X-Ray Diffraction Patterns of Phenols L. J. E. HOFER and W. C. PEEBLES Branch
of Coal-to-Oil Research,
X-ray diffraction analysis is proposed for the positive identification of crystalline phenols. If the phenols have a reasonably high melting point, conversion to the phenyl isocyanate derivative for the purpose of making a diffraction pattern is unnecessary. It is also unnecessary to recrystallize the specimen until the literature melting point is attained. The diffraction patterns of isomers and closely related compounds are distinctly different.
-RAY diffraction analysis
is proposed for the positive identification of crystalline phenols. X-ray powder-diffraction patterns of 51 solid phenole have been made, using characteristic filtered FeK, radiation. Many phenols are susceptible to oxidation on contact with a i r ; b u t such oxidation, although i t lowers the melting point, does not appreciably modify the diffraction pattern. I n the course of x-ray diffraction studies of coal, coal-related materials, and coal-hydrogenation products, it was desirable to establish the diffraction patterns of possible constituents such as aromatic hydrocarbons (IO), hydrocarbon derivatives ( 9 ) , and phenols. Such compilations are of interest in the coal tar, dye, plastics, fuel, pharmaceutical, and other industries. A preceding study by McKinley, Nickels, and Sidhu (24) was confined to the phenyl thiocyanate derivatives of simple liquid phenols. The present study is confined to phenols of high enough melting point to permit the preparation of extruded specimens.
Pattern SO.
24 4 47 36 49 38 b
21 20 42 b
I5
6 37 40 25 18 13 12 23 33 31 19 26 39 8 30 50 29 35 3 b
43 10 32 17 28 45 b
t t
27 51 2 34 9 22 b
41 b
14 46 16 11 48 1 b b
b b b t b b
b
6 b
PROCEDURE
The specimens were very finely ground in an agate morPresent address, 5064 West Tuscarawas St., Canton, Ohio. 1
V, Bruceton,
Pa.
Table I. Melting Points and Three Most Intense Diffraction Lines of Solid Phenols"
44
X
Bureau of Mines, Region
b
Three ___ Stronges t 1st
2nd
12.35 12.3 10.7 6.4
4 64 3 52 5.9 3.86
6 6
11 5
6.4 6.30 6.2
15.1 4.34 10.7 4.05
{ E 3 4.29 6.1 5.85 3.28 3.795 5 8 3 6i5 5.6 5.5 4.46 3.88 5 5 11.5 5.4 .5 . 1 5.4 4 48 5 4 4 26 5 4 3.22 5.4 lo., 5.3 4.68 5 2 4 18 5 2 3.92 5.2 3.91 5.2 5.0 6.3 4 57 5.0 4.33 5.0 4 50 4.97 3.66 4 88 3 37 4 88 ' 4 ,605 4.84 '
