Infrared Quantative Analysis Data. CS-81 ... - ACS Publications

(projection on 100). Beta Angle.122°. ... (5893 A.; 25° C.). 2E = 74°;. 2V = 45°. Dispersion, r > v. Optic Axial Plane. 7 A c. = 7° in obtuse ß...
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CRYSTAL ~~ORPHOLOGY Crystal System. Monoclinic. Form and Habit. Tablets lying on the basal pinacoid { 001 ] elongated parallel to b showing the ortho pinacoid { l o o ) , the hemiorthodome and the prisms { 1101, {210},and 1310). Axial Ratio. a:b:c = 3.198: 1: 1.351. Interfacial Angles (Polar). 901 A001 = 310 810 = 86'20' .~ A 5105&l' (projection on 100) 310 A 3l,0 = 210 A 210 = 64'20' 95'&6 (projection on 100) 210A210 = 110 A 110 = 35"30' 72'4_8' (projection on 100) 110 A 110 =

OPTICALPROPERTIES Refractive Indices (5893 A , ; 26' C.). cy = 1.532 rt 0.002; p = 1.59 i 0.01; y =>2.0. Optic Axial Angles (5893 A.; 25' C.). 2 E = 74'; 2V = 45". Dispersion. r > u. Optic Axial Plane. y d c = 7" in obtdse p. Sign of Double Refraction. Posit'ive. Atute Bisectrix. y . Extinction. p A a = 25' in obtuse p. Molecular Refraction ( R ) (5893 A.; 25" C,). qi/cypy = 1.700. R(ca1cd.) = 45.63; R(ohsd.) = 47.7. FUSION DATA. PDMAB sublimes on heating, the condensate forming as droplets; final melting occurs a t 72.1' C. The refractive index of the melt is 1.6128 at 99-101' C. and 1.6229 a t 82-4' C. ; the resulting temperature

pol},

40'28'

Beta Angle. 122'. X-RAYDIFFRACTION DAT.4 Cell Dimensions. a = 24.43 A.; b = 7.64 A.; c = 10.32 A.

NICHOLSON, Humble O i l and Refining Co., Baytown, Tex.

x or v B. 1. Pts.

1

2

Ij

5,5-Dimethyl4-ethyl-3. :;-hex-

CSH180S

4,6,6-Trimethyl-3thia-2-hep1 tanone

CsHisOS

0-100

12

1

1I

1

Slit

CS-81

(mm) AX or

Concn. mg/ml length

Av

mm

I

Component Range ~

%

racy ~

%

1

8 . 1. Pts.

Slit (mm)

''

AXor

Av

I

Concn. mglml length mm.

Pentamethyldiphenylmethane

I

~

I 1 ~~

Base l i n e - X

1

methyldiphenylethane

0.085~ 1.00

~~

PointInstrument: Perkin-Elmer Model 21, NaCl prism Sample Phase: Solution in carbon disulfide

Successive approx.--

Cell Windows: NaCl Absorbonce Measurement:

Relofive Absorbances"-Analytical Matrix:

12.30~ 0.630

1

Formuh

or v

I

I

ComponentfX

1

Name

I

x

diphenyl (bimesityl)

1

I

0-100

Inverse matrixGraphical&

1

I

No.1

Instrument: Perkin-Elmer Model 21, NaCl prism Sample Phase: Liquid mixtures, without solvent

Calculation:

ACW-

!

1

,

CS-82

D. E. NICHOLSON, Humble O i l and Refining Co., Baytown, Tex.

12.30 0.224 0.044~ 0.092

I

Cell Windows: NaCl Absorbance Meosuremenf:

Ill.

Determination of Diphenyls Related to 1,3,5-Trirnethylbenzene

Determination of Isomeric Thiolacetates in Binary Mixtures D. E.

coefficient of refractive index is 0.00058. On cooling, the melt tends to supercool; however, recrystallization is spontaneous. The rate of growth is rapid and increases as cooling continues. The crystals formed from the melt are coarse-grained spherulites. On a meltback, well-formed crystals are formed. The crystals are tablets lying on 001 and are elongated parallel to b. An off-centered biaxial, positive interference figure is obtained showing an optic axial angle, 2E, equal to 74'. The crystals show high birefringence with normal polarization colors. The growing edge shows a-ell-formed prisms 110, 210, 310. Shrinkage cracks are evident running parallel to a. PDAfAB forms eutectics with azobenzene and benzil with eutectic temperatures of 42-3' and 50.0-0.5" C., respectively; the benzil-PDJZAB eutectic contains 55 zt 1% PDMAB. COSTRIBUTIOXS of crystallographic data for this section should be sent to Kalter C. McCrone, 501 East 32nd St., Chicago 16,

'Formula Weights per Cell. 8 (7.961 calculated from x-ray data). Formula Weight. 149.19. Density. 1.210 (flotation and pycnometer); 1.216 (x-ray).

fidence in the values obtained. The authors would welcome any suggestions as to methods of checking directly the beta and gamma values obtained.

Moferiol Purity: Component 2, 98%; component 1, 50% taminant being component 2.

Colcubtion:

with the con-

Comments: Alternate nomenclature for components; No. 1: 1,3,3trimethylbutyl thiolacetate; No. 2: 2,2-dimethyl-1 -ethylpropyl thiolacetate; Component 2 was determined b y difference.

Inverse matrixGra p hica I-.-.-.-

Point& Successive a p p r o x . - X

Relative Absorbancesa-Anolyficol Mofrix: ComponentlX 9.96~

1 2 3 Moferial Purify:

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

Base line-

0.0378 0.0093 0.0069

12.04~ 0.0043 0.0481 0.0203

14.38~ 0.0037 0.0054 0.0715

Synthesized compounds of approximately 97% purity

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

~~~

These d a t a represent standard publication a n d submission is open t o anyone in accordance with regulations of ANALYTICAL CHEM\IIBTRY. T h e Coblentr Societv is acting only a s a n aid t o t h e journal.

1 120

ANALYTICAL CHEMISTRY

To standardize procedure AXALYTICAL CHEMISTRY r e q ~ ~ e s t hs a t material be sent in quintuplicate t o t h e chairman of the review committee: Robert C. Wilkerson, Celanese Corp. of America, Post Office Box 8, Clarkmood, Tex.