Determination of Diethyl Diethylmalonate in Diethyl Ethylmalonate
cs-12
W. H. WASHBURN, Abbotf Laboratories, North Chicago, 111.
Cell Windows: NaCl Absorbance Measurement:
Component
No.1
1
Name
1 . 1
I
Calculation: Range
%
Formula
1
8.1. Pts.
curacy
%
I
-1-1- 13.52
Diethyl diethylmalonate
L A or 1Len;fh Av
~
1adj.sh.
1
Inverted MatrixGraphical-X
Relafive Absorbances-Analytical
1.340 70 0.229 0.10
1
Base-Line-L
Poini-
Successive ApproxMatrix:
13.52 0.525
Componenflk
1.
MaterialPurity: Reference compounds 99 +% pure Commenfs: In concentrations o f from 70 io SO%, a correction must b e applied due to deviation in Beer's law.
Instrument: Perkin-Elmer Model 12C, NaCl prism Sample Phase: Solution in carbon disulfide
Analysis of Hexachlorocyclohexane Mixtures by Infrared Absorption
CS-13
R. L. HUDSON, Ethyl Corp., Baton Rouge, la. I
Component
20-100
1
2.
1
a-Hexachlorocyclohexane
C6H6C16
6-Hexachlorocyclohexane
~
0-40
CfiHsCls
I
0.8
j
10.95
1
i
12.71
I
0.610 0.108
I
1.0150 1.80
i
0.113
'
1.80
1
0.930 0.162
I
1.0150 1.80
I
0.5
1
13.96
1
12.'50
~
I
I
I
--
0-100
~
I
1
4.
10.8 1
0.400 0.076
~
1.0150 1.80
I
0-20
y-Heptachlorocyclohexane
1
7.
1
6-Heptachlorocyclohexane
o.3
CsHsCli
e-Heptachlorocyclohexane
I 9.
a-Heptachlorocyclohexane
10.
1,2,3,4-Tetra-5-chlorocyclohexene
0.575 0.103
~
1.0150 1.80
I-
Cst'iscI7
0-20
1
1
1 I,
0.4
I 1
1-
~
1
i
0-20
0.4
1
I
13.45
~
0.545 0.098
0.750 0.132
0-20
CgHoC17
--I CfiHsCla
1
12.30
I 1
I
1
0.1
0-20
~
0.3
I ~
i 1
1.0/50 1-80
1.0150 1.80
13.07
0.665 0.117
1.0/50 1.80
11.98
0.505 0.092
1.0150 1.80
Inslrument: Perkin-Elmer Model 12-C, NaCl prism Sample Phase: Solution in carbon disulfide Cell Windows: NaCl Absorbance Measurements: Calculafian:
Base-Line-
Inverted M a t r i d -
Relative Absorbances-Analyfical
Point-X Successive Approx.-
-
Graphical-
Matrix:
Companenis
14.55
10.95
12.71
13.20
13.96
11.05
12.50
12.30
13.45
13.07
11.98
1. 2.
2.035 0.133 0.157 0.018 0.042 0.029 0.103 0.027 0,021 1.216
0.661 0.078 0.049 0.207 0.548 0.039 0.048 0.086 0.030 0,058
0.553 1,220 0.077 0.610 0.054 0.266 0,102 0.390 0.163 0.178
0.038 0.125 1.459 0.052 0.132 0.130 0.070 0.118 0.685 0.040
0.133 0.100 0.044 1.315 0.780 0.600 0.085 0.140 0.018 0,120
0.159 0.057 0.026 0.074 1.526 0.022 0.044 0.075 0.028 0.076
0.046 0.518 0.056 0.122 0.333 2.730 0.218 0.868 0.058 3.720
0.030 0.058 0.029 0.056 0.292 0.405 1.890 0.110 0.056 0.440
0.029 0.043 0.203 0.067 0.551 0.038 0.070 2.115 0.091 0.051
0.097 0.602 0.690 0.046 0.049 0.870 0.337 0.073 2.880 0.041
0.089 0.028 0.027 0.024 0.057 0.029 0.051 0.029 0.050 3.078
3. 4. 5.
6. 7. 8. 9.
10.
~
Range can be increased beyond recommended range by applying a correction to the analytical matrix. Material Purity: Reference compounds 9 9 +% pure. Comments: Notation on hepta isomers used here is the same as reported by K. Kuratoni, Repf. Inst. Sci. Techno/. Univ. Tokyo 4, 236-9 (1 9 5 0 ) . 8-Hexachlorocyclahexane i s only partially soluble in the solvent used. Correctiacs are applied for beta-isomer absorption a t only 3 wave lengths. The corrections are 0.033 absorbance unit at 13.45p, 0.028 at 13.20p, and 0.006 a t 10.951. These corrections assume that the solvent i s saturated with respect to the beta isomer.
1718
0
ANALYTICAL CHEMISTRY
