Infrared Quantitative Analysis Data. CS-9. Determination of Styrene and α-Methylstyrene in...
Transcript of Infrared Quantitative Analysis Data. CS-9. Determination of Styrene and α-Methylstyrene in...
Infrared Analysis of Isomeric Vinyltoluene Mixtures
Name
o-Vinyltoluene
Infrared Analysis of Isomeric Vinyltoluene Mixtures NINA HADDEN and W. F. HAMNER, Monsanto Chemical Co., Texas City, l ex .
Formula
CpHlo
with low Ortho Content NINA HADDEN and W. F. HAMNER, Monsanto Chemical Co., Texas City, Tex.
f 0 . 5
- f 0 . 5
kO.5
cs-8
_ _ _ ~ 12.98
13.35 (Ref.)
9 .10
8 .77 (Ref.)
-- 8 . 9 4
8 .77 (Ref.)
CS-6 Concn.
% lengfh
mm
Concn.
lengfh mm
% Componenf
Range %
ccuracy % A
~
:o rm u fa Range %
kcuracy % A
Name
o-Vinyltoluene 15-90 1 0 . 7 12.98
~ 11.6 (Ref.)
1.37 0.087 0.864 0.058
100
0 .01 0-15 0.500
0.071 0.565 0.077
100
0 . 1
m-Vinyltoluene 10-90 1.27 0.081 0.864 0.058
100
0 .01
k 0 . 7 12.65
11.6 (Ref.)
m-Vinyltoluene I CgHlo 10-90 0,220 0.052 0.200 0.050
100
0 . 1
p-Vinyltoluene 10-90 h 0 . 7 12.15
' 11.6 I (Ref.)
1.09 0 I 071 0.864 0.058
100
0 .01
__
p-Vinyltaluene ~ CgHlo 10-90 0.215 0.052 0.200 0.050
100
0 . 1
Instrumenf: Sample Phase: l iquid
Cell Windows: NaCl Absorbance Measurement: Point_& Calculation: Inverted M a t r i x - X
Analytical Matrix:
Component AI-Ref. A*-Ref. As-Ref.
1. 0.690 0.000 -0.007 2. 0.036 0.515 0.000 3. -0.002 0.019 0.670
Baird recording spectrophotometer, NaCl prism
Malerial Purity:
Reference:
Reference compounds 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 (1941).
Insfrumenf: Sample Phase: l iquid
Cell Windows: NaCl Shutter:
Absorbance Measuremenf: P o i n t X Calculation: Inverted M a t r i L
Analyfical Mafrix:
Perkin-Elmer 1 2C, NaCl prism
For No. 1, LiF; for No. 2 and 3, glass
Compound AI-Ref. Az-Ref.
1 . 3 .000 0.033 2. 0.017 0.160 3. 0.000 0.015
As-Ref.
0.032 0.000 0.405
Material Purity: Comments:
Reference compounds 99.4 mole % or better An accurate value for absorbance of pure o-vinyltoluene
at 12.98~ could not b e measured directly but was derived from known absorbances of m- and p-vinyltoluenes at this point and the observed absorbances of 0, m- and 0, p-vinyltoluene mixtures. Absorbances of al l 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: Perry, J. A., Anal. Chem. 23, 495 (1 951 1. Crout, P. D., Trans. Am. Insf. Elec. Engrs. 60, 1235 (1 941 1.
Determination of Styrene and a-Methylstyrene in Comonomer Mixtures 1. R. KILEY, The Dow Chemical Co., Midland, Mich. cs-9
Slit Concn.
Range Accuracy 0.1. AA or lengfh Component A o r u ( m m ) %
No.1 Name ,Formula! % 1 % Pfs. 1 Av 1 mm Determination of Chloropicrin in Methyl Bromide R. T. SCHEDDEL and 1. R. KILEY, The Dow Chemical Co., Midland, Mich.
cs-7 0-100 1 0 5 8 3 0 265 100 1 C8H8 I 1 ' I ' 10:0641 0 . 1 I. 1 Styrene
Slit Concn. Componenf 1 I AcCu- I or v I (mm) I ms/ml
2. 1 a-Methylstyrene 1 I 0-100 1 h 0 . 5 I 7 . 3 10.240 1 100 0.065 0 . 1
Range racy B 1 AA or le-n'gth No.1 Name 1 Formula 1 % I % 1 PI, I Au 1 mm
fnsfrumenf: Sample Phase: Full strength
Cell Windows: NaCl Absorbance Measurement: Base-line- P o i n t X
Calculofion: Inverse Matrix- Successive A p p r o x . - X
Perkin-Elmer Model 12, NaCl prism
Graphical-
1. chloropicrin CClsNOz 0-5 1 0 . 1 14.15 0.700 180 1 ~ 1 ~ 1 ~ 0.1461 3 . 0
Instrumenf: Perkin-Elmer Model 1 12, KBr prism Sample Phase:
Cell Windows: KBr Absorbance Measurement: B a s e - L i n e X Point-
Calculofion: Inverted Matrix- Successive Approx.
Relative Absorbancea-Analyfical Motrix:
Solution in carbon disulflde
G r a p h i c a l X
Relative AbsorbanceQ-Analytical Mafrix:
Componen f l A 8 . 3 7 . 3
1. 0.510 0.120 2. 0.064 1.670
ComponentJX
1. 14.15 18,250
Material Purify: 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 at 8 . 3 ~ i s obtained from the 0.1-mm cell loaded with carbon di- sulfide.
a Relative absorbances are given as the slope of the Beer's law con- centration curves used expressed in terms of absorbance per 100% of constituent.
Reference compounds 99 +% pure
Maferial Purify: Comments: Samples are compared with known standards of chlaro-
picrin in methyl bromide.
The relative absorbance i s given os the slope of the Beer's iaw con- centration curve used expressed in terms of absorbance per 100% of constituent.
Reference compounds 99 +yo pure
1554 ANALYTICAL CHEMISTRY