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