JANUARY 15, 1937 ANALYTICAL EDITION 49

microbalance. After rolling between the fingers, the capsule is of nitric acid is reduced t o 1 cc. They are charged, heated, and
left on the balance pan for 10 minutes t o reach constant weight. opened, and the precipitate is transferred to the filter as before.
The bomb tubes are constructed of 10-mm. tubing and the amount Before the first weighing of any day the filter tube is wiped with
a dam cloth, placed in the adapter, and heated in the oven at
125’ 8 The adapter is closed with cork stoppers and allowed
to cool, and the filter tube wiped again with the damp cloth and
TABLEI. RESULTS
B Y SEMI-MICROMETHOD
left for a half hour on the pan of the microbalance before weighing.
Sample Halide Calcd. Found Difference After filtration the identical procedure is followed, and this
Mo . Mo . % % % weight can be used &sthe first weight of any succeeding analysis
p-Bromoacetanilide, BrCoHCVHCOCH3 on the same day. Obviously the drying block technic of Pregl
22.30 19.80 37.34 37.79 4-0.45 could be employed if desired.
23.25
48.50
20.30
42.30
37.17
37,12
-0.17
-0.22
The accuracy seems to be of the same order as the semi-micro-
46.20 40.25 37.08 -0.26 determinations. Slightly more time is required, so that economy
26.55 23.30 37.36 +0.02 of material is the only advantage of the micromethod.
58.25 50.65 37.01 -0.33
23.70 20.80 37.36 +o 02
p-Chloroacetanilide, CIC6H4NHCOCHa Analytical Results
39.45 33.20 20.92 20.82 -0.10
58.25 49.10 20.85 -0.07 The data given in Tables I and 11, obtained by under-
26.45 22.40 20.95 $0.03
43.10 36.00 20.66 -0 26 graduate students, indicate that the degree of accuracy is
p-Nitrochlorobenzene, C1CsH4NOz about that normally expected. It is worthy of note that the
41.75 37.90 22.51 22.46 -0 05 use of a larger sample brings no corresponding increase in
29.85 27.00 22.38 -0 13
101.20 92.20 22.54 +O 03 accuracy, showing that the errors in weighing are well within
61.05
45.75
54.75
41.95
22.18
22.68
-0 33
f0.17
those inherent in the method itself. Of the few failures en-
20.75 19.15 22.82 4-0 31 countered, only two were not traced to faulty manipula-
N-(7-bromopropyl) phthalimide, CaH4OnN-CHz-CHz-CHzBr tion.
31.45 22.00 29.82 29.77 -0.05
35.05 24.50 29.75 -0 07
37.15 25.95 29.73 -0 09 Summary
21.85 15.30 29.80 -0 02
63.00 44.05 29.76 -0.06
82.30 57.50 29.74 -0.08 A simplified Carius method is described for the semi-
Methyl-a-phenyl-8-bromo-@-benzoyl propionate (a), ClrHlaOsBr micro- and microdetermination of chlorine and bromine in
37.25 19.90 23.03 22.74 -0 29 organic compounds. The sample is weighed on an ordinary
21.55 11.70 23.11 +o 08 analytical balance in a capsule of silver foil which dissolves
19.65 10.60 22.96 -0 07
21.55 11.60 22.92 -0 11 and allows the halide to be siphoned directly from the bomb
Methyl-o,r-diphenyl-o,8-dihydroxy-y-ohlorobutyrate (91, C I ~ H I ~ O L X tube onto a micro filter tube. The bomb tube is opened with
12.75 5.70 11.06 11.06 0
22.15 9.95 11.11 $0.05 a flame which eliminates the danger of glass chips falling into
20.80 9.25 11.00 -0.06 the precipitate. The method is reliable and convenient and
the results are of the usual order of accuracy.
TABLE11. RESULTSBY MICROMETHOD
Sample Halide Calcd. Found Difference Literature Cited
24-0. Mg. % % % Clark, J . Assoc. Oficiul Agr. Chem., 17, 483 (1934).
p-Bromoacetanilide Kohler and Goodwin, J . Am. Chem. Soc., 49,226 (1927);Kohler
11.660 10.280 37.34 37.52 +o. 18 and Kimball, Ibid., 56, 730 (1934).
10.710 9.395 37.34 0 Ibid., 55, 4637 (1933).
10.666 9.370 37.39 +0.05
12.807 11.240 37.36 +0.02 Pregl, “Quantitative Organic Microanalysis,” 2nd English ed..
p-Chloroacetanilide tr. by Fyleman, p. 149, Philadelphia, P. Blakiston’s Son &
11.161 9.430 20.92 20.91 -0.01 Co., 1930.
7~ 156 6.095 21.07 +O. 15 I b i d . , 4th German ed., p. 129, Berlin, Julius Springer, 1935.
6.226 5.315 21.11 +o. 19
RECEIVED
August 20, 1936.

Preparation of Vehicle Films Free of Supporting Foundation

E. H. BAYOR AND L. KAMPF
Division of Analyzing and Testing, Borough of Queens,
Long Island City, N. Y.

I N THE analysis of paints, etc., useful information con-

cerning their physical characteristics can be obtained by
examination of a film of the vehicle. The following is a
method of preparing such films: The vehicle must first be
separated from the pigment by settling, centrifuging, or filter-
ing with or without the aid of solvents or solvent mixtures.
If a solvent is used, the solvent must subsequently evaporate
so as not t o change the nature of the vehicle. The separated
vehicle is poured on a thin aluminum sheet and allowed to
harden, and the aluminum is dissolved with dilute (1 to 10)
hydrochloric acid to which a drop of platinum chloride solu-
tion has been added. The film is then washed and dried.
To avoid wrinkling of the film during preparation or after-
wards, the authors found it practical to dip the four edges of
the film in molten paraffin, after it dried on the aluminum
sheet. This protects the aluminum underneath from the
action of the acid bath and leaves a metal frame around the
film.
RECEIVED
Sovember 3, 1936.