Determination of Impurities in Trimethylchlorosilane PAUL BROWN and A. LEE SMITH, Dow Corning Corp., Midland, Mich.
cs-43
No.
Concn. wlml length
Component Nome j Formula
1
G. D. GRANT and A. LEE SMITH, Dow Corning Corp., Midland, Mich.
cs-45
!
I 1
Determination of Phenyl to Methyl Ratio in Phenyl and Methyl Containing Polysiloxanes
mm
, Component No./ Name Formula
1
1
%
trichloro-
1 3 . 2 0 p 0.043 I 100 of1 0.0111Ml 0 . 1
,-. , . ,*IO% u.1101
17.2 I
lo
-1-
present
1 3 . 3 8 ~ 0.043
1
100
' 0 . 0 1 0 8 ~ 0.1 3 ~
Dimethyl dichlorosilane
(CH3)2SiCIz1 0-1 ~
I
1
I 10.1
I
1 8 . 6 6 ~'0.415 250 18.910.064~ 0.1 18.4 j
Instrument: Perkin-Elmer Model 1 12, KBr prism Sample Phase: Solution in carbon disulfide Cell Windows: KBr Absorbance Measuremenf: Calculation:
Base I i n e X
Inverted matrixGraphicalX
Colculotion:
Base line-
Inverted matrixGraphicalX
Relofive Absorbancesn-Analytical Componentlh
Point-
A plot of log
P o i n t J Successive approx.-
Matrix:
A dJ gives o straight line through the follow3.2 against log A3.4 Me
ing points;
Mafrix:
17.51~
1 2 3
Cell Windows: NaCl Absorbonce Meosurement:
Successive approx.-
Relative Absorbances"-Analytical Component/A
Insfrument: Perkin-Elmer Model 1 12, CoF2 prism Somple Phase: Solution in carbon tetrachloride
16.35~
18.66~
14.3
0
0
0 0
18.2
0
0
,
Aa.2 - = 9.40 Aa.4
8.33
Material Purity: Reference compounds 99.9% pure Comments: Samples are corrosive and readily hydrolyzed. deposits in cells.
A3.z dJ = 0 . 1 4 0 at - = A3.4 Me -
0.100
dJ
at - = 10.00 Me
M a y leave
Maferial Purity: 95% or better Comments: Ratio obtained i s that o f the actual number of phenyl to methyl groups. Other alkyl or aryl groups interfere.
a Relative absorbances are given os the slope of the Beer's law concentration curves used expressed in terms of absorbonce per 100% of constituent.
a Relative absorbances are given as the slope of the Beer's law concentration curves used expressed in terms of absorbance per 100% of constituent.
Determination of Triglyceride Esters and Fatty Acids in Petroleum-Base Oils (Saponiflcation Value of Industrial Oils) R. W. FOREMAN and JEANETTE A. GRASSELLI The Standard Oil Co. (Ohio), Cleveland, Ohio
Accu-
Component No.1 Nome Formula
I
1
Triglyc- H.&-O-C-O-R~ eride esters H C-0-C-0-I?
0-15%
I I
1 f1%
Aorv 6.1.
Slit fmm) A X or
Pls.
Av
1
!Fatty acids
,1 RCOOH R-olkyl groups
~
length
5.46.1
1 HzC-0-C-0-RI
2
1 Concn.
I
Calculation:
Base I
i
Inverse matrix& Graphical-
n
e
X
0.030
0.025
ANALYTICAL CHEMISTRY
8.94
Material Purity: Soybean oil, chemical saponification value = 188.5 Lauric acid. chemical acid value = 200.3
Saponification No. = 9w
100
Acid No.
= -w t ' %
100
X 188.5 X 200.5
Presence of free sulfur and active sulfur compounds does not interfere with this analysis (will interfere with chemical sap. No.). Presence of unsaponifiable carbonyl compounds or a synthetic ester will interfere with this analysis (position of C=O is clue for such an interference). Point-
Successive approx.-
These data represent standard publication and submission is open to anyone in accordance with regulations of ANALYTICAL CHEMISTRY. The Coblentz Society is acting only aa an aid to the Journal.
1016
0.00
0.00
0.078 100
Insfrumenf: Perkin-Elmer Model 21, NaCl prism Sample Phase: Full strength Cell Windows: NaCl Absorbance Measuremenf:
3.62
calculation of saponification number and acid number.
-5.82 5.46.3
1 2
Range i s that usually encountered in industrial oils and corresponds to saponification volue of 0-20 for (1) and acid value of 0-20 for (2). (I Matrix Is given for calibration based on soybean oil (1). solution in medium white oil, and lauric acid (2), solution in medium white oil.
To standardize procedures, ANALYTICAL CHEMISTRY requests that materia be sent in quintuplicate to the chairman of the review committee: Robert C. Wilkerson, Celanese Corp. of America, Post O 5 c e Box 8, Clsrkwood, Ter.
