Infrared Quantitative Analysis Data. CS-105 Determination of C10

Determination of Isomeric Dimethyl Benzyl Alcohols. D. E. NICHOLSON and S. H. HASTINGS, Humble Oil & Refining Co.,. Baytown, Tex. C5-105. Component...
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acid, 40 mi. of water), transfer to filter tube, and fill tube with water. After a few minutes draw solution through the mat and rinse the flask and tube with several small portions of water, combining washings with the solution. Add a few drops of 5% phenol to decolorize the solution and determine selenite by measuring the color produced by reaction with diaminobenzidine according to the method of C k n g . This procedure will convert selenium in biological materials into selenite and appears to be quantitative \vithin 7. It is, of course, necessary t o be reasona-

bly careful and to determine a reagent blank. I n the Cheng procedure, the use of more concentrated formic acid, thereby reducing the volume, gives more consistent results. In any case, the volume must be kept constant. Diaminobenzidine, synthesized b y the method of Hoste (Z), gives us more consistent results than the commercial material we purchased.

(2) Hoste, J., Anal. Chim. Acta 2, 402 (1948). (3) Hoste, J., Gillis, J., Ibid., 12, 158 (1955). ( 4 ) Olson, 0.E., personal communication, 1952.

LiTERATURE CITED

WORKmade possible by a grant made by the Tektronix Foundation, Portland, Ore., to the Chemistry Department of the University of Portland.

(1) Cheng, K., ANAL. CHEW 28, 1738 (1956).

O s 2

CARLW. BOKHORST JAhlES J. hfATTICE University of Portland Portland 3, Ore.

~~

Determination of Clo-Akylbenzenes

Determination of Isomeric Dimethyl Benzyl Alcohols

D. E. NICHOLSON and S. H. HASTINGS, Humble Oil 8, Reflning Co., Baytown, lex. CS- 105

D. E. NICHOLSON, Humble Oil & Refining Co., Baytown, l e x . Slit

I

No.

Slit Accuracy

Componenf I Range Name 1 Formulo 1 %

%

B.L.

AX or

Concn. glliter Length

Pts.

Av

mm

X or

(mm)

Y

Range

1

3,5-Dimethyl benzyl alcohol

CgH120

% % ~0-100 10.5 1 1 . 8 5 ~

2,4-Dimethyl benzyl alcohol

CgH120

0-100 f 0 . 5

2,5-Dimethyl benzyl alcohol

C~HIZO

-

3

Relotive Absorbancer-Analyficol ComponentlX

0.713 0.394

0.050 0.242 Material Purity:

P o i n t X

Calculofion:

Successive a p p r o x A

22.21~

18.49~

3

1,4-Dimethylbenzene

Base line-

Inverse m a t r i r G r a p h i c a l

Mafrix: 12.35~

0.020 0.202 0.048

0.017

0.345 0.882 0.252

0.202

3

0.998

Successive a p p r o x L

12.20p

0.690 0.109 0.219

0.088

P o i n t X

0.211 0.015 0.017

2 Material Purify:

0.139 0.294

Minimum of 99%

Instrumenf: Perkin-Elmer Model 11 2, NaCl prism Sample Phase: Solution in carbon disulfide

CS- 107

Range

-

Cell Windows: NaCl Absorbance Measurement:

Concn. gllifer Lengfh

Calculation:

mm

-

1 1 2 . 3 5 ~ 0.229 0 . 0 4 4 ~ 0.027

99.9%

Componenf

1,3-Dimethylbenzene

1 G.218 0 . 0 4 2 ~ 0.027

11.85p

0.068

Humble Oil & Reflnlng Co., Baytown, l e x .

2

1 0.202 0 . 0 3 9 ~ 0.027

1

0.110

S. H. HASTINGS and D. E. NICHOLSON

phenone

mm

Component/k

0.180

Determinatioir of 1r3- and 1 ,CDirnethylbenzenes Containing Benzophenone

-

0-100 k 0 . 5

Relative Absorbancet-Analyfical 21.32~

AA or Av

Concn. g/lifer Lengfh

~-

Cell Windows: NaCl Absorbance Measuremenf:

Mafrix:

20.16~

12.20p

(mm)

Instrument: Perkin-Elmer Model 112, NaCl prism Sample Phase: Solution in carbon disulfide

Insfrumenf: Perkin-Elmer Model 11 2, CsBr prism Sample Phose: Solution in carbon tetrachloride

Inverse m a t r i x Graphical-

or v 6.1. Pfs.

Formulo

-

Calculation:

X

Name

2

Base line-

Accuracy

No.

-

Cell Windows: CsBr Absorbonce Measurement:

CS-106

-I

f0.5 CsHlo

0-100

f0.5

i x K o-100 rto.5

5.95p

1 0.200 1 0 . 0 3 5 ~ 1 .oo

I

1 3 . 0 2 ~ 0.690 0.061~

1 1.00 1 1 .oo

Base line-

Inverse matrixGraphical-

P o i n t X Successive a p p r 0 x . X

Relofive AbsorbancerAnalyfical Matrix: ComponentlX

5.95p

13.02~

12.59~

1 2

0.219

0.007

0.002

0.000 0.000

0.272 0.002

0.002 0.277

3 Maferial Purity:

1.3- and 1,4-dimethylbenzenes, 99.5%; 98%

benzophenone,

VOL 31, NO. 12, DECEMBER 1959

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