when no more gas is given off .

The cold mass is powdered finely , added to four times its

0 weight of fuming sulfuric acid (3 per cent SO,) and warmed ° 0 —80 to 7 for a few minutes , till a sample dissolves in dilute alkali . The sulfonation mixture is then poured into ten times its

- th e rimu lin volume Of ice water , and the sulfonic acid of p base wh ich is precipitated is filte re d and washed till free

78 LABORA TORY GUIDE OF INDUSTRIAL CH EMISTRY

crop of crystals separate . The preparation only succeeds in as i cool weather, in summer a resinous mass s usually ob taine d . The crystalline body which separates is known as ° h terpinol and has a melting point at 3 5 C. The body t us obtained is terpin h ydrate which by boiling with dilute h s as hydroc loric acid gives a colorle s oil known terpinol , having an Oder resembling hyacinths . Ni 1 66. obe Oil .

0 of 5 grams benzoic acid .

The benzoic acid is dissolved in an excess of meth yl alcohol h and saturated with dry hydroc loric acid gas . After satura tion the solution is heated for about four hours in a water l h a . T e bath , and then poured into an equ volume of water e is oil which s parates purified by rectification .

e r s il h Prop tie . This O w ich in methyl benzoate h as a v l spe cific gra ity of and b . p . Synthetic Oi of birch .

1 6 . Be nzalde h de 7 y .

50 grams of benzyl chlorid 40 grams of copper nitrate f 500 grams O water .

of e and The mixture benzyl chlorid , copp r nitrate water are heated to boiling in a round bottom flask with upright

for — A condenser on the sand bath a day (8 9 hours) . slow current of carbon dioxid is at th e same time passed through the liquid to prevent oxidation of the benzaldeh yde by o th abs rption of oxygen from e air. During the process

is nitrous fumes are slowly evolved . When the reaction

th e complete , the contents of flask are extracted with ether, and th e l ff th yellow oil remaining , after distil ing O e ether , is well shaken with a saturated solution of sodium bisulfite nd o for Th l a allowed t stand some time . e colorless crysta COMMERCIAL ORGAN IC COMPOUNDS 79

line mas s which separates out is filtered, washed with a little alcohol and ether, and then drained in a porcelain filter . The aldehyde is regained by adding dilute sulfuric acid in h excess and distilling wit steam . The distillate is extracted h h h wit et er, de ydrated over calcium chlorid , decanted and l the ether disti led Off .

Pro e rtie s . C p olorless liquid , known as artificial Oil of °

1 . . almond ; b . p . 79 C ; Sp gr . at

Re action

2 C H CH Cl Cu N 2 C H COH Cu Cl 2 HNO , 5 , ( , , , 8

8 Cinn a ic Ald h d 1 6 . e e . C H CH m y ( , 5 ( This compoun d is the ch ief in gredient of oil of cassia and It ll cinnamon . is prepared artifici a y in large quantities by th e action of caustic soda on a mixture of benzaldehyde and h to . acetalde yde , according the equation

C H COH CH COH C H CH : H H H , , , , , C CO ,O

il l ° ro e rt e s . P p i Colorless O boi ing at 247 C. Ani l 1 69 . so .

5 grams sodium 1 00 grames meth yl acloh ol 20 grams phenol i 40 grams methyl iod d . The meth yl alcoh ol is poured into a round bottom flask connected with an upright condenser . The sodium cut into h h h . W t e small pieces is t en added en sodium has dissolved , th e phenol and meth yl iodid are added . The mixture is h eated on th e water-bath until th e solution h as no longer an

— A a alkalin reaction (2 4 hours) . s much s possible Of the meth yl alcoh ol is distilled Off on the water-bath and water

- A i added to th e amber colored residue . colorless O l separates 80 LABORA TORY GUIDE OF IND USTRIAL CHEMISTRY

w i i . h t out , hich s extrac te d w th ether The et ereal solu ion al is dehydrated over c cium chlorid and distilled , first on the - h as off water bath , until the ether been driven , and then over

A 1 0 the flame . lmost the whole of the residue distils at 5

Re action

1 H H H N H O 2 CH O11 C O a C N . ( ) , ,O C , , , , H H 2 H ONa CH O G OC Na". ( ) C, , , , , ,

r r i P ope tie s . Colorless liquid possess ng an agreeable odor resembling of anise .

REFERENCES

’ d r F m h r i . h i l h Rich e r r n ic Ch e mist . E a . S t P lade ia 1 0 t s O ga y g p , 9 5 . h n r r A Be rnt se . London 1 0 n i mi . 6 a c h e s . . O g C t y , 9

Coh e n . e w ork 1 r i h e mis r . . B . N Y 0 O an c C t . g y J , 9 7 h r r m r . . o n . w ork P tica l anic Ch e ist B . C e Ne Y 0 ac O 1 . g y J , 9 7 m n i D nd h e ir In e r dia r d . Sy th e t c ye stuffs a t t e te p o ucts J . C. Cain T T h 1 0 d . or . London . an . e J p , 9 5 T h h i r n i l il rr d m of Esse t a s . Erne s Lon on e C e st O t . Pe . y J y , 1 8 99 .

- r h l z nd r ni lorin Ma e . G . S u t a P li . London 1 0 a c o tt . u us O g C g J , 9 4 . h f r ni h mi r d rm l d o a c e s . w Practica Me t o s O g C t y Lu ig Gatte ann .

n 06. Londo , 1 9 CHAPT ER V

PIGMENTS AND LAKES

1 o Pi me n ts — P 7 . g . igments are mineral or organic bodies,

us s or ually in oluble in water, oils, other neutral solvents, and

e to a are us d to impart color a b se , by admixture with its

substance . The color of a pigment depends upon the amount and kind

of light which it reflects . It is necessary that the pigment “ ” to be opaque in order give good covering power, that is ,

it should entirely conceal the surface to which . it is applied . The chief pigments are given in the following table :

Wh ite s Blue s Gre e ns White Lead Ultramarine Ultramarine Lead Sulfate Prussian Blue Brunswick Green Lead Oxychlorid Smalt Ch rome Green ’ White Zinc Cobalt Blue Guigne t s Green Zinc Sulfid Copper Blue Copper Greens Barytes Indigo Arse nic Green Gypsum Chinese Blue Whiting Lithophone

Ye llows Re ds Blacks

Chrome Yellow Re d Lead Lamp Black Yellow Ochre Chrome Re d Ivory-Black Cadmium Yellow Re d Ochre Bone-Black

8 1 8 2 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

Orpiment Venetian Re d Litharge Vermilion Gamboge Re alge r Indian Yellow Antimony R e d Carmine

Orange Orange Mineral Umbers Chrome Orange Vandyke Brown Antimony Orange Sepia

M . any other pigments, both natural and artificial are in

as not in use , but they do have a distinctive color, are not cluded in the above classification . For detail description Of these pigments the student is referred to some of the books given in th e list of references . The preparation Of some typical pigments will be taken up in order to give the method employed in handling arti

ficial colors . B 1 1 Pr ussian lue . D f 7 . issolve 1 000 grams of sulfate O iron (fe r rous) in 1 5 liters of water and add 50 grams of d h f hy rochloric acid . To t is solution add a solution o 1 000 grams of fe rrocyanid of potassium and 50 grams of h ydro

f w th e chloric acid in 3 0 liters o water . No slowly add to

00 mixture 4 grams of bleaching powder, when the white precipitate will be changed to a blue one . To hasten the

to h . oxidation , it is well boil wit open steam for a short time

This pigment being finally divided is slow to settle at first , so s hould be allowed to stand for several day s . When the prussian blue has settled somewh at the top liquid is syphoned Off , and the tank again filled with water . This process of washing is continued until the test of the wash water shows PIGMEN TS AND LAKES

only slight traces of sulfates . The pigment is next passe d s into the filter press, wa hed again , removed , dried , and

ground to a fine powder in the ball mill .

id — P 1 000 2 Re d Ox . 1 7 . lace about grams of ferrous sulfate in an iron crucible and heat until nearly all of the ar ff fumes of sulfuric anhydrid e given o . Then add 1 00

u is grams of slaked lime and heat until niform color Obtained . — P 00 1 Ve rmilion . ut 1 1 7 3 . 3 grams of mercury and 4 grams of sulfur into a mortar and triturate until the ingre D die nts are thoroughly incorporated . issolve 76 grams

- tin h 1 va ora 600 . . caustic potas in a 4 inch p g dish, using c c ° of H of water, and add the contents the mortar . eat to 45

se C . , and keep at this temperature for veral hours stirring h a very thoroug ly at frequent interv ls, and keeping the h volume of water constant for the first two ours . The tem ° a pe rature must be regulated not to exceed 45 C. nor less th n ° 40 C. In the course of 2 or 3 hours the mass becomes brown and

h th e then gradually turns a brig t red . When desired ver h a 6 8 milion color is acquired , whic is usu lly after or hours ,

n wash by decanting until free from alkali . Filter by mea s

ss on s of the pre , dry gra s plates at not over 4

1 An n e rmili n timo V o . 1 0 f h 74 . y 4 grams o sodium t io f 2 0 . . o sulfate are dissolved in 5 c c water, making a solution f ° i h o w Mx 1 . . . 0 T . 00 0 4 c c of antimony c lorid with 4 c c . of

P s water . lace the thiosulfate in a ca serole and add the H i antimony solution . eat slowly , and when the red color s developed , filter . 1 ch r n . l D 1 7 5 S e e e G e e . issolve 50 grams of arsenious

x 1 f . o 200 o id in 000 c c . water containing grams of sodium 1 0 f carbonate . Next dissolve 5 grams o copper sulfate in

2000 . . . W c c of water hen both solutions are ready, mix

al e . together, low to s ttle , wash and filter 84 LABORA TORY GUIDE OF INDUSTRIAL CH EMISTRY

Ch r om Ye llo D 1 e w . 2 7 6. issolve 000 grams of lead 8 an d h acetate in liters of water filter if necessary . T en dis solve 1 5 50 grams of sodium dichromate in 8 liters of water

. W e n and mix the two solutions ash by d ca tation, filter and Of is not dry. If all the color precipitated add a little more

lead acetate . m R d — 1 Ch r o e e . W o t 00 7 7 . eigh u 5 grams of lead acetate

' and 1 75 grams of sodiumdich romate ; dissolve each separately

1 0 in liters of water, then mix the two solutions . Allow the

e ff pr cipitate of chrome yellow to settle out, pour O the super n nata t liquor, add a solution of 75 grams of caustic soda in

00 . lf 5 c . c of water, and boil for about ha an hour, or until the h as yellow assumed a red color, then filter, wash and dry .

1 8 Ch rome Oran e . 00 7 . g Dissolve 5 grams of lead acetate

1 0 Of h 1 2 of in liters water, next weig out 5 grams sodium dichromate and 1 25 grams of sulfate of soda and dissolve in

Mx wo 1 0 . i t liters of water the solutions together, allow P off the precipitate to settle . our the clear liquor, then add

f 0 i 1 O n 000 . . a solution 5 grams of caustic soda c c of water,

20 boil the mixture for about minutes, filter, wash and dry . — 1 Satin Wh ite . W 800 7 9 . eigh out grams of lime and after mixing with water make into a thin cream with more

ou 1 00 water . Weigh t 7 grams of aluminium sulfate and dis ix of . M to solve in 5 liters water the two and heat a boil ,

then allow to settle . Decant the clear liquor, wash , and

allow to settle . Filter and dry . 1 h r m r n — m 80 C o e G e e . . Formed by heating chromiu hydroxid .

1 k r n — F 8 1 Brunswic G e e . Of B . our shades runswick Green may be made by using th e proportions given under the l l . su fo lowing separate heads In each case , however , the fate of iron and lead are dissolved in separate vessels and l added to the suspended barytes, while the yel ow prussiate

86 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTR Y

C : olors for the manufacture of lithographic inks, paint colors, colors for kalsomine or wall finishes, colors for wall paper and coated paper surfaces . 8 Lith o ra h ic an d Printin Ink 1 s . 7 . g p g The lakes for

rn h these are ground in va is . They must be fast to water and for high grade inks must possess covering power, fast

In ness to light and varnishing . some cases these inks are required to be transparent .

Pain l — In 1 88 t Co o s . of . r the manufacture paints th e

o pigments are ground with oil r varnish . For th is pur

th e pose lakes must be insoluble in the medium, especially

oil for use in Sign and ornamental painting, as solubility in a h will cause the colors to run into e ch ot er .

Kalsomin e r W all Finish e s — 1 o . 89 . For this purpose th e colors must be in powder form . They are mixed with water of h and then with milk lime or ot er suitable material . On of this account , colors must resist the action lime and should mix easily with water. 1 W all Pa e and Coa e d S face Pa l 0 . ur e o ors 9 p r t p r C .

th e dr These lakes are usually in pulp form , but y powder

n may be used if very finely ground . The colors are ordi arily

n al h n applied by the use of a Sizi g materi , suc as glue , casei ,

For e th e etc . this purpos lakes must be absolutely insoluble in water . im n L — 1 1 Cr so ake . of 9 . This is one the most important lakes and its preparation takes place in three stages : first th e

Of th e preparation cochineal liquor ; second , the preparation

of of hydroxid aluminium ; and third , the combination Of these two .

h . Weigh out 200 grams of coc ineal and mix with 2000 c c .

for n 0 of Of water, and boil five mi utes ; add 3 grams cream f h of o tartar and boil again ; t en add 4 grams alum , boil,

0 a strain , and add to the decoction 5 grams more Of cre m PIGMEN TS AN D LAKES 3 7

i . of tartar . The cochineal liquor s ready To prepare the a 20 al lumina, weight out 4 grams of um (or its equivalent of

a 000 . . sulfate of luminium) , dissolve in 3 c c of hot water, also

2 f h 0 000 . . o ot 1 4 grams of ammonium carbonate in c c water .

Add th e to th e r alum solution carbonate solution , sti ring

h h ot . a re ci i well , t en wash well with water This lumina p p tate is next mixed with coch ineal liquor and the whole boiled

h h s e Off toget er ; w en the crim on lake is formed it is filter d , h was ed and dried . m B i l d r — 1 2 So e as c Co ors use fo Lak e s . f 9 . The use o basic colors in producing lakes depend upon their affinity

and for acid radicles, is best illustrated by example .

1 iole t Lak e — 1 V . 00 93 . Weigh out grams barytes and h h . mix wit 500 c . c of boiling water ; add to t is mixture 2 grams l Wh th e of methyl violet and stir wel . en dye has dissolved ,

2 of add grams of tartar emetic , then a solution 3 grams of

h o w . n n tannic acid in 1 00 c . c . of t ater O allowi g to settle if th e top liquor is high ly colored it is an indication that suffi If cient tannic acid has not been added . necessary , add

n sh . more ta nic acid , wa , filter , and dry

T h e n followi g lakes may be made in a similar manner, h h using t e met od given above .

1 Bl Lake 1 ue . 00 a 94 . grams b rytes , 3 grams tartar h l 6 emetic , 3 grams met y ene blue , grams tannic acid . m n Lake R 1 C i so . 1 00 9 5 . r , grams barytes , 3 grams 6 tartar emetic , 3 grams safranin , grams tannic acid . B n L 1 6 ow ak e . 1 0 0 9 . r grams of barytes , 3 grams tar B tar emetic , 3 grams ismarck brown , and 4 5 grams of tannic acid .

1 L ke 1 a f Scarle t a . 00 O . t 97 gr ms barytes , 3 grams tar ar

1 2 a 4 emetic , gram of safranin , grams aur min , and 4 } grams tannic acid . k — 1 8 Some Acid Colors use d for La e s . 9 . The following 88 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

is a list of acid colors adapted for the manufacture of lakes are r e which p ecipitat d with barium chlorid . The example

given will se rve for the entire list .

Mix 1 1 0 5 parts of sulfate of aluminium in 5 parts of water,

with a solution of 1 0 parts of acid green L . in 1 00 parts of

2 water . Then precipitate with 3 parts of barium chlroid in n a 6 - 640 parts of water . O dding 5 parts of soda as h in 65

parts of water , the alumina is precipitated in the lake, h t us producing a complete se paration .

1 Re ds — A Azo 99 . . cid magenta ; cochineal; Azo crimson i B Azo e soin Azo h e lox n 2 G . S. ; ; p ; ordeaux extra ; Brillian t

B . P B A. T . R . . as 2 L . R crocein 3 ; F t red , ; onceau 5 . L . — n II . B 2 L . 00 Ora e . . G . . O M g range ; andarine G . Y llo — 20 1 e w . s s . Fa t yellow extra ; Fa t light yellow ;

Naphthol yellow S. — 2 2 r n A L . B 0 G e e s . . cid green ; rilliant acid green 6 B . ; B X X Ne w . . G . acid green 3 , 2 0 Bl e — A u s Al P. H 3 . . izarin blue S S E. ; Cotton blue ; a B Fast blue greenish ; G llocyanin ; Indulin . 20 iol — A B . V e ts . 1 R B 4 cid violet 4 , extra, . ext . 8 . ; l Alkali violet ; fast acid vio et . Br — 20 own . . 5 . Fast brown 2 ra — B 06. G A 8 . ys . cid black 2 Th e Alizar in olors 0 . C 7 are very fast to light and water, and are extensively employed in paints as well as litho An graphic inks, etc . example will serve for the class

I

Mix 2 0 43 c .c . of a 1 per cent solution of aluminium sulfate

- 1 2 . . 1 0 s 5 c c of a per cent olution of soda ash .

Wash out three times . To this add

0 of 1 0 3 c . c . a per cent solution of calcium chlorid 0 1 0 7 c . c . of a per cent solution of sodium phosphate .

CHAPT ER VI

DRIER VARNISHES PAINTS AND TA N S, , S I S

2 1 Drie r — Wh f 0 . s . as o en some substances , such acetate f o . lead , acetate manganese , red lead , manganese borate , etc ,

n h dr d are added to pai ts and varnis es, these become y or har

h L x h much quicker than ot erwise . inseed oil mi ed or eated h F h with such bodies drie s muc quicker . rom t is fact h as

th e l th e a a and arisen p an of adding , in manuf cture of p ints “ ” as h for th e of varnishes , driers , t ey are called , purpose facilitating th e drying or hardening . ” A very small quantity of drier will cause the drying Of a large quantity of Oil ; from to 1 per cent of th e weigh t of the oil is usually sufficient . Manganese compounds are more energetic drying agents h than lead compounds . Driers w ich dissolve easily in th e

and are Oil, such as linoleates resinates , more active than

e or n a do not thos which , like red lead ma g nese , dissolve in the Oil . When raw linseed Oil is mixed with lead oxid or manganese

of h th e borate very little t ese is taken up, and rapidity Of

h But h drying is not muc increased . if the Oil be eated with them th ey are more freely dissolved and the treated Oil dries h muc more rapidly .

S of th e h for ome substances w ich are used driers, are , of n h h acetate lead , red lead , ora ge lead , w ite lead , c rome h yellow , lit arge , manganese dioxid , manganese sulfate , manganese acetate , ferrous sulfate and ferric oxid .

Of l a e late years , however, the lino e tes , r sinates and 90 ’ i h m Roge rs Industr a l C e istr y .

D R Y O L R AND PAIN F T R C O T AC O Y.

92 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

1 75 grams of raw linseed oil 75 grams of flake litharge 3 5 grams Of kauri gum 20 grams of granulated manganese

1 000 grams of turpentine .

Oil Cook the , litharge , gum, and manganese together until a drop when cold is brittle . Then after cooling the mass to °

2 0 00 F. . between 5 and 3 , add the turpentine slowly Drie r N 1 1 . D a ad 2 20 o . s . , issolve much le resinate in f turpentine as possible and use only in the cold . O this drier 5 per cent of the amount of Oil which is contained in the paint , is used . 22 1 Paint and Varni R m N sh e o e r o 1 . . v , .

Mi . f x 200 c c . O an ilin with

200 c . c . of benzol

- 1 0 . . c . c of nitro benzol

P n d R m r N II 222 aint a Varnish e ove o. . . ,

of 1 00 c . c . amyl acetate

1 00 c . c . of anilin

of . 200 c . c . benzol

R m r N II 22 P and Varnish e ove o I . 3 . aint , .

1 00 . c c . of wood alcohol f . o . 1 00 c c . benzol

2 m — 2 Rust Re ov r P f i . 4 . e . owdered emery and para f n oil

2 2 . P ote ctive Varni h for Ir n 1 00 5 r s o . Dissolve grams

ffi 1 of para n wax in liter of benzin . 2 26 Fre n ch — di . olish s P . This polish is prepared by solvmg 24 grams of gum com" 1 6 grams of gum arabic 45 grams of gu m shellac in f 1 lite r o alcohol . V N P AN D DRIERS, AR ISHES, AINTS STAINS 93

ni h e s — a th e 2 2 S irit Var s . 7 . p These varnishes are m de in cold and are useful when a quick drying varnish is desired . h 0 0 2 28 Sh e lla c Varnis . . Dissolve 4 grams of shellac in 1 liter of alcohol . h n h 2 2 Fre n c Var is . 9 .

500 grams of white shellac dissolved in d . a an 1 000 c c . of lcohol to this when filtered add

1 50 grams Venice turpentine . — H iri . 2 0 Brown ard S t Varnish . D 1 00 3 . p issolve grams

a 200 2 um of sandar c , grams of orange shellac , 5 grams g

and 0 V r 1 of h . elemi , 5 grams of enice tu pentine in liter alco ol M sh 00 2 1 astic Varni . s 3 . Dis olve 5 grams of gum mastic in 1 liter of turpentine . 2 2 Dammar Varnish 00 3 . . Dissolve 4 grams gum dam

mar in 1 liter of warm turpentine .

oll di n ni 2 2 C o o Var sh . 33 . Dissolve 5 grams of gum cotton in a mixture of 7 20 grams of amyl alcohol and 360 Of grams amyl acetate . il ni h e i 2 O Var s s . l 3 4 . O varnishes are divided commer cially into two groups coach varnishes and cabinet var A l ff nishes . lthough there is very ittle di erence between al them, either in the method of making or in the materi s

used . The process in outline consists of the following stages “ ” i st . as s I melting (or running, it known in the trade) , the “ ”

d . resin or gum ; 2d . boiling the oil ; 3 mixing the melted

li i n th . gum and boi ng o l; 4th . boiling the var ish ; 5 thinning

th . the boiled product ; 6 . clearing R u . f I . nning The running O the gum is carried out in

th e copper kettles heated by direct flame . This part of process must have the utmost care as over-heating will give a poor grade of varnish and under-heating will not 94 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

T o give a uniform product . make a good varnish it re quires experience to kn ow just wh en to stop h eating — “ l oilin . II . Oi B Wh i g ile the gum is being run , the o l

. h th e T h to be used is boiled T is is done in boiling pot. e ° o for 1 t 00 F . to 2 Oil is heated about 5 , hours, when it is

x n ready for mi i g with the gum . — I ixin . m II . M g When the gu h as be en properly melted the necessary quantity of boiling oil is poured into the melted

h h a all th e gum , w ic is stirred energetic lly time .

W th e um and Oil IV . hen g are first mixed a rathe r cloudy

in to h a mass is produced and order make t is tr nsparent , and to th e a h to make v rnis string, it is necessary boil again . The point at wh ich to stop boiling depends upon th e varn ish ; but as a rule wh en a drop taken between th e thumb and finger

strin s wh e n se ar ate d is forms g , the fingers are p , an indication h of t e end point . h —A T innin . V. g fter the boiling operation described

ot its above is completed , the p and contents are removed from the fire and placed at some distance from any flame . h Here it is mixed wit turpentine to a working consistency . Although it is necessary to mix the turpentine with th e var

a h e t ad nish m ss at as igh a temperature as possible , y it is visable to allow th e h ot varnish mass to cool down somewh at ° before adding the turps (350 F) ; this sh ould also be added

h x in small quantities at a time , t is means the mi ing will be

l d h too of prope r y one wit out great a loss turps .

r n — h I le a in and A i . a V . C g g g Fres ly made v rnish is most

to all th e e unsatisfactory use , and best qualities are subj cted to an aging and clearing process before they are sen t out .

th e Thus in standing , more insoluble particles separate out

c me and th e top laye r b e o s clear . T h e following list will serve to demonstrate the manufac ture of oil varnishes in general :

96 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTR Y

By following the general directions given under the head th e of oil varnish, student may be able to produce some very good results with the subsequent list of formulas :

2 0 Extra Fine Co al Varnish . 4 . p

1 50 grams of African copal 300 grams of fin e ligh t coach oil (h ot) 80 thin with 4 grams of turpentine .

2 1 Elas c arnish 4 . ti V .

50 grams African copal 50 grams animi gum 3 00 grams medium coach oil (hot)

thin with 480 grams tu rpentine .

2 2 Tool arni 4 . V sh .

1 50 grams gum kauri

1 50 grams rosin W . G . 1 20 grams strong coach Oil (hot) thin with 288 grams turpentine

240 grams benzin .

R Mixe d Paint 2 . e ad 43 y . There is hardly industry which has made more rapid progress in the past fifteen years h “ ” t an the manufacture of ready to use paints . Near ly every user of paint goes through the stage of desiring to

become his own paint manufacturer, and there are , even at

present , many who fondly imagine that they can prepare

of - mixed paints by means a wooden paddle and a wash tub, capable of ran king as protective and decorative agents with the material compoun ded by the aid of powerful and special

machinery . There h as be en much dissatisfaction in regard to ready x mi ed paints, and justly as numerous brands have been

placed upon the market , which were not much better than V P AN D DRIERS, ARNISHES, AINTS STAINS 9 7

. C chalk and water onscientious manufacturers , however , to have done much bring these frauds to light , and we may h look to a time in the not far distant future , w en all brands of l paint wi l be properly labeled , and the public educated to the requirement of a ready to use paint .

— Son M M in as . Ross Co . FI 0 in e . 1 . i ac G. x g h Ch ,

B n . ook N . r ly , Y

2 Mixin — . In 44 g . the manufacture of ready mixed paint the necessary amount of raw linseed Oil is placed in the

- mixing machine . The body containing coloring matter is

introduced in small portion at a time , new lots being added th only as e paste becomes limpid . The mixture is then run th rough the mill until perfectly 98 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

smooth when rubbed out on glass . It is then thinned as desired . The method Of procedure t aries to quite an extent in diff erent plants al th ough all are based on th e same

general principle . F ro m t h e foll ow i n g fo r m u l a s th e ge n e r a l

method may be Obtained , and various shades pro

duce d .

Wh i e —P 2 . 45 . t our into the can of th e mixer 1 1 60 grams of raw linseed Oil

n . n N . Ross So Co , B rookly , . Y i mot on . Now add slowly a mixture of

2 500 grams Of dry white lead

2 00 of x 5 grams zinc o id .

Mix h t oroughly , or until a smooth paste is Obtained which l th h wi l run easily from e can . Th is paste is passed t rough th e th e so to mill , stones being adjusted as Obtain a product

h A s free from lumps w en rubbed out on glass . fter pa sing h h h h t roug the mill it is t en broug t into the mixer again , and thinned by adding,

1 500 grams of raw linseed oil 1 000 grams Of boiled linseed Oil 3 50 grams of Japan drier

1 50 grams of turpentine . Wh en thoroughly mixed it is run into cans and is ready for use

A quantity of the above thinning mixture should be made

1 00 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

2 8 Ye llow 4 . . 2000 grams white lead 2000 grams zinc oxid 1 00 grams ch rome yellow 1 1 60 grams raw linse ed oil

h 2 t in with 600 grams standard Oil .

2000 grams white lead 2000 grams zinc oxid grams golden ochre 1 00 grams orange yellow 1 400 grams raw linseed oil

2 thin with 8 50 grams standard oil . 2 0 Fl 5 . e sh . 2000 grams white lead 2000 grams zinc oxid 500 grams golden och re 290 grams French ochre 30 gr ams princess metallic I O grams lamp -black 1 1 60 grams raw linseed Oil

2 il thin with 580 grams standard o .

2 1 A le Gre e n 5 . pp . white lead zinc oxid lemon chrome yellow chrome green raw linseed oil h t in with standard oil .

2 2 Li h t Blue 5 . g .

2 2 50 grams white lead 2 2 50 grams zinc oxid 500 grams Chinese blue 1 1 60 grams raw linseed oil h t in with 3 000 grams standard oil . D I RS VARNISHES P IN S AND ST INS R E , , A T A 1 0 1

k B Dar lue . 2 5 3 .

2000 grams white lead 2000 grams zinc oxid 1 000 grams Prussian blue 1 1 60 grams raw linseed oil

000 3 grams standard oil .

2450 grams white lead 2450 grams zinc oxid 2 5 grams lamp black 1 1 60 grams raw linse ed oil

000 a thin with 3 grams st ndard oil .

2 Azure 5 5 .

2500 grams white lead 2 500 grams zinc oxid 1 0 grams Chinese blue 30 grams lemon chrome yellow il thin with 2600 standard o .

2 5 6‘ Slate . white lead zin c oxid lamp -black raw linseed Oil

thin with standard oil .

2 Dark 5 7 . wh ite lead zinc oxid golden ochre Ch inese blue graphite raw linseed oil

n thin with sta dard oil . 1 0 2 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

2 8 . Sa e Gre n 5 g e .

2000 grams white lead 2000 grams zinc oxid 1 300 grams French ochre 580 grams ch rome green 1 80 grams lamp -black 3 0 grams Venetian red 1 20 0 grams raw linseed oil

00 thin with 28 grams standard Oil .

2 Dark Oli e Gre n 5 9 . v e .

3 500 grams golden ochre 600 grams Fren ch och re 980 grams drop black 1 20 grams ch rome green 20 grams lemon chrome yellow 1 3 50 grams raw linseed Oil

0 thin with 345 grams standard Oil .

B k 2 60 run swic G e e . . r n

4000 grams extra deep Brunsw ick green 1 60 grams lemon ch rome yellow 1 1 60 grams linseed oil

h 2 0 a t in with 8 5 grams st ndard Oil .

1 In di n R d 2 6 . a e .

6620 grams Venetian red 1 230 grams princess metallic 2400 grams raw linseed Oil t 0 hin with 543 grams standard oil .

By changing th e proportion of pigment any range of sh ade T h n . e e and tint may be obtai ed above are m rely given , h therefore , to illustrate the met ods of proce dure .

1 04 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY I V N S P N S AND S INS 1 DR ERS, AR ISHE , AI T TA 0 5

. not n portions The finished product should stick to the ha ds , but if such is the case a small amount of th e mixture in excess i of the above may be added . The putty s then allowed to stand several days to sweat when it is again kn eaded with ll of the addition of a sma amount whiting if necessary . Oil in s and W od Fille rs 2 Sta o . 63 . The following list of formulas will serve to illustrate the large class of substances

n o . put o the market as w od fillers and oil stains . They con sist of a base to which various pigments may be added to

ff x produce the desired e ect . The mi ing and grinding is con

x ducted as given under ready mi ed paint .

Fille r Ba 2 6 Stain and se . 1 200 4 . grams of starch is placed in the mixer and worked into a thin paste with 8 1 0

f W 2 grams o water . hen thoroughly triturated 700 grams

oil 1 0 860 boiled linseed , 3 5 grams turpentine and 3 grams of

e Japan added , the whole being run until p rfectly smooth .

h d use T is should be made in large amounts, rea y for , and

S B se d as for labeled , tain a , which is then use a body the

various stains .

2 Li h Oak r A — 6 . t o sh Stain P 5 g . lace in the mixing ma

20 of 60 T o chine 7 grams boiled Oil ; 3 grams turpentine .

x 2 0 80 this Slowly add a mi ture of 4 grams raw sienna, grams h hl i 00 . W n burnt umber , and 4 grams Silica en thoroug y cor or ate d p transfer to mill , grinding until perfectly smooth R when rubbed out on glass . eturn to mixer and thin with f 7 200 grams o stain base .

Work well and can while still in suspension . The following list of oil stains may be prepared by follow ing the general direction given for light oak or ash

2 k n D Oak Stai . 66. ar

3 20 grams silica 3 20 grams burnt Italian sienna 1 60 grams burnt umber 1 06 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

7 20 grams boiled linseed oil 360 grams turpentine

7 200 grams stain base .

in 26 h ta . 7 . C e stnut S

640 grams silica 1 60 grams burnt Italian sienna 80 grams boiled Turkey umber 7 20 grams boiled linseed oil 360 grams turpentine

7 200 grams stain base .

2 Y l r Ma l tain 68 e low Pine o e S . . p

1 60 grams raw Italian sienna 1 20 grams ch rome ye llow 580 grams silica 7 20 grams boiled linseed Oil 360 grams turpentine

7 200 grams stain base .

2 W aln t tain 69 . u S .

9 20 grams burnt Turkey umber 1 20 grams burnt Italian sienna 7 20 grams boiled linseed Oil 3 60 grams turpentine

9000 grams stain base .

2 0 Mah o an Stain 7 . g y .

1 000 grams burnt Italian sienna 1 60 grams burnt Turkey umber 7 20 grams boiled linseed oil 3 60 grams turpentine

9000 grams stain base .

Oil stains are often made from coal-tar colors soluble in

CHAPT ER VII

SOAP AND ALLIED PRODUCTS

2 1 Soa — In of h h 7 . p. the manufacture soap t ere are t ree

- . : general processes employed , viz boiled soaps, half boiled to soaps, and cold made soaps ; but owing the method em ployed they will be taken in the reverse order . In the installation for a miniature soap works it is ne ce s sary to provide a lye tank , kettle , crutcher, frames, Slabber, h h cutting mac ine , c ipper, mill , plod

der press and dies, all Of which may be secured from manufacturers of

th e fol soap machinery . Some of lowing formulas can also be worked out on a small scale by using a good

s sized iron kettle , a mall garden rake with a wooden box to serve as

a frame , and the cake cut by means f h k of a piece o piano wire or t in nife . “ c “ T h e proportlon s g ven hereafter asual?“ £1231 t i for r h avm i B r kl n N are a c utcher g a capac ty oo . y , Y. one ma of hundred pounds , but y be varied to suit the requirements . 2 2 ld m a — Co ade . T h 7 . So p e term cold made soap is applied to those soaps in which the fat and Oil are on ly ffi l ° to sa not 1 20 . heated su ciently me t them , y , over F and h h h the cold lye t en introduced . T is process gives a ard

' soap but is quite apt to contain eith er un sapon ifie d fats or f e e a r lkali . ’ o e rs Industria l Ch e mis t R g ry .

MINIAT R W R K U E SO AP O S.

1 1 0 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

D i f ru r A In e t fo r e IG . 1 . e ta o t t a S F c e . s te a ac e t su r 7 l C h , l m ; B , m j k

rou n in e tt e O u t e t fo r e sc a in ste a a n d con e n sa tion D d g k l ; C , l p g m d ; ,

S i to ac e t E S a ce fo r co n te n ts F or for a ita tion G ase l p j k ; , p ; , W m g ; , C or wor Fri i n t G t for u in r e ct o c u c M a e c a . f m ; H , l h ; , d mp g h g SOA P AN D ALLIED PRODUCTS 1 1 1

S a bbin M in e c in n Co roo n N Ai e . FIG 1 8 . ac . ou . . . l g h H h k , B kly , Y

FI G . in n 1 . ut M i e o in Ai n n t ac . uc e Co roo N 9 C g h H h k . , B kly , . Y. 1 1 2 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTR Y

ll th e l through the mi , setting granite ro lers a little close r and finally se ttin g the roller R th tigh t . epeat e milling se veral times or un til a uniform r i b b on c o m e s from th e kn ife of about

h h n of t e t ick ess paper .

2 Ploddin — 7 5 . g . F ro m th e mill th e soap is pas sed to th e plodder wh ich is a mach ine provided with a T h e s c re w compressor . — in ac in e in 0 i M . ouc FIG . 2 . Ch pp g h H h nose ° Of the plodder is " N “ B . k 0 . mo . A e C , kly , Y sligh tly warmed and the d A milled soap intro uced . s soon as the soap begins to dis

on th e f K charge put forming plate desired or use . eep th e hopper of the plodder

filled , as this will in a meas ure keep out air bubbles and prevent th e soap from being

streaked . T h e first 1 5 or 20 feet should be returned to th e

as plodder , the bars have not

received the full pressure . As soon as th e soap runs smooth and free from streaks it may be cut into any con

ve n ie nt h lengt and presse d . 2 6 P e ssin — 7 . r g . The dies

being adjusted , and the press

' i FIG T ‘ mue r o . ' o S a M 2 1 ° p ll th e h H i well Oiled , faces are t en ou in Ai e n Co roo n H ch k . , B kly , h n moistened wit a stro g salt N , y ,

1 1 4 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

d 2 8 Lau Soa . 7 . n ry p

of a 3 0 lbs . t llow

of oil 30 lbs . cocoanut ° of - 6 Bé 3 0 lbs . caustic soda lye 3 ° s d m a B6 8 lbs . Of o iu c rbonate solution 3 5

i ir 8 ounces Of o l of m bane .

This soap is cut into cake s and dried and is not milled as h in t e case Of toilet soaps .

2 H lf B ile d Soa s 7 9 . a o p . By this process very fine soap

can to be made , almost equal

B ut th e best boiled soaps .

h th e w h wit them , same as it

cold process, great care must be taken to have perfectly

pure stock .

2 8 0 Palm Oil oa — P S . . p lace in th e crutcher

of 1 8 lbs . palm Oil

of a oil 36 lbs . coco nut of 9 lbs . tallow

and heat to a temperature Of ° ‘ 1 60 F . Add 6 ° Bé 3 lbs . Of 3 5 soda H Soa Pre ss . ou h 2 . c m FIG . 3 p ’° “ um 5 °Wl °r ab°ut i e n Co B r n N l3 and h l y f oo . . A k . , kly , Y 3 minutes ; now cover up to

to s for one and h keep warm , and allow tand hour t ree

A of h h l quarters . t the end t is time the c arge wi l have — ° to 1 0 1 80 F . T h e h h e e warmed up 7 crutc er is t n start d . very a w slowly . At first the so p ill be th ick and h ard to crutch

l e h but wi l soon thin down and b come hotter . If after crutc SOAP AN D ALLIED PRODUCTS 1 1 5 ing for 1 0 minutes the soap for some reason does not thin h ot li down and get , throw on a ttle steam, being careful not ° 1 0 to raise th e tempe rature over 8 F. After the soap has l been well crutched and is free from umps , it should be tested by rubbin g some in the palm of th e hand ; if sapon ificatin g is

e l ffi compl te it will form flakes , whi e if insu cient alkali is l f A present it wil remain like a at . lso test for strength on

f h e h the tip o t tongue . The soap s ould have a very little sharp taste ; if too mild add a small amount Of lye until it can just be tasted , but if at first it burns the tongue add a il little more cocoanut o .

A th e of a al or fter addition lk i fat , crutch well and when it begins to th icken (which is sh own by th e soap dropping free from th e paddle in flakes) run into the frame immediately and allow to cool . For laundry soap the perfume is crutched in just before

n h f r a l mfll o n e d . frami g , w ile toilet so p it is on y added whe Eigh t ounces of citronella Oil or other essential oil will f 1 00 o o . perfume lbs . s ap 28 1 Gre e n Cas ile a . t So p .

2 of fallow 8 lbs .

o 28 lbs . Of olive Oil fo ts (green) f il o n O . 1 4 lbs . cocoa ut

° Mix and to 1 0 F the above warm 5 . , then add a mixture of

° 6 of B6 3 lbs . caustic soda lye 33 ° of h - l e B 4 lbs . caustic potas y 3 5 é .

28 2 Tar oa S . . p

2 n il 5 lbs . Of cocoa ut o l 2 5 lbs . Of O ive Oil foots ° f s d - l 3 0 lbs . o caustic o a ye at 33 B6

of e tar 5 lbs . pin

r 5 lbs . Of glyce in . 1 1 6 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

°

h . W 1 0 W . arm the oils, tar and glycerin toget er hen at 4 F crutch in th e lye and continue crutch ing until all are well combined ; cover up and allow to stand one and one -half to two hours . Then follow general directions .

2 L r a 83 aund y So p .

of 3 1 lbs . tallow l 6 bs . Of cocoanut Oil f 1 o W . . 9 lbs . rosin G ° - B é . 3 2 lbs . Of caustic soda lye at 33

M h oil 1 t e . elt tallow and cocoanut , then introduce 9 lbs ll h ll to Of rosin ; when melted we toget er, a ow cool down to ° l th e on 1 0 F . e e 3 , then add the y , letting soap stand for and

th e a half to two h ours . When soap is finished and just

of before framing add 8 lbs . sodium carbonate solution ° B l ll é of . 3 5 and 8 ounces citronel a Crutch we and frame . When the soap has set suflicie n tly long to properly harden it

for is cut into cakes and is ready use , as soon as dry .

28 Do a So . 4 . g p

of ll 50 lbs . ta ow l 5 bs . of cocoanut Oil ° 2 -l e B 7 5 lbs . caustic soda y at 36 6 l f l 5 bs . o strong tobacco so ution of f 5 lbs . powdered sul ur

5 ounces carbolic acid .

The tobacco solution is made by boilin g tobacco stems in h water ; mix the sulfur and tobacco solution toget er . When th e soap is well formed crutch in the warm sulfur and tobacco ;

th e then add carbolic acid and frame . 28 B il d a o e s . 5 . So p Owing to the recovery of glycerin th is process is employed very largely and in fact th e bulk of i h I l soap s manufactured in t is manner . n order to i lustrate this process we will take as an example the manufacture of

1 1 8 LABORA TOR Y GUIDE OF INDUSTRIAL CH EMISTR Y

2 Fin i h in R ff h s . n O t h 89 . g u and save e lye t at has s out al ettled , as it contains kali strength which can be used . h on t e 1 0 . Turn Open steam and add the lbs of palm Oil , l running in a ittle water to thin the soap . If the soap is weak ° B add lye at 5 é . W is h hen the soap finished it should be smoot and shining, h l boiling wit a ro ling motion , and a sample taken on the

Off trowel should slide in flakes . 2 0 F amin — A 9 . r g . llow the soap to settle a few days until ° R n it h as cooled to about 1 45 F . u sufficient for one frame

th e 6 to 8 -ash t into crutcher, and add per cent of soda solu ion ° B h l for 2 h 6 é . C t e at 3 rutc we l minutes, add perfume and h D crutch until smoot . ump into frame and allow to stand

h n n h several days to arden . O setti g it is t en slabbed and f l cut but not milled as in the case o toi et soap .

2 1 R sin a — h o So . O to t e 9 . p wing fact that plain tallow

not h to h soap does lat er , it is always necessary add somet ing to h ff l produce t is e ect , consequent y rosin is used in laundry

f Wh for th e f h soap or this purpose . ile purpose O c eapening and making a h arder product silicate of soda is sometimes l T h l emp oyed . e following formula therefore wi l serve to ll h i ustrate a soap of this c aracter .

1 l 50 lbs . Of ta low f 7 5 lbs . o rosin f 1 . o 5 lbs sodium silicate .

The meth od of manufacture is th e same in this case as for

x l A h h h e . t e the pr vious e amp e fter finis ing , owever, silicate of soda is added as follows :

Put th e of silicate soda into a small kettle and add water , ° boiling un til it registers 5 Bé (h ot) ; th en add soda-ash until ° Bé h l 8 ° Bé l l it registers 7 , t en salt unti it makes whi e boi ing h ot . SOA P AN D ALLIED PRODUCTS 1 1 9

Now run about 70 lbs . of the soap into the crutcher and

h s t e . C add 30 lbs . of hot silicate of oda solution rutch well ; add th e perfume and continue crutch ing until the soap starts

D th e an d as to form . ump into frame treat directed above . Powde — ki 2 2 a . 9 . So p r There are many nds of soap

ar . are powders on the m ket They all, however, prepared

d -ash m is s an s . from soap oda , someti es borax al o used The following will serve as an illustration l l il Eigh t pounds of fa low and 8 bs . of cocoanut O placed ° ° 1 0 1 60 in the crutcher and heate d to 5 to F 8 lbs . of caustic ° lye 33 B6 is now crutched in and the soap allowed to stand f At th e u and or 2 hours . end of this time crutch ntil thin h C - al add h ot water until quite t in . rutch in one h f pound of sulfate of soda which h as been dissolved in hot water and

- h h 2 . as so t en add 5 lbs of soda , keeping the ap thin by W h the addition of hot water . hen t oroughly mixed run into frames an d let stand over night ; th en cut into bar s and open d . W an pile to dry hen thoroughly dry chip grind , when it is ready for use .

2 Soft Soa n a o is o 93 . p. Tra sp rent soft s ap in g od ” “ th e so so demand under name of glycerin ft ap , crown ” il d soap etc . Its chief constituent is linseed O an the lye

i is most suitable s that from caustic potash . The lye pre pared several days before using in order that it may be come

A . clear . very good soap may be made by melting 4 lbs of

h 2 1 rosin in a crutc er or iron kettle and adding lbs . of linseed

- 2 1 . . oil, and lbs of cotton seed oil The temperature is then ° 2 lbs . raised to 1 60 F . and a mixture of 4 of caustic potash ° ° - 2 2 B 1 2 lb s 2 B d . lye 6 and s . of caustic oda lye 5 é intro uced is The mass then crutched for 5 minutes, allowed to stand for 2 hours and crutch ed again until th e soap is smooth It is l is final y run into the container, and when cool ready for

use . 1 20 LABORA TOR Y GUIDE OF INDUSTRIAL CH EMISTR Y

REFERENCES

l m m w de rn andl nd G ce rin e . L L . Ne Mo Soa s C e a L . bo p , s y . a 06 1 9 .

Am ri n r hm e . k 0 can Soa s He Ga n . Y r t a e w o 1 . p y N , 9 4

r l x r n Th e A of Makin . A e an d t Soa de . n o 1 1 . p g Watt Lo , 90 f ll n o F rm . ld ro d A Co e ctio o ae A . . H G b M s . ul W ouch in . o o , ,

’ Ro e rs Indu stri l Ch m g a e istr y . MINIAT U RE T ANNERY . CHAPT ER VIII

LEATHER MANUFACTURE

The object of tanning is to render the skins of animals

As imputresc ible and pliable . only a small amount of h th e leather is required wit hair on , preliminary treatments are necessary to remove it before entering into the actual

tanning process . In conducting the work along this line it will be found best to follow th e outline as given below 2 k in — A h Soa . s t e nn 94 . g the Skins or hides come to ta er

h l th e t ey are usua ly in dry salted or pickled condition , and

e th e al Of and contain b sides s t a large amount blood dirt . The first step th erefore is to place them in a pit containing

water, where they are allowed to remain until soft . They are then rinsed Off in fresh water to remove as much of the i dirt an d blood as possible . When washing s complete the ll “ ” Skins are placed over a round inclined table ca ed a beam . H - an d ere the excess of flesh , ear laps tail are trimmed Oflbv l “ fl h ” means of a sharp kn ife ca led a e s e r . Machines are h also used to accomplish t is result . — 2 De ilatin . 9 5 . p g The next step in the process consists in removing th e hair and epidermis and is usually accomplish ed

b n h y mea s of milk of lime , although ot er substances are some

times employed . The most common method in use is to

a ffi h as prep re su cient milk of lime to cover the skins , to which been added 5 per cent of sodium sulfid on the weight of the

lime . The skins, after being introduced into this mixture , are turned twice each day in such a manner as to bring the ones on

1 2 1 1 22 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

th e top into the bottom of the pit . This treatment requires from 4 to 8 days depending on the nature of the skin ; the proper time being indicated by the ease with which the hair

th e and epidermis are removed when rubbed over with finger . The chemical action which takes place in this treatment is due to the combination of the calcium h ydroxid with the fat surrounding the hair pellicle and that between the fiber

thus forming a lime soap, which loosens the hair and epi

u dermis, swells p and separates the fiber bundles . The hair Old ll itself is only very slightly altered . limes wi unhair h much more readily than new ones , w ich is often advan tage ous for dressing goods ; although for sole -leathers and r others requiring firmness, new limes are p eferred . When properly limed th e skins are removed from th e pit l and allowed to drain . They are again p aced over the beam where their plump condition makes it easy to remove the

fle sh in a to remaining flesh with the g knife , and lso scrape ff o the loosened hair by means of a blunt knife . In case of hides (heavy leather) much of the lime is also worked out

A h fle h in by this means . fter un airing and s g the skins or hides are placed in a pin-mill where they are washed with

or th e running water for half an hour until fine hair, etc . , is have bee n removed . The stock then in the proper condi

tion for the subsequent treatments . 2 in or Batin 6 Pue . 9 . r g g This procedure is carried out

to o flacid in order free the skin from lime , to produce a s ft , ,

Open condition and to smooth down the grain . There are

h u numerous met ods in vog e , most of which depend upon h fermentation for their beneficial action . Some Of t e sub

in n stances use are hen , pigeon and dog ma ure ; sour milk in — the form of dermi former ; fermenting bran ; pue rine and

Mn - a on th e many others . a y non fermenting baits are lso

h n h t . market , t e most commo of whic is lac ic acid

1 2 4 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTR Y

f n water and add to this 1 000 grams o co e . sulfuric acid ; now

600 o heat if necessary , and slowly add grams of syrup gluc se , waiting until the action subsides after each addition before adding the next portion .

W n h as he all of the glucose been added , the liquid will

h for assume a green color, and , w en cool, is ready use .

The skins after being washed from the puer are slated , is that , they are stretched by rubbing the flesh side with a stone slicker which besides stretching th e skin frees it from excess of water . The skins are next placed in the mill, the door adjusted , and the mill revolved . Ten per cent Of the above liquor computed on the weight of the skins is now

out of weighed and diluted with three times its volume water, and this solution introduced through the trunnion of the mill . The skins are then drummed one and a half hours (sheep

of 1 of and calfskin) , at the end which time , per cent sodium

of is bicarbonate dissolved in a small amount water added ,

f n -h are h and drummed or o e alf hour longer . They t en

th e on th e h removed from drum, placed horse over nig t in

to h n th e order drain and ydrate . O removing from drum samples are taken from the th ickest part of several Skins and h placed in boiling water . If t ey remain flat it proves that h . S U the tanning is complete hould t ey curl p, however, it

in T h e h h indicates unde r tann g . skin s ould t en be returned to the mill and worked in a second liquor of one -h alf th e A h strength of the original . fter standing over nig t they

h for one - l are t en washed ha f hour in running water, taken

out to from the drum , put in order remove excess of water,

o out h t smooth and stretch t em .

2 D e in — in 99 . y g . The plugs are put place again . The

to th e for one —h skins now returned drum , worked alf hour with a solution Of 3 per cent hematin paste and 5 per cent ° f - s i of 1 0 F W o soda a h n a small amount water at 4 . hen the LEA THER MANUF ACTURE 1 25

dyeing is finished several plugs are removed while the mill is off s in motion in order to draw the exce s of liquor. The A plugs are then replaced . solution containing 1 per cent of ferrous sulfate and 5 pe r cent of copper sulfate is introduced

1 through the trunnion , and revolved for 5 minutes longer . Li rin 00 Fat u o . 3 . q g The plugs are again drawn and

the skins washed in running water for 1 5 minutes . The fat

1 liquor is next added , which consists of an emulsion of 5 per cent of chip soap in as little water as possible and 1 per cent ° f 1 0 -h al A of ne ats oot oil at 4 F working one f hour . fter and of al a draining, the skins are put out , a coat equ p rts of glycerin and water applied to the grain . They are again al 2 a ac lowed to drain for about hours , put out ,and fin lly t ked W h h out on boards to dry . hen t oroug ly dry they are re mo m ved fro the boards , placed in damp sawdust until soft , and may then be ironed or glazed as desired . 0 1 Ironin — If 3 . g . a dull finish is desired , the skins are V i NO . 1 O l C given a light coat of setine ( acuum ompany) ,

flat- th e ironed with a hot iron and are then ready for market .

02 lazin — For 3 . G g . producing a glaze on leather a solu tion is made as follows

1 00 parts of hematin paste 5 00 parts of water 2 5 parts ammonia 1 0 parts ferrous sulfate 1 00 parts blood or egg albumen 200 parts water

1 0 parts glycerin .

Before glazing the grain is cleared with very dilute acetic

is lactic , or formic acid . The size then well rubbed in , dried ,

i ose ne and glazed under a glass roller . N gr sizes are also m uch used . 1 26 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

0 lo d h r me Co re C o . 3 3 . The chromed skins after stand

for 2 and ing 4 hours are thoroughly washed , put out then

of worked in a solution gambia, sumac , or fustic , standing ° 2 T h h as about . , whic been rendered acid with a very small l z . t amoun t Of sulfuric acid ( 1 o o 300 bs . of solution) . The ° temperature sh ould be about 1 1 0 F and th e skins should

1 to 2 h h be run hours . T is operation s ould be conducted in

-b x out to e of a paddle o . They are next put r move excess liquor and fixed with 5 per cent of tartar emetic by running

1 A of n ow for 5 minutes in the drum . solution basic color is ° h th run i n 2 t F run in t rough e t o ( o 5 per cent at 1 40 . ) and

for 2 l worked 0 minutes . The p ugs are then removed to free the skins from excess of solution and finally fat liquored with a solution of 1 5 per cent of soap and 1 per cent Of n e atsfoot ° il 1 f - f h n h O 0 F . o O t e at 4 r one hal our . removing from drum th e skins are th rown over th e h orse to drain and are ll fina y tacked out , and the following solution applied to the grain : 1 5 0 parts Of acetic an d 4 parts sodium dichromate

1 500 parts water .

W h th hen dry t ey are removed from e boards , placed in

to n h n ar damp sawdust softe , and a finis i g size prep ed as follows 56 parts Of e gg or blood albumen 1 part of sodium dich romate 7 parts of acetic acid 3 00 parts of water is well mixed and th orough ly rubbed in to th e grain ; allowed to h It dry, and t en glazed . is sometimes necessary to apply s h h everal coats before t e desired finis is secured .

0 B h r om T n e h im . N o e a na T 3 4 ath C g . e first really portant advance in ch rome tannin g was made by Augustus

1 28 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

K Cr O 2 HCl 2 KCl 2 Cr O , , 7 , H,O

“ In the dip some chromium dioxid is produced

C1 0 6 HCl 6 Na S O 6 NaCl H 3 , 3 , , , + 3 ,O

+ CQO ,

In the reducing bath we have two stages in the reaction .

6 HCl Na S O Na I . 2 C1 0 sO st , 3 , , , 3 , , 3 S 2 Cr Cl H 0 , 3 2

l a S O H O 2 Cr OH l 2d . 2 CrC N C SO 8 , , , , , , S 2 NaCl

r H l The C O C , is held by the fiber and is probably fin ally H converted to Cr (O ) , by the action of the bicarbonate use d for washing . It will be seen that the two bath method varies from the one bath in the fact that more or less of the precipitated sulfur is taken up by the fiber . In fact , a test to tell whether a chrome tanned skin is one bath or two bath may be made w h by rapping a silver coin in the leather, placing in the ot and n water oven for half an hour oting, that if turned black was - the leather made by a two bath process . l Tann a e 0 Ve e tab e . 3 5 . g g The process employed in the production of leather with the vegetable tan ning materials var y extremely according to the class of leather which is being produced , both in the materials selected and the time

- required . In sole leather tanning, when thick hides are used , many months are frequently needed ; while with th in skin and with the aid of mechanical motion which circulates the is liquor, the process often complete within a few hours . The simplest method of tannage is the old form used for - a sole leather m nufacture , but owing to the time required it a as A b cannot be re dily conducted a laboratory process . rief

s of outline of the proce s , however, many not be out place . LEATHER MA N UFACTURE 1 29

The hides as th ey come from th e liming process are de h aired and washed and then entered into a weakly acid - bath c of l which usually onsists old , nearly exhausted tan iquors .

As old not l ffi these liquors may a ways be su ciently acid , a l of as sma l amount some acid , such lactic acid , is introduced . After the hides have remained from 8 to 1 0 days in the suspenders ” they are usually laid in pits called “ handlers ”

h h 6 8 or 1 0 w ic are worked in series of , , pits , containing the of same number hides . The weakest liquor from the young is est pit run to the suspender daily , a new and stronger liquor is run to the pit holding the oldest and most tanned pack ; as this pack is removed the next in age takes its place while the youngest pack enters the pit containing the weakest d o an s . liquor, on down the series In this way each pack receives a change of liquor of regular graduated strength ; ° f 2 Bkr . h . o 0 passing from per aps a Sp . gr ( ) to one of ° a B r . 0 k . As bout a Sp gr . (4 ) the hides come from the handlers they are completely or nearly colored through “ ” and then pass to the layers . In the layers the hides are dusted with ground bark and r for or emain undisturbed several weeks, until the leather has attained all of th e weigh t and solidity of which it is It capable . is then washed in clear liquor, and scoured with i A stone and brush till the bloom s removed . light coat “ ” of oil is applied on the grain , partly dried and struck out

h on eit er the table or machine and colored as desired . 6 h h 0 . as 3 The finer grades of leat er , such goat , s eep and s al for - l e bookbinding, pocket books , and the like , are usual y tanned with sumac , although other tanning extracts are Often employed . For this method of tanning, the skins are more thoroughly puered than for sole-leath er ; while paddles and drums are largely used to hasten th e absorption of th e tan ning material . F 1 30 LABORA TORY GUIDE O INDUSTRIAL CHEMISTRY

The general method of procedure is given under the head of vegetable tan . Tan 0 Ve e table . 3 7 . g In this process the skins are first

as prepared under chrome tannage , namely, they are soaked to remove blood and dirt then introduced into milk of lime

h s sulfid on n wit 5 per cent of odium the amou t of lime used . h for 6 to 8 The liming s ould be continued days, or until the hair and epidermis are well loosened . They are then de

for haired , fleshed , and are ready the puering process , which is conducted in the same manner as for chrome tannage ; th e process being continued until the grain is smooth , the

l an d h h h al to fibers we l separated , a test wit p enol pht ein , a T h h . e are cut portion , s ows no evidence of lime skins now h and a a al t oroughly washed , are re dy for the ctu tanning process .

8 ue rbrach o Extract ue rbrach o on 3 0 . Q . Q is put the inarke t as a heavy paste and is sh ipped in barrels weigh ing f h 600 . one O t e about lbs It is produced in various places , S principal manufacturers , however, being the tamford

m ffi x M C S C . S e anufacturing ompany, ta ford , onn u cient ° tract is dissolved in water at 70 F . to produce a solution B stan ding at 4 6. The skins are now fastened on sticks by means of hooks and allowed to han g in th e tan liquor in such a manner that th ey may be lifted several times each day in th At of order to agitate e liquor . the end 3 days a quantity of extract equivalent to the weight of the skin is added to the tan liquor and the process continued until completely e struck through . The time requir d is usually about 6 days

for al h a . calfskin , thoug this may v ry to some extent

0 R nnin — h e . e Wh t 3 9 ta g . en properly tanned skins are put

out and shaved . They are then retanned in sumac , using h 1 about 2 per cent on the weight of t e skin and 5 5 per cent for of sulfuric acid in a paddle and run about 2 hours.

1 3 2 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

and flaxse e d softened with the moon knife , filled with and f flaxse d is 1 . o e milk . This mixture prepared by boiling lb

in a bucket of water until a good extract is obtained . For o and to use , take a p rtion of this extract add it an equal ° f 1 20 F se al . o . n volume milk, heat to ,a d apply ver coats If

to th e it is desired produce a grain , leather is boarded , which

consists in rolling under a board having a cork bottom . If smooth dull finish it is allowed to dry and softened by me ans

of staking . If glazed it is coated with e gg or blood albumen and worked

th e h on glazing mac ine .

1 2 Fat Li u o for h r m h e 2 r o e Le a . D 00 3 . q s C t r issolve

600 h ot . W grams of chip soap in grams water hen cool , add

0 of n e atsfoot one . 7 grams Oil , and stir in direction For use take 6 per cent of th is emulsion on th e weight of

the skins . T h e following ' fat liquors may also be found useful

500 grams soft soap 3 00 grams water 1 50 grams ne atsfoot Oil

500 grams soft soap 300 grams wate r 1 30 grams Castor oil i 20 grams linseed o l.

The preparation of ch ip soap and soft soap will be found

th e c on in hapter soap making . 1 Turke Re d Oil — h as 3 3 . y . T is compound kn own also soluble Oil is largely employed in th e tanning industry and may be prepared as follows

P 1 60 of rovide a suitable vessel , place in it grams castor

o R un oil of go d quality . in slowly, taking about an hour LEA THER MANUF ACTURE 1 33

e all 2 over the op ration , and stirring well the time , 4 grams

. A th e r to 2 of strong sulfuric acid llow mixtu e stand 4 hours .

0 . of At the end of this time stir in 1 7 c c . water until the whole mass h as a uniform creamy appearance ; next allow to stand for 24 hours , when it will be found to have settled out into oil to two layers, one of at the p, the other of acid water

Run off below . this through a tap funnel ; next dissolve f 1 0 . o 20 grams of common salt in 7 c . c water and add this to th e ll ll f oil, shaking we as before ; again a ow to stand or 24 off hours . Then run the bottom aqueous layer . Now add concentrated ammonia slowly with constan t stirring into the i oil u . until a clear , transparent liq d is obtained Finally add

to 0 R sufficient water make 3 5 grams, when Turkey e d Oil of 50 per cent strength will have been made . fi n 1 Currie rs Stu Gre ase . 3 4 . g In working heavy leather it is customary to fill the hides with grease which h elps to A give it a body and renders it more pliable . good stuffing grease may be mad e as follows :

1 00 grams of town fallow 50 grams moellon degras 50 grams petroleum jelly

x are melted together . When melted the mi ture is allowed to cool somewhat and 1 00 grams of cod oil stirred in before it sets . n anna e O h is h 1 Combinatio T . 3 5 . g nce a leat er thoroug ly tanned with a vegetable material it is little aff ected by alum or on or chrome , while the other hand alum chromed tan leather is still capable of absorbing a large amount of ve ge table tanning material . A mineral tannage gives a soft flat leather ; while vegetable tannage gives a full plump leath er which can only be made soft by stuffing with a large amount of grease . Conse quently 1 34 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY advantage is taken of the ability of chrome tanned leather h to absorb tannic acid , thus producing a full leather, w ich

t s n retains the sof nes characteristic of mineral ta nage . To carry out the process the skins after being washed from excess of chrome liquor are run in a weak solution of gambia for

h n se veral hours, and may t en be finished in the same ma ner as given for chrome tan ning . Combination tannages also have the advantage over straight chrome in that they may be colored with basic colors in th e same manner as given under vegetable tannage . 1 6 S l ' s 3 . ome vegetable tanning materia s and the content of tannic acid — 8 1 0 per cent Tannin — Larch 9 1 0 per cent Tannin — Saw Palmetto 5 1 3 per cent Tannin Sweet Fern 4 6 per cent Tannin — Alder 1 6 20 per cent Tan nin Common Birch 2 5 per cent Tannin Chestnut Bark 1 7 per cent Tannin Ch estnut Wood 3 6 per cent Tannin — O ak Bark 1 2 1 4 per cent Tannin — Galls 50 60 per cent Tannin — Canaigre 2 5 30 per cent Tannin — Sumac . 1 8 25 per cent Tannin Que rbrach o 20 per cent Tannin — Gambeer 3 5 65 per cent Tannin

- — Divi Divi . 40 45 per cent Tannin — Mimosa 1 2 20 per cent Tannin Valonia 40 per cent Tannin — Myrobalans 28 3 5 per cent Tann in

CHAPT ER IX

WOOD FIBER PULP AND PAPER ,

1 In o 3 7 . a lab ratory manner it is impossible to go very a uf a of h extensively into the m n cture paper, wit out entailing

re . A a g at expense few simple tests may be performed ,

l a re however, which wi l enable the student to more fully pp ciate some of the operations introduce d in th is very important industry . Pape r consists of cellulose fibers matted or felted in a sheet . The raw materials employed are wood pulp, cotton or linen rags, esparto , straw , hemp , flax, jute , etc . 1 8 Wood Pul 3 . p . As the bulk Of paper on the market is

a r d h al m de entirely or in pa t from woo fibers, t is raw materi will be the only one considered in this chapter . For a more detailed account of the processes involved the student is referred to the books of references given at th e end of the chapter . Wood pulp is of two kinds, mechanical and chemical . 1 M l — . c l M 3 9 e h anica Pu p. echanical pulp may be made of O lar in the laboratory by forcing a stick p p , hemlock ,

or - spruce , pine bass wood against a revolving emery wheel , over which a small stream Of water plays continuously . The resulting pulp is passed through se veral screens to re

in move suflicie n tly disintegrated particles . The finely di vide d pulp is then brought into a settling tank when it is washed , bleached , filled and colored as subsequently de h m scribed under the treatment of c e ical pulp . 20 Ch e mical Pu l is 3 . p . Chemical pulp prepared by the 1 36 W F P P AN D 1 OOD IBER, UL PAPER 3 7

sulfite soda process, the process, or by the sulfate process . h s e T e soda proces is largely us d for soft woods . The bar k Th is removed by shaving . e wood is then chipped in a

machine , or by hand by cutting across the grain . To sepa

rate the knots , the chips are thrown into water where the

heavy parts go to the bottom , thus leaving the clear wood on

tO . p The digester is nearly filled with chips, which are then ° of 0 B covered with a caustic liquor about 1 6. The cover of the digester is safely screwed in place , and the charge

is heated until a pressure of 90 lbs . obtained ; which pressure “ ” 1 ff is held from 8 to 0 hours . The e ect of this cooking is to reduce the wood to a soft mass of grayish-brown color ; while the liquor becomes dark brown and h as increased

somewhat in density . Now Ope n the valve of the digester

to Much very slowly in order release the pressure . car e must be take n he re to avoid an ossibilit o an e x losion y p y f p . If h as the process been conducted properly , the stock will all crumble to a pulp which togeth er with the “ black liquor is transferred to a suitable apparatus when it is systematically as s l w hed , and the wa h waters saved until their density fa ls ° B below 8 é . ° r o 8 B This liquo may be evap rated to a density of 3 6, “ ” Th e when it may be burned . black ash thus Obtained may be re causticize d with milk of time and from 80 to 90 of per cent the original soda recovered . The pulp Obtained

i is above s thoroughly washed . It then passe d through a screen to remove the larger particles . 2 1 Ble ach in — ul 3 . g . The washed p p is next placed in a vessel provided with some form of agitator where it is mixed hl with a weak solution of calcium hypoc orite . Only a clear o o e s lution of bleaching p wder should be us d , so that no dirt as will be introduced into the insoluble residue , it will cause ° is ° spots in the paper . If the liquid heated to 90 or 1 00 F 1 38 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

is A or a little acid added , the process hastened . lum forms

aluminium hypochlorites with bleaching powder solutions , “ ” which is very eff e ctive ; a slightly ac id alum or bleaching

i 1 8 2 alum s commonly employed . From to 5 parts of bleach

i 1 00 r A ing powder s used for each pa ts of pulp . s soon as e bleached , the process is stopped ; otherwis the fiber is liable

to be chlorinated , and color again taken up . The excess of

in is or hypochlorite the pulp washed out with water , is

d ad as - estroyed by ding an antichlor, such sodium thio sul

fate . The action of the antichlor is as follows :

2 Ca lO Na s O H O 2 NaCl 2 CaSO (C ) , , , , , , + 2 HCl

l s The pu p must be thoroughly wa hed after bleaching,

even when antichlors are used , since injurious substances

may be left in the pulp . O as ther materials than bleaching powder, such ozone ,

h or hydrogen peroxid , sulfurous acid , liquid c lorin , sodium

as peroxid have been suggested for bleaching, but yet the hypochlorites are the most employed .

2 2 Th e Pa e r Mak in Proce ss . 3 . p g The first operation furnishing or charging the stack ; the kinds and quantity of material employed depend on the quality of th e paper to

. an d be produced In order to give the paper body, weight , “ ” al is greater smoothness, mineral filler on loading materi employed . This must be exceedingly fine , and not have too high a spe cific gravity or soluble in water . It must be free from dirt , grit , and mica . The loading is done after the ll fiber h as been well beaten with water . The fi er is thor

n oughly mixed with pulp , and then the sizi g material added , and the whole beaten until a perfect mixture of all the ma te rials are obtained . Some of the fillers which are employed s in paper making are clay, chalk , and calcium ulfate , while a good size may be prepared from rosin with a concentrated

1 40 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

s b h answer the purpo e very well , it only eing necessary to ave two polished rolls in place Of the usual machine having only

one polished roll . — z 00 . . Of 2 Rosin Si e . 3 4 . Into an iron kettle place 7 c c

20 f - B water and dissolve in this grams O soda ash . ring to a f A boil and Slowly add 1 50 grams O powdered rosin . large

amount of carbon dioxid is generated , consequently the kettle sh ould be of sufficie nt capacity to prevent the liquid from

passing over the side . In order to avoid too great a loss by t evaporation , water is added from time to ime , the level being regulated by means of a stick having a notch cut at the d original height of the liquid . When all of the rosin has is is a solved , the mixture llowed to cool , and is practically a - A 2 5 per cent solution of rosin soap . stronger size may be

made by using less water .

e Case in Siz . This size is prepared by dissolving casein

- 1 or in cold soda ash (5 to ) borax solution . It is applied in

the same manner as that given for rosin size . 2 Colore d Pa e r 3 5 . p The pulp colors described in Chapter VI may be added to the pulp in the beater in any

. V amount desired to produce the required shade ery Often , is however, the color produced by direct application of coal

as l tar dyes , the general method of procedure being fo lows : The pulp and filler are introduced into the pulping machine

and well worked . The requisite amount of color, previously

i v l and d ssol ed in water , is now added , wel worked in , then al - followed by the rosin size and um . The well beaten mass is then worked into sheets and treated as given above . To produce light shades 5 per cent of color on the weight l of the dry pu p is used . For medium shades 1 per cent is employed . For heavy shades as much as 3 per cent may be necessary . The dye stufls used for coloring pulp may be any acid color W F P P AN D P P OOD IBER, UL A ER 1 4 1

O or direct cotton color . ther colors will require agents . l The fo lowing list of colors may be found of service . Uranin O soluble Dianil red

E n n osi , all brands Dia il sc arlet E all rythrosin , brands Dianil blue A all cid violet , brands Dianil brown N aphthol yellow, all brands Dianil black O range , all brands Direct black

REFERENCES

Practical a e r makin . G . Cla e rton . London 1 0 P p g pp , 9 7 .

dl . nd h r on P e r Makin . . Be a e Lo n 0 C a te s a C o 1 . p p g , 9 4 d r n . Lon on 1 0 . T he P h e m t . Ste e s 8 ape C is v , 9

f r kin . r A T e x Book P e Ma C. F. C oss and E t o a . . Be van p g J . — don 00 n 1 1 06. Lo , 9 9

li rf . D in f r . d n e o Pa e Pul u u E urt Lon o 1 0 1 . y g p p J s , 9 CHAPT ER X

USEFUL DATA

m r n i n 26 Th e rmo e te Co ve s o s . 3 . r In order to convert Centigrade (Ce lisus) into Fahrenheit (above freezing-point)

i 2 th e multiply by 9 , d vide the product by 5 , and add 3 to quotient . To convert Fahrenheit above freezing-point into Centi

2 grade , subtract 3 , multiply the remainder by 5 , and divide the product by 9 . R r F To convert eaumu into ahrenheit , multiply by 9 ,

2 to . divide by 4 , and add 3 the quotient

O R u 2 T convert Fahrenheit into eaum r, subtract 3 , mul i l t . p y the remainder by 4 , and divide the product by 9 l 2 Me n ration of o ume . 3 7 . su V The standard gallon measures 23 1 cu . in . and weighs lbs . One cubic foot contains gallons and weigh s ounces or lbs .

For of of of facility computation , the weight a cubic foot

1 00 0 or water is usually taken as ounces lbs . ° ° 0 2 Water expands from 4 to 0 2 to the amount of . 0 467

00 2 1 . 7 5 for each degree giving an increase of 1 cubic foot in

cubic feet . 28 To Com ute Volume of a e f . d o 3 p Cub . Multiply a si e a cube by itself and that product again by a side .

2 TO Com ute Volume of a Pa all l i do ul . o e M 3 9 p r e p p n . i l t p y length by breadth and that product again by depth . 0 To Com ute Volume of a lin de 33 . p Cy r . Multiply area of base by height .

1 44 LABORA TORY GUIDE OF INDUSTRIAL CHEMISTRY

m m a n 2 To Co u te Volu e of Co e . M . 33 . p ultiply the area

- of the base by perpendicular height, and take one third of

product . To Com u te Volume of a Frustum of a Cone — Add 3 3 3 . p . together square of the diamte rs of greater and lesser sides and product of the two diameters ; multiply the sum by

. 78 54 and this product by height ; then divide the last product

by 3 .

Exa — W mple . hat is the volume of frustum of a cone di

ame te r and ss of greater le er ends being 5 and 3 feet, and

hei8ht 9 feet .

49 X -78 54 38 4 846

X 9 cubic feet . 3

m u te Volume of S h e re M To Co . 33 4 . p p ultiply the cubic of the diameter by 5 236. — Example . What is the volume of a sphere the diameter h being 1 0 inc es . 3 1 0 1 000 1 000 . 2 6 and X 5 3 cubic inches . This rule will apply to the measurement Of kettles which

- as a rule are one half a sphere . If the kettle is a combination of a sphere and cylinder the me asu rement of each may be made and the contents thus

s determined . In all of the above mea urements it is a simple matter to ascertain the number of pounds by multiplying the number of cubic feet by 5 and then by the spe cific h gravity of t e substance in question . h Of 33 5 . The weig t per pound a few common substances may be found useful as indicated in the following table USEFUL DA TA 1 45

SO LIDS

Substance Substance

1 0 7 .

ncre te . 1 9 2 . Co

r i . . Ea th , so l 0 1 7 .

te 8 to An thrac i . 4

Lime s n e . k . to Ca in g .

LIQUIDS AND SEMI SO LIDS

Substance Substance

pe r . Cu . Ft .

T c ute th e we i t of a bo in oun s e r cubi f t i i e th e o omp gh dy p d p c oo , d v d i spe c ific grav ty by 1 6.

To Com ute Pre ssure of a Fluid u on Bottom of its 3 36. p p

n nin e —Ml e Co tai g V sse l. u tiply area of bas by height of

fluid in feet , and product by weight of a cubic foot of fluid . To Com ute Pre ssure of a Fluid u on a Ve rtical 3 3 7 . p M p , Incline d or an Surface . , y ultiply area of surface by height of center of gravity of fluid in feet , and product by weight of cubic foot of fluid . 1 46 LABORA TORY GUIDE OF INDUSTRIAL CH EMISTR Y

i Example . What s pressure upon a mping side of a

1 d pond of fresh water 0 feet square an 8 feet in depth .

Center of gravity 8 2 4 feet from surface . 2 1 0 Then X 4 X lbs . 8 E uivale n ts of Me tri c We h and e asure 33 . q ig ts M s

1 o p und 453 . 59 grams

1 oz . avoirdupois grams

1 U . S. gallon liters l 1 U . S. iquid oz . cc . grains per imperial gallon parts per

P e arts p r X grains per imperial gallon .

s . Grain per U S. gallon parts per

P . l 8 U S. arts per X 5 3 grains per ga lon . Table of Multi le s 339 . p .

Centimeters X inches .

Centimeters X feet . C ’ entimeters cubic X apothecaries fluid ounces.

Diameter of a circle X circumference .

U . S. Gallons X liters .

m . U . S. Gallons X 565 i perial gallons

S. . G U . allons , imperial X gallons

l . U . S. Ga lons X pounds of water

Gal 1 0 . lons, imperial X pounds of water

G . allons, imperial X liters

Grains X grams .

Inches X meters . IMnches X millimeters . iles X kilometers . O t unces, roy X ounces of avoirdupois .

Ounces avoirdupois X ounces troy . P ounbs i . , avoirdupois X k lograms

F 1 48 - LABORA TORY GUIDE O INDUSTRIA L CH EMISTRY

Units or Com utin Saf e Strain th at ma b om 3 43 . f p g y e h e

N s Hause rs and Cable s by e w Rope , .

ROPEs IIAUSERS CABLES

Circum White Tarre d Wh ite Tar re d Wh ite Tarre d Des cription

4 3 3 3 3 Strands Strands Strands Strands Strands

Lbs . Lbs . Lbs . Lbs . Lbs . L . bs Lbs .

White

Illustrat o W w can be r a a i n . hat eight bo ne with s fety by manila rope of 3 strands having a circumference of 6 inches ?

2 6 X lbs . USEF UL DA TA 1 49

E a i P r W i h an d B lk W e i h s . va o ve owe e e t u 3 44 . g t p r t r p g

of difi e re n t Fue ls .

5 a ’ T ‘ é e 5 :i B 0 3 22 M 133 Ef f 5 EEE 5

n t in . mbe r an ma x. e ac Mou a Cu l d , P h min 29 Fo re st 4 1 -7 8 Duff ryn Be a ve r Me adow . 39 -

ar me i an . Lac awann a -8 C l , W g k 45 Blossbur gh 9 7 2 Le high 40 -5 Ne wc as tl e 8 76 44 COKE Pitts bu rg 8 2 4 7 8 Natu ral Sydn e y 7 99 47 2 C u mbe rlan d

o e r i Va . . 6 2 MISC LLA OUS Cl v H ll , 7 7 49 E NE

I d . k . an n e lton n . arcoa O a C , 7 3 4 4 7 Ch l Sc otc h 7 08 43 8 Pe at 1 50 LABORATOR Y GUIDE OF IN D USTRIAL CH EMIS TR Y

P e ssure and Te m e a u e of Sa u ate d 3 45 . r p r t r t r Ste am

- m . T r tm Pre ssur . n . T m Pra m : Sq. In e p a 1 Sq I e p rature fg g aL$ g

1 5 2 LABORATORY GUIDE op INDUSTRIAL CHEMIS TRY

of Satu ate d Ste am contin u Pre ssu re and Te mpe rature r , e d

m T m rature Pr e ss ur e S . In . Te e r ature Pre ssure 1 Sq In . e pe q p Lfif o Lg .

6 Fri orifi c Mix u e s . 3 4 . g t r

Fa ll of Fall of Mixture s Parts Te mpe rature Te mpe r ature

Se a sa lt S now ° ° Amm on iu m Ca lc iu m 4 0 to 73 ° ° n itrate 1 5 to 2 5 c hlorid

S now or

powde re d ice

Amrri on u m ° ° 68 to 9 1 ll lor :il c

° 0 S n ow or 5 to 1 8 powde re d ice USEF UL DA TA I 53

f P lle S e e d o u s . 3 47 . p y

f an d ve l e V an d v spe e d o driving dri n pu l ys .

d e of e n D and diam ter driving and driv pulleys . f v R and 7 number o re olutions .

dr d —DR R —dr ’ R r D

In a train of pulleys the final velocity V VD D D d d d , etc ) ” ) ” — U i of Ele c rical Re sis a ce T h e oh r 3 48 . n t t t n . m e pre ° h ff to l sente d by t e re sistance o ered at 0 C . an unvarying e ec of tric current by a column mercury grams in mass , of - e of e h of a constant cross sectional ar a, and a l ngt centimeters .

i of r T h e a r wh h U e . m . Cu e e 3 49 n t r nt p , ic is an unvary in g current passed th rough a solution of silve r nitrate in

e an d h f 00 1 1 1 wat r deposits silver at t e rate o . 8 grams per second . 0 U i f El c Mi F c h o e t o o e o e . T e l h 3 5 . n t r t v r vo t is t e pre s sure which ii ste adily applied to a conductor wh ose re sist

one h m ll n of one ance is O wi produce a curre t ampe re .

i f an i T h lo 1 U o u . e u mb h h h . co t e 3 5 n t Q t ty , w ic is quantity of electricity transferred by a curre nt of one ampere in one second .

2 i ci a ad h h U of Ca a . r h . t e a 3 5 n t p ty The f , w ic is cap city of a conde n se r ch arged to a potential of 1 volt by 1 coulomb of electricity . U i k 7 W . oule h h 1 0 . to 3 5 3 n t of or The j , w ic is equal h f h . e h a units o work in t e C . G . S syst m and w ic is practic lly equivalent to the energy expended in one second by an h ampere in an o m.

n i f P e watt h h to U t o ow . 3 5 4 . r The , w ic is equivalent

e r e the work done by one joule p s cond . 1 54 LABORA TOR Y GUIDE OF IN D USTRIAL CH EMIS TR Y

REFERENCES

’

i . d c l n n u l. h n l w Van Nostran s Ch e m a A a o C se n . Ne Y J O ork , I 90 7 ’ i ’ k k d n e r c . h rl Me ch an ics an E ne s Po e t Boo C a e s H . Hasw g e ll .

w rk 1 6 Yo 0 . Ne , 9 l A Pocke t Book for Ch e mists . T h omas Ba e . London 1 02 y y , 9 .

1 56 IN DEX

PAGE

1 6 In u in . 1 d l (S S . )

0 In l Drie rs 9 du in (W . S . ) Dye ing 2 5

n r 1 2 1 1 Dye i g Le a the 4 , 3 Dye T e sts on Cotton 3 9 Iron Su lfate Va t

E e c tr ica l Un its l La ke s Eosin Laund ry Soaps EOSi“ G rou p Le ad Ace tate E u i a le nts Of Me tr ic S ste q v y m Le ad Nitra te Et e r h Le athe r Ma n u fac tu re Evapora tion

E a orati e owe r of Fue s . v p v P l Lilac

Lixiviation Logwood La ke s Logwood on Wool Fas t G re e n 0

Fa t Liquoring Fat Liquors for Ch ro me Le athe r Fe rrous Ammon iu m Su lfate Magne siu m Chlorid Filte r Pre ss Mastic Va rn ish Fi te r acu u l , V m Me chan ica l Pu lp Filtra tion Me n su ration of Vol ume Fre n c h Polish Me rce rize d Cotton Fre n c h Va rn ish Me tallic Mordan ts Frigo rific Mixtu re s Me thyl Viole t Me thyle ne Blue Me tric Equ ivale n ts Mordant D y e s Glazing Mordan ts of Me ta llic T an n ate s G re e n C astile Soap

N a t o e ow 5 . Ha l f B oile d Soap ph h l Y ll Ne r i O il Han d Frame ol Niobe on Hyd rosu lfite Vat Nitrobe nzol

P-n itrace tan ilid

P-n itran ilin IN DEX

Se ttling T an ks

l n 0 i e a rn i 0 O i Sta s Sh llac V sh 0 0 0 0 0 0 0 0 0 O il Va rn ishe s Silk O ne B ath Ch rome Soaking Skin s O range II Soap O rga nzin e Soap Powde r O xidation Co lo rs Soda Ash Sodiu m Bisu lfite Soft Soap Solu ble O il Palm O il Soap Spe cific G ravity Pape r Making Spe e d of Pulle vs Pic ric Ac id Spirit Colors Pigme n ts Spirit S ta in s Potassiu m Ch rom a te Spir it Va rn ish otassiu Dic ro ate Sta in Re o a of P m h m s, m v l Potass iu m Pe rmangan a te Ste a m Jac ke t Ke ttle Potas s iu m Sod iu m T a r t ra te Strain on Rope s Primu lin S u blim ation P ru ss ian Blue S ubstan tive Dye s - n 0 0 0 0 0 i Pue ri g 0 0 0 0 0 P Su lfan lic Ac id Pu tty S u lfu r Dye s Pyknome te r

T a ble of M u ltiple s Que r brac h o Extrac t T ann ic Ac id Mo rd a n ts T a r Soap T e mpe rature for Ste a m Pre s

su re

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