h
Principal Liner d , A. 11.0 7.28 6.76 6.23 5.68
IIIx
d, A.
111,
1
4.45 4.26 4.13 3.85
2
3.10
5
8
7
2 2 2
5.12 4.54
I
Refractive Indices (.5893 A.). N , = 1.544; N , = 1.550; N , = 1.604; geometric mean 1.5fi2. Molecular Refraction. 69.4 o h served; 70.4 calculated. Optic Axial Angle (5893 A,). 21' = 38" calculated from refractive indices; 42' using .Mallard's constant.
Analysis of Diphenylamine, Diphenyl Ether, and Azobenzene Mixtures
No.
Name
CSM-55
Formulo
~
I
Diphenyl amine
Cx2HIIN
Diphenyl
C,&hoO
0-100
1
~-~ _ _ _ _ _ _ 2
040
erne,
10
melts at 132' C. When the melt is cooled slowly, an unstable form crystallizes, which, upon reheating, slowly undergoes a solid-solid phase transformation to the stable form.
OPTICAL PROPERTIES
L. R. KILEY, The D o w Chemical Co., Midland, Mich.
5
FUSION PROPERTIES.Tolbutamide
Figure 2. Orthogonal and clinographic projections of tolbutamide crystals
Foriiiula Wciglits per Cell. 1. Formula Weight. 270.34. Density. 1.263 (x-ray); 1.215 (flotation).
5
3.39
Dispersion. r > u, strong. Optic Orientation. a = 1'; b = X. Common Crystal Orientation. (010) showing centered obtuse bisectrix interference figure. Optic Sign. Positive.
96.
Figure 1. Tolbutamide crystals showing supplementary twinning 180 XI
2 2
LITERATURE CITED
(1) Forist, A,, Chulski,
T.,Melabolism 5,
807-12 (19561.
C~KTRIRUTIONS of crystallographic &ita should be sent to W. C. McCrone, 500 Ihst :Srd S t , Chicago 16,Ill.
Determination of Toluene in Methylcyclohexane E. A. McCRORY a n d R. T. SCHEDDEL
CSM-56
I h e D o w Chemical Co.. Midlmd. Mich.
Vo.
Nome
1
Toluene
~Rmge Formulo %
~
CiHa
0-0.4
h
ACC".
7_ %
10.002
&0.3 ]11.52s 10.400 100 0 . 0 7 4 ~ 0.1
or
Y
6.1.
mcy
PI'.
_~0.380 Ij 100
13.7s 13.41.40
o.069M
I
0.9
~
I
zene
.
Instrument: Perkin-Elmer Model 12C. NaCi prism Somple Phose; Full strength
040
I
Instrument: Perkin-Elmer Model 12, NaCI prism Smmple Phase: Solution in carbon d i d f l d e
Cell Windows:
NoCl Absorbonce Meorumment:
Bore l i n e a -
Inverse matrix .~ GraphicalX ~
Point&
Cdculotion:
Successive mpprox.-
Compaoentlh
2.88
I
0.215
2 3
0.000 0.000
Moteriol Purity:
Inverse motrixGraphical2
Relmtire Abrorbanc=i'-An.lytical
Relotire A b * ~ , b ~ " ~ ~ c - A " ~ Matrix: i~ti~~l
"
Bore I i n e L
P o i n t L
NaCl
Absorbonce Measurement: Colruiotion:
Cell Windows:
11.52 0.108 0.953
12.92
Component/X
0.103
1
0.018
2.288
0.152
Reference compounds 9 9 +% pure
Relative obrorboncer ore given 01 the dope o f the Beer's low concentrotion curves used expressed in terms of absorbonce per IOOVo con$tituent.
Moterid Pvrity:
Successive approx.-
Motrix:
Reference compounds 9 9 + %
13.7~ 155.2 pure
The relative abrorbancer are given 01 the dope o f the Bcer'r low :oncentrotion curve used expressed In terms o f obiorbonce per 100% of :O"stil"ent.
VOL. 30, NO. 9, SEPTEMBER 1958