Infrared Quantitative Analysis Data. CS-68 Analysis of Carbon

Infrared Quantitative Analysis Data. CS-68 Analysis of Carbon Tetrachloride For Trace Impurities. L R. Kiley, and R T. Scheddel. Anal. Chem. , 1959, 3...
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is 14.315 granis per cc., and the U--i"\' bond distance for coordination number 6 is 2.4449 A.

were plotted against 9 tan q (where @ is the complement of the Bragg angle), and the calculated least sauares fit was linearly extrapolated to 6 tan 9 = 0. The y intercept obtained was 4.8897 A. After correcting for the refraction of filtered copper radiation by UK, the precision lattice constant is 4.8899 A. at 26'. Therefore, the theoretical density

LITERATURE CITED

E.,~ ~s. c., ~ Kilson. 8 . S., McDonald, R.h.,J . d m . Chem. SOC.70,99 (1948).

(1) Rundle, R.

ACKNOWLEDGMENT

The authors wish to thank 0. H. Kriege and B. D. McCarty for their analytical assistance, and Vernon B. Taylor for his general assistance.

~

CRYSTALLOGRAPHIC data for publication in this section of - ~ I A L Y T I ~ A CHEMISTRY L should be sent to K , C. RicCrone, Jr., 1lcCrone Associates, 501 East 33nd St., Chicago 16, Ill.

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Determination of Geranyl Acetate in Geranyl Formate A. J. FENTON, The Procter a n d Gamble Co., Cincinnati, O h i o

x

slit

B I. Points

(mm)

Concn. gll length

Ax

mm

I

1

Component Name Formula

No.

- ' - I - ' -1 i

Accuracy

' Range i %

%

1 C I ~ H ~ O O ?0-20

Geranyl acetate

~

&0.2

I-___-

I

I

,I

CS-66

1

8.1 7.938.22

1

1

300

200

0.040~I 0.05

Calculation:

L. R. KlLEY a n d R. T. SCHEDDEL, The D o w Chemical Co., Midland, Mich.

CS-68 Sllt

I I

1

2

x

~ccuracy

Componei I Range Name Formula %

No.1

%

or v B 1. Pts.

11

Concn.

(mm)

70

A x or Av

length mm

1,Z-Dichloroethane

~

Instrument: Perkin-Elmer M o d e l 321, NaCl prism Sample Phase: Solution in carbon disulfide Cell Windows: NaCl Absorbance Measurement:

Analysis of Carbon Tetrachloride for Trace Impurities

2-Propanone

~

Base line

Graphical ~

Relative Absorbance-Analytical Matrix: Camponent/h

Carbon disulfide

- ____I _ _ _ _ _

8 . 1 ~ 4

1.67

1

5.86.8

Material Purity: Reference compounds 99 +Tc pure Comments: The absorbance i s expressed as the slope o f the Beer's l a w curve in absorbance p e r 1007' of constituent. Calibration curve passes through -0.033 absorbance a t 0% acetate.

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Trichloromethane

_____ 5

'

8 . 2 ~ 0.491

100

7.5- ' 0 . 0 4 4 ~0.1

1

8.6

I______---

C2HC13 0-0.15

Trichloraethylene

-1-

0-0.151&0.05

CHC13

0 . 0 3 9 ~ 0.1

zkO.005

~

I 1

10.711 0.782 100 10.60 . 0 5 4 ~ 0.1 10.9

_ _ _ ~ _ _ _ _ _ _ _ _ _ _

I

Determination of Citronellyl Acetate in Citronellyl Formate A. J. FENTON, The Procter a n d Gamble Co., Cincinnati, O h i o

Na.1

1

i

Component Name Formula Citronellyl acetate

I

I

I

Range

Accuracy

%

%

C12H2202 0-20

*0.3

CS-67

slit

6.1.

hm)

Concn. g/l length

Paints

Ax

mm

8.1 7.75

0.300

200

Cell Windows: NaCl Absorbance Measurement: Calculation:

Relative Absorbance-Analytical Matrix:

5 6

Componentlx 1

8 . 1 ~ 1.68

1 0 . 9 5 ~ 0.821 10.80.05611

100 0.1

11.2

Base l i n e - X

Inverse matrix--G r a p hica I L L

Material Purity:

0.068 0.000 0.000 0.000 0.000

0.000

0.000

2.740 0.000 0.000

0.000 0.000

Point-

Successive opprox.-

Relafive Absorbances"-Analyticol Matrix: Component/X 3.35 5.75 6.5

Graphical

Base line

, 10.005

Instrument: Baird Associates M o d e l A, NaCl prism Sample Phose: Full strength

1 2 3 4

Calculation:

0-0.15

I

0.040~ 0.05

Instrument: Perkin-Elmer M o d e l 321, NaCl prism Sample Phase: Solution in carbon disulfide Cell Windows: NaCl Absorbance Measurement:

C?CId

I

x __

Perchloroethylene

0.000 0.000

0.458 0.000 0.000 0.000

8.2

10.7

10.95

0.000

0.000

0.000 0.000

0.000 0.000 0.000 0.000 0.032

0.000

0.000 0.047 0.000

0.000

0.000 0.000

0.000 0.093

Reference compounds 99 +% pure

Material Purity: Reference compounds 99 +% pure Comments: Absorbance expressed as slope of Beer's l a w curve in absorbance p e r 1OOyo o f constituent. Calibration curve passes through 0.075 absorbance a t 07, acetate.

O4 Relative absorbances a r e given as the slope o f the Beer's l a w concentration curves used expressed in terms o f absorbance per 0.157, o f constituent.

These d a t a represent standard publication a n d submission is open t o anyone in accordance with regulations of ANALYTICAL CHEMISTRY. T h e Coblentz Society is acting only a s a n aid t o t h e journal.

T o standardize procedures. ~ K A L Y T I C A LCHEMISTRY reques-s t h a t material be sent in quintuplicate t o t h e chairman of the reT-iew coiiimittee: Robrrt C. Wilkerson, Celanese Corp. of America. Post Office Box 8. Clarkwood. T e x .

VOL. 31, NO. 1, JANUARY 1959

157