Industrial and Engineering Chemistry : analytical edition, Vol. 17, No. 5

INDUSTRIAL

AND

ENGINEERING CHEMISTRY

S C I E N C E I S P O W E R

G O O D N U T R I T I O N F O R A M E R I C A

lib,"* rt" 0 . 0 0 0 » n 02 •

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■»¡Bijy* ... o.« ; S " o.«=!

. starts in the laboratory!

Purity d iflnid — not to "moxi- mum limits"— but to ft» dmci- mof by actu al lot an alysis.

That's tho story of tho Bakor's Analyzod label.

Someone has said, "W hat w e eat w e are!” But few real­

ize that good health frequently is charted in the lab­

oratory !

Soils vary in chemical content and so do crops that are grown on them ! The feed intake o f livestock frequently determines the nutrient values o f meat, eggs, m ilk, etc.

Vitam in and mineral fortification o f food has been made possible through laboratory analysis. Laboratory analysis has indicated not only the need for but also the degree of enrichment necessary. Truly, America’s good health

starts in the laboratory.

In the laboratories (product control room s) o f many of the leading food and food processing manufacturers, you w ill find effective tools to measure good nutrition.

¡B a k ers

They are Baker’s Analyzed C.P. Chemicals and Acids.

The reason these Reagents have been selected is unique, for Baker’s Analyzed C.P. Chemicals bear this distinc­

tion. Each bottle has the actual lo t analysis on the label.

T he small percentages o f impurities by lot analysis, as found by Baker’s analysts, are printed on the label.

Chemists w ho work in terms o f third and fourth decimal exactness know the value of the actual analysis rather than a statement o f maximum lim its o f impurities.

So on your next order, be sure to specify Baker’s Ana­

lyzed C.P. Chemicals and Acids. Y our favorite laboratory supply house can supply you.

J. T. Baker Chemical Co., Executive Offices and Plant:

Phillipsburg, N. J.

Branch Offices: New York, Philadelphia and Chicago.

m

n P n H F M I T A I S A N !) AH i n s

F O R R A P I D , A C C U R A T E A N A L Y S E S

F I S H E R

Electro Analyzer

O perates Directly on Alternating

Current

The Fisher Improved Electro Analyzer facilitates the rapid quantitative determination of metallic elements in solutions. It eliminates the need for expensive, cumbersome motor generators and rheostats, since it is a self- contained unit that operates directly from a 110 volt, 60 cycle, A.C. line.

The Fisher Electro A nalyzer will make two similar determinations simultaneously. The voltage and am perage at the electrodes can be varied from zero to 36 watts (a maximum of six volts and six amperes), thus providing ample range to select the optimum current for each particular separation.

This new instrument is also an efficient source of power for electrolytic polishing, charging storage batteries, electroplating and many other applications where direct current within its capacity is required.

The bakelite panel of the Electro A nalyzer is engraved and filled with permanent white.

The sides of the case are also of bakelite to protect it from fumes and spattering.

Fisher Improved Electro Analyzer,

for use with IIO volt, 5 0 - 6 o cycle A . C . , w ithout electro de s or glass stirrer.

Ea ch , $ 1 5 0 .0 0

G / o S S

Stirrer/

for use with E le ctro A n alyze r. Edch, $1.00 (Prices of p latin um e lectrod es on request)

M a n u fa ctu rers— D istrib u to rs

Fisher Scientific Co. ^{q E im e r and Am end}

717 Forbes S t., Pittsburgh (19), Pa. G r e e n w ic h and M o rto n S t r e e t s

2109 Lo cu st S t ., St. Louis (3), Mo. New York (14), New York

H e a d q u a rte rs fo r L a b o ra to ry S u p p lie s

e

F i s h e r El e c t r o An a l y z e r

M E T E R

RIGHT SPINDLE

POWER LEFT

SPINDLE

'»©S'

P O W E R

POWER

HIGH

M O TO R

?oU}

INDUSTRIAL ^{a n d} ENGINEERING CHEMISTRY

A N A L Y T I C A L E D I T I O N

OTEK

W A L T E R J . M U R P H Y , E D IT O R • IS S U E D M A Y 19, 1945 V O L . 17, NO. 5 C O N C E S U T IV E NO. 10 ' O h

Manuscri-pt Editor: G . G l a d y s G o r d o n

R . P . C h a p m a n

J. R . C h u r c h i l l

B. L. C l a r k e

Lawrence T. Hallett, Associate Editor

M anuscript A ssistant: S t e l l a A n d e r s o n

Advisory Board T . R. C u n n i n g h a m

G. E . F. L u n d e l l M . G. M e l l o n

M ake-up Assistant: C h a r l o t t e C . S a y r e

R . H. M ü l l e r

B. L . O s e r

H. H. W i l l a r d

ANALYTICAL CONTROL FOR AM M ONIA S Y N ­ TH ESIS

C on trol R e q u ir e m e n ts in TVA P l a n t ...

Earl H. Brown and M aurice M. Feiger 273 D e te r m in a tio n of O xides of C arbon in H ydrogen-

N itro g en M i x t u r e s ...

Earl H. Brown an d M aurice M. Feiger 277 C o n tin u o u s D e te r m in a tio n o f A m m o n ia A ctivity

in A m m o n ia c a l S o lu tio n s . Earl H. Brown, James E. C line, M aurice M. Feiger, and R. Bowen Howard, Jr. 280 C o n tin u o u s D e te r m in a tio n of C arbon D ioxide by

E le c tr o c o n d u c tiv ity in C o n c e n tr a tio n s Up to 2 Per C en t . Earl H. Brown an d M aurice M. Feiger 283 C o n tin u o u s P h o to m e tr ic D e te r m in a tio n of B i­

v a le n t C opper in A m m o n ia c a l S o lu tio n . . . . Earl H. Brown an d James E. Cline 284 D e te r m in a tio n of A rgon in A m m o n ia -S y n th e sis

G a s e s ... Earl H. Brown an d James E. Cline 286 C o n tin u o u s D e te r m in a tio n of C arbon M onoxide

in C o n c e n tr a tio n s U p to 3.5 Per C en t by E lectr o ­ c o n d u c tiv ity ...Earl H.

Brown, M aurice M. Feiger, an d R. Bowen Howard, Jr. 287

C o n tin u o u s D e te r m in a tio n of M eth y l B rom id e in A t m o s p h e r e ...

Dwight Williams, G eo rg e S. Haines, an d F. D. Heindel 289 D e te r m in a tio n o f Low C o n c e n tr a tio n s of M eth yl

B rom id e in A tm o sp h ere . . . . Dwight Williams 295 D e te r m in a tio n of T o ta l S u lfu r in R u b b e r ...

C. L. Luke 298

L aboratory C orrosion T ests R. M. Burns 299 F actors C a u sin g L u b rica tin g Oil D eterio ra tio n in

E n g in es . . ...

R. E. Burk, E. C. Hughes, W. E. Scovill, an d J. D. Bartleson 302 A n alysis of H yd roflu oric-N itric A cid S ta in le ss S teel

P ic k lin g B a t h ...

W illiam E. McKee an d William F. Hamilton 310 D e te r m in a tio n o f W ater in Dry Food M a teria ls . .

C. M. Johnson 312 D e te r m in a tio n o f W ater in L iq u id P etro leu m F ra c­

t io n s ... O. T. Aepli an d W. S. W. M cCarter 316 F ast G ra tin g S p ectrograp h . A ccessories an d T e c h ­

n iq u e s for S tu d y in g R a m a n E f f e c t ...

Robert F. Stamm 318 A u to m a tic A p p aratu s for E lectr o ly sis a t C on trolled

P o t e n t i a l ...James J. Lingane 332

BOOK R E V I E W ...333 M ICROCH EM ISTRY

M icr o d e term in a tio n o f A cetyl G roups in A ceta tes o f S u g a rs an d G l y c o s i d e s ...

Ray C larke and Bert E. C hristensen 334 R eport of C o m m itte e o n A n a ly sis o f C om m ercial

F a ts a n d O i l s ...

E. W. Blank, E. W. Colt, F. G . Dollear, J. L. Laing, J. Fitelson, C. P. Long, J. E. Maroney, R. T. Milner, L. B. Parsons, H. A. Schuette, S. O. Sorensen, L. M.

Tolman, F. C. Woekel, V. C. M ehlenbacher, C hairm an 336

T h e A m erican C hem ical S ociety assum es no resp o n sib ility fo r th e sta te m e n ts a n d opinions a d v an c e d b y co n trib u to rs to its pu b licatio n s.

32,000 copies of th is issue p rin te d . C o p y rig h t 1945 b y A m erican C hem ical Society.

P u b lish ed b y th e A m erican C hem ical Society a t E a sto n , P a . E d i­

to rial Office: 1155 16th S tree t, N . W ., W ash in g to n 6, D . C .; telephone, R epublic 5301; cable, Jiech em (W ashington). N ew Y o rk E d ito ria l B ran ch : 60 E a s t 42nd St., N ew Y ork 17, N . Y .; telephone, M u rra y H ill 2-4662.

C h icag o E d ito ria l B ra n ch : 310 S o u th M ichigan A venue, C hicago 4, 111.;

telephone, W ab ash 7376. B usiness Office: A m erican C hem ical Society, 1155 16th S tree t, N . W ., W ash in g to n 6, D . C. A d v ertisin g Office: 332 W est 42 n d S tree t, N ew Y o rk 18, N . Y .; telephone, B ry a n t 9-4430.

E n te re d as second-class m a tte r a t th e P o st Office a t E a sto n , P a., u n d e r th e A ct of M arch 3, 1879, as 24 tim es a y e ar— In d u s tria l E d itio n m o n th ly on th e 1st, A n aly tical E d itio n m o n th ly on th e 15th. A cceptance for m ailing a t special r a te of postage p rovided fo r in Section 1103, A c t of O ctober 3, 1917, au th o riz e d Ju ly 13, 1918.

R em itta n ce s an d orders fo r s u b scrip tio n s a n d fo r single copies, notices of changes of ad d ress a n d new professional connections, a n d claim s fo r m issing num bers should be se n t to th e A m erican C hem ical Society, 1155 16th Street, N. W ., W ash in g to n 6, D . C. C hanges of ad d ress for th e In d u s tria l E d itio n

m u st be received on or before th e 18th of th e preceding m o n th an d fo r th e A n aly tical E d itio n n o t la te r th a n th e 3 0 th of th e preceding m o n th . Claim s fo r m issing n u m b ers will n o t be allow ed (1) if received m ore th a n 60 days from d a te of issue (owing to th e h azard s of w artim e d elivery, no claim s can be honored fro m su b scrib ers o u tsid e of N o rth A m erica), (2) if loss was d ue to failu re of n o tice of change of ad d ress to be received before th e d a te s specified in th e preceding sentence, or (3) if th e reaso n fo r claim is "m issing from files".

A n n u al su b scrip tio n — In d u s tria l E d itio n a n d A n a ly tic al E d itio n sold only as a u n it, m em bers $3.00, n onm em bers $4.00. P o stag e to co u n tries n o t in th e P an -A m erican U nion $2.25; C an a d ia n po stag e $0.75. Single copies—

c u rre n t issues, In d u s tria l E d itio n $0.75, A n aly tical E d itio n $0.50; b ack nu m b ers, In d u s tria l E d itio n $0.80, A n a ly tic al E d itio n prices on re q u e st;

special ra te s to m em bers.

T h e A m erican C hem ical Society also publishes Chemical and Engineering News, Chemical Abstracts, an d Jo u rn a l o f the A m erican Chemical Society.

R ates on req u est.

Each tim e you see the Harshaw trademark, whether on tank car, package or small laboratory bottle, remember it identifies chemicals that will help to do a better job . . . truly reflecting the integrity of the maker. • Harshaw will always guard the quality o f its chem icals. . . chemicals which you identify by the Harshaw trademark . . . and which you buy with confidence.

For more than 50 years Harshaw has persevered in ceaseless research and field investigation. As a result, thousands o f manufacturers have been supp lied w ith hundreds o f different chem icals w hich have helped th em . . . and w hich in addition have proved a source o f satisfaction to them and to us.

P, 2 > Vi ¡ S 3

the H A R S H A W C H E M I C A L - •

1945 East 97th Street, C le ve la n d 6, O h io

B R A N C H E S I N P R I N C I P A L C I T I E S

May, 1945 A N A L Y T I C A L E D I T I O N 5

On Sentry Duty

★ A heavily armed soldier guards a ship­

ment of food for the hungry m illions of devastated Europe . . .

★ A laboratory technician guards the qual­

ity of foods being processed.

Both performing vital functions, both using the finest o f equipment—equip­

ment such as the Spencer Refractometer w h ich is a standard laboratory control instrument of canners, dairymen, oleo­

margarine producers and others. Through­

out these industries the refractometer is used to determine sugar content or total dissolved solids—to determine the times

when condensation or hydrogenation S C I E N T I F I C I N S T R U M E N T D I V I S I O N O F A M E R I C A N O P T I C A L C O M P A N Y or other processes have progressed to the proper point.

For complete information about the many Spencer instruments w hich can help you m aintain the quality o f your product w rite Dept. P48.

encer

L E N S C O M P A N Y B U F F A L O , N E W Y O R K

6 I N D U S T R I A L A N D E N G I N E E R I N G C H E M I S T R Y Vol. 17, No. 5

This n e w com pact filter photom eter em b od ies the most recen t im provem ents in d esig n for efficien cy, sensitiveness, attractiveness, and econom y. Its use in the control or clin ica l laboratory for ch em ical analyses offers m any advantages. W here sp eed , accu racy, and freedom from "hum an elem ent" errors are desirable, the

"Photelometer" m ethod of determ ining concentrations of colored solutions is rapidly rep lacin g older, slow er m ethods. R eadings are now b ein g applied to d e ­ term inations su ch as m olybdenum , titanium, vanadium , or m anganese in steel;

for lead, copper, iron or vitam ins in foods; for hem oglobin and blood chemistry;

and m any other colorim etric procedures.

The N ew "Photelometer" is a barrier-layer type instrument consisting of basically a low voltage ligh t source, an adjustable ligh t aperture, a three-color filter holder, recep ta cles for tubular or rectangular absorption cells, a sin gle photoelectric cell, and a sensitive current-m easuring instrument with a 2 ^ -in c h scale. The scale reads from 0 -1 0 0 in 50 divisions.

The b asic parts are m ounted in an attractive plastic ca se m easuring 4% in ch es h ig h by 10% in c h e s lo n g by 4 in ch es w ide. The 115-volt A C instrum ents are eq u ip p ed with constant voltage transformers to supply constant intensity of light w h en operated on a controlled freq u en cy pow er lin e.

No. 12346 "Photelometer" Industrial Type B -2 Including a p ackage of (1 2 ) No. 12344G C ells and blue, green, and red filters:

No... A C For v o l t s ...1 1 5 AC 6 0 cy cles 6 DC P r i c e ... S 1 1 0 .0 0 $ 1 0 0 0 0

CENCO "PHOTELOMETER" In d u s tria l T y p e B-2

CENTRAL SCIENTIFIC COMPANY

SCIEN TIFIC IN STRU M EN TS L A B O R A T O R Y A P P A R A T U S

REG U S PAT 0»

NEW YORK TORONTO CHICAGO BOSTON SAN FRANCISCO

May, 1945 A N A L Y T I C A L E D I T I O N

R i g i d l y controlled particle size is one of the factors which make Isocel a more acceptable catalyst than plain aluminum chloride. The bauxite used in Isocel as the carrier for aluminum chloride is prepared to uniform particle size, and control is maintained throughout the manufac­

ture of Isocel. The aluminum chloride is thus pre­

sented in a lower concentration per unit of reac­

tant space, yet uniformly dispersed. Isocel may be used with very sensitive or very active com­

pounds, where reaction with finely powdered A IC I3 is too rapid or severe, and in processes where lump A IC I3 produces complications.

An important use of Isocel today is the con­

version of normal butane to isobutane for the enrichment of akylation feed stocks deficient in isobutane. Its value as an isomerization catalyst in refinery operations has been amply proved.

Other reactions are constantly being studied.

In many of them, the use of Isocel as a catalyst has unmistakable advantages, and it is safer to handle and less corrosive.

ISOCEL

has a potential application in e ve ry fie ld in w hich alum inum chloride is used as a catalyst. These seven fields are typical:

1. Reaction of organic halides with aromatic hydro­

carbons.

2. Reaction of anhydrides of organic acids with aro­

matic hydrocarbons.

3. Reaction of oxygen, sulfur and sulfur dioxide with aromatic hydrocarbons.

4. Cracking of aliphatic and aromatic hydrocarbons.

5. Polymerization of unsaturated hydrocarbons.

6. Alkylation of aromatic hydrocarbons.

7. Isomerization of aliphatic hydrocarbons.

Our well-staffed laboratory and experienced engineers are availab le to help solve your special catalytic problems. W h y not enlist their aid? There is no obligation. W rite Attapulgus C lay Company (Sales Agent), 260 South Broad Street, Philadelphia 1, Pennsylvania.

P O R O C EL C O R P O R A T I O N • B A U X I T E A D S O R B E N T S A N D C A T A L Y S T S

8 I N D U S T R I A L A N D E N G I N E E R I N G C H E M I S T R Y Vol. 17, No. 5

tecuian, • • • w it h p r o v is io n

T h e G -E X R D B a c k R e fle c t io n C a m e r a Fo r X - R a y D if f r a c t io n T e c h n ic s

W hen x-ray diffraction technics call for precision lattice parameter determination, here is a proved and invaluable instrument. The G-E X R D Back Reflection Camera incorporates ideally precise execution o f the basic Sachs design . . . with provision for: oscil­

lation and rotation o f the film ; eccentrically rotating the sample to permit integration o f an area; assem bling the camera for symmetrical focusing technics for minimum exposure. For full information about G-E X-Ray diffraction equipment for precision research and control— or to request the services o f G-E’s corps o f experienced diffraction engineers in helping you apply x-ray diffraction to your individual problems — write or wire today, to Department N45.

☆ ☆ ☆

GENERAL (g) ELECTRIC X -R A Y CO RPO RATIO N

2012 JA C K S O N B L V D . CHICAGO (12). ILL./ U. S. A.

V Ï8 9 S [ O U R F I F T I E T H Y E A R O F S E R V I C E ! 1945 /

May, 1945 A N A L Y T I C A L E D I T I O N 9

awaWr.i. t

L U S O R B E N T F O R IL L U M IN A N T S

Absorbs all the gases in the illuminants group, i.e ., ethylene, propylene, butylene, acetylene, benzene and toluene. Requires fewer passes than fuming sulfuric acid, has no vapor pressure, absorbs less saturated hydro­

carbons and does not attack rubber tubing.

C O S O R B E N T F O R C A R B O N M O N O X ID E

Supplied in either liquid or powder form. Has no vapor tension, forms stable compound w ith carbon monoxide, is fast and active. Absorbs ethylene, propylene and acety­

lene, also oxygen slow ly.

Complete information on reagents for gas analysis is given in the new Burrell Catalog 80. If you have not already received your copy, w rite to Jkirrell Tech­

nical Supply C o., 1936-42 Fifth A ve., Pittsburgh 19, Pa.

LUSO RBEN T r« um «dominantst J

AA9-7 l ?

-* «-(if!**,«, r-rui.-“»"

,

B U R » * I

SPEED YOUR GAS AN ALYSIS WITH THESE REAGENTS

«OSORBEW*

U Q U lD r o p M it * A im » ptiofl ° i

V, C^N<..A3»7Z£I V

wtumled ^

b u r r e l i

co*T>

W ,CAl 5UPP17 *

av.. .

JBtBBtti j

° * S O »b eNT

«0*^ combined catalog a n d m a n u a l describes the la te s t equipm ent a n d

methods fo r g a s a n a ly sis.

O X S O R B E N T F O R O X Y G E N

Fast, clean and accurate, removes oxygen in a few passes and forms a stable compound w ith it. Absorbs four times its volume of oxygen. Rises cleanly in the capillary and is slig h tly acid — preventing sticking stopcocks.

BURRELL

. ..

__

10 I N D U S T R I A L A N D E N G I N E E R I N G C H E M I S T R Y Vol. 17, No. 5

* )m fr u H A e d

PALO-MYERS WATER STILLS

Other Palo-Myers apparatus available:

Partical size measuring apparatus pH equipment

Chemicals and solutions for ASTM, AOAC, and APHA analyses

Pumps—vacuum Thermometers Stirrers Ovens

Electrolytic apparatus Automatic burettes

Assure Chemically Pure W ater...

Available for ^{e a r l y} d e l i v e r y

Preference for Palo-Myers Water Stills is recognition of the fact that more and more careful consideration is being given today by chemists to the need for chemically pure water.

Basic improvements in design and op­

eration achieved in Palo-Myers Water Stills include—

• V E R TIC A L C O N D E N S ER . . . assures greater stability, easy release o f gases and elim ination o f progens.

• ECONOMY . . . is effected by the most efficient m ethod o f heat exchange be­

cause the water enters at the lowest and hottest point o f condenser.

• MULTIPLE BAFFLES . .. designed to pre­

vent foam ing and im purities entering condenser.

• EASIER TO MOUNT . .. due to compact construction, requires lim ited amount of space or can be supported on w all bracket.

Regular sizes Vi to 10 Gallons per hour

—Stills 100 Gallons per hour if desired.

I n q u i r i e s i n v i t e d — s t a t e c a p a c i t y r e ­ q u ir e d p e r h o u r a n d m e th o d o f h e a tin g .

CAPACITY PRICES

G. P. HR. GAS ELECTRIC STEAM

Vi $49.50 $56.00

^{$ . . . .}

1 64.00 75.00 65.00 2 95.00 110.00 95,00 5 170.00 270.00 150.00 10 360.00 540.00 210.00

P rices s u b je c t to c h a n g e

I “P A f â -M Y E R S inc.

S I READE STREET, NEW YORK 7, N. Y.

May, 1945 A N A L Y T I C A L E D I T I O N 11

T h e V i s i b l e G u a r a n t e e o f I n v i s i b l e Q u a l i t y

KIMBLE GLASS COMPANY • .

NE W YORK • C H I C A G O • P H I L A D E L P H I A • D E T R O I T • 8 0 S T 0 N

• V I N E L A N D , N. J.

I N D I A N A P O L I S • S A N F R A N C I S C O

12 I N D U S T R I A L A N D E N G I N E E R I N G C H E M I S T R Y Vol. 17, No. 5

D eterm ination o f com parative m elting points in th e M erck Research Laboratories.

F ine chem icals for th e professions and industry since 1818.

MERCK has

THE RIGHT COMBINATION

for Laboratory Chemicals

r — M E R C K & CO., In c . f^/iianu^actuK in^ <&Aemi6U R A H W A Y , N. J . - ~ >

I In d . Eng. C hem .— 5-15-45

Please send m e th e following ch arts: N a m e ... I

I

□ S ensitivity of Q u alitativ e R eactions C o m p an y ... - ...P o sitio n ...

□ Periodic C h art of th e E lem ents S t r e e t... I

□ S ensitivity C h a rt C it y ...S ta t e ...

!

A corner o f th e M erck Packaging Laboratory. Stock points strategically located from coast to coast.

May, 1945 A N A L Y T I C A L E D I T I O N

It M es fears to Make a

ss Blower

T here is no short course in glass b lo w in g . Y ou learn the lo n g , hard way. For glass b lo w in g is an art w h ich requires sp ecial aptitude. In the past its secrets w ere handed d ow n from father to son. Even today there are w h o le fam ilies o f glass b low ers at C orning.

A ll o f w h ich explains h o w a war can affect a lam p shop. M en and w om en can be taught to operate autom atic m achines— even lathes— overnight. But you cannot train a lam p sh op craftsman in a day, a m onth or even a year.

W ar has made severe inroads o n our lam p sh op s w here the hand fabrication o f laboratory glassw are is perform ed. W e ll over tw enty per cent o f C o m in g ’s glass b low ers are in military service. Few could be replaced.

H ow ever, despite such handicaps, lam p sh op output has actually increased several fold . By w o rk in g m ore shifts and lo n g er hours, by adding new facilities and d evisin g n ew ways o f sp eed in g production as m uch as is p o ssib le on hand w ork , the dem ands o f the Arm ed Forces and war industries are b ein g met.

Soon, heavy war dem ands may ease. T h en , w ill you no lo n g er have to wait, but also your requests for special apparatus can be m et prom ptly. A nd to all this w ork, C orning can bring the n ew sk ill, the new techniques and the advanced m ethods, war production has added to C orning R esearch in Glass.

“ P yrex,” “ V ycor” a n d “ C om ing” are registered trade-m arks a n d indicate m anufacture by C O R N I N G G L A S S W O R K S . C O R N I N G , N E W Y O R K

■ % j r

P V R c X

B A L A N C E D F O R A L L - A R O U N D US E

brand LASORA TORY GLASSWARE

I N D U S T R I A L A N D E N G I N E E R I N G C H E M I S T R Y Vol. 17, No. 5

Type MU-86 Crucible Furnace.

Multiple Unit Laboratory Furnaces are stan­

dard in most laboratories. In m any cases, however, they are the active apparatus in industrial research program s being carried on in the search for better materials and improved processes. A case in point is the use of an M U -8 6 Crucible Furnace by H. P. Burchfield in his research on “ Iden­

tification of Natural and Synthetic Rubbers.”

(*lnd. & Eng. Chem. Anly. 16,424,1944.)

S ee. 'Ifo u l JlaluvuU osuf. S u p fiiif. 2)ecU eA.

ie * u l jjO-'i B u ile tU t - 6 3 9

U T Y E L E C T R I C C O M P A N Y

Î R A O C M A R K

LABORATORY FURNACES

MULTIPLE UNIT

ELECTRIC EXCLUSIVELY

REG. U. S. PAT. OFF.

M I L W A U K E E . W I S C O N S I N

May, 1945 A N A L Y T I C A L E D I T I O N 15

EE

D O W C O R N I N G

S I L I C O N E S

D OW CORNING, first in silicones,

is fully equipped with new plant and facilities for

the production and distribution o f an expanding line o f silicone products

American industry has been quick to utilize the new Dow Corning Silicones—to see the potentialities inherent in their higher order of heat stability, chemical inertness, water resistance, and dielectric properties. Dow Corning is now supplying, directly or through selected distributors, the following silicone products:

0 Water-white, odorless, inert

FLUIDS Silicone Liquids . . . notable for their low rate of viscosity change over a wide tempera­

ture range, low vapor pressure, water repellency, and good dielectric properties.

0 Ignition Sealing Compound

4 easily applied silicone waterproofing ^{. an} compound having excellent dielectric properties, corona resistance, and the consistency of petroleum jelly. It neither hardens nor melts at temperatures ranging from — 40° F.

to 400° F.

0 Special Low Temperature Compound y . . . an oxidation resistant lubricant and sealing compound developed for use at temperatures as low as — 70° F.

E E A lubricating Silicone Grease for

31 special applications in the tempera­

ture range of —70° F. to 190° F.

E E A lubricating Silicone Grease ^for

4 | special applications where operat ing temperatures range from 0° F to 400° F.

D O W C O R N I N G C O R P O R A T I O N M I D L A N D , M I C H I G A N

A D D R E S S A L L I N Q U I R I E S T O B O X 5 9 2

-

Insulating Varnish . . . recom­

mended because of its extreme heat stability for impregnat­

ing, coating and bonding, and waterproofing inorganic insulating materials such as asbestos, mica, and Fiberglas cloth, tape, and sleeving. Other special purpose silicone resins and compounds are available.

D C STOPCOCK GREASE

A chem ically resistant Silicone G rease for lubricating stopcocks and other ground glass joints.

E E PLUG COCK GREASE

A Silicone Grease that affords easy operation of lubricated plug valves over wide temperature ranges in most diffi­

cult services.

16 I N D U S T R I A L A N D E N G I N E E R I N G C H E M I S T R Y Vol. 17, No. 5

H O S K IN S PRODUCTS

E L E C T R I C H E A T T R E A T I N G F U R N A C E S • • H E A T IN G E L E M E N T A L L O Y S • • T H E R M O C O U P L E A N D LEA D W IR E • • PY R O M ETER S • • W E L D IN G W IR E • • H EA T R E S IS T A N T C A S T IN G S • • E N A M E LIN G FIX TU R E S • • S P A R K PLU G E LE C TR O D E W IR E • • S P E C IA L A L L O Y S O F N IC K E L • • » R O T E C T IO N TUBES \

# The heating coil in this FH combustion furnace is made of 7 G auge (.144") Chrom el-A wire. That is to say, the unit is very heavy and is made of the most durable of the Nickel-Chrom ium alloys. In use, Chromel takes on a thin skin of oxide, which clings tenaciously to the metal, is virtually air tight— and thus acts as a protective coating for the w ire against progressive oxidation. We make the wire and we make the furnace. They belong together— as a good team. A faithful com­

bination that results in a Hoskins Com­

bustion Furnace, that is more or less the

standard, the world around. Write to your

dealer or to u s . . . . Hoskins M anufacturing

Com pany, Detroit 8, M ichigan.

May, 1945 A N A L Y T I C A L E D I T I O N 17

No. 2060 G ra tin g Spectrograph

F o r unexcelled sp e c tru m p h o to g ra p h y — av ailab le w ith e ith e r a 24,400 o r a 36,600 line p er inch original concave g ra tin g giving a lin ear dispersion o f 6.95 and 4.64 A p e r m m in th e first o rd e r a n d 3.48 an d 2.32 A p e r m m in th e second order resp ectiv ely .

No. 2050 M ultisource U nit

F o r exciting th e sp e c tra o f sam ples a n d pro­

v id in g in one u n it an d in a su p erio r m an n er, a v irtu a lly infinite v a rie ty o f co n tro lled ty p es o f e x c ita tio n ; ran g in g from th e e q u iv a le n t ex c ita tio n o f a high v o ltag e s p a rk , a high v o ltag e A .C . a rc o r a D .C . arc a n d all in te r­

m e d ia te cases.

No. 2380 M otor Driven Electrode C u tte r and Saw F o r m ach in in g c arb o n elec tro d e tip s to specific shapes.

No. 3500 B riq u e ttin g Press F o r b r i q u e t t i n g b o r i n g s a n d m illed chips o f m e tallic m a te ria ls a n d p o w d e r s o f n o n - m e ta l li c m a te ria ls in to specim ens s u it­

able for sp ectro g rap h ic analysis.

No. 2300 Developing M achine (above)

F o r ra p id a n d c o n siste n t film a n d p la te processing p ro v id ed b y a g ita tio n an d a c c u ra te te m ­ p e ra tu re control.

No. 2397 M icro-Pipette (righ t)

F o r c o n v e n ie n tly a n d accur­

a te ly m easu rin g sm all q u a n ­ titie s o f solutions.

No. 2351 Plate Dryer F o r im m e d ia te d ry in g o f p la te s in from one to tw o m in u te s. F ilm D ry e r also available.

No. 2250 Com parator-D ensitom eter

F o r c o n v en ie n t w av elen g th a n d d e n sity m easu re m e n ts—

av ailab le for e ith e r film o r p la te sp ectro g ram s— w ide range o f m a s te r p la te s also av ailab le.

No. 2375 C a lcu la tin g Board (right)

F o r th e d ire c t read in g o f sam ple com position from the tran sm issio n read in g s o b ta in e d from th e C o m p a ra to r- D en sito m eter.

T h e above spectrographic u n its a re b u t a few o f th e m a n y pieces o f “ m a te d ” e q u ip m e n t offered by A R L - D I E T E R T . T h e s e a c c e s ­ sories w o rk v e ry well n o t on ly w ith A R L - D I E T E R T S p ectro ­ g ra p h s, b u t also w ith sp e c tro ­ g ra p h s o f o th e r m ak es an d ty p es.

W h e th e r a m o to r g e n e ra to r s e t is needed, a sp e c tro g ra p h for pre­

cise an aly sis, o r j u s t a few feet o f g ra p h ite electrodes, A R L -D IE ­ T E R T is p re p a re d to ta k e care o f y o u r sp ectro g rap h ic needs or p r o b l e m s in a n e f f i c i e n t a n d p ro m p t m an n er.

A.R.L. * DIETERT

A P P L I E D R E S E A R C H L A B O R A T O R I E S 4336 SAN FERNANDO RD., GLENDALE 4, CALIF.

H A R R Y W. D I E T E R T C O . 9330 ROSELAWN AVE., DETROIT 4, MICH.

18 I N D U S T R I A L A N D E N G I N E E R I N G C H E M I S T R Y Vol. 17, No. 5

A .H .T . CO. S P E C IF IC A T IO N

MICRO ELECTROLYTIC O U TFIT

BASED ON CLARKE-HERM ANCE ELEC TR O LYTIC CELL

4786-K .

C la rk e -H erm a n ce M icro Electrolytic O utfit

4786-L.

C la rk e -H erm a n ce M icro E lectrolytic Cell

A. O u ter Vessel E . T h erm o m eter B. G lass F ram e F . In n e r E lectrode C. P um ping T u b e G. O u te r E lectrode D. R insing T u b e

M ICRO ELECTROLYTIC OUTFIT, CLARKE-HERM ANCE, A.H .T. Co. Specification. For the identification, separation and determ ination of sm all quantities of m etallic ions in liquid samples.

T ests can be m ade w ith 4 to 5 m l of electrolyte, all of which can be forced betw een the electrodes several tim es each m inute w ithout causing excessive spraying. See B everly L. Clarke and H . W. Hermance, The Jo u rn a l o f the A m erican Chemical Society, Vol. o f, N o . 3 {M arch, 1932), pp. 877-885; and Em ich- Schneider, M icrochem ical Laboratory M a n u a l, E nglish E d. {1932), p. 152.

E lectrolytic Cell A is w ater jacketed, w ith stopcock a t b ottom which facilitates draining th e cell an d washing the electrodes in situ. Jack et is supplied w ith flattened arm for heating th e cell by a micro bu rn er; w ater jack e t is 50 m m outside diam eter; electrode com partm ent is 90 mm deep X 21 m m inside diam eter.

Glass F ram e B consists of superim posed and con­

centric glass tu b es w ith cage-like lower section. In use th e inner electrode fits inside th e rods, resting on th e flared base of th e lower tu b e; th e o u ter electrode

fits outside th e rods, resting on sm all lugs attach ed to th e rods.

Com plete outfit as shown in illustration consists of:

E lectrolytic Cell complete w ith therm om eter 0 to 110° C in 2° divisions, inner an d o u ter platinum electrodes and rinsing tu b e D ; S upport w ith base of Coors porcelain and rod of alum inum alloy; E lectrode Clam p w ith binding posts and holder; Spring-G rip Clam p for th e Cell, w ith holder;

Micro B urner w ith needle valve a d ju stm en t; and Power U n it com plete w ith connecting leads.

4786-K . M icro E lectro ly tic O utfit, C la rk e -H e rm a n c e , A .H .T . Co. Specification, com plete o u tfit as show n in illu stra tio n , for use on 115 v o lts, a.c., b u t w ith o u t ru b b e r tu b in g co n n ectio n fo r B u rn er a n d P u m p in g T u b e ... 122.75 4786-L. M icro E lectro ly tic Cell, C la rk e -H erm a n ce , of P y rex glass, co nsisting of Vessel A, glass fram e B, p u m p in g tu b e C, rinsing tu b e D , th e r­

m o m eter E , 0 to 110° C in 2° divisions, a n d in n e r a n d o u te r p la tin u m electrodes F a n d G ; w ith o u t electrode clam p or connecting

le a d s ... 41.25

4785-N . P o w e r U nit, in v e n tila te d sh ee t m etal case 12 X 7 X 6 inches, co n tain in g d ry disc rectifier, v a ria b le tra n sfo rm e r for delivering stepless d.c. up to 5 am peres, v o ltm e te r 0 to 10 v olts, a m m e ter 0 to 5 am peres, e x tra safety fuse a n d sw itch for chan g in g p o la rity of elec­

tro d e s 70.00

M o r e d e t a i l e d i n f o r m a t i o n s e n t u p o n r e q u e s t .

ARTHUR H. T H O M A S COMPANY

R E T A IL — W H O L E S A L E — E X P O R T

LABO RATO RY APPARATUS AND REAGENTS

W E S T W A S H IN G T O N S Q U A R E , P H IL A D E L P H IA 5, U .S.A . Cable Address “ B alance,” Philadelphia

INDUSTRIAL ^{a n d} EN G IN EERIN G CHEM ISTRY

P U B L I S H E D BY

T H E A M E R I C A N C H E M I C A L S O C I E T Y W A L T E R J. M U R P H Y ,

E D I T O R

A N A L Y T I C A L C O N T R O L F O R A M M O N I A S Y N T H E S IS

k i O D E R N industry often autom atically records pH, temperature, pressure, etc., for reasons of plant efficiency, and analysis of individual spot samples is com m only used in the control of an industrial process.

Where process materials are gaseous or liquid, methods o f continuous analysis are often possible, though these have not received the attention their importance ju sti­

fies. Individual papers involving continuous analysis do not permit the analyst to include details which would enable readers to appreciate the over-all advantages and the lim itations o f continuous analysis.

It is for this reason that we take particular pleasure in publishing the following seven articles on “A nalyti­

cal Control for Ammonia Synthesis”, prepared by Earl H . Brown and co-workers a t Tennessee Valley A uthority, W ilson D am , Ala. In these we have an ex­

cellent representation o f developm ent and application in this type of analysis for control of an im portant in­

dustrial process.

Further, to illustrate the conventional approach of the analyst in the determ ination of a specific compound and the compromises needed to develop a procedure for continuous recording, two articles on determining m ethyl bromide in air follow im m ediately after the group of seven.

L. T. Ha l l e t t, Associate Editor

Control Requirements in the T V A Plant

E A R L H . B R O W N a n d M A U R IC E M. F E L G E R 1

The analytical control requirements for the T V A synthetic ammonia plant are given. A description of the control laboratory and a flow sheet of the process showing the sample points are also included, with a table describing the samples analyzed, constituents deter­

mined, methods used, and frequency of determinations.

T

H E R E has been a trem endous expansion in th e production of synthetic am m onia since th e outb reak of W orld W ar II.

T he synthetic am m onia p lan t of th e Tennessee Valley A uthority a t Wilson D am , Ala., one of th e plants constructed since the be­

ginning of th e war, w ent into full production in Septem ber 1942.

Miller and Junkins (f) have described th e m odern pressure- synthesis process employed an d m entioned some of the methods developed for process control.

T he successful operation of this process depends upon the m aintenance of close, reliable analytical control. T his paper de­

scribes the control laboratory and th e analytical requirem ents for process control, while subsequent papers in th is series describe m ethods and instrum ents for continuous analysis w hich h ave been developed by the TVA.

1 P re s e n t ad d ress, W orks L a b o ra to ry , G en eral E lec tric C o., F o r t W ayne, In d .

D ESCRIPTIO N O F C O N T R O L L A B O R A T O R Y

T he central control la b o rato ry is a glass-walled room, 16 feet wide and 60 feet long, inside th e m ain building, and is readily accessible to th e p lan t operators. Samples for th e more im por­

ta n t determ inations are brought directly to th e lab o rato ry by sam ple lines. T here is a sm all lab o rato ry in th e gas p la n t in which analyses for th e control of sem i-w ater gas production are made.

Efficiency and convenience were em phasized in th e lay o u t and equipm ent of th e laboratory in order to give th e m axim um use of th e ra th e r lim ited space available. T h e th erm al conductivity cabinets an d electroconductom etric analyzers occupy about one th ird of th e laboratory. One technician per shift operates and services these units. All analyses of th e copper solution are m ade a t a separate bench, and another bench is used for th e preparation of reagents and for miscellaneous analyses. A bank 273

274 I N D U S T R I A L A N D E N G I N E E R I N G C H E M I S T R Y Vol. 17, No. 5

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of three O rsat analyzers is located along one wall near th e outlets of th e sam ple lines. A bench w ith glass-blowing equipm ent is provided for the emergency repair of glass ap p aratu s during pe­

riods when th is regular service is n o t available.

A small storeroom in th e basem ent below the laboratory serves the im m ediate needs for chemi­

cals and apparatus.

P L A N T A N A L Y T I C A L REQ U IREM EN TS

In th e TVA am m onia p lan t th e synthesis mix­

tu re is derived from sem i-w ater gas by catalytic oxidation of m ost of th e carbon monoxide w ith steam , and subsequent purification of th e hydrogen- nitrogen m ixture. In th e purification process the concentration of carbon dioxide is reduced to about 0.7% by scrubbing w ith w ater a t 17 atm os­

pheres’ pressure. T he residual carbon monoxide and carbon dioxide are rem oved by scrubbing w ith cold am m oniacal copper solution a t 121 atm ospheres. T he am m oniacal copper solution contains cupric ammino, cuprous ammino, am­

m onium , form ate, an d carbonate ions, and un­

combined amm onia. T he gas next passes through th e caustic scrubbers where any rem aining traces of carbon dioxide can be rem oved by scrubbing w ith sodium hydroxide solution. A ctually, ow­

ing to th e high efficiency of carbon dioxide rem oval in th e w ater and copper scrubbers, th e caustic scrubbers have not been operated. T he purified hydrogen-nitrogen m ixture is fed into th e cir­

culating gases of th e synthesis system a t a rate sufficient to replace th e gas rem oved as am m onia an d th a t discarded to control th e concentration of inert gases.

T h e laboratory supplies analytical d a ta for th e control of: (1) th e quality of the raw gas and of th e finished product, (2) th e steam -gas and hy­

drogen-nitrogen ratios, (3) th e conversion in th e w ater gas and synthesis converters, (4) th e puri­

fication of th e hydrogen-nitrogen m ixture, and (5) th e regeneration of th e solution used for absorb­

ing hydrogen sulfide from th e sem i-w ater gas and of th e copper solution used in th e final rem oval of oxides of carbon from th e synthesis m ixture.

A sum m ary of th e p lan t analytical require­

m ents for th e control of these factors follows.

T he num bers given in parentheses refer to th e sam ple point designations shown in Figure 1. T he sam ple points on tra in 1 have odd num bers while those on tra in 2 h ave even num bers, b u t this system does n o t apply w here th e sam ple point is common to th e tw o train s comprising the TVA p lan t. Sam ple p o in t designations, as well as th e constituents determ ined an d th e methods

used, are given in T able I. T he de- t e r m i n a t i o n s m arked by an as­

terisk are m ade by special m ethods de­

veloped in th e TVA r e s e a r c h l a b o r a ­ tories; these new developments are described in sub­

sequent papers.

t t

I i m u

May, 1945 A N A L Y T I C A L E D I T I O N 275

Sam ple P o in t N o.

Gas P la n t GS-1, 2, 3, 4

GS-5GS-6

GS-7 GS-8

GS-9 GS-10 GS-11 GS-12 GS-13

G S-14, 15, 16, 17 D -5

D -6 D -8A B H y d ro g e n S ection

H S-1, 2, 3, 4 H S-5, 6, 7, 8

Table I. Sample Points and Analyses for Control of the Ammonia-Synthesis Process

S am ple

C o n stitu e n ts

D e term in e d M eth o d F req u e n c y of

D e te rm in a tio n

R aw gas fro m g en erato rs G as fro m blow ru n

R aw gas to so d a ash s cru b b er R aw gas fro m so d a ash s cru b b er Soda a sh so lu tio n to actifiers Soda ash so lu tio n fro m actifiers

R aw gas in h o ld er

R aw gas fro m ho ld er, before blow gas a d d itio n B low gas in h older

B low gas fro m h older B oiler feed w a ter B la st gas fro m sta c k R aw gas to coke filter R aw gas fro m coke filter R aw gas, e x it R o o ts blow ers R aw gas to p rim a ry c o n v erte rs C o n v erte d gas fro m sec o n d a ry co n v erters

H S-9, 10 R aw gas fro m s a tu r a t o r tow ers H S-11, 12, 13, 14 G as from p rim a ry co n v erters

H S-15 R aw gas to s a tu r a to r , a fte r blow gas a d d itio n H S-16

H S-17 C o n v erte d gas in h older C o n v erte d gas to com pressors

P u rific a tio n Section PS -11, 12 PS -13, 14 PS -15, 16 PS -17, 18 PS -19 S y n th esis S y stem

SS-19, 20

C o n v erte d gas to w a te r scru b b ers G as fro m w a ter scru b b ers G as fro m co p p er scru b b ers G as from c au stic scru b b ers V en t gas fro m b reak d o w n ta n k M ak e -u p gas to s y n th esis

SS-21, 22

SS-23, 24 SS-25, 26

SS-27, 28 SS-29, 30

SS-31 SS-32, 33 SS-34, 35

G as to am m o n ia c o n v erte rs

G as fro m a m m o n ia c o n v erte rs G as a t c irc u la to rs

G as to am m onia-cooled condenser B leeder gas

P u rg e gas fro m degasifier

A n h y d ro u s am m o n ia, w ater-cooled condenser A n h y d ro u s a m m o n ia, am m onia-cooled condenser SS-36, 37 A n h y d ro u s a m m o n ia fro m weigh ta n k s SS-38 V en t gas fro m a b so rp tio n to w er

SS-39 A q u a a m m o n ia

C o p p er S o lution S y stem ĆS-1

C S-2W C S-3S C S-4S C S-5S C S-6S C S-7S C S-8S C S-9S C S-10 CS-11

C o p p er so lu tio n a t H .P . p u m p su ctio n

E x it co p p er s cru b b er B ase of reflux to w er 1st p re h e a te r, reflux to w er 2 n d p re h e a te r, reflux to w e r 1st sectio n , re g e n e ra to r 2 n d sectio n , re g e n e ra to r 3 rd sectio n , re g e n erato r 4 th sectio n , re g e n erato r L ow -pressure p u m p su ctio n F ro m oxidizing to w er

* Special m eth o d s developed in TV A resea rc h la b o ra to rie s.

Na, Hz, COa, C O , C H4, Oa

02

H 2S H2S

H S " , S .C N -, SaO s"", to ta l a lk a lin ity , H2S

T o ta l alk a lin ity

H S " , S C N - , H C O s", S2O8- - , C O3 , H2S, to ta l a lk a lin ity Specific g ra v ity

N 2, H2, C O2, CO, C H4, O2 N2, H 2, C O2, CO, C H4, O2 Na, H 2, C O2, CO, C H 4, O2 N 2, H 2, C O2, CO, C H 4, O2 0 2

N2, H 2, C O2, CO, C H 4, O2 D u s t

D u s t D u s t

S team -g as ra tio C O2, CO, O2 H 2

N t, H2, C O2, CO, C H 4, 0 2 Steam -g as ra tio C O2, CO, O2

HaN t, H 2, COa, C O , C H 4, Oa Na, Ha, COa, CO, C H 4, Oa Ha

Na, Ha, C O2, CO, C H 4, Oa Na, Ha, COa, CO, C H 4, O2 Na, Ha, COa, C O , C H 4, Oa CO, COa

CO , COa, Oa CO

COaNa, Ha, COa, CO, C H 4, Na

C O + COa Ha Na, Ha, C H 4 Ha, N H j, A Na + A, Ha, C H 4 N H ,

NH»

N H j N H s, A N H s

Na + A, Ha, C H 4

NHi

Na + A, Ha, C H 4 A

N H . Na, Ha N H i Oil Oil W a te r Oil, w a ter N H 3 N H s N H s a c tiv ity B iv a le n t co p p er

C u + +, C u +, COa, N H s, H C O O H B iv a le n t co p p er

B iv a le n t co p p er B iv a le n t copper B iv a le n t co p p er B iv a le n t co p p er B iv a le n t co p p er B iv a le n t copper B iv a le n t co p p er

C u + +, C u +, COa, N H s, H C O O H C u + +, C u +, COa, N H s, H C O O H

O rsat D aily

O rsat E v e ry 8 h o u rs or

as req u ired T u tw eiler titr a tio n E v e ry 2 h ours T u tw e ile r titr a tio n E v e ry 2 h ours

T itra tio n E v e ry week

T itra tio n E v e ry 2 ho u rs

T itra tio n D aily

H y d ro m e te r D aily

O rsat As re q u ire d

O rsat D a ily (com posite)

O rsat As req u ired

O rsat D aily (com posite)

M odified W in k ler E v e ry 8 hours

O rsat As req u ire d

G ra v im e tric D aily

G ra v im e tric D aily

G ra v im e tric D aily

V olum etric H o u rly

O rsat E v e ry 8 ho u rs

T h e rm al co n d u ctiv ity C o n tin u o u s

O rsat D aily

V olum etric H o u rly

O rsat D aily

T h e rm al co n d u ctiv ity C o n tin u o u s

O rsat E v e ry 3 d ay s

O rsat As req u ire d

T h e rm a l c o n d u ctiv ity C o n tin u o u s

O rsat E v e ry 3 d ay s

O rsat D a ily (com posite)

O rsat As req u ire d

E le c tric a l c o n d u c tiv ity * C o n tin u o u s

O rsat D aily

E lec tric a l c o n d u ctiv ity * C o n tin u o u s E le c tric a l co n d u ctiv ity * C o n tin u o u s

O rsat D aily (com posite)

E lec tric a l c o n d u ctiv ity *

T h e rm a l co n d u ctiv ity C o n tin u o u s C o n tin u o u s

O rsat E ve^y 3 d ay s

T h e rm al c o n d u ctiv ity C o n tin u o u s

O rsat E v e ry 3 d ay s

A b so rp tio n an d titr a tio n D aily T h e rm al c o n d u ctiv ity C o n tin u o u s A b so rp tio n a n d titr a tio n D aily

T h e rm al co n d u ctiv ity * C o n tinuous A b so rp tio n a n d titr a tio n D aily

O rsat D aily

A b so rp tio n a n d titr a tio n As req u ired

O rsat As req u ired

T h e rm al co n d u ctiv ity * As re q u ire d A b so rp tio n a n d titr a tio n As req u ired

O rsat As req u ired

A b so rp tio n a n d titr a tio n As req u ired

G rav im etric As req u ired

G ra v im e tric D aily

V olum etric D aily

S am e as SS-34, 35 As req u ired A b so rp tio n a n d titr a tio n

Specific g ra v ity As req u ired

As req u ired E le c tric a l co n d u ctiv ity * C o n tin u o u s

P h o to m etric* C o n tin u o u s

G ra v im e tric a n d v o lu m etric D aily

V olum etric As req u ired

P h o to m etric* C o n tin u o u s

V olum etric As re q u ire d

P h o to m e tric * C o n tin u o u s

V olum etric As req u ired

P h o to m e tric * C o n tin u o u s

V olum etric As req u ired

V olum etric As req u ired

G ra v im e tric a n d v o lu m etric As req u ired G ra v im e tric a n d v o lu m etric As req u ired

Ga s Pl a n t. Coke is analyzed for carbon, sulfur, an d ash;

th e fusion p o in t of th e ash also is determ ined. Boiler w ater (GS-13) is analyzed in connection w ith th e tre a tm e n t to m ini­

mize boiler corrosion.

Raw gas is produced by blowing steam first u p an d th e n down through a h o t bed of coke u ntil th e bed cools; air is th en blown through th e bed u n til th e coke reaches th e proper tem p eratu re for th e repetition of th e steam cycle. (A portion of th e gas pro­

duced on th e a ir blast is used to ad ju st th e nitrogen content of th e raw gas.) Gas sam ples from th e various phases of th e cycle, up-steam , back-steam , an d blow runs, are analyzed (GS-1, 2, 3, an d 4) for hydrogen, nitrogen, carbon dioxide, carbon monoxide, m ethane, an d oxygen in order to check th e q u ality of th e gas produced.

T he raw gas is passed th ro u g h a w ater scrubber, w here it is cooled and p a rt of th e d u st and coke breeze is rem oved, and th en

through a soda ash scrubber to rem ove th e hydrogen sulfide pro­

duced as a by-product in th e gas-production cycle. T he gas en­

tering (GS-5) and leaving (GS-6) th e hydrogen sulfide absorber is analyzed for hydrogen sulfide to determ ine th e completeness of rem oval. A fter absorption of th e hydrogen sulfide, th e soda ash solution is regenerated by blowing air through it in th e tw o actifier towers. A djustm ent of th e composition of th e solution is controlled by th e analysis of sam ples tak en a t th e entrance (GS-7) and the exit (GS-8) of th e actifier towers.

T he raw gas from th e hydrogen sulfide absorbers contains considerable dust, m ost of w hich m u st be rem oved to prevent excessive clogging of th e hydrogen p lan t cata ly st beds. This d u st is rem oved by passage through a coke filter. Samples tak en a t th e entrance (D-5) and th e exit (D-6) of the coke filter and a t th e entrance to th e hydrogen system (D-8AB) are ana­

lyzed for d u st as a check on th e operation of th e filter and of th e gas generators.