+
+
compounds were examined under a microscope and found to crystallize as small, \\.ell defined octahedra (K20sC16) and rhombic dodecahedra (K20sBr,).
found 9.729 0.02 z and 10.30 0.03 A for K20sC16 and K20sBr6,respectively. The lattice constant of the former compound corresponds rather closely t o the value reported by the Sational Bureau of Staiidards for (SHJ2PtCl6 ( 3 ) . The authors' intensity determinations differ considerably from the visual estimates of 1\IcCullough (2) and seem to follow m acceptablc ordrr of variation with the planes of r d w t i o i i . In addition, both
ACKNOWLEDGMENT
The authors express their thanks to
H. J. yearian, Department of Purdue t-niversity, for the use of his laboratory facilities.
LITERATURE CITED
(1) Gilchrist, R., Bur. StandardsJ * Research 9, 282 (1932). ( 2 ) ,1fcCullough, J. D., Z. Krist. 94, 143 (1936). (3) Swanson, H. E., Gilfrich, N. T., Ugrinic, G. hl., S a t l . Bur. Standards, Circ. 539 (1955). (4) Swanson, H. E., Tatge, E., Ibid., 539 (1953). CRYSTALLOGRAPHIC data for publication in this section should be sent t o W. C. 1tcCrone. 500 East 33rd St.. Chicago 16, Ill.
Analysis of 2-Bromoethanol, 1.2-Dibromoethane, 1,1,2,2-Tetrabromoethane, and i -Bromo-2-(2-bromoethoxy)-Ethane Mixtures cs-57
1. R. KILEY, The Dow Chemical Co., Midland, Mich.
Instrument: Perkin-Elmer M o d e l 12, NoCl prism Sample Phase: Solution in carbon disulfide No.1
AA or Lengfh Av 1 mm
Name
1 2-Bromo-
1
0-20
C?H:BrO
~
zt0.3
2.8p 2.7 2.9
10.5
8.44y
ethanol
-I
-1-
2
1,2-Dibromoethane
CnHdBrz
0-50
Cell Windows: NaCl Absorbance Meosurement:
0.090 100 0 . 0 4 9 ~ 0.1
Calculofion:
___ -I
Relative Absorbancera-Anolyticol
0.300 100 0.071p1 0 . 1
1
1 Bromo-2-(?-bromoethoxylethane
C,HaBriO
1,1,2,2-Tetrabromoethane
CsH2Brr
0-50
!
Successive approx.-Mofrix:
2.8
8.44
8.92
14.25
1 2
0.945 0.000 0.000 0.000
0.234 0.648 0.194 0.015
0.187 0.013 0.916 0.037
0.058
8 . 9 2 ~ 0.350 0 . 0 7 7 ~ 0.1
3 4
0.003 0.002 0.446
I
I
- -~ ~ _ _ 4
1 f0.3
Inverse m a t r i x - X GraphicolL-
Point-X-
ComponentlX
-.
3
Base l i n e - L
_ _ _ I_ _ _ _ _ _ 1 4 . 2 5 ~ 11.400 1 100 0 . 2 4 5 ~ 0.1 I
Materiol Purify:
Reference compounds 99 +% pure
Relative absorbances are given as the slope o f the Beer's l a w concentration curves used expressed in terms of obsorbance p e r 100% o f constituent.
Analysis of 2,4-Dichlorophenoxyacetic Acid 1.
R. KILEY,
The Dow Chemical Co., Midland, Mich.
CS-58 ~ - _ _ _ ~ - - _ _ _ _ _
I
~- l
Component Name Formula
I
No.
.
1 2,4-Dichloro-
ICsH,ClrOs
%%d
I
2 2,6-Dichloro-
1'
1
1
I
-
l
phenoxyacetic ocid
phenoxyacetic acid
-~
~
4 Di-(2,4-di1 chlorophenoxyocetic I acid
%
AC~U-
racy
%
1 1
X or B.L. Pts.
1
Slit
Concn.
(mm) 1 mg/ml
1 AA or
1
Av
Instrument: Perkin-Elmer Model 12, N a C l prism Sample Phase: Solution in acetone
1 Length
1
mm
Cell Windows: N a C l Absorbance Measurement: Calculation:
1
I
~13.58
1
~1
0.800 '~0.140p
100 0.1
~
10.139pl 0.1 0-20
l1- _
10.5
1
-1-1
9.39p0.450 100 10*094p'
I
These d a t a represent standard piibliration and submission is open t o anyone in accordanre with regulations of ..\SAI,STICAL CHEMISTRY.T h e Coblentz Society is acting only as a n aid t o t h e journal.
Base line-
Inverse m a t r i x - X Graphical---
~
~
Relotive Absorbancesa-Analyticol
Point
2-
Successive approx.---
' Matrix:
~
ComponenflA
13.85
13.58
13.00
1 2
0.426 0.084 0.168 0.165
0.148 0.254 0.122 0.145
0.149 0.212 0.888 0.208
_ _ _ I_ _ _ f0.5 1 3 . O O p ~ o . 8 O o 1 ~
-___ _ _ _ Ci4H&lrOll
l__l__l___
k
,
-_______-
1
150-1001 f1.0 113.85pl1.000 1 100 10.174pl 0.1
_______
1
l
Range
3 4 Moterial Purity:
9.39 0.235 0.213 0.215 1.240
Reference compounds 99 +% pure
Relative absorbances a r e given as the slope o f the Beer's law concentration curves used expressed in terms o f absorbance p e r 10070 of constituent.
T o standardize procedures, ASILYTICALCHEMISTRY requests t h a t material be sent in quintuplicate t o t h e chairman of t h e review committee: Robert C . Wilkerson, Celanese Corp.. of America. Post Office Box 8, Clarkson, Tex.
VOL. 30, NO. 10, OCTOBER 1958
1709
