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The Students' Guide in Quantitative Analysis - Free Ebooks Library

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DISTILLATION OF PETROLEUM, i^t<br />

of about 500 c. c. capacity ; connect this with a Liebig's<br />

condenser, and arrange for distill<strong>in</strong>g <strong>in</strong> the usual manner.<br />

Through the tubulus of the retort <strong>in</strong>sert a thermometer.<br />

Provitk ten glass cyl<strong>in</strong>ders of 50 to 75<br />

c. c. <strong>in</strong> capacity,<br />

and mark each with a file, so as to show the volume occu-<br />

pied by 25 c. c. of liquid. <strong>The</strong>se cyl<strong>in</strong>ders are to serve as<br />

recipients of the distillate.<br />

Pour 250 c. c. crude petroleum <strong>in</strong>to the retort, and apply<br />

heat very gently at first, <strong>in</strong>creas<strong>in</strong>g gradually, and f<strong>in</strong>ally<br />

heat<strong>in</strong>g until the residue <strong>in</strong> the retort is coked. Collect<br />

25 c. c. of the distillate <strong>in</strong> the first cyl<strong>in</strong>der, and note the<br />

temperature <strong>in</strong>dicated by the thermometer <strong>in</strong> the retort<br />

collect the second 25 c c. <strong>in</strong> another recipient, note also<br />

temperature, and cont<strong>in</strong>ue <strong>in</strong> this manner, chang<strong>in</strong>g the<br />

recipient for every 2$ c c. until the whole liquid has dis-<br />

tilled over.<br />

B. — Exam<strong>in</strong>ation of the Distillates.<br />

Determ<strong>in</strong>e the sp. gr. of each distillate by float<strong>in</strong>g <strong>in</strong> it<br />

a small Baumd Hydrometer, note the color of each sam-<br />

ple, and determ<strong>in</strong>e its flash<strong>in</strong>g po<strong>in</strong>t by means of Taglia-<br />

bue's *' Open Tester," a figure and description of which are<br />

found on page 41, Vol. HI. of the "American Chemist."<br />

To test the flash<strong>in</strong>g po<strong>in</strong>t, proceed as follows : pour a<br />

small quantity of the sample to be e.Kam<strong>in</strong>ed <strong>in</strong>to the open<br />

cup, which is surrounded by a vessel of water. Light the<br />

lamp beneath and apply heat very gradually the tempera-<br />

;<br />

ture should not rise faster than two degrees a mmute.<br />

<strong>The</strong> thermometer bulb should dip beneath the surface of<br />

the oil. From time to time test the <strong>in</strong>flammable vapors<br />

which arise from the surface of the oil, us<strong>in</strong>g a small flame,<br />

flitt<strong>in</strong>g it quickly across the surface, and not<strong>in</strong>g simultane-<br />

ously the height of the thermometer at the moment of<br />

ignition. Record results with each distillate.<br />

;

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