Determination of Phenethyl Acetate in Phenethyl Formate A. J. FENTON, The Procter and Gamble Co., Cincinnati, Ohio
I Range
onent
1
racy
B.L.
[mm)
Determination of 4-Nitrochlorobenzene in :2,4-Dinitrochlorobenzene
cs-74
length
% % Points AX mm _ _ - _ _ _ _ ~ Phenethyl /-CIOHI~O~ 0-20 3 ~ 0 . 2 9 . 7 0.400 100 acetate 9.23 0 . 0 4 1 ~ 0.025 -
-I 1
~
~
Insfrument: Perkin-Elmer Model 32 1, NaCl prism Sample Phase: liquid Cell Windows: NaCl Absorbance Measurement: Calculafion:
B. E. SEEBER and 8. B. WHITCOMB, National Aniline Div., Allied Chemical Corp., Buffalo, N. Y.
Companenf Name Farmula
1
No.1
1
I
4-Nifrochlorobenzene
1
%
%
C S H ~ N O ~ C 0-4 I
Cell Windows: NaCl Absorbance Measurement:
Graphical
Calculation:
9.7p 1.23
1
Range
zk0.2
X orv 5.1. Pfs.
Slit [mm) AX or Av
9.9
0.40 500
Qi;lo/
Concn. mg/mf length
mm
0.1
fnsfrument: Baird-Atomic, Model B, NaCl prism Sample Phase: Solution in chloroform
Base line
Relative Absorbance-Anofyfical Matrix: Componentlh
I1 11 1I I I1 Accuracy
cs-75
Base l i n e x
Inverse matrixGraphical&
Point-
Successive apprax.-
Relafive Absorbances-Analytical Matrix: Component/X
9.9 2.80
Materi;rl Purity: Reference compounds 99 +% pure Comments: The absorbance i s expressed as the slope of the Beer’s l a w curve in absorbance per 1 0 0 ~ o of constituent. The calibration curve passes through 0.23 absorbance at 0% acetate.
98 +%.
These d a t a repreaent s t a n d a r d publication a n d submission is open to anyone in accordance with regulations of ANALYTICAL CHEXISTRY. T h e Coblenta Society is acting only a s an aid t o t h e journal.
To standardize procedures, AX-~LYTICAL CIiEarrsmy requests tliat material be s e n t in quintuplicate t o t h e chairman of t h e review committee: Robert C . Wilkerson, Celanose Corp. of Binerica, Post Office Box 8, Clarkwood, Tex.
1 Material Purify:
2,4-Dinitrochlorobenzene 99 +%, 4-nitrochlorobenzene
~
No. 1 80. Uranyl DisaIicyIa,te Trihydrate, U0 2 (CsH40HC O0)2.3H20 V. AMIRTHALINGAM and V. M. PADMANABHAN Chemistry Division, Atomic Energy Establishment Trombay, Bombay, India
D
the preparation of yellow triclinic uranyl disalicylate dihydrate crystals ( 1 ) for detailed structure analysis (to be reported in another paper), tiny orange-brown hexagonal prismatic crystals are isolated from the same mother solution. Detailed thermogravixnetric studies of both the URING
orange-brown and yellow compounds which were dried over calcium chloride in a desiccator re m l e d that they are of the same compcsition except for the water molecule content. Calculation showed that thk orange-brown compound contains three water molecules per molecule.
Partial Powder X-Ray Diffraction Pattern of Uranyl Di:dicylate Trihydrate hk,
110 001 101 111 20 1
300 211 220 310 301
d, A. (Cdcd.) 8.553 7.161 6.446 5.492 5.149 4.938 4.411 4.275 4.109 3.980
d , A.a
(Obsd.) 8.52 7.14 6.43 5.51 5.15 4.91 4.42 4.28 4.11 4.02
d, 4,.
I
hkl
m vs vs vs
400 102 401 32 1 212 500 330 420 331
ni m w
m
m vw
(Cnl-d.) 3.736 3.479 3.271 3.071 3.018 2.C63 2.551 2.E01 2.t849
d, A: (Obsd.) 3.72 3.47 3.28 3.09 3.03 2.98 2.85 2.79 2.66
1
ANALYTICAL CHEMISTRY
CO
= 7.16A. No. of Molecules in Unit Cell. 2
=
12. Density. 2.192 grams per cc. (calculated), 2.120 grams per cc. (measured). Space Group. PG (no systematic absences). OPTICALPROPERTIES Uniaxial Negative. Refractive Indices (A 4358). no = 1.657. n , = 1.653. Geometric Mean. 1.655. Rfolecular Refraction. 99.6 cc. Color. Orange brown.
s
ACKNOWLEDGMENT
m in
The authors thank Jagdish Sliankar for his interest during the progress of the work.
ni m IT
w 111
w
a G.E.C. 143.2-niin. diameter powder camera Straumani,j mount,ing, (CuKi,) 1.5418 A.
622
X-RAP DIFFR.4CTION DATA Cell dimensions. a. = 17.10 A.
LITERATURE CITED
(1) Llanoilovic, 1,. RI., B u l l . Inst. Nuclear Sci., “Boris Kidrich,” Belgrade, 8 , 105 (1958). CRYSTALLOQRAPHIC data for publication in this section should be sent t o W. C. hIcCrone, Jr., McCrone Associates, 501 East 32nd St., Chicago 16, Ill.
