October 15, 1932 INDUSTRIAL AND ENGINEERING CHEMISTRY 445

LITERATURE CITED (5) Selvig, W. A,, Bur. Mines, Rept. Investigations 3003 (1930).
( 6 ) Selvig, W. A., Bur. Mines, Tech. Paper 8, revised, 42 (1929).
(1) Am. Soo. Testing Materials, Standards, Part 11, pp. 551-6, 1927.
(2) Fieldner. A. C., Selvig, W. A., and Parker, W. L., J. IND.ENQ.
CHIDM., 14, 695-8 (1922). RH~CH~IVED December 21, 1931. Presented before the Division of Gas and
(3) Jones, M. C. K., et al., Ibid., Anal. Ed., 2, 325-8 (1930). Fuel Chemistry at the 83rd Meeting of the American Chemioal Society,
(4) Remmey, G.B.,J. Am. Ceram. Soc., 14, 358-84 (1931). New Orleans, La.,March 28 to April 1, 1932.

Improved Distillation Trap

EDWARD
S. WEST,Washington University School of Medicine, St. Louis, Mo.

T HE diagram represents a trap for use as a connecting bulb

in Kjeldahl distillations which has been found superior
to the ones in common use. It was originally used in a still
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for conductivity water and is now employed by the writer

wherever an efficient distillation trap is required, It has the
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advantage of operating entirely without spattering and of

efficiently removing fine spray from the vapors. The ap-
paratus is easily made. ‘INNER TUBE TO HAVE
I n operation, vapors pass up the inner tube, through the 11 \\ 1 8 HOLES- 27,DIA.
side holes at the end, and are deflected down through the wet
narrow annular space between the inner tube and cap. The
vapors again change direction a t an angle of 180 degrees and I.D. OF TE~TTUBL
pass out between the wet walls of the cap and bulb. Con- NOT LE55 THAN 151
densed liquid returns to the boiling flask through a hole a t the
bottom of the inner tube near its seal to the outer tube. The
space between the walls of the inner and outer tubes, around
and above this hole, must be sufficiently narrow to hold by
capillarity a column of water which will prevent steam blow-
ing through it. CE DETWELN MALLS
The dimensions given are satisfactory, but may be varied T LE55 THAN ‘Ill,
IN INNER TUBE
rather widely except that the space between the inner and
outer tubes must not be too wide, nor the return hole too
large, and the exit holes a t the end of the inner tube must be
large enough to allow passage of the vapors a t a low pressure
to prevent blowing through the return hole. Traps with
practically any desired efficiency may be made by simply
lengthening the inner tube and cap.
This apparatus may be obtained from Arthur H. Thomas
Company, Philadelphia, Pa. July 26, 1932
RECEIVED

An Identification Test €or Oxalic Acid

EARLER. CALEY,Frick Chemical Laboratory, Princeton University, Princeton, N. J.

SINCE 4 several carboxylic acids form more or less insoluble

calcium salts, the usual calcium oxalate precipitation test
for oxalic acid is not an especially distinctive means for
identifying the acid, and may lead to confusion in certain
instances. The following specific precipitation reaction for
free oxalic acid is based upon the fact that sodium oxalate is
sparingly soluble salt, whereas the normal sodium salts of
practically all other known carboxylic acids are freely soluble
in water.
Dissolve 0.10 gram of the solid organic acid in 2.0 cc. of
cold water and add 1.0 cc. of approximately 6 N sodium
hydroxide solution. Shake the mixture vigorously for 1 or 2
minutes. The separation of a white crystalline precipitate
indicates oxalic acid.
The proportions of weights and volumes given were those
found to give the optimum results in a series of experiments
bearing on this point. Any marked deviations from these
details may vitiate the test. The weights and volumes may,
of course, be reduced in proper proportion in case a sample as
large as 0.10 gram is not available for examination.
This reaction is not of value for the detection of oxalic acid
in mixtures, but is intended solely as a simple identification
test for the free acid in order to distinguish it readily from
other solid, water-soluble, carboxylic acids. Tests made on
a number of such acids using this procedure yielded negative
results even when samples larger than 0.10 gram were taken.
Among those examined were the following representative
ones: citric, crotonic, glycollic, maleic, malic, malonic,
mandelic, succinic, and tartaric. As far as the writer has
been able to determine, the only carboxylic acid that will give
a precipitate in the above test is dihydroxytartaric acid.
However, it is not likely that confusion could arise from this
source in view of the unstable character of this acid and the
special means required to obtain it.
RECEIVED
September 8, 1932.