Infrared Analysis of Isomeric Vinyltoluene Mixtures with l o w Ortho Content NINA HADDEN and W. F. HAMNER, Monsanto Chemical Co., Texas City, Tex.
Infrared Analysis of Isomeric Vinyltoluene Mixtures
CS-6
NINA HADDEN and W. F. HAMNER, Monsanto Chemical Co., Texas City, l e x .
cs-8 Concn.
Concn. Range Name
Formula
%
o-Vinyltoluene
CpHlo
0-15
I
m-Vinyltoluene
%
%
Name
~
kO.5
10-90
CgHlo
10-90
p-Vinyltoluene
I
I (Ref.)
Cell Windows: NaCl Absorbance Measurement: Point_& Calculation: Inverted M a t r i x - X Analytical Matrix:
As-Ref.
1. 2. 3.
3.000 0.017 0.000
0.033 0.160 0.015
0.032 0.000 0.405
Perry, J. A., Anal. Chem. 23, 495 (1951 1. Crout, P. D., Trans. Am. Insf. Elec. Engrs. 60,
Component
AI-Ref.
A*-Ref.
As-Ref.
1.
0.690 0.036 -0.002
0.000
-0.007 0.000 0.670
2. 3. Malerial Purity:
Material Purity: Reference compounds 99.4 mole % or better Comments: An accurate value for absorbance o f pure o-vinyltoluene a t 12.98~could not b e measured directly but was derived from known absorbances o f m- and p-vinyltoluenes a t this point and the observed absorbances o f 0 , m- and 0 , p-vinyltoluene mixtures. Absorbances o f all wave lengths were measured for somples and Crout's method (2) was used to calculate the results. In actual practice any size ceii may be used because normalization cancels out differences in cell length.
Reference:
1.
1
1
Name chloropicrin
Formula CClsNOz
~
1
%
%
10.1
0-5 ~
1
B1 PI,
No.1
I I
14.15 ~
Slit
(mm)
AA or Au
I 1
Concn. ms/ml le-n'gth
2.
1
1
Name
a-Methylstyrene
1
C8H8
I
I
0.700 180 0.1461 3 . 0
Cell Windows: NaCl Absorbance Measurement:
1
Pfs.
1 0 5 '
h0.5
I
I
8 3 '
1 1
Concn.
Av
mm
% lengfh
0 265 100 10:0641 0 . 1
7 . 3 10.240 0.065
1
100 0.1
Point-
Successive Apo pxr. Motrix:
14.15 18,250
12, NaCl prism
Base-line-
Relative AbsorbanceQ-Analytical
Relative Absorbancea-Analyfical
0-100
fnsfrumenf: Perkin-Elmer Model Sample Phase: Full strength
Cell Windows: KBr Absorbance Measurement:
Base-LineX
0-100
%
Slit (mm) AA or
mm
Calculofion:
Inverted MatrixGraphicalX
%
,Formula!
1
Styrene
11
A oru Range Accuracy 0.1.
Instrumenf: Perkin-Elmer Model 1 12, KBr prism Sample Phase: Solution in carbon disulflde
Calculofion:
cs-9
1. R. KILEY, The D o w Chemical Co., Midland, Mich.
cs-7 I.
or v
1235 (1941).
Determination of Styrene and a-Methylstyrene in Comonomer Mixtures
R. T. SCHEDDEL and 1. R. KILEY, The D o w Chemical Co., Midland, Mich.
I 1
99.4 mole % or better
Perry, J. A., Anal. Chem. 23,495 (1 951 1. Crout, P. D., Trans. Am. Inst. Elec. Engrs. 60,
1235 (1 941 1.
Determination of Chloropicrin in Methyl Bromide
AcCuracy
0.515 0.019
Reference compounds
Component
No.1
1.09 100 0 071 0.864 0 . 0 1 0.058 __
12.15
' 11.6
3, glass
Az-Ref.
Range
h0.7
Instrumenf: Baird recording spectrophotometer, NaCl prism Sample Phase: liquid
AI-Ref.
I I
1.27 100 0.081 0.864 0.01 0.058
12.65
8 . 9 4 0.215 100 0.052 8 . 7 7 0.200 0 . 1 0.050 (Ref.)
Compound
1 1
k0.7
11.6
Analyfical Mafrix:
Componenf
11.6
(Ref.)
Absorbance Measuremenf: P o i n t X Calculation: Inverted M a t r i L
Reference:
10-90
m-Vinyltoluene
9 . 1 0 0 , 2 2 0 100 0.052 8.77 0.200 0 . 1 (Ref.) 0.050
Insfrumenf: Perkin-Elmer 1 2C, NaCl prism Sample Phase: liquid Cell Windows: NaCl Shutter: For No. 1, LiF; for No. 2 and
1.37 100 0.087 0.864 0 . 0 1 0.058
1 0 . 7 12.98 (Ref.)
-p-Vinyltaluene
mm
A
~
f0.5
%
15-90
o-Vinyltoluene
lengfh
ccuracy
%
:o rmufa
mm
A
_ _ _ ~ f 0 . 5 12.98 0 . 5 0 0 100 0.071 13.35 0.565 0 . 1 (Ref.) 0.077
10-90
CgHlo
Range
~
lengfh
kcuracy
%
Componenf
Inverse MatrixGraphical-
P o i n t X Successive A p p r o x . - X
Mafrix:
Componenf l A
8.3
7.3
1. 2.
0.510 0.064
0.120 1.670
Maferial Purify: Reference compounds 99 +yo pure Comments: Samples are compared with known standards of chlaropicrin in methyl bromide.
Material Purify: Reference compounds 99 +% pure Commenfs: Results o f this analysis are best checked by preparation of a known mixture on which a check analysis i s then mode. Component 1 at 7 . 3 ~ i s obtained from the 0.1 -mm cell loaded with carbon tetrachloride ond 1 a t 8 . 3 ~i s obtained from the 0.1-mm cell loaded with carbon disulfide.
The relative absorbance i s given os the slope o f the Beer's iaw concentration curve used expressed in terms o f absorbance per 100% o f constituent.
a Relative absorbances are given as the slope o f the Beer's law concentration curves used expressed in terms o f absorbance per 100% of constituent.
ComponentJX
1.
1554
ANALYTICAL CHEMISTRY
