Infrared Quantative Analysis Data. CS-118. Determination of C10-C11

Infrared Quantative Analysis Data. CS-118. Determination of C10-C11 Naphthalenes. D E. Nicholson, and S H. Hastings. Anal. Chem. , 1960, 32 (2), pp 29...
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{ O l O ) , macropinacoid { loo}, and basal pinacoid { O O l ) ; (1011 and (011) are most predominant. Polysynthetic twinning on (110) and (170). Axial Ratio. a : b : c = 0.9750:l: 0.8045 (x-ray) ; not determined morphologically owing to multiple reflections caused by twinning.

hkO, with h # 2n. The corresponding space group is I 2/m 2/m 2/a. The literature space group is given as tetragonal P 4/nnm or a subgroup ( 5 ) . All Weissenberg patterns showed twinning on both (110) and (lio). Observations with a n electron microscope showed the twinning to consist of two sets of extremely fine, multiple, parallel layers. The latter were approximately 2000 A. in thickness, giving rise to continuous visible spectra on the crystal faces when these vvere viewed with an optical microscope. Tabulated powder diffraction data n-ere derived in the same manner as for a-A1Bl2.

ACKNOWLEDGMENT

Crystals n-ere obtained from A A. Giardini, of this laboratory (melt technique), and from P. G. Cotter, U.S. Bureau of Mines, Norris, Tenn. (aluminotherniic method). R. Lefker, of this laboratory, programmed the machine computations of d-spacings. G. Katz and L. Toman, also of this laboratory, assisted in some of the physical determinations.

X-RAYDIFFRACTION DATA Space Group. I 2 / m 2/m 2/a [tetragonal P 4/nnm or a subgroup (5)1. Cell Dimensions. a = 12.34 & 0.01 A , ; b = 12.631 & 0.005 A.; c = 10.161 =t 0.001 A. [Tetragonal, a = 12.55 A.; c = 10.18A. ( 5 ) ] . Formula Weights per Cell. 15.8. Formula Weight. 156.82. 0.003 grams per Density. 2.600 cc. (pycnometric in toluene).

LITERATURE CITED

*

CRYSTAL ~IORPHOLOGY Crystal System and Class. Orthorhombic, pseudotetragonal; orthorhombic bipyramidal class. Form and Habit. Pseudotetragonal bipyramids, rarely octagonal prisms with bipyramidal terminations; forms observed are orthorhombic bipyramid { 112 1, orthorhombic prism ( 110] , brachydomes { 011 1 and (021) , macrodomes { 101] and { 201 ]. brachypinacoid

OPTICALPROPERTIES Refractive Indices. 01, p, and y > 2.20. Surface Character. Continuous spectra in visible light, due to grating effect of twin lamellae.

FUSIOS BEHAVIOR Melting Point. 2200 helium a t 50 p.s.i.1.

I

50" C. (in

Determination of

Determination of Polymethylbenzyl Benzoates D. E. NICHOLSON, Humble O i l 8 Refinina- Co.,. Bavtown, . , lex.

*

cs-117 I

Slit

CRYSTALLOGRAPHIC data for publication in this section should be sent to W. C. McCrone, 501 East 32nd St., Chicago 16, Ill.

Cl~-CII Naphthalenes

Concn.

, I

Component Formula Name

8 . 8 5 ~0.112 I 0.028~ 0.027

0-100 &I

-

2,4,5-trimethyl benzoate -1-1-

benzyI-2,5dimethyl benzoate 2,4-Dimethylbenzyl-2,4dimethyl benzoate

,1

0-100 & I 112.23~ 0.218 10.042

2 2,4-Dimethyl-

3

-1-1

~

0-1001 A1

CisH2002

1 ~

Naphthalene

1-Methylnaphthalene 2-Methylnaphthalene 1,2,3,4-Tetrahydronaphthalene

oil 8 Rennins

1 1

Slif

Range

Accuracy

%

%

X or v

0.100

--CllHlo 0-100 h0.5

0.301

1 0.100

16.00p 0.214

1 0.100

I

I

CllHlo

--- I CloHlz

0-100 f0.5 I

Cell Windows: CsBr Absorbance Measuremenf:

Inverse matrix-Graphical-

Successive a p p r o x . 2 -

1 2 3 Material Purify:

298

0

8.85~ 0.398 0.127 0.220 9 8 % minimum

ANALYTICAL CHEMISTRY

Base line-

Inverse matrixGraphical-

P o i n t X Successive o p p r o x - L

Relafive Absorbances-Analyfical Matrix:

Relafive Absorbances-Analyfical Matrix: Componenf/X

Calculafion:

Concn. glliter lengfh mrn

0.389 1

Cell Windows: NaCl Absorbance Measuremenf: Calculation:

Av

0-100 h0.5

lnsfrumenf: Perkin-Elmer M o d e l 1 12, CsBr prism Sample Phase: Solution in carbon tetrachloride

P o i n t X

(mm) AX or

8.1. Pfs.

Jnsfrurnenf: Perkin-Elmer Model 21, NaCl prism Sample Phase: Solution in carbon disulflde

Base line-

C0.n

CS-118

CloHs

0.027

12.99~~0.255 1 10.048~ 0.027

HASTINOS, Humble

E* NICHOLSoN and 5. Baytown, Tex.

12.23~ 0.012 0.154 0.080

12.99~ 0.021 0.047 0.185

Componenflk 1 2

3 4 Material Purify:

20.98~ 16.150 0.251 6.908 0.101 99.5% minimum

18.68~ 0.072 3.507 0.015 0.046

16.00~ 0.302 0.115 1.111 0.048

23.02~ 0.030 0.377 0.042 1.459