Vol. 68 butyl peroxides have also been prepared having ¿-butyl alcohol of crystallization.3. The pyrolysis of ¿-butyl hydroperoxide has been studied at 95-100°and at 250°. At 95-100°¿ -butyl alcohol and oxygen are the only products formed, while at 250°the products formed are acetone, methyl alcohol, ¿-butyl alcohol, formaldehyde and water.4. The pyrolysis of di-¿-butyl peroxide has been studied at 200, 250 and 300°. Acetone and ethane are the only products formed.5. A free radical mechanism has been proposed to explain the pyrolysis of both ¿-butyl hydroperoxide and di-¿-butyl peroxide.Cambridge 39, Massachusetts
The trialkylsilicyl fluorides were very stable and did not respond t o the action of sodium in liquid ammonia and therefore could not be analyzed by the sodium-liquid ammonia4 method.The fluorine was qualitatively determined in each compound by oxidation with chromic acid in sulfuric acid solution to silicon tetrafluoride which was passed into aniline6 t o form a solid addition compound. TABLE I PROPERTIES AND ANALYSES OF TRIALKYLSILICYL FLUORIDES Trialkyl-B. p., Euorides mm.) n% d'54 % Calcd. Found silicyl 'C. (745 Yield, Carbon, ' % Ethyl' 109 1.3900 0.8354 45.0 53.66 52.50 Propyl 175 1.4107 ,8339 62.0 61.28 60.93 Butyl 224 1,4250 ,8372 70.1 65.97 65.96 Amyl 267 1.4305 ,8389 57.6 69.10 69.10 (4) Vaughn and Nieuwland, I n d . Eng. Chem., Anal. Ed., 3, 274 (1931). (5) Comey and Jackson, Am. Chcm. J . , 10,166 (1888). Table I.
The compounds were analyzed quantitatively for carbon by a modified Chalmer'se method which is a wet combustion method. The results of this analysis are given in
SummaryA study was made of the reaction between silicon tetrafluoride and ethyl, propyl, butyl and amylmagnesium halides.Three new trialkylsilicyl fluorides were prepared.The fluorine atom in trialkylsilicyl fluorides is very inactive, much less reactive than the corresponding bromide or chlorides.The reaction between alkylmagnesium halides and silicon tetrafluoride is completed in less than one hour. NOTRE DAME, INDIANA (6) Chalmer, I n d . Eng. Chem., Anal. E d . , 4 , 1 (1932).
SummaryPossible spectrophotometric methods which could replace the present system of grading crude green soybean oils are given below in order of convenience. The limits are approximate values.
Measurement of optical density of crude oils at 700 mμ in 21.8‐mm. tubes. Grade 2 limits would be at optical densities of 0.5 and 0.7
Measurement of refined oils at 690 mμ in 21.8‐mm. tubes. The limits for Grade 2 would be at optical densities of 0.4 and 0.6.
Measurement of refined oil at 670 mμ in 8.0‐mm. tubes. Limits would be at optical densities of 0.4 and 0.6.
Measurement of refined and bleached oils at 670 mμ in 21.8‐mm. tubes. Limits would be at optical densities of 0.1 and 0.7.
Measurement of optical density of crude oils at 670 mμ in approximately 4‐mm. I.D. tubes. Limits would be at optical densities of 0.4 and 0.7.
Measurement of optical density at 670 mμ of crude oils in 15% solutions of oil in carbon tetrachloride in 21.8‐mm. tubes. Limits would be at optical densities of 0.5 and 0.7.
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