Infrared Quantitative Analysis Data. CS-6. Infrared Analysis of Isomeric

100. 0.1 instrument: Perkin-Elmer Model 1 2, NaCI prism. Sample Phase: Full strength. Celt Windows: NaCI. Absorbance Measurement: Base-Line-. Point—...
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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