ANALYTICAL CHEMISTRY
1884
M.. and Linmne. J. J.. "Polaropraphy," P. 215, New York. Interscience Publishers, 1941. (3) L i n w e . J. J.. IND.ENG.CHEM.,~ I L ED.. . 18.429 (1946). CHEM..20,984 (1948). (4) Meitea, L.. and Meites, T., .4ar~. ( 5 ) Ritvner. H.. IND.ENG.CHEU..ANAL.ED.. 17,41-3 (1945). (6) Sherman. M., Foundru, 78, 94 (1050) (2) Koithoff, I.
yield satisfactory results for nickel and zinc in copper-base alloys. N o results for the copper, lead, and tin were reported, as that of the is in daily use in foundry and familiar to moEt chemists. LITERATURE CITED
(1) Allaopp.
W.E., .4NnL. CHEM.,21, 428 (1949).
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5 1. N-Phenyl-2-naphthylamine
Sign of Douhle Refraction. Pl'egative Acute Binectrix. b = a.
Contributed by W. C. MCCRONE, Armour Researoh Foundation of Illinois I n s t i t u t e .of Technology, Chicago 16, Ill.
Prinoioal Lines
PHENYG~-NAPHTHYLAMINE can be recrystallized from rnethNinol, ethanol, ether, benzene, or acetic acid. The best crystals for x-ray and optical work are obtained either from methanol or by sublimation. Recrystallization from methanol even with liberal use of deoolodaing charcoal gave reddish brown crystals; the product from sublimation, however, was colorless. There is little or no effect of the coloring material on other optical properties.
d 9.12 6.45 3.51 4.83 4.35 4.30 4.16 4.02 3.92 3.80 3.68 3.53 3.47 3.21
I/Ir 0.30 0.10 0.28 1.00 0.03 0.33 0.53 very weak 0.08 0.14 0.20 0.03 0.09 0.13
3.12 2.99 2.91 2.86 2.81 2.79 2.58 2.37 2.28 2.23 2.15 2.41 1.88 1 84
0 16 0 21 very weak 0 07 0 05 Very weak very weahvery weak very weal, Very weahvery weak very weak very weak Very weah-
e
C
I
F i g u r e l . Fusion Preparation of Phenyl-2-naphthylamine
CRYSTAL MORPHOLOQY
Crystal System. Orthorhombic Orthographic Proje,ction of Typical Crystal of Phenyl-2-naph t h y l a m i n e
Figure 2.
,
I"I,.
Axid Ratio. a:b:e = 0.942:1:0.412. Interfacial Angles (Polar). 201 A 201 = 98'34'. 110 A i i n = 92" 34'. X-RAYDIPFRACTION DATA Cell Dimensions. a = 17.45 A.; b = 18.25 A.; e = 7.52 A. Formula Weights per Cell. 8. Formula Weight. 219.27. Density. 1.237 (flotation and pycnometer); 1.226 (x-ray). OPTICAL PROPERTIES Refractive Indexes (5893 A,; 25' C.). a = 1.636 =t 0.005 B = 1.82 0.01. Y = 1.92 =t 0.002 (cslculated). The cargille index medium 1.512 when saturated with phenyl-2naphthylamine mtohes the alpha refractive index of that eom-
+
nn,."'i _rY+ IIII".."
-.
0
81 ~~
~
l "
pptic Axial Angles.
Molecular Refraction ( R ) , R(aalcd.) = 70.4. R(obsi3.) FUSIONDATA.Pheuyl-Z-nitprl~nyliLlmnewnen rearysmineen from methanol several times shows a micro melting point of 107108' C. and an equilibrium melting point of 107.8" C. The melt solidifim spontaneously to give many spherites. The unit crystals are coarse rods and the nucleation rate rises rapidly as the temperature falls t o mom temperature. The rate of crystal gmwth is rapid at all temperatures between the melting point and mom temperature. A meltback gives broad rods showing o tie axis interference figures with 2V = 65" 1) > r, (-). A txymol mixed fusion gives well-formed rods &ith all refractive indenes ereater than thvmol. " . nardel _ ~ extinction, and a 79' profile aGgIe.
(5893 A.; 25' C.). 2V = 65'.
Dispersion. v > 1. Optic Axial Plane. 001,
2H
=
~
Cos~nrsn~rona of orystallogra~lhiodata for this section should be aent to Walter C. MoCrone. su~ervisor, AnalYtiChl Section, Armour Research Foundation oi the Illinois Institute of Technology, Chiaago 16, Ill.
