Infrared Quantative Analysis Data. CS-78. Determination of

Infrared Quantative Analysis Data. CS-78. Determination of Naphthalene and Ethyl Chloride in Tetraethyllead. R P. Curry. Anal. Chem. , 1959, 31 (5), p...
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Determination of Polyacrylonitrile in Coatings

Determination of Acetate and Formate in Geranium Algerian and Geranium Bourbon

M. 1. A D A M and M. H. SWANN, Coating and Chemical Laboratory, Aberdeen Proving Ground, Md.

Component

!

No1 Name

1

1

Slit hm) AA or

Accu-

% ; ("7'1'7

Acrylo- CsH3N nitriiel

1 I 0-6

cs-77

6f.lf;s.

~

1 ~

Av

~

Cell Windows: NaCl Absorbance Measurement: Calculation;

Base l i n e - X

Inverse matriGraphicalX

2

CioHs

I1 1 1 k: 1 ~

Base line

Graphical

2

Determination of 1-Hexyne and 1-Hexene in Iso-octane Solution

%

g/ml length mm

Component

12.80~10.381 1100 0.069~ 0.103

2

~

CS-80

R. P. CURRY, Ethyl Corp., Baton Rouge, La.

1

'E'

0

1.46

Material Purity: Reference compounds 99 f % pure Comments: Calibration curves made up using geranyl acetate and formate in toluene.

Concn. Slit

8.6~

2.14 0

1

length mm

Rage ry 0-1 10.03

0.300 200 0-30 f0.3 8.1 7.57- 0.040~ 0.05 8.92

Relative AbsorbancesAnalytical Mafrix: Component/A 8.lp

cs-7a

ACCU-

1

mm

-

Formate CiiHisOz (as geranyi formate)

Calculation:

R. P. CURRY, Ethyl Corp., Baton Rouge, La.

Naphthalene

Points

0.319 200 10.3 8.6 7.57- 0.038~ 0.05 8.92

Cell Windows: NaCl Absorbance Measurement:

4.48~ 5.99

Determination of Naphthalene and Ethyl Chloride in Tetraethyllead

1

%

Instrument: Perkin-Elmer Model 321, NaCl prism. Somple Phase: Solution in toluene

Successive approx.-

Relative absorbances are given as the slope of the Beer's l a w concentration curves used expressed in terms o f absorbance per 100% o f constituent.

I

%

(as geranyl acetate)

-

Material Purity: Reference compound was an acrylonitrile-butadiene copolymer which was assayed b y a standard Kleldahl procedure. Comments: 1 Quantltative toluene dilutions ( b y wt.) o f the assayed acrylonitrilebutadiene copolymer were used to prepare standards. 2 Resin solutions that are too viscous are quantitatively diluted (by wt.) with toluene in such a way that the experimental absorbance i s a t 4.48 p . 3 A line drawn parallel to the zero line and tangent to the absorption minimum a t 4 . 9 0 ~was used as a base line. 4 A rock salt plate was placed in the reference beam.

Component Name Formula

6.1.

Concn. g/l Length

~

I

1-Hexyne

1-Hexene

~

CBHlo

CBHls

~

0-15 0-20

I

I

zt0.3

I

3 . 0 5 ~ 0.046 2/10 1 0 . 0 2 8 ~ 0.114

~

2/10 6.08~ 0.102 10.08~ 0.036~ 0.114 0.224 0.049~

f0.2

, f0.5 I

I Instrument: Perkin-Elmer 21, NaCl prlrm Sample Phase: Solution In iso-octane

Instrument: Perkin-Elmer 21, NaCl prism Somple Phase: liquid Cell Windows: NaCl Absorbance Measurement: Calculation:

Cell Windows: NaCl Absorbance Measurement: Bore line-

Inverse matrixGraphical A

A

Point-

1

No./

Range

Accuracy

f0.3 4.48 0.060 comment 14.90 (comment (31 3) 0.0093p/ 2.02

Relative Absorbancesa-Analytical Matrix: CornponenilA

'

nt Formula

Instrument: Perkin-Elmer Model 21, NaCl prism Sample Phase: Dilution o f resin solution with toluene

cs-79

A. J. FENTON, The Procter and Gamble Co., Cincinnati, Ohio

Concn. mg/ml length mm

Base line-

P o i n t X

PointX Successive approx.--

Relative Absorbances"-Analytical Matrix Component/X 12.80~

1

1.12

2

0.000

Calculation:

inverse m a t r i r GraphicalX

Successive approx.-

Relative Absorbances"-Analyfical Matrix:

7.82~ 0.000 0.143

3.05~ 3.04

6.08~

10.08/,i

1

0.000

0.000

2

0.000

2.69

3.82

ComponentlX

Material Purify: Reference compounds 99 +% pure Comments: A highly refined TEL sample was run for obtaining reference points; however, the following equations for base line absorbance were A4.50 + 0.064; A (ethyl chloride) found to b e satisfactory: A (naphthalene) Aa.sop+a.lss. A4.50~ i s absorbance of sample compared to air in reference beam.

Moterial Purity: Reference compounds 98 $% pure Comments: Other 1 -alkynes and 1 -alkenes will interfere. In the particular application involved, 1 -hexyne was the only alkyne possible from the reaction. Two wave lengths are used for 1-hexene to check against other hexenes.

Relative absorbances are given as the slope o f the Beer's law concentration curves used expressed in terms of absorbonce per 1 % of constituent.

Relative absorbances are given as the slope o f the Beer's law concentration curves used expressed in terms of absorbance per 100% of constituent.

These data represent standard publication and submission is open to anyThe Coone in accordance with regulations of ANALYTICAL CHEMISTRY. blenta Society is acting only as an aid to the journal.

To standardize procedure, ANALYTICAL CHEMISTRY requests that material be sent in quintuplicate t o the chairman of the review committee. Robert C. Wilkerson, Celanese Corp. of Arnerioa, Post O 5 c e Box 8, Cla;kwood, Tes.

=

=

960

ANALYTICAL CHEMISTRY