Industrial and Engineering Chemistry : analytical edition, Vol. 10, No. 10

IN D U S T R IA L and ENG OIE E RING C H E M I S T R Y

V o l. 30, C o n s e c u tiv e N o . 39

H arrison E. H ow e, E d itor

Re f r a c t i o n, Di s p e r s i o n, a n d Re l a t e d Pr o p e r t i e s o f

Pu r e Hy d r o c a r b o n s...

...A. L. Ward and S. S. Kurtz, Jr. 559

D e t e r m i n a t i o n o f M e r c u r y w i t h s - D i p h e n y l c a r b a -

z i d e ...F. W. Laird and Sister Alonza Smith 576

Q u a n t i t a t i v e S p e c t r o g r a p h i c E s t i m a t i o n o f T r a c e

E l e m e n t s i n B i o l o g i c a l A s h ...Paul H. Bell 5 7 9

V i s c o s i t y o f A n i l i n e b e t w e e n 2 0 ° a n d 1 0 0 ° C . . . .

. ... L. A. Steiner 582

Li q u i d Ba t h Me l t i n g Po i n t Ap p a r a t u s...

... E. C. Wagner and J. F. Meyer 584

De t e c t i o n o f Sm a l l Am o u n t s o f Ph e n o l p h t h a l e i n

... Eugenia H. Maecliling 580

G l a s s V a p o r - D e n s i t y B a l a n c e ... I. H . Simons 5 8 7

Mo d e r n La b o r a t o r i e s :

T h e U n i v e r s i t y o f D e l a w a r e C h e m i c a l L a b o r a ­

t o r y ...Albert S . Eastman 5 8 8 T h e A m erican C h em ical Society assum es no re s p o n sib ility for the

ANALYTICAL EDITION

20,200 Copies of This Issue Printed

O ctober 15, 1938

tfSLt jg:

Vol. 10, N o. 10

Mi c r o c h e m i s t r y:

Pa p e r a s Me d i u m f o r An a l y t i c a l Re a c t i o n s . .

...Beverly L. Clarke and H. W. Hermance 591

De t e r m i n a t i o n o f Io d i n e...

A. C. Bratton and J. F. McClendon, with the tech­

nical assistance of William Foster and Ralph White 600

U s e o f T r a u t z ' s M i c r o - D u m a s M e t h o d w i t h A p p a ­

r a t u s o f P r e g l ...Charles W. Beazley 605

Re l a t i v e Va l u e o f Ce r t a i n Az o De r i v a t i v e s o f

8 - Hy d r o x y q u i n o l i n e a s An a l y t i c a l Re a g e n t s . .

...Thomas Boyd with Ed. F. Degering and R. Norris Shreve 606

De t e r m i n a t i o n o f Ca r b o n a n d Hy d r o g e n . . . .

... Samuel Natelson, S. Steven Brodie, and Edwin B. Conner 609

De t e r m i n a t i o n o f Io d i n e i n Bi o l o g i c a l Ma t e r i a l s

...Norman L. Matthews, George M. Curtis, and Wallace R. Brode 612

E s t i m a t i o n o f C o p p e r , Z i n c , a n d C o b a l t ( w i t h

N i c k e l ) i n S o i l E x t r a c t s . . . P . L. Hibbard 615

ents a n d opinions a d v a n c e d b y c o n trib u to rs to its p u b lic a tio n s.

P u b l i c a t i o n O ffice : E d i to r ia l O ffice : R o o m 706, M ills B u ild in g , W a s h i n g t o n , D . C .

T e le p h o n e : N a t i o n a l 0848. C a b l e : J i e c h e m ( W a s h in g t o n )

P u b lish e d b y th e A m erican C hem ical S o ciety , P u b lic a tio n Office. 2 0 th &

N o rth a m p to n S ts., E a s to n , P a . E n te re d as second-class m a tte r a t th e P o st Office a t E a s to n , P a ., u n d e r th e A c t of M arch 3, 1879, as 48 tim es a y ear.

In d u stria l E d itio n m o n th ly on th e 1st; A n a ly tic al E d itio n m o n th ly on th e l o th ; N ew s E d itio n o n th e 10th a n d 2 0 th . A ccep tan ce fo r m ailin g at special r a te of p o stag e p ro v id e d fo r in S ectio n 1103, A c t of O cto b er 3, 1917.

a u th o riz e d J u ly 13, 1918.

A n n u a l su b sc rip tio n ra te s : In d u s t r i a l a n i> En g i n e e r i n g Ch e m i s t r y

co m p lete $6.00; (a) In d u s t r i a l Ed i t i o n S3.00; (6) An a l y t i c a l Ed i t i o n

E a s t o n , P a .

A d v e rtis in g D e p a r t m e n t : 332 W e st 4 2 n d S t r e e t , N ew Y o rk , N . Y.

T e le p h o n e : B r y a n t 9-4430

$2.50; (c) Ne w s Ed i t i o n $1.50; ( a ) a n d (b) to g e th e r, $5.00; F o reig n postage to .e o u n trie s n o t in th e P a n A m e ric a n U n io n , $2.40, (a) $1.20; (6) $0.00; (c) 50.60. C a n a d ia n p o stag e o n e -th ird th e se ra te s. Single copies: (a) $0.75;

(6) $0.50; (c) $0.10. Special ra te s to m em bers.

N o claim s c an be allow ed fo r copies of jo u rn a ls lo st in th e m ails unless such claim s a re receiv ed w ith in s ix ty d a y s of th e d a te of issue, a n d no claim s will be allow ed fo r issues lo st as a re s u lt of in sufficient n o tic e of ch an g e of a d d ress. (T en d a y s ’ a d v an c e n o tice re q u ire d .) “ M issing fro m files'’

c a n n o t be acc e p te d as th e reaso n fo r h o n o rin g a claim . C h arle s L. P a rso n s, B usiness M an a g e r. M ills B u ild in g , W a sh in g to n . D . C ., U . S. A.

INDUSTRIAL AND ENGINEERING CHEMISTRY VOL. 10, NO. 10

M o r e A c c u r a t e

^—

M o r e R a p i d — M o r e R e l i a b l e T h a n a

C o l o r i m e t e r

P

H O T E L O M E T R 1C m ethods of analysis replace m any of the usual colorimetric m ethods w ith slight modifications in procedure. N o comparison standards are needed. A single calibration for any par­

ticular unknow n holds indefinitely. Such simplification in laboratory practice greatly facilitates the work and saves m uch tim e in im p o rtan t analyses. For example, in the colorim etric determ ination of m olyb­

denum in steel, preparation of a new reference sam ple is required every few hours; w ith the “ Photel- om eter,” a single calibration holds indefinitely.

P R E SE N T ANALYTICAL APPLICATIO NS FOR “ PIIO T ELO M ETE R ”

Food A n a ly sis L ead in m ic ro g ra m s C opper

Iron C a ro ten e F lavin

S te e l A n a ly sis M o ly b d e n u m M a n g a n ese C opper C h r o m iu m T ita n iu m V a n a d iu m

W ater A n a ly sis A m m o n ia M a g n e siu m C a lc iu m S u lp h a te s N itr a te s N itr ite s A lu m in u m C h lorin e

M isce lla n eo u s C h ro m e P la tin g

S o lu tio n s S u lp h ite L iq u o rs

T a n n in L iq u o rs S o d iu m C h r o m a te S o d iu m D ic h r o m a te

For F ull In fo rm a tio n , A sk For B u lletin No. 104F

CHICAGO

1700 Irving Pk. Blvd.

Lakeview

Station

S C I E N T I F I C

INSTRUMENTS

LA BO RATORY A P P A R A T U S

B O S T O N 79 Amherst St.

Cambridge A Station

New York • Boston • C H I C A G O • Toronto • Los A n g e l«

C E N C O - S H E A R D - S A N F O R D

P H O T E L O M E

(Patent Nos. 2,051,317 and 2,051,320)

T E R

OCTOBER 15, 1938 ANALYTICAL EDITION 5

CEMENT ANALYSIS requires ACCURATE ALKALI DETERMINATIONS

For vital analytical accuracy many cem ent chemists préfer the J. Lawrence Smith m ethod for detecting minute quantities of alkali. This procedure requires a calcium carbonate reagent with particularly low alkali content, such as—

CALCIUM CA RB O N A TE A.R. L O W A L K A L I

(Mallinckrodt)

Refined to predeterm ined standards, this reagent has been especially developed for use in the J. Lawrence Smith method of alkali determ inations. I t is always uniform in composition and reaction.

O th e r Reagents for the Cement Chemist

AM M ONIUM O XALATE SO DIUM AM M O NIUM PH O SPH A TE PO T A SSIU M CARBONATE SODIUM ACID PH O SPH A TE

PO T A SSIU M H Y D R O X ID E SO DIUM CARBONATE PO T A SSIU M PERM ANG ANATE SO DIUM H Y D R O X ID E

Send for the new catalog of Mallinckrodt Analytical Reagents and Laboratory Chemicals showing maximum limits of impurities of nearly 500 chemicals for research and control labo­

ratories.

C H E M I C A L W O R K S

2nd & Mallinckrodt Sts. C H IC A G O M O N T R E A L 72 Gold St.

ST. L O U IS , M O . P H IL A D E L P H IA T O R O N T O NEW Y O R K , N. y .

INDUSTRIAL AND ENGINEERING CHEMISTRY VOL. 10, NO. 10

A w o rld , yet unseen and u n k n o w n , aw aits th e co m p letio n o f the g ian t 200-inch telescope, b ein g erected on M o u n t P alo m ar, C alifornia. Sci­

entists anxiously aw ait the m om ent w hen the h u g e "eye” can be focused on d istan t p lanets to determ ine, am o n g o th e r th in g s, w h a t types of life, if any, exist in th e far reaches of the universe.

T h e task o f co n stru c tin g such a telescope, o f g rin d in g and p o lish ­ in g the en o rm o u s m irro r to a deg ree o f p erfectio n never b efore attained,

is in itself am azing. B ut w h a t o f the researc h chem ists w h o stru g g led lo n g h o u rs to d eterm in e th e sta n d ­ ard s o f m aterials to be used in the co n stru c tio n o f this scientific in ­ strum ent?

T h e stan d ard s set by th e lab o ra to ry chem ist fo r such vital re searc h w o rk are necessarily exacting. So, to o , are th e stan d ard s estab lish ed fo r the m anufacture o f M erck R eag e n t C hem icals w h ich are used by exact­

in g chem ists.

Catalog on request.

M E R C K & C O . I N C . ^/M tinu^acùiK hiÿ (o/iem i ⁴ t ⁴ R A H W A Y , N . J

OCTOBER 15, 1938 ANALYTICAL EDITION

THE NEW WILL CATALOG

T he new Will C atalog is as m uch a necessity in m odern laboratories as are th e thousands of item s it lists and describes. C ontaining m ore th a n 900 pages with thousands of illustrations, i t is a com pact, easily re­

ferred to source of com prehensive inform ation for every purchaser of laboratory supplies.

W ith every item indexed, cross indexed an d arranged in alphabetical order, i t m akes the locating of inform a­

tion on any desired equipm ent or m aterial as easy as looking up a w ord in th e dictionary.

T he new F ifth E ditio n of the W ill C atalog, like earlier editions which served as buying guides in so m any labo­

ratories, lists every necessity for th e m ost m odern

laboratory work. Obsolete item s have been . weeded out, their place tak en b y th e m ost m odern equipm ent and m aterial. I t is the first general laboratory supply catalog to incorporate the new “P Y R E X ” Laboratory

Ware reduced price lists.

T his catalog is th e last word in labo rato ry equipm ent and supplies. Y ou need i t on your lab o rato ry shelf- F or your copy w rite us on your laboratory, business or institution letterh ead —or fill in th e attac h ed coupon and a ttac h to business card or letterhead.

C O R P O R A T I O N

4 7 R U S S E L L S T R E E T

R O C H E S T E R , N. Y.

Please send me the N ew W ill Catalog.

N a m e ...

T i t l e ...

C o m p a n y ...

C ity a n d S t a t e ...

L A B O R A T O R Y A P P A R A T U S A N D C H E M I C A L S

8 INDUSTRIAL AND ENGINEERING CHEMISTRY VOL. 10, NO. 10

HOSKINS PRODUCTS

ELECTRIC HEAT TREATING FURNACES • • HEATING ELEMENT ALLOYS • • THERMOCOUPLE AND LEAD WIRE • • PYROMETERS » • WELDING WIRE

• • HEAT RESISTANT CASTINGS • • ENAMELING FIXTURES * • SPARK PLUG ELECTRODE WIRE • • SPECIAL ALLOYS OF NICKEL • • PROTECTION TUBES

H O SKIN S MANUFACTURING CO M PAN Y, DETROIT, MICHIGAN

BACK IN 1910

This H o s k i n s F u r n a c e Is N o w 2 8 Y e a r s Old, B u t Is S t i l l i n U s e .

The Western Railroad Supply Company use this little Hoskins Furnace in solder­

ing eyelets on wire leads. “ A girl will clean and dip about 1200 leads per hour, at both ends,” they say. The Chrome! element has, of course, been replaced many times, but the cost of the furnace has long since been

“ charged off.” A good investment, indeed. For full description of all Hoskins Furnaces, send for Catalog 56.

If yo u h a ve a n y problem , in vo lvin g heat, w e lik e ly can g iv e you some help.

A s makers of Chromel heating-element a llo y s w e ’ll g la d ly help you w ith your electric heating problem s. O r if you need an a llo y to w ithstand heat, w e ’ll tell you about A llo y 502, that is a v a ila b le in cast and hot-rolled form s. . . . If you w ish to m easure temperatures, w e ’ll sh o w you h o w Hoskins Pyrom eters and Chromel Couples can be applied to the job. You are invited to w rite us.

If you are interested in heat resisting castings, w e invite ' you to send for folder, "E V E R Y SH A PE A N D FO RM .”

The Chrome! elements of Hoskins Furnaces are noted for their durabil­

ity. They are hard to w e a r out, but you’ll find them easy to renew.

•

(Right) Hoskins Port­

ab le M eter, with a Chromel couple, is h a n d y fo r " c h e c k ” purposes.

[Left) Hoskins High

Tem perature Com­

bustion Furnace, b e ­ ing used to calib rate platinum couples.

OCTOBER 15,1938 ANALYTICAL EDITION 9

13 Litre Capacity

I N T E R N A T I O N A L E Q U I P M E N T CO.

352 W E S T E R N A V E N U E M a k e r s o f F in e C e n tr ifu g e s B O S T O N , M A S S .

N e w M o d e l

I n t e r n a t io n a l S erum C entrifuge

T h is n ew I n te r n a tio n a l S e r u m C e n tr ifu g e o f 13 litr e ca p a c ity h a s a sp eed o f 2,200 R .P .M . w ith R .C .F . o f 2,100 x g ravity.

T h e n e w d e s ig n e m b o d ie s s e l f c o n ta in e d fe a tu r e b y h a v in g t h e a d ju s ta b le sp eed v ertical m o to r m o u n te d o n s u p p o r tin g fra m e.

T h e drive fr o m th e m o to r to t h e c e n tr ifu g e c o n s is ts o f th r e e vee b e lts an d grooved p u lle y s.

T h e c e n tr ifu g e s h a ft is flexib ly m o u n te d , im p a r tin g a s e lf-b a la n c in g effect to th e r o ta tin g p a r ts, for s m o o th e r r u n n in g .

T h e n e w m o d e l is e q u ip p ed w ith in d ic a tin g ta c h o m e te r a lso v ib r a tio n d a m p en ers u n d er b a se o f th e c e n tr ifu g e .

S p e cia l a llo y c a s t s te e l tr u n n io n cu p s are fu r n ish e d for carryin g 10-1,000 m l. g la ss b o ttle s or m e ta l c o n ta in e r s o f 1.3 litr e c a p a c ity .

T h e r e is a n I n t e r n a ti o n a l f o r a n y j o b

10 INDUSTRIAL AND ENGINEERING CHEMISTRY VOL. 10, NO. 10

A C O M P LE T E A S S O R T M E N T OF

"PYREX"

^{b r a n d}

LABORATORY GLASSWARE

IN OUR STOCK FOR IMMEDIATE SHIPMENT

Of the 235B items of

“ Py r e x”

brand Laboratory Glassware listed in the new catalogue LP-18 (August, 1938) of the Corning Glass Works, 610 are listed in the current 1044-page edition of our catalogue LABORATORY APPARATUS A N D REAGENTS, published in 1931. This was the entire assortment available at that time.

W e n o w m a in t a in , in a d d itio n , c o m p le t e s to c k s o f t h e r e m a in in g 1743 i t e m s lis t e d i n t h e n e w C o r n in g c a ta lo g u e L P -1 8 , fo r im m e d ia t e s h ip m e n t , a t m a k e r ’s c u r r e n t p r ic e s.

Among the more important of the new items listed in this catalogue are the following:

In te r c h a n g e a b le gro u n d jo in t s , c o n n e c tio n s , a d a p ters, sto p p ers, an d sto p c o c k s, o f sta n d a rd ta p er

“ L ife tim e R e d ” G ra d u a ted W are

“ E co n o m y R e d ” H o sp ita l W are C orn in g C ertified V o lu m e tr ic W are F ib rou s G lass (G lass W ool)

M ou ld ed F u n n e ls , 60° a n g le , p la in a n d flu ted M icr o -C h em ic a l W are

The

“ Py r e x”

items not listed in our catalogue can be conveniently ordered of us under the maker’s numbers as printed in the new Corning catalogue LP-18, which is now being distributed directly to consumers by the Corning Glass Works.

The entire assortment of “P Y R E X ” brand Laboratory Glassware is now on permanent display in our sales room.

O u r a vera g e s to c k o f “ P Y R E X ” b r a n d L a b o r a to ry G la ssw a re is over 5000 p a c k a g e s , so t h a t s h ip m e n t o f a n y u su a l a s s o r tm e n t ca n be

m a d e o n th e s a m e d a y o rd e r is received .

AR TH U R H. T H O M A S C O M P A N Y

RETAIL— W HOLESALE— E X PO R T

LA B O R A TO R Y A P PA R A TU S A N D REAG ENTS

W EST W ASH IN G TO N SQUARE P H ILA D E L P H IA , U.S.A.

Cable Address, “ B alance,” Philadelphia

IN D U STR IA L «»a ENGINEERING CHEM ISTRY

ANALYTICAL EDITION ♦ H a r r iso n E . H o w e , E d ito r

Refraction, Dispersion, and Related Properties o f Pure Hydrocarbons

Arranged for U se in the A nalysis o f H ydrocarbon M ixtures 1

A. L . W A R D , T h e U n ite d G a s I m p r o v e m e n t C o ., P h ila d e lp h i a , P a ., A N D S . S . K U R T Z , J R ., T h e S u n O il C o m p a n y , M a r c u s H o o k , P a .

I

N T H E technical analysis of hydrocarbon mixtures and in m ost phases of research on pure hydrocarbons and hydrocarbon mixtures there has long been a well recognized need for concise tables listing sound values for the physical properties of hydrocarbons of the various homologous series and for graphs showing the more im portant relationships th a t m ay be used in the analysis and study of hydrocarbons (25, 41, 66, 87,125, 155,157, 158).

This paper presents a mass of data collected by the authors over a period of years and recently revised and correlated to make the information as useful as possible. The available d a ta for the members of the common hydrocarbon series boil­

ing between 10° and 200° C. or slightly higher have been thoroughly com bed; some data for higher boiling compounds are included, but, in this article, no attem p t has been made to tabulate or evaluate d ata for mixed type hydrocarbons such as those covered by the excellent article of Mikeska {102).

The d ata tabulated are (1) boiling point a t 760 mm. (or 10 m m .); (2) density d?0; refractive index n™; (3) dispersion nF — nc and two derived constants; (4) the refractivity inter­

cept, n — d /2 (88); and (5) the specific dispersion (nF — nc) /d (155). These are first tabulated in detail for ten classes of hydrocarbons; tables containing averaged d ata for specified boiling ranges are then presented, and graphs are drawn based on these averaged properties. A few graphs are also pre­

sented showing the relationship between density and refrac­

tive index for groups of paraffin and olefin isomers.

In the tables the compounds are arranged in the order of their boiling points, and in the graphs the other properties are in general plotted against boiling point, since this arrange­

m ent is especially convenient in analytical and research work w ith hydrocarbon mixtures which are obtained by distillation.

A consideration of the change in density and refractive in­

dex w ith change in tem perature is given and curves are pre­

sented showing the coefficient of cubical expansion as a func­

tion of boiling point and the change in density per degree as a function of density.

I t is also shown th a t the introduction of the K urtz-W ard (88) frequency coefficient into the Sellmeier-Drude equation gives

1 N o r e p rin ts of th is a rtic le h a v e b e en m a d e . T h o se in te re s te d m a y p u rc h a se s e p a ra te copies of th is issu e of th e An a l y t i c a l Ed i t i o n s olong as th e s u p p ly la sts fro m th e B usiness M a n a g e r of th e Am e r i c a n Ch e m i c a l So c i e t y, M ills B ldg., W a sh in g to n , D . C . T h e p ric e is fifty c en ts to n o n ­ m em b ers of th e So c i e t y a n d fo rty cen ts to m em b ers.

an equation th a t accurately expresses the relationship be­

tween refractive index and density in the case of the excellent d ata of Gibson and Kincaid (67) for benzene over the tem pera­

ture range of 25° to 45° C. and the pressure range of 1 to 1200 bars.

T a b u la te d D a ta for th e P h y s ic a l P ro p er ties o f P u re H yd rocarb on s

In Tables I to X are tabulated the properties of some in­

dividual hydrocarbons representing 10 series arranged in the following order:

Noncyclic Paraffins Monoolefins

Nonconjugated diolefins Conjugated diolefins Monocyclic

Naphthenes (saturated) Monoolefins

Conjugated diolefins Aromatics

Polycyclic

Dicyclic saturated Tricyclic saturated

The d ata have been selected from the large mass of d ata in the literature as being the best now available, consideration being given to the reliability of the author and to the relation­

ship between the different physical properties as a function of the constitution of the hydrocarbon.

In a limited number of cases in which there is little to choose between sets of data, two or more sets have been averaged.

In a few cases in which no sound d ata are available, question­

able values have been included and indicated. Except in rare instances, this has been done only in the case of hydrocar­

bons of types for which few data are available. In m ost in­

stances, references to the original literature are given; other­

wise reference is made to one of the recent tabulations.

In preparing these tables it was decided to tabulate boiling points to the nearest 0 C. only and to correct to 760 mm. using the chart of Wilson (169), unless the pressures were very low, in which case they were corrected to 10 mm., using the chart of Nelson (108). Pressures differing by only a few millimeters from 760 were corrected w ith a special large-scale chart de­

rived from Wilson’s equation.

359

560 IN D U ST R IA L A N D E N G IN E E R IN G CHEM ISTRY VOL. 10, NO. 10

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