INDUSTRIAL a n d ENGINEERING CHEMISTRY
A N A L Y T I C A L E D I T I O N
V O L U M E 18 , N U M B E R 2 I S S U E D F E B R U A R Y 23 , 1946 C O N S E C U T I V E N U M B E R 4
Assistant to Ed ito r: N . A . P A R K IN S O N
M anuscript E d itin s: 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 IL L B. L . C L A R K E
E D IT O R : W A L T E R J . M U R P H Y A ssociate Editor: L A W R E N C E T . H A L L E T T
Att/siant Editors
M anuscript R eview ing : S T E L L A A N D E R S O N A d visory Board
T. R. C U N N IN G H A M G . E. F. LU N D ELL M . G . M E L LO N
C ontributing Ed ito r: R. H . M U L LE R
M ake-up: C H A R L O T T E C . S A Y R E
R. H . M U LLER • B. L . O SER H . H . W ILLA R D
Tabulated D iffraction Data for Tetragonal Isomorphs . . . L . K. Freve l, H . W . Rinn, and H . C . A nderson A p p lic a tio n of C o lo rim etry to A n a ly s is of Corrosion-
Resistant Steels . . . ...O sc a r I. M iln e r
C olorim etric Determ ination of N itrites . *
B. F. R ider w ith M . G . M ello n Rapid Estimation of Effect of Pressure upon Boiling Points
of O rg a n ic C o m p o u n d s ... C a rl Bordenca N ephelom etric Determ ination of Sm all A m o unts of Sodium F. K. Lind say, D. G . B raithw aite , and J . S . D Am ico
83
94
9 6
99
101 Colorim etric Determ ination of Phenols . . • • • •
Louis Lykken, R. S . Treseder, and V ic to r Zahn 104 A n a lysis of Ternary M ixtu re s of M e th ylc y clo h e xa n e -
T o l u e n e - A n il in e ... • • • • • • _ ’
C . S. C a rlso n , A . E. Schubert, and M . R. Fenske 1 0 9 3apid Photom etric Determ ination of Iron in A lum inum
A l l o y s ... ... • • M ich ael Stevens Pepi 111 Chemical Determ ination of V ita m in A in D ried W h ° ]e Eggs
C . R. Thompson, M . A . E w a n , S . M . H a u g e , B. B Bohren, and F. W . Q uackenbush 113 Measuring Coverage and Film Thickness of Printing Ink and
Paint Film s . . R o l f B u c h d a h l a n d M a r g a r e t F. P o l g l a s e . 11b
’pectrophotometric Procedure for Q uantitative Estimation of V itam ins D . . . Jam es B. De W itt and M . X . Su llivan 'recipitation of Platinum M e ta ls b y O rg a n ic M onosulfides J . E. C u rrah , W . A . E. M cB ry d e , A . J . C ruikshank, and F. E. Beamish lexam ethylenetetram ine in Separations of Titanium and
Columbium . ...K a r l W . T r a u b Termination of M e ta llic C opper in Cuprous O x id e -C u p ric
O xid e M ixtu re s . . . Irvin Baker and R. Stevens G ib b s 11 7
120
122
1 2 4 irm ination of M agnesium in A lu m in u m A llo y s . . . •
H e n ry C . Deterding and Richard G . Taylo r
Determination of M enthol in Pepperm int O i l . • • • • ■ J S . Jo n es and S . C . Fang A c c e le ra te d A g in g Test for Insecticidal A e ro s o ls Containing D D T ...Ly le D. G o o d h u e and W . R. B alling er Determination of Traces of A c e t y le n e in L iq u id O x y g e n in
R ectifyin g Columns • H . P. M cK oon and H e n ry D. Eddy Determ ination of Cuprous C h l o r id e ..., ■ • • • • L e w is F. H atch and Reedus Ray Estes Determination of M oisture in Sugar Solutions with Karl
Fischer Reagent . . . . F. W . Z erb an and Louis Sattler Ap paratu s for Flash-Distillation of Butadiene . . . .
A . P. H ob bs and M . R. Rector Sim ple H yd rostatic G ravitom eter for Rapid Determ ination of
S p ecific G ra v ity of L i q u i d s ... • • • • • • W illia m Seaman and J . J . H ugonet
1 3 0
131
1 3 3
1 3 6
1 3 8
1 4 0
141
1 4 4 M IC R O C H E M IS T R Y
M icrodeterm ination of Saponification N um ber of Fats and O ils . . . . Kalman M a rca li and W illia m Rieman III Colorim etric M icrom ethod for Determ ination of A n tim o n y in Biolog ical M aterials with Concomitant Determ ination of B ism u th ... Evan W . M cC h e sn ey T 4 6 M icrodeterm ination of M ercu ry in B io lo g ical M aterial
Ja c o b C h o la k and Donald M . H u bbard 1 4 9 N O T E S O N A N A L Y T I C A L P R O C E D U R E S
V e rsa tile E lectro nic R e la y . . • • • • • • • • • • ■ Joseph G . Baie r, J r . , and Paul E. M illin g to n Kettle for M easuring Sm all Residues in Low-Tem perature
Fractional D i s t i ll a t i o n ..., • • • , * • * , * ' G ra y T . Ham blen and Jo se p h C . Thorstenberg H o t Stage for M icro sco p ic O bservations between Room Temperature and 3 5 0 ° C . . . • • • • • • • • M a rjo rie J . V o id and Todd M . Doscner V a ria b le Pressure M anostat . . . . H ugh B. Donahoe,
Robert R. Russell, and C a lv in A . V a n d e rW e rr Improved A d so rp tio n V e s s e l . - • Robert B. A n derson
1 5 2
1 5 3
1 5 4
1 5 6 1 5 6
Instrumentation in A n a ly s is . . R. H . M u lle r (A d v t . S e c t.) 25
erican Chemical Society assumes no responsibility for the statements and advanced by contributors to its publications. V ie w s expressed In the are those of the editors and do not necessarily represent the official 1 the American Chemical Society.
W e acknowledge with thanks the action of J . T. Baker Chemical C o . in releasing the front cover of this issue for editorial purposes.
Copyright 194 6 by American Chemical Society.
3 7,2 0 0 copies of this issue printed.
d. by the American Chemical Society at Easton, Pa. Editorial Head- 5 16th Street, N . W „ Washington 6 , D C .j telephone, Repub lie 5301/
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R E S E A R C H . . .
G AVE REBIRTH TO THE R U B B E R I N D U S T R Y
S ynthetic ru b b e r and th e prom ise o f ad d itio n al n atu ral ru b b e r play a dual ro le in the o ncom ing, around-the-clock o p e ra tio n o f ru b b e r factories.
And in this speed-up peace p ro g ra m , th e chem ist has a re al ally in B aker’s A nalyzed C. P. Chem icals and Acids, low in sulphur derivatives. F o r the am o u n t o f su lph ur p re sen t in vulcanized ru b b e r o r in various c o m p o u n d in g agents is o n e o f m any im p o rta n t tests.
T h e re are several B aker’s A nalyzed C. P. R eagents th a t have extrem ely lo w indexes o f su lp h u r im pu rities—C .P . B arium C hloride, Potassium C hlo rate, B rom ine, M ineral Acids and E schka’s M ixture. M oreover, this lo w s u lp h u r c o n te n t is plainly set fo rth on th e la b e l—<
2« actual analysis o f the lot. T h is is vitally im p o rta n t to chem ists w hen m eth o d s m ust quickly yield an accurate, d ep en d ab le evaluation.
T h e fact th a t you k n o w the lim its o f vital im p u ritie s in y o u r lab o ra to ry reagents, and k n o w th e m in advance to th e decim al, is im p o rta n t in c o n tro llin g th e quality o f any p ro d u c t.
W e u rg e you to ask y o u r favorite chem ical d istrib u to r for q u o tatio n s on B aker’s A nalyzed C .P. Chemicals an d Acids. R egardless o f w h ere you m ay be located th ere is a B ak er d istrib u to r ready an d eag er to serve y ou p ro m p tly .
J . T. B a k e r C h e m ic a l C o ., Ex e cu tive O ffices and Plant: P h illip sb u rg , N . J . Branch O ffices: N e w Y o rk , P h ila d e lp h ia , Boston a n d C h ica g o .
P u r it y d e f i n e d — n o t '
" m a x im u m lim it * " - but t h e d e c im a l b y a ctu a l a n a ly s is .T h a t 's t h e *tor th e B a k e r ’s A n a ly z e d I
F ebiuary, 1946 A N A 1 Y T I C A L E D I T I O N
M E E T M E T A L I U R G I S T ’ S N E E D S
Now you can select a m etallurgical microscope th a t exactly fits your needs, and in addition provides th e m echan
ical advantages for which Spencer M icroscopes have long been famous.
F o r these new instru m ents offer a wide choice of equipm ent and m any o u t
standing features for convenience and speed in operation:
r literature describing the new Spencer Metallurgical Microscopes in detail, write dept. B -48 today.
American O ptical
COMPANY S cientific In stru m en t Division
Buffalo 15, N ew Y ork
# V A R IE T Y O F E Q U IP M E N T
for te a c h in g , ro u tin e e x a m in a tio n , a n d re sea rc h . . . elev en s ta n d a r d c o m b in a tio n s o f sta g e s , o p tic s, illu m in a to rs , a n d b o d y tu b e s (fixed o r a d ju s ta b le m o n o c u la r a n d in clin ed o r v e rtic a l b in o c u la r).
• W ID E R A N G E A D JU S T A B L E S T A G E h a s b o th slid e a n d ra c k a n d p in io n a d ju s t m e n ts to h a n d le u n u s u a lly larg e o r sm all specim ens.
« b r i l l i a n t, u n i f o r m i l l u m i n a t i o n
fro m a n e w ly d esig n ed v e rtic a l illu m in a to r t h a t is sim p le to o p e ra te , s tu r d y a n d a l
w ay s cool en o u g h to h a n d le . I t h a s a u n iq u e c o a te d re flecto r fo r m ax im u m efficiency . . . b u ilt-in in te n s ity c o n tro l . . . q u ic k ch a n g e nosepiece.
• L A R G E , S T U R D Y , R E S E A R C II-T Y P E S T A N D w ith m ic ro m e te r screw fine a d ju s tm e n t . . . in te rc h a n g e a b le b o d y tu b es . . . g ro o v ed b e a rin g su rfa ce s for long w ear.
H E V I D U T Y E L E C T R I C C O M P A N Y
9 I . ^ l*M.< I»» o»«. A«v. I*!?,««.»
8 _ ■*■“ V«-» £*U*»iMf ■t -yr’r
j ^ « u WipptifüNiT rjcrvc wcAtmci. -. <
M & & * tW * *i l . ? t ft«OM S1 X _ .^ .;’■1 . ,;c!
9 For over thirty years M U LT IP LE UN IT Electric Laboratory Furnaces have played an activ e part in in d u stria l scientific rese a rch . They are s ta n d a rd in most laboratories. See your laboratory supply dealer or send for d e scrip tiv e bulletins.
LABORATORY FURNACES MULTIPLE UNIT ELECTRIC EXCLUSIVELY
. REG, U. S. PAT. O FF.
M I L W A U K E E , W I S C O N S I N
MERCK
Reagent Chemicals
M an y tons of glass of various ty p es are in daily use th ro u g h o u t th e M erck p lan t a t R ahw ay, N . J. M a n y chem ical processes are possible only because th e glass chem ist has m ade available th e m any kinds of glass necessary for the success of su ch operations.
R egardless of ty p e — lim e soda glass, lead -contain ing glasses, chemical glassware, o r optical glass—th e glass chem ist is called up on to devise form ulas for b atch es, an d to te s t raw m aterials as well as finished products.
T o a large degree, he also m u st control d u rab ility , th erm al expansion, elasticity, tensile stren g th , and m an y o ther physical properties.
W e are p ro u d t h a t th e exacting glass chem ist uses M erck A nalytical R eagents in m aking his rigid te sts an d analyses because, like th e glass he has provided for our use, th e y are of highest q u a lity an d dep end ability .
ACID HYDROFLUORIC Merck Reagent
C o n fo rm s to A. C . S. S p ecificatio n s A ssa y : M in im u m 4 7 % H F
Ma x i m u m Im p u r i t i e s
N o n-volatile... 0.003 % Chloride (C l)... 0.003 % Fluosilicic acid (H z S iF e)...0.25 % Sulfate (SO4) ... 0.005 % Sulfite (S 0 2) ...0.005 % H e av y m etals (as P b ) ...0.0005%
Iro n ( F e )...0.0005%
ACID PERCHLORIC 70%
Merck Reagent
C o n fo rm s to A. C . S. S pecifications
M a x i m u m Im p u r i t i e s
N on-volatile... 0.005 % C hloride (C l)... 0.001 % Fluorine ( F ) ... 0.0001%
N itro g en com pounds (as N ) . . .. 0.003 % S ulfate (SO4) ... 0.005 % A m m onia (N H3) ... 0.001 % Iro n ( F e ) ... 0.0008%
L ead (P b ) b y P ith iz o n e . .n o t detectable
M E R C K & CO. , I nc .
d ía n tifío c fa k itu fRAH WAY, N . J .
N e w Y o rk , N . Y . • P h ila d e lp h ia , P a . • S t. L o u is, M o . • E lk to n , V a. • C h icag o , 111. • L o s A ngeles, C alif.
I n C a n a d a : M E R C K & C O ., L td ., M o n tre a l, T o ro n to , V alley field .
S o m e o f th e M erck R e a g e n ts u se d b y
G la ss C h e m ists
SODIUM CARBONATE ANHYDROUS Merck Reagent
C o n fo rm s to A. C . S. S p ecificatio n s
Ma x i m u m Im p u r i t i e s
Insoluble... 0.010 % M o istu re ... L0 % Chloride (C l)...0.003 % A m m onium com pounds (as N ). .0.001 % P h o sp h ate (PO4) ...0.001 % N H -iO H p re c ip ita te ... 0.010 % Silica (S1O2) ... 0.005 % Sulfur com pounds (as SO4) 0.003 % A lum inum (A I)... 0.002 % A rsenic (A s)... 0.0001 % Calcium and M agnesium precip .0.015 % H e av y m etals (as P b ) ...0.0005%
Iro n ( F e ) ... 0.0005%
P otassium (K )...0.02 %
POTASSIUM CARBONATE ANHYDROUS Merck Reagent
C o n fo rm s t o A. C . S. S p ecificatio n s
M a x i m u m Im p u r i t i e s
In so lu b le... 0.010 % M o istu re ... 1*0 % C hloride and C hlorate (as C l).. .0.003 % N itrogen com pounds (as N ) . . . . 0.001 % Pho sp h ate (PO-i)... 0.002 % S ulfur com pounds (as SO4) 0.004 % N H4O H precip itate a n d Silica. .0.01 % Silica (Si0 2) ... 0.005 % Arsenic (A s)...0.0000%
C alcium & M agnesium precip. . 0.01 % H e av y m etals (as P b ) ... 0.0005%
Iro n ( F e ) ...0.0005%
Sodium (N a) (flame t e s t ) . . a b t. 0.02 % February, 1946
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. 18, No. 2
THE METALLURGICAL A N D CHEMICAL INDUSTRIES
A d e ta i le d d e sc r ip tio n o f th e Q u a n t o m e t e r is n o w a vailable f o r d is tr i b u ti o n . Your in q u i r i e s are in v ite d .
m e n t. F o r these in d u s trie s th e Q u a n to m e te r e lim in a te s th e la b o ra to ry b o ttle n e c k a n d th u s allow s a su b s ta n tia l sp eed u p in p r o d u c tio n a n d a larg e o v e ra ll im p ro v e m e n t in q u a lity c o n tro l.
D I R E C T R E A D I N G C U T S T I M E
B asically th e m e th o d u tilizes th e tim e-tested p ro c e d u re s o f sp e c tro ch em istry w h e re in a s p a rk is p assed to th e sa m p le to b e an aly z ed , a n d th e lig h t p ro d u c e d is d is
p e rse d in to a s p e c tru m by m ean s o f a d iffra c tin g m e d iu m . H o w ev er, th e Q u a n to m e te r does n o t p h o to g r a p h the sp e c tru m . In s te a d , a lin e fo r each e le m e n t to b e d e te rm in e d is selected fro m th e s p e c tru m a n d its e n erg y is m e a s u re d by m e a n s o f m u l ti p li e r p h o to tu b e s w hich c o n v e rt th e lig h t receiv ed d ire c tly in to e le c tric a l energy.
By u tiliz in g a n in t e r n a l s ta n d a r d a n d a n in te g r a tin g c irc u it in c o n ju n c tio n w ith re c o rd e rs, each o f w h ic h is c a lib ra te d d ire c tly in th e p e rc e n ta g e c o m p o s itio n o f th e e le m e n t it m easu res, d ire c t re a d in g is ach iev ed .
H I G H P R E C I S I O N
By th e e lim in a tio n o f o n e o f th e c h ie f v a ria b le s in s p e c tro g ra p h y —th e p h o to g r a p h ic e m u lsio n —a n d by th e a d d itio n o f m ean s for ra p id c a lib ra tio n , th e Q u a n to m e te r p ro v id e s h ig h p re c isio n a n d re lia b ility . T h e p re s e n t p r o d u c tio n in s tru m e n ts , d e v e lo p e d a n d te ste d o v er a p e rio d o f th re e years, are fin ish ed p ro d u c ts in every d e ta il, a n d a re n o w re a d y to p e rfo rm th e ir w o n d e rs fo r in d u s try .
S H A R R Y W . D I E T E R T C O . 4336 SAN FERNANDO RD., GLENDALE 4 , CA LIF. 9330 ROSELAWN A V E., DETROIT 4, MICH.
E L E V E N E L E M E N T S IN O N E M I N U T E A d ire c t-re a d in g m e th o d o f sp e c tro c h e m ic a l analysis is n ow a v a ila b le , u tiliz in g a g ro u p o f n e w in s tru m e n ts te rm e d th e “ Q u a n to m e te r .” W ith th ese in s tru m e n ts , a sa m p le can be an aly z ed q u a n tita tiv e ly fo r as m a n y as elev en e le m e n ts in o n e m in u te o r less.
1 his m e a n s th a t th e d re a m o f m a n y a n a n a ly s t a n d m e ta llu rg ist h as fin ally com e tru e , w h e re in an aly sis can lead a n d c o n tr o l th e e x a c t c o m p o u n d in g a n d re fin in g o f a n allo y a t every' stag e in th e process. I n th e c o m p e ti
tive p o stw a r w o rld , w h ich d e m a n d s c o m p le x alloys h e ld to close to le ra n c e s a n d to lo w e r costs, m e ta l p r o d u cers can o n ly m e e t th is c h a lle n g e by b e in g a b le to p ro d u c e every h e a t ex actly a c c o rd in g to sp ecific atio n a n d in less tim e th a n a t p re s e n t.
H U G E S A V I N G S P O S S I B L E
T h e Q u a n to m e te r m akes th is p o ssib le by p e rfo rm in g th e analysis o f a sa m p le fo r a g ro u p o f ele m e n ts in o n e o p e ra tio n , a n d d o in g it m u c h faster th a n h a s h e re to fo re b een p o ssib le by an y m ean s. T h is re su lts in larg e savings by th e e lim in a tio n o f h e a t re je c tio n s, by re d u c tio n o f fu rn a c e tim e necessary to p ro d u c e alloys, a n d by o b v ia t
in g m a n y c o n tro l costs. In fact, in a h ig h ly c o m p e titiv e m a rk e t, su ch savings m ay re p r e s e n t th e d ifferen ce b e tw een a p ro fit a n d a loss in o v e ra ll o p e ra tio n s . E x actly th e sam e factors a p p ly in m a n y o th e r in d u s tries w h e re a n a ly tic a l c o n tr o l is th e a ll im p o r ta n t ele-
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
2 3 0 0 3 BACTERIOLOGY
BREW ER ANA ERO BIC CULTURE D ISH COVER.
Used w ith a solid m edium containing a reducing agent. M akes possible th e cultivation of anaerobes and m icro-aerophiles, in th e sm allest hospital or m obile lab orato ry. R equires no anaerobe jars or
seals. Each S0-70
16040 FERTILIZER
K JELD A H L CONNECTING BULB, Cylindrical, w ith two curved tip s inside th e bulb, new design with drainage bole at seal.
D iam eter o f bulb
m m . 4 5 5 5
L e n g t h o f b u l b m m .
100 120
E a c h
s i .io
1.20
2 8 0 0 5 -S T ESSENTIAL OILS
IO D IN E FLASK. M ade of K im ble R esistant glass.
250 ml. size is req u ired in A.S.T.M. M ethod D29-40 for shellac (W ijs M e th o d ); 500 m l. size is used in A.S.T.M. M ethod D555-39 (H anus M eth o d ).
Capacity m l.
125 25 0 5 0 0
Q uantity in Case
2 4 2 4 24
Each S0.90
1.00
1.10
1 Case S1 9 .4 4 2 1 .6 0 2 3 .7 6
16 005-ST METALLURGY
FLEM IN G - M A R TIN A B SO R PTIO N BULB, two bulb style, w ith $ joints, for absorption of C 0 2 in determ ination of carbon in steel by direct com bus
tion. Each $4.00
C o n s u lt le a d in g l a b o r a t o r y S u p p ly H o u se s th ro u g h o u t th e U n ite d S ta te s a n d C b n a d a fo r K im b le la b o r a t o r y ^ G la s s w a r e to m ee t Y O U R n e e d s .
V isit o u r Booth 342-343 at the E xposition of Chem ical Industries1 /Vcm> Y o rk, Feb. 25 to Mar. 4 /
Vol. 18, No. 2
C H E M I C A L W O R K S
m m m Ê Ê m m m iam m m ,tm iim '" " Ê" " ll^ l""''""""""""""BmÊmÊÊÊÊÊÊÊÊÊÊÊÊÊÊÊÊÊÊmÊmamimiÊÊÊÊÊÊmÊÊaimÊtmm
Mallinckrodt Street, St. Louis 7, Mo.
72 Gold Street, N ew York 8, N. Y.
C h ica g o • P h ila d e lp h ia • Los A n g e le s ■ M ontreal
WHEN YOU USE MALLINCKRODT ANALYTICAL REAGENTS, y o u n e e d n o t c h e c k th e ir u n if o r m d e p e n d a b l e p u rity .
Y o u c a n b e s u re o f t b a t e v e ry tim e y o u b u y . S e n d for tb e M a ll in c k r o d t A n a l y t i c a l R e a g e n t c a ta lo g to g e th e r w itK a n y specific in f o r m a t i o n d e s ir e d o n M a l
lin c k r o d t c h e m ic a ls to fit y o u r s p e c ia liz e d o p e r a tio n s .
A lw a y s S p e cify R eagen ts In M a n u fa c tu re rs O rig in al P ack ag es
Uniform •' Dependable
•Purity
February, 1946
R A Y C O N T R O L
/Îv tv M M C V tC C Û t& C
M A N
« é / i f i e n t c v i e
A N INSTRUM ENT C O M B IN IN G SPEED A N D G O O D
POWER
B u lletin a v a ila b le upon re q u est.
This sp ectro g raph is d esigned p rim arily fo r use in Ram an sp ectro sco p y. H o w ever, b e
cause of its high lum inosity, it is e q u a lly w ell suited fo r w ork in the fields o f phosphores
cence and fluorescence in the visib le reg io n . Future incorpo ration o f electronic equipm ent fo r d irect intensity m easurem ents has been a n ticip ated in the present d esig n.
The dispersing system consists o f three e x c e p tio n a lly la rg e , extra -d en se flint prisms of exce lle n t o p tical q u ality. The collim ating
lens is a cem ented ach ro m at, e sp e c ia lly co r
rected fo r sp h erical a b e rra tio n . The out
standing fe a tu re o f this sp ectro g rap h is the photo g rap hic c a m e ra . This is o f the reflecting cam e ra type with a co rrecting m eniscus, and it w orks at an ap e rtu re of f / 3 . 5 . The fron t alum inized sp h e rical m irror has been p ro
tected so that cle an in g w ill not harm it.
A sp e cia l film ho ld er has been constructed, which eclip ses only 1 0 % of the light tra v ersing the prism system .
T h e o re tic a l C a m e ra D efin itio n (sm a llest circle o f co n fu sio n ). 3/jl S p e c tra l R e g io n .
Len g th o f S p e ctru m Ï
R e so lv in g P ow er.
4 0 0 0 -6 5 00 A units 93 mm
{
.5 A in th e v io le t 1 .5 A in the g re e nR A Y C O N T R O L C O M P A N Y
9 7 5 E A S T G R E E N S T R E E T P A S A D E N A 1, C A L I F O R N I A
B. F. Goodrich Chemical Company
h a s a v a i l a b l e f o r s a l e t h e s e o r g a n i c c h e m i c a l s
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. 18, No. 2
Purity 92 % ; . , • • • • • • • • • • • • • • * * * * * * * *
... Ethyl a n d Dimethyl
c t í s— ^
... —n o , —i • Mercaptothiazoles c h , - C - s
« A v a i l a b l e in comm«
) C S H - , - S
A v a i l a b l e 1- c o m m e r c i a l
N-Nitroso Diphenyl Amine
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• ^ a, y C i > c 5 H« — ■■— : — Ä S -Ä » - c - .
poril'y 9 7 % : m erc ap to tb ia c o le s... • • • • • • *
...
q I O ' O j Mixed Aliphatic Thiazyl % - c~s J i
Diphenyl p PhenyleneBiemine ; Dl^ £
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For o d ,iit!o n al in fo rm atio n p le a s e w rite B. F. G o o d rich Chem ical Co m p an y, D e p artm en t CA-2, Rose B uilding, C le v e la n d 1 5 , O h io .
B. F. G oodrich C hem ical C om pany « „ ss;u ..
February, 1946 A N A L Y T I C A L E D I T I O N
WEL L K N O W N T H R O U G H O U T T H E W O R L D A S L E A D E R S IN D E V E L O P I N G A N D M A N U F A C T U R I N G
I N D U S T R I A L H E A T T R E A T I N G E Q U I P M E N T
V':.' iv
S O L D E X C L U S I V E L Y T H R O U G H L A B O R A T O R Y E Q U I P M E N T D E A L E R S
Efficient, d e p e n d a b le , ad vanced in design . . . these superb furnaces a re an asset to an y lab or shop.
Accurate, d e p e n d a b le tem perature control plus every p ractical provision fo r o p erato r ease and sa fe ty makes them favo rites e ve ryw h e re.
Engineered and built b y the le a d e rs in industrial heat treating developm ent, these furnaces give you your money's worth in d u rability and trouble-free service.
The Lindberg Box Furnace fo r fast, accurate, econom
ical heats, up to 2 0 0 0 ° F. Ideal fo r m etallurgical tests and chemical an alyse s. Transform er is built-in. Step less” Input Controller and Indicating Pyrom eter a re housed in a se p a ra te metal case.
The Lindberg Pot-Crucible Furnace fo r dual-purpose service a t heats up to 2 0 0 0 ° F. As a pot furnace it han
dles salt or le a d bath immersion tem pering, hardening and annealing, cyaniding and aluminum heat treating.
It is e q u a lly effective as a crucible furnace fo r deter
mining critical points of steel, melting base metals, calib rating thermocouples and other useful shop and
" la b ” jobs.
The Lindberg Combustion Tube Furnace provides heats up to 2 5 0 0 ° F. It d e p e n d a b ly handles carbon determ ination o f steel b y the volum etric method o f analysis as w ell as gravim etric typ e determinations of all allo y steels including stainless and heat resisting steels. Com pletely self-contained with transform er, control and pyrom eter.
The Lindberg Hot Plate fo r controlled " la b ” and shop heating up to 9 5 0 ° F. Built-in Input Control assures fast, accurate tem perature regulation.
Your lab o ra to ry equipment d e a le r has these furnaces a v a ila b le now. H e’ll be g lad to give you prices and fuli information. Se e him to d a y.
L I N D B E R G E N G I N E E R I N G C O M P A N Y
2450 WEST HUBBARD STREET • C H IC A G O 12, ILLINOIS
Vol. 18, No. 2
CHICAGO APPARATUS COMPANY CHICAGO K Ä 5 S
BECKMAN pH METER
Laboratory M o d e l G
This instru m en t is re c o m m en d ed for all types of re s e a rc h a n d p re c is e lab o rato ry p H investigations w h e re m axim um versatility a n d a c c u ra c y a re essential. It is also id e a l for m easu rem en t of oxidation a n d re d u c tio n potentials.
F e a t u r e s i n c l u d e :
C ontinu ous in d icatio n of c irc u it u n b a la n c e (elim inates th e key ta p p in g of ballistic m ethods).
Built-in te m p e ra tu re com pensation.
D irect m illivolt re a d in g s for o xidatio n -red u ctio n m easu rem en ts.
S ealed glass e lec tro d es a re sm all a n d un u su ally sturdy; re q u ire m inim um m ain ten an c e.
l b e m ad e on ex c eed in g ly sm all (0.005 ml)
of th e p ro p e r electro des.
in c a b in e t w ith lock a n d key, self co n tain e d s ta n d a rd cell, a n d b atteries; th e 2 3^" glass-C alom el elec tro d e assem bly for pH w ork o n 3 ml sam ples, buffer solution for stan dard izing , sa tu ra te d KC1 solution for th e C alom el electro d e. C a b in e t size 11 ¡Hi x 11 x 9", n e t w eig h t 20 lbs.
N o . 75210 B e c k m a n p H M e t e r , L aboratory M odel G c o m p le te $205.00
A vailable for P rom pt D elivery
M o re a n d m o r e A m e r ic a ’s m o s t e x a c t in g a n d p r o g r e s s iv e s c i e n t i f ic a n d i n d u s t r i a l la b o r a t o r ie s u s e t h e A C C U L U T E se r v ic e r e g u la r ly i n t h e p r e p a r a t io n o f t h e i r s t a n d a r d v o lu m e t r ic s o l u t io n s . A C C U L U T E a m p o u le s h o ld t h e p r e c is e e q u iv a le n t o f t h e n o r m a lit y s t a t e d o n t h e la b e ls , s o t h a t w h e n c o n t e n t s a r e d i l u t e d t o 1,000 m l . , t h e s t a t e d n o r m a l it y r e s u l t s a n d n o s u b s e q u e n t s t a n d a r d iz in g i s r e q u ir e d .
T h e u s e o f t h e A C C U L U T E s e r v ic e s a v e s t i m e , a s s u r e s u n i - fo r m it y i n t i t r a t i o n . U s e o f A C C U L U T E i s t h e M o d e r n W a y o f h a v in g o n h a n d — w h e n n e e d e d — v o lu m e t r ic s o l u t i o n s o f p r o v e n a c c u r a c y .
A C C U L U T E c a r b o n a t e fr e e a lk a lie s c o m e t o y o u i n p a r a ffin a m p o u le s , s o t h a t t h e A C C U L U T E a m p o u le s m a y b e p u r c h a s e d in q u a n t i t i e s a n d k e p t o n h a n d t o r e s p o n d t o u r g e n t n e e d s a s trie c o n t e n t s o f t h e a m p o u le s a r e i n d e f i n i t e l y s t a b le .
A C C U L U T E s t a n d a r d v o lu m e t r ic s o l u t i o n se r v ic e i s c o m p l e t e - o v e r 80 d if f e r e n t s u b s t a n c e s o f v a r io u s n o r m a l it i e s a v a ila b le t o m e e t y o u r in d iv id u a l r e q u ir e m e n t s . W r ite fo r p r ic e l i s t . A -5 0 -U
C o m p le t e i n s t r u c t i o n s o n h a n d l i n g A C C U L U T E a n d , w h e r e n e e d e d , a d v ic e o n e n d p o i n t s , t i t r a t i o n s a n d s c ie n t if ic re e r e n a r e s u p p lie d w i t h e a c h a m p o u le
a r e s o t h a t a n
b y s im p ly
t h r o u g h
P A R A F F I N
o f t h e a m p o u le a r e tr a n s fe r r e d t o a 1000 m l. v o lu m e t r ic f la s k a n d t h e b o d y o f t h e a m p o u l e i s w a s h e d o u t w i t h a w a s h in g b o t t l e , a llo w in g t h e w a s h t o flo w i n t o t h e v o lu m e t r ic fla s k . D ilu t e c o n t e n t s o f t h e fla s k t o 1000 m l.
w i t h d is t ille d w a t e r a n d t h e s t a n d a r d v o lu m e t r ic s o l u t i o n i s p r e p a r e d .
ANACHEM1A 70 E.45 St., NEW YO RK 17, N Y. j
C H E M I C A L S P E C I A L T I E S
D IS T R IB U T O R S
(Stocks M aintained for Prompt Shipm ent) E . H . S A R G E N T & C O . , 1 5 5— 165 E . Superior St., Chicago 1 1 , III.
19 59 E . Jefferson, Detroit 7 , M ich .
Serves: The M id d le W est, G u ll States and Mounta.n Slates of the West
S T A N D A R D S C IE N T IF IC S U P P L Y C O M P A N Y
G E N E R A L L A B O R A T O R Y S U P P L Y C O . , 3 2 0 M arket S t., Paterson 3 , N . J . Sherwood 2-505 0
Serves: N ew Jersey
P H IPP S * B IR D , Sixth and Byrd Sts., Richmond, V a . Serves: V irg inia, North Carolina, South Carolina 34— 38 W est 4th St.
N ew York 1 2 , N . Y
rgrnia, rsortn Carolina, oout W IL L C O R P O R A T I O N
Rochester 3, N . Y . . . . . .P i ai a wic\y/ v n D V
A C C U R A T E r n K i v F K i i F K i T
' C l. 'C l
Just Dilute A cculute
IN F O O D S A N D C O N F E C T I O N S ! U . S . P . g l y c e r i n e , p u r e , s w e e t , a n d w h o le s o m e , i s a v a l u a b l e in g r e d i e n t i n i t s e l f — a n d a ls o o f f e r s a d v a n t a g e s i n t h e d e r i v a t i v e s t h a t c a n b e m a d e f r o m i t .
IN TEXTILES! G l y c e r i n e is u s e d i n d y e b a t h s , p r i n t i n g p a s t e s , a n d s p r a y - d y e s o l u t i o n s e m p l o y e d i n c o l o r i n g a n d p r i n t i n g m a n y t y p e s o f t e x t i l e s . T h e u s e o f g l y c e r i n e - d e r i v e d a l k y d r e s i n s i n t h e t e x t i l e f ie ld i s g r o w i n g .
IN D R U G S A N D C O S M E T IC S ! G l y c e r i n e h a s b e e n a k n o w n a n d t r u s t e d s t a n d b y f o r g e n e r a t i o n s in t h e m a k i n g o f p h a r m a c e u t i c a l s . I t i s a ls o a m a t e r ia l t h a t o f f e r s e v e r - n e w p o s s i b i l i t i e s .
Vol. 18, No. 2
IN R E S IN S ! G l y c e r i n e is a n i m p o r t a n t c o m p o n e n t i n t h e m a k i n g o f a l k y d r e s i n s , u s e d f o r a u t o m o t i v e f i n i s h e s a n d f o r f i n i s h e s o n r e f r i g e r a t o r s , s t o v e s , a n d o t h e r h o m e a p p l i a n c e s , b e c a u s e i t i s e f f ic ie n t a n d h i g h - b o ili n g , a n d o f f e r s c o m p le t e a v a i l a b i l i t y o f a l l t h r e e o f i t s h y d r o x y l g r o u p s . P i c t u r e d a b o v e i s a d e p t h g a u g e u s e d to m e a s u r e t h e t h i c k n e s s o f p a i n t .
What’s News In Chemistry?
-Glycerine!
G
l y c e r i n ! : , k n o w n f o r g e n e r a t i o n s t o c h e m i s t s , i s s t i l l s o m e t h i n g n e w , s o m e t h i n g e x c i t i n g i n i t s p o s s i b i l i t i e s , b o t h f o r p r o d u c t s f o r h u m a n c o n s u m p t i o n a n d f o r u s e i n i n d u s t r y .G l y c e r i n e i s c h e m i c a l l y s t a b l e u n d e r o r d i n a r y c o n d i t i o n s , a n d b y p r o p e r c h o i c e o f c o n d i t i o n s m a n y o t h e r u s e f u l c h e m i c a l s c a n b e m a d e f r o m i t .
F o r i n s t a n c e , g l y c e r i n e i s a n i m p o r t a n t c o m p o n e n t o f a l k y d
r e s i n s , u s e d i n m a k i n g p r o t e c t i v e c o a t i n g s a n d i n p r o c e s s i n g t e x t i l e s . I t i s u s e d i n m a k i n g e s t e r g u m , a n i m p o r t a n t c o n s t i t u e n t o f v a r n i s h e s .
I t i s o n e o f t h e b a s i c m a t e r i a l s u s e d i n m a k i n g m o n o g l y c e r i d e s , e m p l o y e d i n s h o r t e n i n g a n d m a r g a r i n e s . A n d i t i s u s e d i n m a k i n g p o l y g l y c e r o l s , w h i c h a r e h i g h e r - b o i l i n g , m o r e v i s c o u s g l y c e r i n e - l i k e s u b s t a n c e s u s e f u l i n t h e m a n u f a c t u r e o f s o m e o f t h e r e s i n s .
B e c a u s e o f i t s m a n y a d v a n t a g e s , s o m a n y m a n u f a c t u r e r s d e s i r e g l y c e r i n e f o r s o m a n y p u r p o s e s t h a t t h i s v e r s a t i l e m a t e r i a l i s m o r e i n d e m a n d t h a n e v e r b e f o r e .
G LY C ER IN E PRODUCERS’ ASSOCIATION
295 Madison Avenus, New York 17, N. Y., D e p L H -1 5 , te su rd i Headquarters. Chicago. III.
The latest developm ent in Refrigerated Centrifuges, the International Model PR-1 offers the laboratory analyst practically all of the ad v an tages of the larger perm anent type installations plus portability. C en
trifuge and compressor are combined in one attractive cabinet m ounted on casters, and both units are operated from a single cord and plug which can be connected to the ordinary lighting circuit.
C onstant tem peratures plus or minus 2° can be m aintained, and usa
ble accessories illustrated here include the m ullispeed attachm en t and high-speed heads for six 7 ml. tubes or four 25 ml. tubes at 18,000 R .P .M ., conical angle heads for 15, 50 and 100 ml. tubes a t speeds up to 5,000 R .P .M ., the four-place pin type head for 250 ml. bottles at 2,600 R .P .M ., as well as the conventional horizontal tube carrying heads. T he compressor is of ample capacity to cool the interior of the guard bowl to 32° F. or lower w ith any of this equipm ent operating at maximum speed and a room tem perature of 80 I .
Although not previously announced, the Model PR-1 has already been supplied to Army, N avy and civilian laboratories, and has been suc
cessfully used in research on the chem istry of the influenza bacillus.
The features of the machine will at once suggest countless applications, and complete details will gladly be furnished on request.
W idth 28" Length 44" H eight 42" W eight 850 lbs.
I N T E R N A T I O N A L E Q U I P M E N T C O M P A N Y
B O S T O N 3 5 , M A S S A C H U S E T T S
A. H . T . CO. S P E C IF IC A T IO N
B O ER N E R S H A K IN G A P P A R A T U S
Providing a shaking motion which can be varied from gentle agitation to violent swirling
pj !5 t Fig* 1 Fig' 2
W a te r u n d e r g o in g s h a k in g in M e r c u r y u n d e r g o in g s h a k in g r q0*1 ivr — w r 5 0 0 m l fla sk a t t a c h e d t o v e r - in 5 0 0 m l fla sk a t t a c h e d to t i c a l r o d of B o e r n e r S h a k e r . v e r t ic a l r o d of B o e r n e r S h a k e r . .F ro m p h o to g r a p h b y " s t o p F r o m p h o to g r a p h b y " s t o p S h o w in g m e th o d of s h a k in g 5 0 0 m l fla sk s . a c t i o n " c a m e r a . a c tio n ' c a m e r a .
SHAKING APPARATUS, BOERNER, A. H . T. Co. Specification, oscillating platform type, with autom atic tim e switch. Designed especially for shaking flasks, test tubes and micro test slides in the Boerner-Jones-Lukens flocculation tests b u t useful also for m any other shaking procedures involving containers up to 500 ml capacity. Consisting of a floating platform attached to four vertical Stain
less steel coil springs which are fastened to the under surface of the platform and to the corners of a supporting m etal base. The base is provided with rubber feet and enclosed in a m etal guard.
Shaking is produced b y a double-ended 7 « h. p. m otor bolted to th e m iddle of th e underside of th e p latfo rm in such m anner th a t th e axis of th e sh a ft is horizontal. E ccentrically secured on th e m otor sh aft are tw o w eights w ith aligned centers so th a t , in operation, th e p latfo rm oscillates in a generally elliptical p a th which, opposed b y th e tension of th e supporting springs, results in com pound oscillations producing a violent shaking a n d sw irling m otion. T h e p latform for slides, te s t tu b e racks, etc., is 13 inches sq u are an d covered w ith sponge rubber. On it are m ounted, on opposite sides, tw o Stainless steel rods, 12 inches high X 34-inch diam eter, for a tta c h in g special heads above th e level of th e p latfo rm for shaking sep arato ry funnels, bottles, flasks, etc.; or, by m eans of N o. 3220-B Clam p, flasks or b o ttle s up to 500 ml capacity.
T h e u p p er ends of th e shaking rods can be m ade to v ib rate violently o r gently, as desired, b y changing th e height of th e flasks, etc., on th e rods a n d by a d ju stin g th e ir position above o r beyond th e p latfo rm ; also, if necessary, by adding a counter w eight to th e opposite rod a t m ost advantageous height.
C om plete w ith au to m atic tim in g device w hich can be se t for a m axim um in terv al of 28 m inutes in steps of l/2 m in u te and sw itch for operation w ith o u t tim er. O verall height, 19K inches; pow er consum ption 40 w atte.
8927-M . Shaking A pparatus, B oerner, A. H . T . Co. Specification, as above described, com plete w ith cord a n d plug, b u t w ith o u t flasks and clam ps show n in illustration. F o r 110 volte, 60 cycles, a. c... 52.50
C la m p , o f s ta m p e d s te e l, w ith h o ld e r ; f o r s e c u r e ly a t t a c h i n g fla sk s , e tc ., to v e r t i c a l ro d s of a b o v e S h a k e r . T a k e s c o n t a in e r s u p to 2 in c h e s d ia m e t e r of n e c k ... 1.85 M u ltip le S h a k in g H e a d , fo r a t t a c h m e n t to v e r t ic a l ro d s o f a b o v e S h a k e r fo r
s h a k in g f o u r s m a l l fla sk s, b o tt le s , e tc ., u p to 125 m l c a p a c it y a n d w ith n e c k s f ro m 18 to 2 8 m m o u ts id e d ia m e t e r . W i th f o u r a d j u s t a b l e S p r in g - G r ip C la m p s of n ic k e l p l a t e d b r o n z e a n d c la m p h o ld e r f o r a t t a c h m e n t to
r o d ... 6 . 0 0
S e p a r a t o r y F u n n e l S h a k in g H e a d , fo r a t t a c h m e n t t o v e r t ic a l r o d of a b o v e S h a k e r fo r s h a k in g tw o s e p a r a t o r y fu n n e ls , 6 0 , 125 o r 2 5 0 m l c a p a c ity , in in v e r te d p o s itio n . O f c a s t a l u m in u m , -with r u b b e r c o v e re d r in g s a n d s p r in g s fo r h o ld in g f u n n e l s to p p e r in p o s i t i o n ... 16.50
89 29. 8 9 2 9 -B .
A R T H U R H. T H O M A S C O M P A N Y
R E T A I L — W H O L E S A L E — E X P O R T
LABORATORY 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, P A ., U .S.A .
Cable Address "Balance” Philadelphia
INDUSTRIAL a n d ENGIN EERING CHEMISTRY
P U B L I S H E D B Y
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
Tabulated Diffraction Data for Tetragonal Isomorphs
L . K . F R E V E L , H . W . R IN N , A N D H . C . A N D E R S O N , The D ow Chem ical C om p any, M id la n d , M ic h .
C
O M P O U N D analysis of crystalline solids by isomorphism depends for its u tility on the av ailab ility of system atically arranged rep resen tativ e diffraction p a tte rn s of the various known crystal stru ctu res. T h e ta b u la tio n of th e cubic stru ctu res (S) has been found useful an d th e effectiveness of the m ethod has prom pted th e com pilation of th e tetragonal structures. The procedure for com paring diffraction p a tte rn s of isomorphous substances has been described ad eq u ately (4), hence only the ta b u lated diffraction d a ta for tetrag o n al isomorphs are presented in th is paper.Figures 1, 2, 3, a n d 4 depict rep resen tativ e diffraction p attern s of 40 tetrag o n al stru c tu re s designated as in th e “S tru k tu rb er- ich t” (2, 5-9). T h e p a tte rn s are arranged in sets an d w ithin each set th e sim plest stru c tu re w ith the highest sym m etry {11) is listed first. T h e averaged relative intensities, based largely on the D ow file of stan d ard s, refer to D ebye-Scherrer-ITull p attern s taken w ith M o K a radiation. F o r each stru c tu re only reflections com patible w ith th e respective space group are shown. T he intensities of superposed lines were resolved by calculating th e appropriate s tru c tu re factors. T o round o u t th e available pow
der d ata, som e fifty substances were synthesized an d th eir dif
fraction p a tte rn s carefully indexed.
G E N E R A L P R O C E D U R E F O R ID E N T IF Y IN G A N O N C A T A L O G E D P A T T E R N
(1) P lo t the log d values an d corresponding relative intensities of the unidentified p a tte rn on a narrow strip of paper; (2) verify th a t the p a tte rn is noncubic (3) ; (3) find an isom orphic p roto
ty p e am ong th e rep resen tativ e diffraction p a tte rn s for the aniso
tropic crystal stru ctu res; (4) com pute th e la ttic e constants and check th e ap p ro p riate classification tables (for th e tetragonal
Table II. Statistical Data on Tabulated Tetragonal Substances
Table 1. X - R a y Pow der Diffraction I
Data
d , k X Ix (AMJ
7 . 2 5 0 . 0 6 001
3 . 7 5 1.00 (100) 101
3 . 6 0 0 . 1 5 002
3 . 1 0 1.00 (100) 110
( 2 .9 8 ) (0.01)
2 . 7 8 0 .6 3 102
2 . 3 5 0 . 7 5 (75) 112
2 .1 9 0 . 6 3 200
2.11 0 . 2 5 2 0 1 , 103
1 .9 0 0 . 4 0 2 1 1 , 113
1 .7 2 0 . 2 5 212
1.68 0.20 104
1 .6 2 0.02 20 3
( 1 .5 9 ) (0.01)
2 2 0 , 114
1 .5 5 0 . 1 5
1 .5 2 0 . 1 5 2 2 1 , 213
1 .4 3 0 . 0 8 2 2 2 , 301
1 .3 9 0.10 2 0 4 , 3 10
1 .3 5 5 0.02 3 1 1 , 302
F ilt e r e d M o K a w as u s e d to o b ta in t h e p o w d e r d if f r a c tio n d a t a , d — n t e r p l a n a r s p a c in g . ~ *= r e l a ti v e in t e n s i t y . T h e l a t t i c e c o n s ta n ts f o r th e
Ii
u n k n o w n p h a s e a r e a = 4 .3 8 k X , c =» 7 .2 3 k X ; — *= 1.G5.
D o m in a n t s t r u c t u r e s N r *=» n u m b e r o f e x a m p le s
Nr Sr.Vr
C o n f ig u r a tio n s f a v o r in g te tr a g o n a l s y m m e tr y
P r e v a le n c e of p r im iti v e la tti c e s P r e v a le n c e o f b o d y - c e n te r e d la tti c e s n hko *“ a v e r a g e n u m b e r o f o b s e r v e d p r is m re fle c tio n s p e r p o w d e r p a t t e r n
p r o b a b i l i t y o f.o b s e rv in g {hko}
H O*, C 4 , C i l , O B 2 0 , . . . 3G, 3 3 , 1 8 , 1 7 , . . . 0 .1 1 , 0 .1 0 , 0 .0 G , 0 . 0 5 , . . . T e t r a h e d r a l , o c t a h e d r a l , s q u a r e ; li n
e a r ; 4 n -c y c lic 5 3 %
477o
%
vhko
1 hko
Jl
4 . 4 ;
(m o , i-soo, öjw) ** ( 0 . 0 5 , 0 . 9 3 , 0 . 9 0 ) a v e r a g e r e l a ti v e in t e n s i t y of
I h ko J
n[ALf) = p r o b a b i lit y t h a t JAW! is t h e nob s tr o n g e s t p o w d e r r e fle c tio n o f a te tr a g o n a l s t r u c t u r e
a v e ra g e a x ia l r a t io
(
/ n o /ooo J o s o \ _ 7i ’ / i ’ Jl / ' Pa (1 0 1 . 1 1 2, 1 1 0, 2 1 1 , 2 0 0 )0 . 2 2 , 0 . 1 3 , 0 . 1 3 , 0 .0 8 ) Pa( 1 0 1. 2 0 0, 2 1 1, 1 1 0, 1 1 2)
0 . 1 3 , 0 . 1 0 , 0 . 0 8 , 0 . 0 8 ) Paf 110. 2 1 1 , 101, 2 0 0 , 112)
0 . 1 0 , 0 . 0 8 , 0 . 0 8 , 0 .0 5 ) 1 . 5 1 ; 0 . 3 1 S - S 6 . 7 -
( 0 .3 8 , 0 .5 1 , 0 . 1 7 ) ( 0 .3 0 . ( 0 .1 5 ,
(0 . 10,
system check T ables I I I an d IV ); (5) confirm th e identification of th e unknow n phase b y a q u a lita tiv e spectroscopic analysis or b y sp o t tests.
T he following example illu strates th e procedure:
Colum ns 1 an d 2 of T ab le I give th e pow der diffraction d a ta of a phase encountered in a m agnesium flux sam ple. A fter plotting log d an d the corresponding relativ e intensities on a strip of paper, one checks first th e index scale for th e cubic system (S) and finds th a t the substance is noncubic. Proceeding to th e tetragonal system an d com paring system atically th e unknow n p a tte rn w ith those of Figures 1, 2, 3, an d 4, one m akes th e follow
ing observations: T he first indication of a fit w ith th e d a ta is noted for C l l w ith ^ = 1.64 (o ~ 4.4 k X , c ~ 7.2 k X ) . However, th e lines 7.25, 2.78, 1.72, 1.68, 1.62 k X are n o t accounted for by this stru ctu re and th e in ten sity agreem ent of th e indexed lines is n o t satisfactory. S tru c tu re C38 perm its indexing all th e lines for - = 1.65 (o = 4.38 k X , c = 7.23 k X ) b u t gives poor agreem ent a
w ith th e relative intensities. Checking T ab le I I I u n d er C38, one fails to find a substance agreeing w ith th e com puted lattice constants. A sim ilar situ atio n is encountered fo r stru ctu re D3i w ith ~ = 2.32 (a = 6.20 k X , c = 14.5 k X ) a n d for stru ctu re D O 22 w ith - = 1.65 (a = 8.75 k X , c = 14.5 k X ) . S tru ctu re E O 1, how
ever, accounts for all the lines an d m atches th e relative intensi
ties well. Looking under E O 1 for ^ = 1.65 (a = 4.38 k X , c = 7.23 k X ) , one identifies th e unknow n as B aF C l. Spectroscopic analysis confirms B a as a m ajo r constituent. T he fa in t lines 2.98 a n d 1.59 k X belong to a n unidentified m aterial present in low concentration. (In com pleting th e com parison of th e iden
tified p a tte rn w ith th e rem aining tetrag o n al structures, one finds only p a rtia l m atching w ith stru ctu res H O 4, H O 7, an d HOg.) 83
