Warming the column

In a typical analysis the columns are cooled to about —75° C. by dry air precooled by liquid N2. Then the gas sample is injected into one column by a Perkin-Elmer sampling valve the second column is for reference. After sampling is complete, the liquid N2 is removed, and the air flow is continued for about 5 minutes or long enough to warm the columns to about —10° C. and remove the 03. Yields, as percent of current, are calculated from the gas chromatographic, amperage, sample volume, and total gas flow measurements. 

The actual apparatus used to separate berkelium from californium, for example, is a dark column of resin surrounded by a glass jacket which serves merely to contain a vapor that warms the column so the process will go on faster at a high temperature. 

Cholestenone. Place a mixture of 1 0 g. of purified cholesterol and 0-2 g. of cupric oxide in a test-tube clamped securely at the top, add a fragment of Dry Ice in order to displace the air by carbon dioxide, and insert a plug of cotton wool in the mouth of the tube. Heat in a metal bath at 300-315° for 15 minutes and allow to cool rotate the test-tube occasionally in order to spread the melt on the sides. Warm with a few ml. of benzene and pour the black suspension directly into the top of a previously prepared chromatographic column (1) rinse the test-tube with a little more benzene and pour the rinsings into the column. With the aid of shght suction (> 3-4 cm. of mercury), draw the solution into the alumina column stir the top 0 -5 cm. or so with a stout copper wire to... 

The carbon monoxide product is removed from the top of the column and warmed against recycled high pressure product. The warm low pressure stream is compressed, and the bulk of it is recycled to the system for process use as a reboder medium and as the reflux to the carbon monoxide column the balance is removed as product. The main impurity in the stream is nitrogen from the feed gas. Carbon monoxide purities of 99.8% are commonly obtained from nitrogen-free feedstocks. 

Dicyclopentadiene (50 g, 0.38 mole) is dissolved in 100 ml of anhydrous ether. Platinum oxide (0.25 g) is added, and the mixture is hydrogenated in a Parr apparatus at an initial pressure of 50 psi. Initially the reaction mixture becomes warm. The absorption of 2 mole equivalents of hydrogen takes 4-6 hours. The mixture is filtered by suction to remove the catalyst, and the filtrate is distilled at atmospheric pressure through a short fractionating column. 

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