Infrared Quantitative Analysis Data. CS-112 Determination of C10-C12

Determination of C10-C12 Alkylbenzenes. D. E. NICHOLSON and S. H. HASTINGS,Humble Oil & Refining Co.,. Baytown, Tex. CS-1 12. Component. Range...
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Determination of Cl&2 D. E. NICHOLSON and 5. Baytown, l e x .

1

_

1,2,3,4-Tetromethylbenzene

2

n-Amylbenzene

3

Pentamethylbenzene

4

H. HASTINGS,

Component Name Formula

No.

Hexamethylbenzene

Alkylbenzenes

C1oHla

Humble Oil 8 Reflning Co.,

Range

yo

_

X or

Accuracy

Yo

_

0-100 &0.5

Y

6.1. Ptr.

_

Slit (mm) A i or

-

Av

Concn. g/Iiter length mm

~

18.22~ 0.279

~ _ _ - - CllHl6 0-100 h0.5 18.54~ 0.293 ClIHle

Calculation:

Relative Absorbances-Analytical

1 2

1 0.100

3 4

0-100 4~0.5 18.98~ 0.309

~ CIZHIU 0-100 f0.5 '-

1 0.100 -

-

-

Base line-

Inverse m a t r i r Graphical-

ComponentlX

P o i n t X Successive approx-

Matrix:

18.22~ 0.926 1.295 0.062 0.069

18.54~ 0.119 1.254 0.051 0.069

18.98~ 0.049 0.320 0.644 0.046

Material Purity: 99.5% minimum ~ Comments: "Determined from mass spectrometry and the interference coefficients shown above are then applied, effectively reducing the infrared spectrometry to the analysis of a three-component system.

To standardize procedure, ANALYTICAL CHEMIBTRY requests that material be sent in quintuplicate to the chairman of the review committee: D. E. Nicholson. Research and Development Division. Humble Oil Refining Co., P.O. Box 3950, Baytown, Tex.

Lithium

M. R. NADLER and CHARLES P. KEMPTER Los Alamos Scientific Laboratory, University of California,

T

Cell Windows: CsBr Absorbance Measurement:

~

1 0.100

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

186.

Instrument: Perkin-Elmer Model 1 12, CsBr prism Sample Phase: Solution in carbon tetrachloride

cs-112

crystal structure of lithium was determined by Hull ( I ) , who found a body-centered cubic lattice with 2 atoms per unit cell; the space group is 0; - Im3m. The X-Ray Powder Data File contains one lithium data card (1-1131) which lists only four interplanar spacings with no Miller indices assigned. The material used for this paper was Fisher lithium metal. The spectrographic analysis results are shown in Table I. The x-ray sample was prepared by pressing freshly cut lithium through a circular steel die 0.18 mm. in diameter and then sealing a 7-mm. length of lithium wire in a Lindemann glass capillary with molten paraffin. The use of a mineral oil bath for the cutting and pressing operations resulted in a highly reflective sample. X-ray diffraction studies were carried out on a Norelco unit using a 114.59mm. DebyerScherrer camera. The 47hour exposure was made a t 25" C. using iron filtered cobalt radiation. The purpose of this long exposure was to bring out the very weak (222) reflection. The Debye-Scherrer data are shown

-JS

Alamos, N.

HE

Table 1.

Spectrographic Analysis of Lithium

(P.p.m.) Major Li