8 INDUSTRIAL AND ENGINEERING CHEMISTRY VOL. 9, NO.

connections are tight and that the tubing contains no air bubbles, Materials, “1933 Book of Standards,” Part 11,p. 891; Federal
Place the condenser in position so that the lower end extends Specification VV-L-791a for “Lubricants and Liquid Fuels;
General Specifications (Methods for Sampling and Testing),”
directly into the upper end of the buret just above the water Method 300.13,p. 80.
level or connect to an adapter siphon, G, which discharges into (8) Hillebrand, W. F., U. S. Geol. Survey, Bull. 700, 102 (1919).
the buret. The cooling water ahould be 15.5’ C. or colder. (9) Ibid.. 700. 232 (1919).
I~ ~ I

Ice water may be desirable for low-boiling hydrocarbons. (10) Hoyt, L. ’F., and Pemberton, H. V., J. IND.ENG.CHEM., 14,
54, 340 (1922).
Weigh 100 grams ( *0.5 gram) of the soap (cut into cubes of (11) Munson, L. S., and Walker, P. H., J. Am. Chem. SOC.,28,663
about 1-om. edges) or 50 grams ( ~ 0 . 3gram) of boap powder (1906); Assoc. Official A m Chem.. Official and Tentative
and transfer to the evolution flask. Add about 10 grams of gum Methods of Analysis; U.S. Dept. Agr., Bur. Chem., Bull.
arabic (commercial) and 100 cc. of distilled water. Place the 107, 241 (1908).
(12) Poetschke, P., J. IND.ENQ.CHDM.,5, 645 (1913).
flask in position with 100 cc. of sulfuric acid (1t o 3) in a dropping (13) Procter & Gamble Co., Oil and Soup, 13, 6-10 (1936).
funnel, C, carried in the stopper. Connect with the steam line, (14) Soap Analysis Committee, Am. Oil Chemists’ SOC.,Ibid., 11,
wash the flasks and the condenser, making sure that the stoppers 90-5 (1934).
are tightly fitting and held in place by wiring. Rubber connec- (15) Ibid.. 12. 10 (1935).
tions in the lines between the evolution flask and condenser (16) Ibid., 12, 10Lll (1935); Wolff, H.,and Scholze, E., Chem.-
Ztg., 38,369,382,430 (1914).
should be avoided. (17) Trevithiok, H. P.,Soap, 7, No. 6, 29 (1931).
Add the acid t o the sample slowly to avoid excessive frothing.
While adding the acid, turn on the steam cautiously, so adjusting RECZIIVED
September 12, 1936. Presented a t the 92nd Meeting of the
American Chemical Sooiety, Pittsburgh, Pa., September 7 t o 11, 1936.
the pressure by a bleeder valve that just enough steam flows to Approved by the Supervisory Committee on Standard Methods of Analysis.
prevent any liquid from backing into the steam trap flask, and by the Council as official for the American Chemical Society,
When all the acid has been added, turn on enough steam to
cause brisk distillation, taking care that no liquid is carried over
from the evolution and wash flasks and that the condenser water
does not become warm.
Continue the distillation until there is no increase in the
A Simple Laboratory
volume of the upper layer for 45 minutes or no small droplets
can be noted in the condensate. Ozonizer
When distillation is completed, shut off and drain the condenser
water, and allow the steam to heat up the condenser to drive out W. SHEEHAN AND W. CARMODY
the last traces of volatile hydrocarbon. Shut off the steam as The Neville Company, Pittsburgh, Pa.
soon as vapor begins to issue from the lower end of the condenser.
I
Immediately open the stopcock of the dropping funnel t o prevent
caustic being drawn into the evolution flask.
Stopper the buret and allow its contents to come to room
B

c
A QUICKLY assembled ozo-
nizer that can be operated
for relatively long periods to
temperature or bring them to a dehite temperature by immersing
give satisfactory yields is shown
the buret for 1 t o 2 hours in a water bath held at 25” C. in Figure 1, which is self-ex-
Read the volume of the upper layer t o the nearest 0.01 cc. The
planatory. It has been con-
volume multipled by the specific gravity equals the weight of 0
structed of a 600-mm. Pyrex
the volatile hydrocarbon. The specific gravity should be de-
condenser with extended side
termined at the temperature a t which the volume is read. A
arm, and from other materials
small Sprengel tube made of 3-mm. glass tubing is convenient E available in a laboratory. It
for this purpose. B is s i m p l e i n c o n s t r u c t i o n ,
Calcdation. quickly assembled, relatively in-
GO. of volatile hydrocarbon X specific gravity X 100 e x p e n s i v e , a n d can be dis-
weight of sample mantled into service as a stand-
per cent of volatile hydrocarbon
ard condenser.
For some samples the volatile hydrocarbon content may be The transformer u s e d was
so low that a larger sample than 50 or 100 grams is desirable. o b t a i n e d from a neon sign.
The size of the evolution flask may need t o be increased if larger Several were tried, r a n g i n g
samples are used. The amount of water in the evolution flask from 10,000 volts upwards; all
and acid used should also be correspondingly increased. Y
*- were satisfactory, and although
FIGURE 1. DIAQRAM OF
not a stockroom item with most
Literature Cited APPARATUS laboratories, they can be readily
Assoc. Official Agr. Chem., Official and Tentative Methods of A . Brass wire obtained from any neon sign
E N Rubber atop ers agency. Used transformers are
Analysis, p. 115 (1930); U. S. Dept. Agr., Bur. Chem., Bull. C.’ 6 per cent sulyuric acid
107, 169 (1908). D 15 000-volt transformer always avaiIable.
Assoc. Official Agr. Chem., Official and Tentative Methods of E: Alhninum foil The units are supported in
C. 600-mm. condenser
Analysis, p. 14 (1930). L. Ground
Ibid., p. 282; U. S. Dept. Agr., Bur. Chem., Bull. 107,53(1908). M. Oxygen
ordinary ring stands, insulation
Bennett, H.C., J. IND. ENQ.CHIM., 13, 813 (1921). T. 0501162 (oxygen) being provided by means of cork
Com. on Analysis of Commercial Fats and Oils, Ibid., 11, 1163 or rubber between the outer foil
(1919): Assoc. Official Agr. Chem., Official and Tentative and the support. Several can be used in series by making the
Methods of Analysis, p. 317 (1930).
Corn. on Methods of Analysis and Specifications of Commercial proper sealed connection.
Soaps and Soap Products, J. IND. ENQ.CHEM.,14, 1159-63
(1922). November 7,1936.
RECEIVED
Dean, E. W.,and Stark, D. D., Ibid., 12,486 (1920); Bidwell,
G.L., and Sterling, W. F., Ibid., 17, 147 (1925); Church, A.
K.,and Wilson, J. H., Soup, 7, No. 11, 35 (1931); Oil a n d
Soap, 9,253 (1932); “Standard Method of Test for Water
in Petroleum Products and Other Bituminous Materials,”
Serial Designation D-95-30,American Society for Testing